REGION I, EPA-NEW ENGLAND DATA VALIDATION FUNCTIONAL GUIDELINES
FOR
EVALUATING ENVIRONMENTAL ANALYSES
U.S. EPA-NEW ENGLAND
Region I
Quality Assurance Unit Staff
Office of Environmental Measurement and Evaluation
Parti
Attachments J-Q
July 1996
Revised December 1996
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Attachment J
Data Validation Report - Blank Forms
i. DQO Summary Form
ii. ORDA/IRDA Form
iii. TeTeph rie Regional/Laboratory
Communication Form
iv. Data Validation Worksheets
v. Chain-of-Custody Form
vi. Traffic Report
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Site Name
Site Location
Assigned Site Laotude/Longinide____________________________
CERCLA Site/Spill Identifier No. 0! ________ lncIudc Operable Unit)
Phase ERA SA/SI prr .-R1 RI (phase I. etc.) ES .D RA post.RA
(circle one) Other
EPA-NE - DQO SUMMARY FORM Page____ of ____
- paratc Form should be completed for each sampling event. Refer to Attachment A for instructions art completing this form. A chment B for a complete list
ic parameter codes and Attachment C for an example of a completed form.
EPA Program: TSCA CERCLA RCRA DW NPDES CAA
Other
Projected Date(s) of Sampling_______________________
EPA Site Manager_______________________
EPA Case Team Members_________________
2. QAPJP Title and Revision Date___________________________________________________________________________________
Approved by of Approval:___________________________________
Title of Approving Official: Organizaoon:_____________________________________
‘If other than EPA. record date approval authority was delegated:
EPA Oversight Project (circle one) Y N Type of EPA Oversight (circle one) PRP or FE Other.________________
Confirmatory Analysis for Field Screening Y N If EPA Oversight or Confirmatory % splits_____________________
Are comparability criteria documented 1 Y N
3.
a. Matrix Code’
b. Parameter Code 1
C. Preservation Codes
d. Analvocal Services Mechanism
C. No of Samole Locations
Field QC:
f. Field Dunlicate Pairs
g. Esuiomeni Blanks
Ii. VOA Trio Blanks
L Cooler Tetnoerature Blanks
). Bottle Blanks
k. Other_______________
I. PES sent to Laboratory
Laboratory QC:
________
Tn. Reaaeni Blank
n. Duolicaic
0. Mama Soike
p. Mama Spike Dunlicate
q. Other._
4.
Site Information
Site Dimensions
List all potentially contaminated matrices_________________________________________________________________________________
Range of Depth to Groundwater_______________________________________________________________________________________
Soil ‘Types Surface Subsurface Other._____________________________________
Sediment Types’ Stream Pond Estuary Wetland Other_________________ Expected Sail/Sediment Moisture Content High Low
When
multiple macncei will be sampled during a sampling event, complete Sections 5-10 for each mama. Mama Code’________
S. Data Use (circle all that apply) Site irwcst igaaon/Asscssnient PRP Detcmiinatiori Removal Actions
Nature and Extent of Contamination Human and/or Ecological Risk Assessment Remedranori Alternatives
Engineering Design Remcdial Action
I Post .Remedial Action (quarterly monitoring) Other_______________
Draft DQO Summary Form 11/96
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if anolicable
COCa Acoon Levels
Analytical Method-Qusitalatron Limits
T1
(circle tec1 ruque) Bailer I.ow flow pwnp ( egion I method: Yes No) Perisialac Pump
Posiuve D placement Pump Faucet or Spigot Other_____________________
Split Spoon Dredge Trowel Other ________________
Procedures (SOP name, No Rev. #. and date)___________________________________________________________
Sample L .ocauons_________________________________________________________________
or Composite
sampled: Yes No
(circle) ORP pH Specific Conductance Dissolved O Temperature Turbidity
Other________________________________________________________________
Methods xid Psr4meters
tide/SOP name Method/SOP
Identification number
Revision Date
Target Parametets
(VOA. SV. Pesr/PCB. Metals. C CC)
Cntcrw (circle one) 1. Recion I, EPA-NE Data Validation FunctioriaF Guidelines icr Evah,atu,e Environn,ened Analyses. Pan I I, III
or IV
2. Other Approved Validation Criteria:____________________________________________
(circle cg ) U U I Painal Tier I D:
Performing Data Validation Prime or Subcoriu-acinr (circle one)
Number______________________________
(e.g. ST/J’T. E’ ..ACS. etc.) Work Msignntcnc No._________________________________________
FoimPEide Date of DQO Summai Form Compicoon
Matrix Codes 1 - Refer to Attachment B, Part I
Parameter Cod& - Refer o Auathm nt B, Pi zt 11
Preservation Cod&
I. HCI to pH 2 7. K Cr O 7
2. HNO 8. Freeze
3. NaH O 9 Room Temperature (avoid excCistvc hear)
4 11 . 50. 10. Other (Specify)
5. Cool @ 4C (± 2) N. Not preserved
6 NaOH
* - To supplement Matrix Codes and/or Parameter Codes contact the QA Unit
Draft DQO Summary Form 11/96
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ATI7ACHMENT A
Guidance for Completion of DQO Summary Form
DISTRIBUTION:
1) Copies of completed DQO Summary Forms should be included in the QAPJP/SAP.
2) A. Copies of completed DQO Summary Forms for all CLP RAS work requested by EPA Site
Managers, EPA contractors, including RACS, ROC, and START, and other Federal Agencies
under Interagency Agreements, i.e., ACOE, and States under Cooperative Agreements should be
sent with the quarterly sample projections to the Region I RSCC. Completed DQO Sumznaxy
Forms for CLP RAS work be received by the RSCC prior to the sampling event.
B. Copies of completed DQO Snmmary Forms for non-CLP DAS work performed for EPA Site
Managers and EPA contractors j j be received by the Region I RSCC pnor to the sampling
event.
C. DQO Summary Forms for non-CLP work performed under Interagency Agreements, Cooperative
Agreements, and Grants must be completed prior to the sampling event, sub mitted to the
‘Authorizing Organization’, as delegated by EPA, and included in the site documents.
3) Copies of completed DQO Summary Forms also must be included in the Data Validation Report or Tier
I Validation Cover Letter (refer to Part I of the ‘Data Validation Manual’ in the Region 1, EPA-NE Data
Validation Functional Guidelines for Evakiatiny Environmental Analyses) , December 1996, cr most recent
revision.
INSTRUCTIONS:
Note: A separate Form should be completed for each sampling event. For sampling events involving multiple
environmental matrices, complete Sections 5-10 for each matrix and ensure that the two-lener matrix code
is identified in Section 5. Enter the page number and total number of pages in the top right hand corner
on the Form.
Section 1:
• Circle the appropriate EPA Program(s) involved in multi media, multi-programmptic sampling
events including, TSCA, CERCLA (i.e. Superfund), RCRA, DW (Drinking Water), NPDES,
CAA (Clean Air), or fill in the blank for ‘Other:______ ‘.
• List projected date(s) of sampling. The sampling dates should be inclusive of all matrices tha will
be sampled during this sampling event.
• Record the EPA Site Manager’s name.
• List the names of the other EPA Case Team Members.
• Enter the site name. Use the NPL site name. If an NPL site name does not exist, then use iM
site name assigned under CERCLIS.
• Record the name of the city/town and State where the site is located in the ‘Sit Location” field.
• Record the ‘Assigned Site Latitude/Longitude’. Those numbers should be identical to thbse
contained in CERCLIS database. Contact the EPA Site Managcr to obtain correct
Latitude/Longitude.
• Record the CERCLA site/spill identifier number, including the operable unit nimber. Contact
the EPA Site Manager to obtain the correct identifier numbers.
• Circle the appropriate phase of Superfund site work (ERA: Environmental Risk Assessment,
SA/SI: Site Assessment/Site Investigation, RI: Remedial Investigation, FS: Feasibility Study, RD:
Remedial Design, RA: Remedial Assessment, post-RA: post-Remedial Assessment, i.e., quarterly
monitoring). For non-Superfund site work, identify sampling event phase in the ‘Other” field.
Att. A - Draft DQO Summary Form 11/96
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Section 2:
• Record the complete title of the final QAPJP and revision date.
• Enter name of the Approving Official.
• Record date that the QAPJP was approved.
• Enter title of the Approving Official.
• Enter name of organization that has approval authority. This will be EPA, unless approval
authority has been delegated by EPA to a State or other Federal Agency.
• If another organization has been delegated approval authority, then enter the date that EPA
delegated approval authority (date of Quality Assurance Management Plan approval).
• Identify whether the project sampling event is an EPA oversight project, circle Yes or No.
• Indicate type of oversight by circling either Potentially Responsible Party (PRP) or Federal
Facility (FF), or complete the blank for Other: -.
• Identify whether confirmatory sampling and analysis is being performed to verify field screening
results, circle Yes or No.
• If EPA oversight or confirmatory analysis will be performed, record the percentage of split
samples to be collected and analyzed.
• If EPA oversight or confirmatory analysis will be performed, identify whether comparability
criteria are documented in the approved QAPJP or SAP, circle Yes or No.
Section 3:
a) List the two letter code for each matrix for samples that will be collected. Refer to Appendix B
for a correct list of matrix codes. If a matrix does not have a corresponding code, then attach a
description of the matrix to the DQO Summary Form.
Note: The matrix codes correspond to the matrix identifiers contained in the New
England Sample Tracking System (NESTS) database. The current list of matrix
codes are not intended to include all types of environmental matrices. However,
they do represent groupings of similar-type matrices that potentially contain similar
analytic interferences. For example, the matrix code GW (ground water) includes
water from monitoring wells, supply wells, and public wells.
b) For each matrix, identify the analytical parameters for samples that will be collected by recording
the appropriate parameter code. Refer to Appendix B for a current list of parameter codes. If
an analytical parameter does not have a corresponding code, then the method title and/or SOP
name, method and/or SOP identification number, and method and/or SOP revision date should be
included and recorded in Section 9 of this Form.
Note: The parameter codes correspond to the analytical method parameters utilized
In NESTS database. Appendix B Includes a comprehensive list of analytical methods
that have been used historically for Region I site work.
C) For each matrix and parameter, identify the preservation technique that will be used by recording
the appropriate preservation code. Refer to the reverse side of this Form for a list of preservation
codes.
d) Record the analytical service(s) mechanism that will be used for each matrix and parameter;
- CLP-RAS (CLP-Routine Analytical Service) This service may be utilized by EPA site
managers, EPA contractors including, RACS, ROC, and START contracts. It may also
be utilized under Interagency agreements, i.e., by the ACOE, and under Cooperative
Agreements with the States.
- RACS-DAS (Remedial Alternative Contracting Strategy-Delivery of Analytical Services)
- ROC-DAS (Regional Oversight Contract-DAS)
- START-DAS (Superfund Technical Assessment and Remediation Contract-DAS)
- EPA-NERL (EPA-New England Regional Laboratory)
2 Ait. A - Draft DQO Summary Form 11/96
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- Regional EPA-NE analytical contract
- State-Non-CLP
- Other Federal Agency Non-CLP
- If another analytical mechanism will be used, describe in detail on a separate page and
attach to the Form.
e) Record the number of discrete locations that will be sampled for each parameter. The ‘No. of
Sample Locations count should include the site and background locations sampled.
• Record the number of each type of field QC sample that will be collected and sent to the
laboratory for analysis for each matrix and parameter.
o Record the number of Field duplicate sample pairs (which will equal “1 for each pair of field
duplicates) that will be collected.
g) Enter the number of equipmentirmsate blanks.
h) Enter the number of VOA Trip blanks.
1) Enter the number of Cooler Temperature blanks that will be used.
j) Enter the number of Bottle Blanks that will be analyzed.
k) Describe any other field QC samples and the total number that were collected and that will be sent
to the laboratory.
I) Enter the number of PESs that will be sent to the laboratory in accordance with EPA Region I
Performance Evaluation Program Guidance , July 1996.
Note: The total of ‘c-i” equals the total number of samples sent to a laboratory for each
matrix and parameter.
• Record the number of each type of laboratory QC sample that will be analyzed with the samples
received.
m) Enter the tnirumum number of reagent blanks that will be analyzed.
n) Enter the number of laboratory Duplicates that will be analyzed.
o) Enter the number of matrix spikes that will be analyzed.
p) Enter the number of matrix spike duplicates that will be analyzed.
q) Describe any other laboratory QC samples and the total number that will be analyzed.
Section 4:
• Enter the approximate site dimensions with units.
• List all potentially contaminated matrices, regardless of whether or not they will be sampled
during this sampling event.
• For well sampling, complete ‘Range of Depth to Groundwater’ to ensure proper pump is utilized.
• For soil sampling, circle Surface or Subsurface or complete Other:____________
• For sediment sampling, circle Stream, Pond, Estuary, Wetland, or complete Other:__________
• For soil/sediment sampling, circle expected moisture content: High or Low. Note: Analytical
methods used for high moisture content samples should ensure that P00-specified dry
weight quantitation limits are achieved.
3 Mt. A - Draft DQO Summary Form 11/96
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Section 5:
When multiple matrices will be sampled during a sampling event, complete Sections 5-10 for each matrix
and enter the Matrix Code.
• Identify the two-letter matrix code for which the information is provided in sections 5-10.
• Circle the potential uses for sample data such as, site investigation/assessment, PRP determination,
removal actions, nature and extent of contamination, human and/or ecological risk assessment,
remediacion alternatives, engineering design, remedial action, post-remedial action, i.e., quarterly
monitoring. A space is available for other potential uses of data.
Section 6:
• Briefly summarize the project DQOs. This section should describe the specific objectives of the
sampling event, i.e., to identify health risks to children, ages 1-6, residing on the site who might
be exposed to surface soils located in the area, or to characterize the extent of groundwater
contamination. Identify the purpose of sampling, the decisions that will be made using the data,
action level information, and any related information needed to identify that appropriate analytical
and field sampling methods were chosen. Complete the table with the following information:
contaminpnts of concern (COC), COC action levels and analytical method quantitation limits for
each COC. Note: Since this information will be used by data validators to identify potential
data usability issues for the user, it is imperative that it is clear and concise.
Section 7:
• Circle applicable sampling technique(s) used and/or complete “Others to describe an innovative
sampling technique or one that is not listed.
• Identify the SOPs that will be utilized for sample collection. Include SOP name, identification
number and revision number and/or date.
• Record the discrete Background sample station location number(s) that will be sampled.
• Circle if samples will be “grab or composite”.
• To indicate potential Hot spocs on site, circle Yes or No.
Section 8:
• Identify the field data that will be collected including, ORP, pH, specific conductance, dissolved
02, temperature, and turbidity. A space is available to indicate other field testing that will be
performed.
Section 9:
• If an analytical method does not have a Parameter code (required information in Section 3), then
the method title and/or SOP name, method and/or SOP identification number, and method andior
SOP revision date should be included. Auacb a separate page if additional space is needed.
• Record the specific parameters required for analysis.
4 Att. A - Draft DQO Summaiy Form 11/96
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Section 10: In accordance with Region I QA policy, all data must be validated in accordance with the
most recent revision of Part I the “Data Validation Manual: The Data Quality System” of
the Region I, EPA-NE Data Validation Functional Guidelines of Evaluating Environmental
Analyses .
• Circle the data validation criteria required by the QAPjP and/or SAP. In most cases, the QAPJP
and/or SAP should cite the most recent revision of the Region I. EPA-NE Data Validation
Functional Guidelines of Evaluating Environmental Analyses and identify the applicable Functional
Guideline criteria procedures that will be used to validate the data: Part lI-Volatile/Senaivolatile
Data Validation Functional Guidelines, Part lll-Pesticide/PCB Data Validation Functional
Guidelines, and Part IV-Inorganic Data Validation Functional Guidelines.
If modified criteria or alternate data validation criteria will be utilized, the modified or alternate
criteria must be documented in an approved QAPjP and/or SAP as stipulated in Part I, the Data
Validation Manual: The Data Quality System, December 1996 revision of the Region I. EPA-NE
Data Validation Functional Guidelines of Evaluating Environmental Analyses , December 1996
revision.
• Circle the Region I Validation Tier that will be used.
• If a partial Tier III data validation is required, then the subset receiving a partial Tier III should
be specified (e.g., benzene, VOA. etc).
• Identify the company performing the data validation. Circle either Prime or Subcontractor.
Secuon 11:
• Record the field sampling contractor companyforganization name
• Contract number
• Name of contract
• Work assignment number
• Name and title of person completing Form
• Completion date of the DQO Summary Form
5 Att. A - Draft DQO Summary Form 11/96
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ATTACHMENT B - PART I
Matrix Codes’
Aqueous:
DW - Drinking Water
GW - Ground Water
LE - Leachate (includes porewater)
SW - Surface Water
WW - Waste Water (includes scrubber blowdown)
Solid:
SE - Sediment (includes tidal sediments)
SO - Soil
Biota:
BD - Bird Tissue
CF - Crawfish Tissue
F! - Fish (includes whole fish)
MU - Mussel (includes clam, quahog, and oyster tissue)
OF - Offal
PL- Plant
FF - Fish Fillet
Wastes:
AS - Ash (includes incinerator ash and boiler aggregate)
DU - Dust (includes concrete dust and fines)
0! - Oil (includes waste oil)
SL - Sludge
WD - Wood (includes chips, cuttings, and driilings)
WT - Waste (includes both solids and liquids)
ST - Still Bottoms
Miscellaneous:
AR - Air Samples
DN - DNAPLs
LN - LNAPLS
WI - Wipe Samples
PC - Paint Chips
CT - Concrete
Att. B, Part I - Draft DQO Summary Form 11/96
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ATE ACJIMLNT II- PART II
PARAMETER CODES
PARAMETER CODE/METHOD
IDENTIFICATION NUMHER
MEUIOD TITLE
REFERENCE
PARAMETER NAME
OLM O3.IF
USEPA CLP Statement of Work fur Orgaiiics Analysis - OLMO3 1
1
Full organics (VOA. SV. P/F) CL? SOW Organic Analysis
OLMO3. IF
L1SEPA CL? Statement of Work (or Organics Analysis - OLMO3, 1
1
Pesticide/Aroclors Analysis CLP SOW Organic Analysis
OLM O3. IS
USEPA CLP Statement of Work for Organics Analysis - OLMO3 I
I
Semivolatite Organics Analysis CL? SOW Organic Analysis
OLMO3. IV
USEPA CLP Statement of Work for Organics Analysis - OLMO3 1
1
Volatile Organics Analysis CLI ’ SOW Organic Analysis
1003
Ilalogenated Hydrocarbons
2
NIOSII 1003 Volatile on Charcoal Tubes
12/90-Dl
USEPA CL? Statement of Work for Analysis of Polyclilonitated Dibenzo-p-Dioxins
(PCDD) and Polyclitonnated Dibenzofurans (PCDF), DFLMI.0, Rev. 12/90
3
12/90 SOW Dioxin/Furan Analysis
130.1
Hardness, Total (mg/L) as CaCO,, Colorimetric, Aulomaled EDTA
4
Hardncss-Colonmetric , Automated EDTA
130.2
hardness. Total (mgIL) as CaCO,, Titrimeinc, EDTA
4
Hardness-Titrimetric. EDTA
13112007
Toxicity Characteristic Leaching Procedure and Determination of Metals and Trace
Elements in Water and Wastes by Inductively Coupled Plasma-Atomic Emission
Spectrometiy
S & 7
TCLP Extraction-Metals Analysis
131 13.IF
Toxicity Characteristic Leaching Procedure and IJSEPA CLP Statement of Work for
Organics Analysis . OLMO3 I
5 & 1
TCLP Extraction-Full Organics Volatile, Semivolatile,
PcsticidelPCB Analysis
131 l3. IP
Toxicity Characteristic Leaching Procedure and USEPA CLP Statement of Work (or
Organics Analysis - OLM OJ.I
5 & I
TCLP Extractjon-PesitcidelPCB Analysis
131 l3.IS
Toxicity Characteristic Leaching Procedure and USEPA CL? Statement of Work for
Organic; Analysis . OLMO3 I
5 & I
TCLP Extraction-Semivolatile Analysis
131 13JV
Toxicity Characteristic Leaching Procedure and USEPA CL? Statement of Work for
Organics Analysis - OLMO3J
5 & 1
TCLP Extraction-Volatile Analysis
13118000
Toxicity Characteristic Leaching Procedure and Detemitnation of Organic Analytes by Gas
Chromatography
5
TCLP Extraction-Full Organic;
13118080
ToxicIty Characteristic Leaching Proccduie and Determination of Oiganochlorinc Pesticides
and PCBs by Gas Chromatography
5
TCLP Extraction PesticidefPCli Analysis
13118240
Toxicity Characteristic Leaching Procedure and Determination of Volatile Organics by Gas
Chromatography/Mass_Spectronietry_(GC/MS)
S
TCLP Extraction-Volatile Aiialysis
13118270
Toxicity Characteristic Leachiiig Procedure and Determination of Sernivolalile Organics by
Gas Chmomatograpliy/Mass_Spcciroiiietry_(GC/MS)_Capillary_Column_Technique
5
TCLP Exiraciion-Seniivolatile Analysis
At’ ‘ iri It r’ —1 , nçir ciiiiiiiiu-v dQfi
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AITACIIME L’ART ii
PARAMETER CODES
PARAMETER CODE/METHOD
IDENTIFICATION NUMBER
METHOD TITLE
REFERENCE
PARAMETER NAME
160 1
Residue. Filterable. Gravimetric. Dried at 180 C
4
TOtal Dissolved Solids (TDS)
160.2
Residue. Non-filterable. Gravinseinc. Dried at 103-105 C
4
Total Suspended Solids (TSS)
160 3
Residue• Total, Gravimeinc, Dried at 103-105 •C
4
Total Solids
1613
Tetra- through Octa- Chlorinated Dioxins and Furans by Isotope Dilutions I 1RGC/IIRMS
6
Dioxin/Furan High Resolution Analysis
200.7
Determination or Metals and Trace Elements in Waler and Wastes by Inductively Coupled
Plasma - Atomic Emission Specnometry (Rev.4 4. 1994)
7
ICP Metals Analysis-Full List
200.7XX
Determination or Metals and Trace Elements in Water and Wastes by Inductively Coupled
Plasma - Atomic Emission Spectrometry (Rev.4.4, 1994)
7
IC? Metals Analysis-XX Specific Metals
200.9/CD
Determination o( Trace Elements by Stabilized Temperature Graphue Furnace Atomic
Absorption Speclrornetry (Rev 2 2. 1994)
7
Graphite Furnace-Cadmium
20 09/SB
Determination ol Trace Elements by Stabilized Temperature Graphite Furnace Atomic
Absorption Spectrornetry
7
Graphite Furnace-Anhiniony
200.9AS
Determination ol Trace Elements by Stabilized Temperature Graphite Furnace Atomic
Absorption Spectromeiry
7
Graphite Furnace-Arsenic
204.2/SB
Antimony AA. Furnace
4
Graphite Furnace-Antimony
206 2
Arsenic AA, Furnace
4
Graphite Furnace-Arsenic
2 1321CD
Cadmium AA, Furnace
4 -
Graphite Furnace-Cadmium
2320.8
Alkalinity, Titration Method
8
Titration Method-Alkalinity
23408
Hardness by Calculation
B
hardness-Calculation
2340C
hardness, EDTA Tmirimetric Method
8
Hardness Titrimeinc. EDTA
25408
Total Solids Dried at 103-105 •C
8
Total Solids
2540C
Total Dissolved Solids Dried at ISO C
8
Total Dissolved Solids (TDS)
25400
Total Suspended Solids Dried at 103-105 •C
8
Total Suspended Solids (TSS)
300 MCI
Ion Chromatography
Determination Inorganic Anions in AQ by IC
300 OF
Ion Chromatography
Ion Chrom -Fluoride
300 0N03
Ion Chromatography
Ion Chirom -Nitrate
310 1
Alkalinity Titrimetric (phI 4 5)
4
Titrimetric Alkalinity
2 All. B, Pan 11 - Diafl DQO Sulnmaxy Form 11/96
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ATI’ACHMENT II- PART 11
PARAMETER CODES
PARAMETER CODE/METHOD
IDENTIFICATION NUMBER j
F METHOD TITLE
REFERENCE
PARAMETER NAME
310 2
Alkalinity. Calorimetric. Automated. Methyl Orange
4
Colorimetric-A lka liiiiiy
3 I I3BFAS
Metals by Electrothermal Atomic Absorption Spectronielry
8
Graphite Furnace-Arsenic
3 1 13B/CD
Metals by Electrothermal Atomic Absorption Spectrometry
8
Graphite Furnace-Cadmium
31 I3BISB
Metals by Electrothermal Atomic Absorption Speclromeiry
8
Graphite Furnace-Antimony
325.2
Chloride. Colorinietnc, Automated Ferricyanide AA II
4
Colorimettic-Chlonde
323 3
Chlonde, Titrimetnc. Mercunc Nitrate
4
Titrimeiric-Ch loride
335.2
Cyanide. Total. Tnnrnetric; Specsrophotometric
4
Titnmelric-Total Cyanide
340.2
Fluonde. Potentiomeiric, Ion Selective Electrode
4
Electrode-Fluoride
350.1
Nitrogen. Ammonia, Colorimctric, Automated Phcnatc
4
Colorimetric-Ammonia
350.2
Nitrogen. Ammonia, Colorimetric; Titrinreiric; Potentiornetric-Distillation Procedure
4
Colctrimetnc. Titrimetric, Electrode-Dist.-Ai,unoiiia
350.3
Nitrogen, Ammonia, Pocentiorneinc. Ion Selective Electrode
4
Electrode-Ammonia
351 2
Nitrogen, Kjeldattl. Total. Colorimeiric, Semi-Automated Block Digester, AA II
4
Colorlinetric Semi-Auto-Total Kjeklahl N (Tl(N)
351 3
Nitrogen. Kjcldahl. Total, Colorimei,ic, Tiirimetnc: Potentiometric
4
Colorimetric, Titriinetr,c. Electrode-Total Kjeldalil N (1KN)
352.1
Nitrogen, Nitrate, Colorinictrtc. Bn cinc
4
Coloriinetric-Nitraic
353.1
Nitrogen. Nitrate-N,tnte. Calorimetric. Automated. Ilydrazine Reduction
4
Calorimetric, Auto.. llydr-Red -Nitrate
353 2
Nitrogen, Nitrate-Nitrite, Colorimetric. Automated, Cadniiuin Reduction
4
Coloriinetric, Auto . Cd -Red-N ilrate
353.3
Nitrogen. Nitrate-Nitrite. Speciroptiotometric, Cadmium Reduction
4
Spectra , Cd-Red-Nitrate
354 1
Nitrogen. Nitrite, Spectrophiotometric
4
Spectrophotometric-Nitrite
365 1
Phosphorus. All Forms, Colorinietric, Autoiiiatcd, Ascorbic Acid
4
Colorimetric. Auto. Ascorbic Acid-Phosphorus
363.2
Phosphorus, All Forms. Coloriniciric, Ascorbic Acid. Single Reagent
4
Colonmelric, Ascorbic Acid. I Reag-Phiosphorus
365.3
Phosphorus. All Forms, Colorirnetric, Ascorbic Acid, Two Reagent
4
Colonmetric, Ascorbic Acid. 2 Reag-Phosphorus
365.4
Phosphorus. Total. Coloriniesric. Autornaied, Block Digescor AA II
4
Colorimetric. Auio -Phosphorus
370 I
Silica. Dissolved. Calorimetric
i
Calorimetric-Silica
375 I
Sullate. Colorinictric, ,‘iitoniaicd. Chloranilatc
4
Colorinictric. Automated-Sulfate
Au R P-’-’ r .riri c urilimil1rv ii ó
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,VrFACIIMEr I’AR’l’ 11
PARAMETER CODES
PARAMETER CODEIMETHOD
IDENTIFICATION NUMBER
METHOD TITLE
REFERENCE
PARAMETER NAME
375.3
Sulfate, Gravimetric
4
Gravimetric -Su lfate
375 4
Sulfate. Turbidiniecric
4
Turbidimetric-SulFate
376.1
Sullide, Titrinietric. Iodine
4
Titnnietric.Su llide
376 2
Sulfide, Colonmeinc, Methylene Blue
4
Colorinietzic-SulIide
403
Bicarbonate
Bicarbonate
405.1
Biochemical Oxygen Demand BOO (5 day, 20C)
4
5 Days 20C -BOO
410.1
Chemical Oxygen Demand. Titriinetric, Mid-Level
4
Titnmetric -COD Mid. Level
410.2
Chemical Oxygen Demand. Titrinictric, Low Level
4
Titrimeiric-COD Low Level
410.3
Chemical Oxygen Demand. Titrimeiric, high Level [ or Saline Waters
4
Titrimetno-COD High Level
410.4
Chemical Oxygen Demand. Colorimetric, Automated; Manual
4
Spectrophotomecric-COD Manual/Auto
4110
Determination of Anions by Ion Chromatography
B
Anions
413.1
Oil and Grease. Total Recoverable, Gravimetric, Separatory Funnel Extraction
4
Gravlmeiric-Oil & Grease
413.2
Oil and Grease, Total Recoverable, Speclrophotometnc. InFrared
4
Oil and Grease (0 & G) - IR Spec.
415.1
Organic Carbon, Total, Combustion or Oxidation
4
Combustion or Oxidation-TOC
415.2
Organic Carbon. Total, UV Promoted, Persulfate Oxidation
TOC-Low Level, LIV Promoted
418.)
Petroleum Hydrocarbons, Total Recoverable, Spectrophocornelnc, Infrared
4
IR Spec-TPII, Petroleum Ilydrocarbons
4l8. ITP II
Peiroleurn Hydrocarbons, Total Recoverable. Spectrophocorneinc. Infrared
4
Total Petroleum llydrocarboiis
4500-PIE
Phosphorus, Ascorbic Acid Method
8
Ascorbic Acid-Phosphorus
4500-P/F
Phosphorus, Automated Ascorbic Acid Reduction Method
8
Auto. Ascorbic Acid-Phosphorus
4500F1C
Fluoride, Ion-Selective Electrode Meiiiod
8
Electrode-Fluoride
4500N02B
Nitrogen (Nitrite) Colorimnetric Method
8
Colorin ictricNiirite
4 SOONO3E
Nitrogen (Nuii-aic) Cadmium Reduction Method
8
Cadmium Red. Manual-Nitrate
4500N03F
Nitrogen (Nitrate) Automated Reduciton Method
8
Cadmium Red. Auto .-Nitrate
4500N03 1 1
Nitrogen (Nitrate) Automated Ilydraziiie Reduction
8
Automated flydrazine-Nitrate
4 Alt. B, Part II - Dralt DQO Summary Form 11/96
-------
ATIACHMENT II - 1’ART II
PARAMETER CODES
602
Purgeabie Aromatics (Trsp-GC/PID)
I0
Purgeable A romatucs Trap-GC/P 1D
PARAMETER CODE/METHOD
IDENTIFICATION NUMBER
METHOD TITLE
REFERENCE
PAItAME1ER NAME
4500S1D
Sulfide, Methyletie Blue Method
8
Methyletic Blue Sulfide
4500S1F
Sulfide, lodometric Method
8
lodometric-Sullide
4500S04C
Sulfate, Graviunetruc Method with Ignition of Residue
8
Grav.+lguiiion-Sullate
4500S 04D
Sulfate, Gravimeinc Method with Drying of Residue
8
Grav.+Diying-Sulfate
4500S 11D
Silica, Molybdosilicate Method
8
Molybdosilicate-Silica
504 I
1,2-Dibromethane (EDS). I.2-Dibromo-3-chloropropane (DBCP), and 1,2.3-
Trichloropropane (123 TCP) in Water by Microextractuon and Gas Chromatography (Rev.
1.1, 1995)
9
EDB. DBCP & I23TCP, Microextraction & CC
5210/B
Biochemical Oxygen Demand (BOD), 5 Day BOD Test
8
5 Day-BOD
5220/C
Chemical Oxygen Demand (COD). Closed Reflux, Tutrinietric Method
8
Titruuuictric-COD Mid Level
5220/D
Chemical Oxygen Demand (COD). Closed Reflux. Colorimetnc Method
8
Spectropliotometruc-COD Manual/Auto
524.2
Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas
Chromatography/Mass Spectrometry (Rev. 4 0. 1992)
9
Measurement of Purgeablc Organic Compounds in Water. Capillary
Column by CC/MS
524 2+
Measurement of Purgeable Organic Compounds in Water by Capillary Column Gas
Chromatography/Mass Spectroinetry (Rev. 4.0. 1992)
9
524.2 PIus Additional Compounds
-
525 2
Determination of Organic Compounds in Dunking Water by Liquid-Solid Extraction and
Capillary Column Gas Chromatography/Mass Spectrometry (Rev. 2 0, 1995)
9
Determination of Organic Coitipounds in DW by Liquid Solid
Extraction Capillary Column by CC/MS
5310/B
Total Organic Carbon (TOC) Combustion-infrared Method
8
Combustion-Infrared-TOC
53 10/C
Total Organic Carbon (TOC) Persulfate-Ultraviolet Oxidation MeiJicid
8
Persulfate-UV Oxidation-TOC
5310/D
Total Organic Carbon (TOC) Wet-Oxidation Method
8
Wet-OxidationTOC
551.1
Detection of Chlorination Disinfection Byproducts and Chlorinated Solvents, and
Ilalogenated Pesticides/i ierbicudes in Drinking Water by Liquid/Liquid Extraction and Gas
Chromatography with Election-Capture Detection
9
Det. Chioro. Disin Dyprods. Cliloro SoIv. by LL.&GC
5520/B
Oil and Create Partition-Gravuiteuric Method
8
Gravirnetric-OtI & Grease
5520/C&F
Oil and Grease Partuuion-liifrarcd Method and hydrocarbons
8
IR SreCIPIJ. Pctuolcuin, ilydrocarboit
601
Purgeable llalcca,boiis (Trap-GC/I iaII Detector-Electrolytic Conductivity Detector)
10
Purgeable I lalocarbons Trap-GC/ELCD
At, fl P- ’ II flr’.fl flfl( r I/or.
-------
A1TACILMI PART H
PARAMETER CODES
PARAMETER CODE/METhOD
IDENT IFICATION NUMBER
METHOD TITLE
REFERENCE
PARAMETER NAME
608
Organochlorine Pesticides and PCBs by (GC/ECD)
JO
Organochloriiie Pcst PCB•GCIECD
624
Purgeables (Trsp-GC/MS)
10
Purgeable Trap-GCIMS
625
Base/Neutrals and Acids (CC/MS)
JO
Basc/Neutrals&Acids Extr CC/MS
80 ISA
Nonhalogenated Volatile Organics by Gas Chroniaiograpliy
S
Noiil*alogenaled Volatile Org CC
808 0A
Organochlonne Pesticides and Polychlonnated Biphenyls by Gas Chromatography (Rev. I.
1994)
5
Organoclilorine Pest &PCB by CC/ECD
8240B
Volatile Organics by Gas ChromatograpliylMass Spcctromctry (GC/MS) (Rev.2. 1994)
5
Volatile Organic Compounds by CC/MS
8270B
Semivolalile Organic Compounds by Gas Chroniatograpliy(Mass Spectroinesry (GC/MS).
Capillary Column Technique (Rev. 2. 1994)
5
Semivolatile Organic Compounds by CC/MS
8290
Polychlorinated Diberuodioxins (PCDDs) and Polyclilonnated Dibenzolurans (PCDFs) by
I ligb.Reaolulion Gas Chromatography/High Resolution Mass Spectromeiry
(F 1RGC/IIRMS) (Rcv.0. 1994)
5
PCDDS & PCDFS by HRGC/MS
ASTM2974
Standard Test Method for Moisture. Ash and Organic Matter of Peat and Oilier Organic
Matter
11
TCOC - TOT Combustible Org Cotileiti
ASTMD4ZZ
Standard Test Method for Particle-Size Analysis of Soils
I I
Grain Size Analysts
ILMO4OCN
USEPA CLP SOW for Inorganics Analysis - ILMO4 0
12
- Cyanide Inorganic CLP SOW
ILM O4 OMT
USEPA CLP SOW for Inorganics Analysis - ILMO4.0
12
Metals (no CN) Inorganic CLP SOW
ILMO4OTL
USEPA CLP SOW for Inorganics Analysis - ILMO4 0
12
Metals & Cyanide Inorganic CLP SOW
TO-I
Detennirialion of Volatile Organic Compounds in Ambient Air using Tersax Adsorption and
CC/MS
13
VOC-AIR. Tenax Tubes
TO- 14
Deteinunalion of Volatile Organic Compounds in Ambient Air Using Sununa Passivated
Canister Sampling and CC Analysis
13
VOC-AIR. Sumrna Canisters
TO-2
Detemsination of Vol ti1e Organic compounds in Ambient Air using Carbon Molecular
Sieve Adsorption and CC/MS
13
VOC-AIR. Carbon Molecular Sieve
NOTE: The method number is incorporated into the Paranieer Code
REFERENCES.
I. USEPA CLP Statement of Work for Organics Analysis, Multi-Media. Multi-Concentration, OLMO3.I. August 1994
2. NIOSII Manual of Analytical Methods (Second. Part I), NIOSI! Mouiitoring Methods, Volume I.
6 Au. B, Part 11 - Draft DQO SUHUIIaIy Form 11/96
-------
AlT ACI1MENT B - PART 11
PARAMETER CODES
3. USEPA CLP Statement of Work for Analysis of Polychiorinated Dibenzo-p .Dioxins (PCDD) and Polychiorinated Dibenzofurans (PCDF). DFLMOI 0/DFLMOI.l - Rev 12/90 and Rev. 9/91
4. Methods for Chemical Analysis of Water and Wastes, Enviro,itii—uiial Protection Agency, EPA-600/4-79-020
5. Test Methods for Evaluating Solid Waste, Physical/Chemical Methods, SW-846, Third Edition. July 1992 and Updates
6. Method 1613- Tetra- Through Octa- Chlorinated Dioxins and Furans by Isotope Dili.ii’nis IIRGC/HRMS. EPA 821-D-94-0O5. October 1994. Rev B.
7. Methods for tue Determination of Metals in Environmental Samples. EPA/600/4-9l/010, June 1991, and Supplement I. EPA-600/R-94/1 11. May 1994.
8. Standard Methods for the Examination of Waler and Wastewater. 19th Edition, 1995
9 Methods for the Determination of Organic Compounds in Drinking Water, December 1988. EPA/60014-881039 and Updates
10. Code of Federal Regulations, 40 CFR. Part 136. App A
II. American Society for Testing and Materials
12 USEPA CLP Statement of Work for Inorganics Analysis. Multi-media, Multi-concentration, ILMO4.O
13. EPA Compendium of Methods for the Determination of Toxic Organic Compounds in Ambient Air. EPA-60014-84-041, May, 1987.
‘ • i Pr,1 1 nnr
-------
REGION I, EPA-NE ORGANIC REGIONAL DATA ASSESSMENT (ORDA)*
CASE #: ___________________ SITE NAME: ___________________
LAB NAME: _________________ # OF SAMPLES/MATRIX: __________
SDG #: ___________________ VALIDATION CONTRACTOR: ______
SOW #/CONTRACT #: _________ VALIDATOR’S NAME: ___________
EPA-NE DV TIER LEVEL: ______ DATE DP REC’D BY EPA-NE: ______
TPO/PO: *ACTION ____ r I ____ DV COMPLETION DATE: __________
ANALYTICAL DATA OUALITY SUMMARY
VOA PesrIPCB
1. Preservation arid Contractual Holding Times ________ ________ ____________
2. GCIMS / GC/ECD Instrument Performance Check _______ _______ __________
3. Initial Calibration _________ ________ ____________
4. Continuing Calibration ________ ________ ____________
5. Blanks ______ ______ _________
6. Surrogate Compounds ________ ___________
7. Inernal Standards ________ ________ ____________
8. Matrix Spike/Matrix Spike Duplicate ________ ________ ____________
9. Sensitivity Check ________ ________ ___________
10. PE Samples-Accuracy Check ________ ________ ____________
11. Target Compound identification ________ ________ ____________
12. Compound Quantitation and Reported QLs ________ ________ ___________
13. Tentatively Identified Compounds ________ ____________
14. Semivolatile Cleanup/PesticidefPCB Cleanup ________ ________ ____________
15. Data Completeness ________ _________ ____________
16. Overall Evaluation of Data ________ ________ ____________
o = Data had no problems or were qualified due to minor contractual problems.
m = Data were qualified due to major contractual problems.
z = Data were rejected as unusable due major contractual problems.
ACTION ITEMS: (z items)________________________________________________________
AREAS OF CONCERN: (m items)_______________________________________________
COMMENTS:
*This form assesses the analytical data quality in terms f contractual compliance only. It does not assess sampling
errors and/or non -contractual analytical issues that affect data quality.
*a Check ACTION” only if contracaial defects resulted in reduced payment/data rejection recommendations.
Vajidator: _____________________________________________ Date: _____________________
INSTR JCTIONS ON REVERSE SiDE
12/96
-------
GtJ [ DANCE FOR COMPLETIIS,!G THE ORDA
The ORDA form provides the laboratory’s CLP-TPO and other contract management personnel ‘ith an overview
of the contractual analysis and reporting deficiencies found in an analytical data package and identifies those
contractual deficiencies that resulted in reduced payment/data rejection recommendations/actions. The ORDA form
is used to summarize analytical data quality only in terms of contractual compliance. Sampling errors and non-
contractual analytical errors that affect data quality are not summarized on this form, but rather are documented in
the Tier I Validation Cover Letter and Tier Il/Ill Data Validation Reports. For instance, if the sampler did not ship
the samples until after the holding time had expired, a notation would not be made on the ORDA form since the
laboratory is not responsible for the sampler’s actions.
The ORDA form should be completed as follows:
1. Fill in all of the header information (with the exception of the TPO Action/FYI field): Case Number, Site
Name, Laboratory Name, number and matrix of samples in the data package, SOC Number, Validation
Contractor, SOW#/Contract#, Data Validacor’s Name, EPA-NE Data Validation Tier Level (i.e., I, II, III
or partial 1 1/111), Date the Data Package was received by EPA-NE, and the Data Validation Completion
Date.
2 Summarize the contractual problems discovered during data validation by fraction and by evaluation criteria
in the “Analytical Data Summary table, and in the ‘Action Items” and ‘Areas of Concern’ sections as
described in items 3 through 6 below. Use the Data Validation Memoranda as a guide when completing
the ORDA form.
3. The following qualifiers must be utilized o document contractual problems on the ORDA forms.
o = Data had no problems or were qualified due to minor contractual problems
m = Data were qualified due to major contractual problems
z = Data were rejected as unusable due to major contractual problems
4 11 the data were acceptable, or were qualified due to minor contractual problems, enter the qualifier “o ”
into the appropriate column (fraction) and row (evaluation criteria). No further documentation is necessary
on the ORDA form. An example of a minor problem would be a sernivolatile compound that slightly
exceeded the SOW-specified %RSD initial calibration criterion.
5 If the data were qualified due to major contractual problems, enter the qualifier “in” into the appropriate
column (fraction) and row (evaluation criteria). Use a different superscript (ms, rn, etc.) for each major
contractual problem identified and provide a brief description of each major problem in the “Areas of
Concern’ section. An example of a major contractual problem resulting in data qualification would be a
semrvolatjje internal standard that had extremely low area counts (below the lower limit of the SOW-
specified acceptance criterion) and reanalysis was not performed.
6. If the data were rejected as unusable due to major contractual problems, enter the qualifier “z’ in the
appropriate column (fraction) and row (evaluation criteria). Use a different superscript (z 1 , , etc.) for
each major contractual problem identified and provide a brief description of each major problem in the
‘Action Items’ section. An example of a major contractual problem resulting in data rejection would be
contractual holding time criteria that were exceeded for volatiles.
7. Complete the TPO Action/FYI field using the information contained in the “Action Items’ and “Areas of
Concern” sections. TPO Action should be indicated with a check mark (V) in the space following “Action”
only if the contractual defects resulted itt reduced payment or data rejection. If no TPO Actions are
indicated, then a check mark (v’) should be placed in the space following ‘FYI”.
8. The validator who completed the ORDA form must sign his(her name in the Validator ” field and enter
the ORDA completion date in the ‘Date’ field.
-------
[ Reference to Case No(s) :
Contract Laboratory Program
REGiONAL/LABORATORY COMMUNICATION SYSTEM
Telephone Record Log
Date of Call: ___________________________________________
Laboratory Name: ___________________________________________
Lab Contact: ________________________________________
Region: ___________________________________________
Regional Contact: ___________________________________________
Call Initiated By: ____ Laboratory ____ Region
In reference to data for the following sample number(s):
Summary of Questions/Issues Discus5ed:
Summary of Resolution:
Signature Date
Distribution: (1) Lab Copy, (2) Region Copy, (3) SMO Copy
-------
EPA-NE
Data Validation Worksheet Cover Page - Page 1
Site Name
Reference No.
REGION I ORGANIC DATA VALIDATION
The following data package has been validated:
Lab Name _________
Case/Project No. ____
SDG No. ________
No. of Samples/Matrix
SOW/Method No.
Sampling Date(s) -
Shipping Date(s)
Date Rec’d by lab
Traffic Report Sample Nos.
Trip Blank No. ________
Equipment Blank No. ____
Bottle Blank No. _______
Field Duplicate Nos. _____
PES Nos. ____________
The Region I, EPA-NE Data Validation Functional Guidelines for Evaluating Environmental Analyses ,
revision _________ was used to evaluate the data andlor approved modifications to the EPA-NE
Functional Guidelines were used to evaluate the data and are attached to this cover page: (attach modified
Criteria from EPA approved QAPjP or amendment to QAPJP).
A Tier II or Tier III evaluation was used to validate the data (circle one). If a Tier II validation with a
partial Tier III was used, then identify samples, parameters, etc. that received partial Tier III validation
The data were evaluated based upon the following parameters:
- Overall Evaluation of Data
- Data Completeness (CSF Audit - Tier 1)
- Preservation & Technical Holding Times
- GCJMS & GC/ECD Instrument Performance Check
- Initial & Continuing Calibrations
- Blanks
- Surrogate Compounds
- Internal Standards
- Matrix Spike/Matrix Spike Duplicate
Region I Definitions and Qualifiers:
- Field Duplicates
- Sensitivity Check
- PE Samples/Accuracy Check
- Target Compound Identification
- Compound Quancitation and Reported
Quantitation Limits
- TiCs
- Sernivolatile and Pesticide/PCB Cleanup
- System Performance
A - Acceptable Data
I - Numerical value associated with compound is an estimated quantity.
R - The data are rejected as unusable. The R replaces the numerical value or sample quantitation limit.
U - Compound not detected at that numerical sample quantitation limit.
UI - The sample quantitation limit is an estimated quantity.
TB, BB, EB - Compound detected in aqueous trip blank, aqueous bottle blank, or aqueous equipment
blank associated with soil/sediment samples.
Validator’s Name
.Company Name Phone Number
Date Validation Started
Date Validation Completed
12/96
-------
EPA-NE
Data Va1ida ion Worksheet Cover Page - Page 2
Check if all criteria are met and no hard copy worksheet provided. Indicate NA if worksheet is not applicable
to analytical method. Note: there is no standard worksheet for System Performance, however, the valid
must document all system performance issues in the Data Validation Memorandum.
VOA/SV workshee :
VOA/SV-PestJPCB COMPLETE SDG FILE (CSF) AUDIT ____
VOA/SV-PescJPCB-I PRESERVATION AND HOLDING TIMES ____
VOAISV-II GC/MS INSTRUMENT PERFORMANCE CHECK (TUNING) ____
VOAISV-Ifl INITIAL CALIBRATION ____
VOAISV-IV CONTINUING CALIBRATION ____
VOA/SV-PCstIPCB-V-A BLANK ANALYSiS ____
VOAJSV-PestIPCB-V-B BLANK ANALYSIS ____
VOA-VI VOA SURROGATE SPIKE RECOVERIES ____
SV-VI SV SURROGATE SPIKE RECOVERIES ____
VOA/SV-VI I INTERNAL STANDARD PERFORMANCE ____
VOA/SV-Pest/PCB-VIJI MATRIX SPIKE/MATRIX SPIKE DUPLICATE ____
VOA/SV-Pest/PCB-D( FIELD DUPLICATE PRECISION ____
VOA/SV.PestJPCB-X SENSITIVITY CHECK ____
VOA/SV-Pe tPCB-XI ACCURACY CHECK ____
VOAISV-PestJPC B-Xfl TARGET COMPOUND IDENTIFICATION ____
VOA/SV-PestJPCB-X1fl SAMPLE QUANTITATION ____
VOA/SV-XIV TENTATIVELY IDENTIFIED COMPOUNDS ____
VOA/SV-XV SEM VOLATILE CLEANUP
TABLE Il-WORKSHEET OVERALL EVALUATION OF DATA
Pest/PCB wcrksheecs :
VOA/SV-PestJPCB COMPLETE SDG FILE (CSF) AUDIT
VOA/SV-PesUPCB-I PRESERVATION AND HOLDING TIMES
PestIPCB-IIA GC/ECD INSTRUMENT PERFORMANCE CHECK-
RESOLUTION
PestIPC B-llB GC/ECD INSTRUMENT PERFORMANCE CHECK-
RETENTION TIMES
Pest/PCB-I [ C GC/ECD INSTRUMENT PERFORMANCE CHECK-
ACCURACY CHECK OF INITIAL CALIBRATION
PesUPCB-III) GC/ECD INSTRUMENT PERFORMANCE CHECK-
PESTICIDE DEGRADATION
Pest/PCB-III INITIAL CALIBRATION
PesIPCB-IV CONTINUING CALIBRATION
VOiVSV-Pest/PCB -V-A BLANK ANALYSIS
VOAJSV-Pest/PCB-V.B BLANK ANALYSIS
Pest/PCB-VI SURROGATE COMPOUNDS:
SPIKE RECOVERIES AND RETENTION TIME SHIFT
Pesc/PCB-Vfl PESTICIDE CLEANUP
VOAjSV-Pest/PCB-VIII MATRIX SPIKEIMATRLX SPIKE DUPLICATE
VOAJSV-Pest/PCB-IX FIELD DUPLICATE PRECISION
VOA/SV-Pest/PCB -X SENSiTIVITY CHECK
VOA/SV-Pest/PCB-XI ACCURACY CHECK
Pesc/PCB-XII COMPOUND IDENTIFICATION
VQA/SV-Pest/PCB-XIH SAMPLE QUANTITATION
TABLE Il-WORKSHEET OVERALL EVALUATION OF DATA
I certify that all criteria were met for the worksheets checked above.
Sisnature:_____________________ Name:_____________________
Date: ___________________________
12 /96
-------
The data validator generates a Data Validation Report, applicable to Data Validation Tiers II and III, that consists
of the following components in the order specified below: (Refer to Section 11 for a description of each of the
Data Validation Report components).
1. Organic Regional Data Assessment/Inorganic Regional Data Assessment
(ORDAJIRDA) Form
2. Data Validation Memorandum
a. Narrative
b. Table I-Qualifier Recommendation Summary Table
c. Table Il-Overall Evaluation of Data
d. Table Ill-Tentatively Identified Compounds
e. Data Summary Tables
3. Standard Data Validation Worksheets
a. Manual
b. Automated Data Review Reports (i.e., CADRE)
4. Support Documentation
a. Copy of non-CL? analytical method, e.g., DAS methods, modified EPA methods
b. Copies of PES Score Reports/Vendor PES QC Acceptance Limits
c. Copies of Telephone Logs/Communication Forms for:
• RSCC communications
• Requests for laboratory data resubmissions/clarifications
• Communications with samplers resolving sampling problems
• Communications with TPO/Lead Chemist to report contractually-deficient data
for rejection/reduced payment
• Communications with EPA Site Manager concerning possible data rejection
• EPA Site Manager authorization for alternate DV tier
d. Copies of data supporting recommendations for reduced payment resulting from CSF
Audit and/or PE sample result evaluation
e. OriginaL data to support recommendations for data rejection/non-payment identified from
Tier II or Tier III data validation
f Copies of field sampling notes and/or field report supplied by field sampler
g. Copies of EPA-approved amendments to QAPJP and/or SAP describing modified criteria
to be used for validating site data
5. CSF Completeness Evidence Audit
6. DQO Summary Form
The data validator is responsible for implementing all corrective actions required by the contractor Lead Chemist
in response to EPA-NE data validation oversight findings.
12/96
-------
EPA-NE i Validation Woikslicct
Overall Evaluation of Data - Data Validatioii Meinoranduiii - Table 11
VOLATILE ORGANICS
Analytical Method
DQO (list all DQOs) II Sampling and/or
Appropriate
Ycs or No
I___________________
I
Measurement Error
Sampling
Var lablliEy**
Potential
Issues
Usability
Aiialytical
Error J
Sampling
Error*
* The evaluation of “sampling error” cannot be completely assessed in data validation.
* * Sampling variability is not assessed in data validation.
Validator:
Date:
12/96
-------
EPA-NI [ a Validation Worksheet
Overall Evaluation of Data - Data Validation Meiiioraiidum - Table LI
SEMI VOLATILE ORGANICS
Analytical Method
DQO (list all DQOs) Sampling and/or
Appropriate
Yes or No
Measurement Eiror
Variability** Ii Usability
Sampling 0 Potential
Issues
II
lytical
Error
Sampling
Error*
* The evaluation of “sampling error” cannot be completely assessed in data validation.
** Sampling variability is not assessed in data validation.
Validator:
Date:
12196
-------
EPA-NE - Data Validation Worksheet
VOA/SV - Pest/PCB
COMPLETE SDG FILE (CSF) AUDIT
Organic Fractions:___________________________________________
Missing Information Date Lab Contacted Date Received
Valjdator: _________________________ Date: _______
12/96
-------
EPA-NE - Da t
VOAISV - I’cs
aIioii
.1
12/96
Sampler:
Co in aiiy : —
1. I’RESERVAiiON AND HOLDING ‘lIMES.
________________________ Contacted: Yes No Date:___________
Circle saniplc nttiiibcrs viili exceeded technical holding tiiliC or UiiiittC(l j)rCSCrV8tIOI I.
List all rcquiicd preservation codes and circle omitted llcscrvation codes.
Circle all excccdcd technical lioldijig tilnec.
ldciitily extraction technique after “II of Days”/( t Extraction Code).
Samnic No
(I A No)
Mau*
rIot
Code
D uo
Saopted
VgA
}
I it’ lA
i’ 1 5 1/ 11 1 1
Alodyced
I)ale
1
rI C O ,, i,nip
J i or t)iys
to Aitaf
1
•
Aciltin
j
J I nUocicd
I I)ue
Sn.ii
I ol Ihys
to Lot: Jo
An,Iy :ed
I),le
E 01
o1 i s
to Anal
A bmi
hale
rtitoctrd
101111)3 I l),lc
SIIII , Atl.1I)7c*J J
to mU 1(
or D i ’ ,
font, I ‘tir
to An I
Actn i
Preservation Code:
1. Cool @4°C (± 2°)
2. Preserve tviili llCl to at least p11 2
3. Protect from light
4. Freeze
5. Room Temperature (Avoid excessive heat)
(*Ex(rnct loll Code:)
L/L - Liquid/Liquid
SON - Sonication
SEP - Separatory Funnel
SOX - Soxhlct
SPE - Solid Phase Extraction
Action Code:
J - Estimate (J) Detected Values
UJ - Esiimatc (UJ) Non-Detected Values
R - Reject (R) Non-Detected Values
Validator:
Date:
-------
EPA4 ata Validation Woikslieet
VOA/ v-u
II. CC/MS INSTRUMENT PERFORMANCE CI IECK (‘FUN ING)
List all Instrument Performance Checks that ate outside method QC Lulling acceptance criteria.
Volatile
Iiistrwuicuit Perloruuiaiice Check
(Cotuiponuud Name)
Analysis
Date and ‘fiuuie
lush nnieiit
lou(s)
Affected
l’em cent
Relative
Abuimulan
QC
Linuitc
Samples Affected
Action
Coinuiients:
Senilvolatile
Instrument Perfonuinuce Check
(Conipouuid Nauuie)
Amia lyslc
Date and Time
lnstrwiiemmt
lou(s)
Affected
Percent
Relative
Abundance
QC
Lhmiults
Samples Affected
Action
Continents:
If tuning compounds and criteria are different from those specified in CLP SOW OLMO3. 1, then the vahidator should include a COPY of time immethod-
specific tuning criteria with this worksheet.
Validator:_________________________________________ Date:__________________
12/96
-------
EPA-NE - Data Validation Worksheet
VOA/S V-HI
11!. INITIAL CALIBRATION - List all analytes that are outside calibration ciitciia.
Validator: ________________________ Date:
hate of
ICAL
hiistruiticiit
I’ni aineter
1 1a(i i’c
Couipotiiul
% RSD
RRV
S aiiiplec
Alfected
A(ieii
Comments:
12/96
-------
EPA-NE - Data Validation Woikslicet
VOA/SV-IY
IV. CONI’INUING CALIBRATION - List all aiialytes [ haL arc outside caliUration ctilcria.
Date of
ICAL
Date of
CCAL
Iuis(runiciit
Parameter
l 1n1i ix
Compound
%L)
liKE
Saiiiplcs Affected
Actioii
Comments:
Validator: Date:
12/96
-------
• - NE - Data Validation Wozkshect
VOA1SV - l’est/I’CIJ-V-A
V. BLANK ANALYSIS
List the blank contamination below. Coticcifli atioli Level: _________
Sampler: Company: _______________________ Contacted: Yes No Date:_______
1. Laboratory: Method, Storage aiid Itistritment Blanks
I)ate
Extracted
Date
Aitalyzed
Parnnieter/
Matrix
Sample No.
(Blank Type) .j
I
l,icti-i,riiciit/
Cotuiiin
Cuiiipuuitd
Coiic.
(units)
2. Field: Equipment (Rinsate), Trip and Bottle Blanks
Date
Extracted
Date
j Airalyzcd
l’nraiiieterl
Matrix
Sample No.
(Blank Type)
Iiislruiiiciit/
Column
Compound
Coiic.
(iiiil(s)
Validator:
Date:
12196
-------
- Data Valic.Iaion Woikshce
VOA/SV - l’est/PCB-V-B
3. Blank Actions — List the inaxiiiiuin coiicenliations of blaiik COIIIpOUIIdS
Couipouiid
iypc or Itlatik
J)afe fllnitk
Sa uiuplcd/Origina(cd
l%1a’c.
Cotic.
(itiuits)
Acliout
Le ’cl
(itiui(s)
S.’iii, 1 ile
QL
Sniupkc
Al Iccied
Actituti
Vahidator:
Date:
12/96
-------
EPA-NE - Data Validation Worksheet
VOA-VI
VI. VOA SURROGATE SI’IKE RECOVERIES - List all surrogate compound rccovcrics (hat nie outside method QC acceptance ciitena.
Method
Volatile Method QC Acccptauicc Ci itci Ia
Toluctic-d 8
BFB
DCE-d 4
Oilier.
OLMO3.2
Water Soil
88-110 84-138
Water Soil
86-115 59-113
Water Soil
76-114 70-121
OLCO2.1
NA
80-120
NA
Oilier:
Sample Nuiuiber/Matrix
% Recovery
% Recovery
% Recovery
% Recovery
Action
Date:
Validator:
12/96
-------
EPA-NE - Data Validation Worksheet
Sv-VI
VI. SV SURROGATE SPIKE RECOVERIES - List all sutlognie compound rccoveiics that ale outside method QC acceptalice em item ia
Method
2-PP
Avid Method OC A
2.4.6-TBP
Water Soil
10-123 19-122
l5-130
ceutauce Critci la
2-C1’-dA
Method
Hasc/Ncutial Isletliod QC Acccptuiicc Ciilciia I
NBZ-d 1
2-FBP
TP II-d 14
l,2-DCB-d 4
Other:
OLMO3.2
Watcr Soil
35-11423-120
Water Soil
43-11630-115
Water Soil
33-141 18-137
Water Soil
16-11020-130
OLCO2.l
40-110
30-110
20-l’l0
NA
Oilier:
Sample
Nuiiibcr/Matrix
% Recovery
% Recovery
% Recovery
C
% Recovery
% Recovety
Action
OLM O3.2
OLCO2. 1
Oilier:
Saiiiple Nutitber/Matrix
Plieiiol-d
Water
10-1102
Soil
4-113
15-115
% Recovery
Water Soil
21-11025-121
15-1 10
% Rcco crv
% Recovery
Water Soil
33-110 20-130
NA
% Rccoveuy
Otlicr
% Recovery
Actioii
- Validatom-:
* Advisory Surrogates - OLMO3.2
Date:
12196
-------
EPA-NE - Data Validation Worksheet
VOA/SV-VI I
VII. INTERNAL STANDARD PERFORMANCE
List the internal standards that are outside the area count and retention time method QC acceptancc cruet-ia.
IS Area Count method QC acceptance criteria:__________________________________________
IS Retention Time method QC acceptance criteria:
Sample
1)a e and
Tinie
Iuis(riinieiit
Pat anicter
IS
Outside Area
IS At en
UI
Acceptable
Action
Number
(TRY)
Analyzed
Count and/or
IUI’ Criteria
Shift
Range
(IS at ca rn I tT shift)
Validator:
I)ate:
12/96
-------
EPA-NE - Data Validation Worksheet
YOA/SV - Pcst/PCJJ-VI1I
VIII. 1\IATRIX SPIKE/MATRIX SPIKE DU I’LJCATE - List all MSIMSI.) analytcs that are outside method QC acceptance
criteria.
Use a separate worksheet for each MS/MSD pair.
Validator:
Matrix ______________ Concentration Level _____________
Sample II
Paraiiietcr
Co iipoiiiid
r.is
%Rcc
E iSD
%Itcc
RPI)
T IctIiod QC iiiiiits
Co ,icciilraliu ,i
% ItSI)
Action
% Rcc
RI’E)
U,is 1 ,ikcd
MS
MSI.)
Saiiiiile
Date:
12/96
-------
EPA-NE - Data Validation Worksheet
VOA/SV - Pest/PCB-IX
IX. FIELD DU I’LICATE PRECISION - List all field duplicate atialytes that aic outside criteria.
Use a separate worksheet for each field duplicate pair.
Sample Number _________ Duplicate Sample Number ________ Matrix ________
Parameter
Conipound
Sample
Cojic.
Saiiipte QL
D uplicate
Couic.
Duplicate QJ
RPI)
QC Acceptance
Criteria RI’D or
Action
SQL,
2xSQL
SQl.
2xSQL
NM
* For instances where one duplicate result is ND (or repom ted less thami the sample QL).
Does the MS/MSD data indicate acceptable laboratory precision?
Comments:
YN
Contractor Name:
Dale:
Date Contacted:
Sampler Name: ________________________
Reason for Contact and tesolutiori obtained:
Validator:
12/96
-------
EPA-NE - Data Validation Woikshcct
VOA/SV - Pcst/PCB-X
X. SENSITIVITY ChECK (Method Detection Liiiiit Study)
List all compounds, surrogates, and internal standards that arc outside thc MDL ctitcria.
• Has an appropriate MDL study been subriiiiied with seven replicates for each coinpoutid and matrix of inteiest 1 Y N
• Date of l’reparationlAnalysis: _________ Within I yeai? Y N
• Instrument l.D.: ________ Same as samples? Y N
• Columnmi 1.1).: Same as samples? Y N
Matri.
Compound
MDL > QL
f.kthod QC Liinit
< 80% or > 120%
IS Oulciik Area Cotmi
amllor It F Criteria
RSI) > 20%
Snuiples Allected
Aclion
If an
(Lab
MDL study has not been submitted, use only time LFB results to evaluate data.
oratory Fortified Blank) - List all LFB compounds, surrogates and internal standards that are outside criteria.
•
•
S
Has an appropriate and complete LFB been submitted at the proper frequency?
Does it contain all target compounds at the method-required QLs?
Was the LFB spiked with a standard from a source (vendor) independent of the calibration standard?
Y N
Y N
Y N
Matrix
Conipoutici
Mctiiwl QC Li,iiits
< 60% or > 140%
Other:
IS Outside Area
Count aiidlor ItT
Criteria
Samples Aifected
Action
Validator:
Date:
12/96
-------
EPA-NE - uata Validation Worksheet
VOA/SV - PestII’CB-XI
XI. ACCURACY CHECK (Performance Evaluation Results) - List all analytes that ale outside criteria
SDG No: CASE: _____
Are more than one-half of the PES aiialytes within criteria for each palamelci. Y N
I’E
Sample
Auiipule
Number
l’arauieter
Type of
I’ES
Mali i?c
Auialyte
Coiic.
Region I E1’A
I’ES Scorcs
No n-EPA I’ES
Scores**
Sauipfes Affected
Action
Nuitiber
* For Region I PESs indicate the Region I PES Scote Report Result: Action high; Action Low; TCL MISS; TCL CONTAMiNANT; TIC
HIT; TIC MISS; TIC CONTAMINANT
** For Non-EPA PESs indicate the Non-EPA PES Score: PES COMPOUND MISS; PES COMPOUND CONTAMINANT; PES COMPOUND
HIT (% Recovery Limits)
Validator: ____________________________________________________ Date: _______________
12/96
-------
EI’A-NE - Data Validatioii Woiksliect
VOA/SV - l’est/ I’CB-XII
XII. TARGE1’ CO!\II’OUND IDENTIFICATION - List thc aualylcs (hat ate outside the acceptance ciilcria.
Sample Nimnilier
Coimipound
ISIS bus
RWf
Ac(iomi
Vahidator:
Date:
12/96
-------
LVA-NE - Data Validation Worksheet
VOA/SV - Pcst/PCB-XIII
XIII. SAMPLE QUANTITATION
Recalculate, from the raw data, the concentrations for one positive detect and one reptirtcd sample (lualititation limit for a tion-detect in a diltitcd samimple or soil sample
per fraction. (Note: i\lthough Section XIII, C. 1 .a, requires that one calculation for each fraction in each sample be performed, time validator is only rcquirc(l to
reproduce an example, for each fraction, of one positive detect and one salimpic qtiantitation limit calculatioii on this worksheet.)
Do all soil/sediment samples have % solids greater than 30%? Y N
If no, list sample numbers --
Fraction
Calculation
VOA
Sample No
Reported_Compound
Reported Value-
Not Detected Compound
Reported Quantilammon Limit-
DNA
Sample No.:
Reported_Compound
Reported ValueS
Not Detected Compound
Reported Quantitation Liuiiit
rest lc lde/PCB
Sample No.
Reported Compound:
Reported Value:
Not Detected Compound:
Reported Quaniitation Limit
Validator:
Date:
12/96
-------
tri -NE - Data Validation Worksheet
VOA/SV-XIV
XIV. TENTATIVELY IDENTIFIED COMPOUNDS (TICs)
List the 5 TICs having [ lie highest concentration for cacti sample Parameter.
Validator:
Date: ______________
12/96
Sanipic Number I Parameter J Crnn anmud Riti’ Est. Coiic. Action
-------
EPA-NE - Data Validation Worksheet
VOA/SV-XY
XV. SEIsII VOLATILE CLEANUP - List all analytes that are outside method cleanup QC criteria.
Cleanup
Procedure
Instrument if
or Lot if
L)ate/Timc GI’C
Calibrated or
Check Solution
Analyzed
Coiiipound
% Rec
,
QC
Liiiiits
Satiiples Affected
Aclion
Did the GPC column meet; resolution requirements?
peak shape requirements?
retention time shift requirements?
Was the GPC calibration, Silica Gel cleanup checked at (lie method required frequency with correct compounds
Y
Y
Y
and concentrations? Y
or N
or N
or N
or N
Were all compounds less than QL for (lie GPCISilica Gel/Acid-Partition blank?
Y
or N
Did the blank surrogate recoveries and IS area counts and RTs (if added) meet method QC acceptance criteria?
Comments:
Y
or N
Validator: Date:
12196
-------
Inorganic Traffic Report Case No
& Chain of Custody Record
(For Inorganic CLP Analysis)
E’I’A United States Environmeniat protection Agency
Contract Laboratory Program
Code Account Code
2 Region No Sampling Co
4 Dale ShiPPed [ Carrier
(Enter
6 Matrix
in Column A)
1 Surlace Waler
2 Ground Water
3 Leachate
4 Field OC
5 Soil/Sediment
7 Waste (High
only)
6 Oil (High only)
8 Other (sp’cify
in Column .4)
(Enter
7 Preservative
in Column 0)
I HCI
2 HNO3
3 NaOH
4 H SO 4
5 K 2 CR 2 0 7
7 Other (specify
in Column 0)
6 Ice only
N Not preserved
J K
Sample Field QC
Initials Qualifier
-Bi.v,k s s . .
0 D ,DhC .1Ie
P = fl ’naai’
P C Prfo,n E af
— liar a OC Sampi
Information
Sampler (Name)
Airbill Number
Program
Sampler Signature
5 Ship To
ATTN
3 Purpose Ea:iyAcaon Lolernr
Lead PA 11 F 5
F1SF REM hIRD
CLEM Ac on
lPRP RI LEIRA
Ii 1ST st L1O&M
LJFED ESl LINPLD
Site Spill ID
CLP A
Sample Matrix
Numbers (from
(from Box 6)
labels)
Oilier
B
Conc.
Low
Med
High
C D
Sample Preser
Type vative
Com / 1rom
Gra ox 7
e
—
E — RAS Analusis
F
Regional Specific
Tracking Number
or Tag Numbers
G
Station
Location
Identilier
H
Mo/Day!
YearfTirne
Sample
Collection
I
Corresponding
CIP Organic
Sample No
— —
iO
—
re
— 17 1
0
Z
•0
m o c
> - 0 o
2 ii 0. 0
for Case Page I Sample(s) To be Used (or Laboratory QC lAdditional Sampler Signatures IChain ol Custody Seal Number(s) —
(YIN) I I I
—o1————I I I
CHAIN OF CUSTODY RECORD
by (Signature)
Date /Time
I
Received by (Signature)
Relinquished by (Signature)
Date /Time
I
Received by (Signature)
by (Signature)
Date
I
Time
Received by (Signature)
Relinquished by (Signature)
Date / Time
Received by (Signature)
— .
—
Relinquished by (Signature)
Date
‘Time
Received for Laboratory by.
(Signature)
Date I Time Remarks
Is custody seal intact? YIN/none
U
I . ,
a.
U
Ca
4
DISTRIBIJTION. Green - Region Copy
White -Lab Copy for Reiurn to Regior.
Pink - CLASS Copy EPA Form 9110.1
Yeliow- Lab Copy br Return to CLASS
SEE REVERSE FOR AoDIrior AL STANDARD INSTRUcT IONS
SEE REVERSE FOR PURPOSE CODE DEFINITIONS
-------
>
U i
________________ ______________________________ a:
•li
N
0
SEE REVERSE FOR ADDITIONAL STANDARD INSTRUCTIONS
SEE REVERSE FOR PURPOSE CODE DEFINITIONS
United States Envuronmentat Protection Agency
Contract Laboratory Program
Traffic Report
& Chain of Custody Record
(For Organic CLP Analysis)
Case No
iProjecl Code Account Code
2 Region No
Sampling Co
4 Date Shippe 1 Carrier
6 Matrix
(Enter
in Column A)
1 Surface Water
7 Preservative
(Enter in
Column 0)
1 HCI
Regional Information -
Sampler (Name)
Airbill Number
2 Ground Water
3 Leachate
4 Field OC
2 HNO3
3 NaHSO4
4 H2S04
Non-Superiund Program
Sampler Signature
5 Ship To
- 5 Soil/Sediment
— —-— -—_____________ 3 Purpose Early Achon
lonq Term 6 Oil (High only)
Sile Name F 1 CLEM Action 7. Waste
Lead ITIPA I1FS
LISF L I I REM RD (High only)
in Column A)
Cily.Stale - [ IPAP I 1 RI LIRA 6 Other (Specify
Spill ID V1ST [ SI III O&M
LJFED L_JESI LJNPLD ATTN
A B C D E F G H I
CLP Matrix Conc Sampl Preser RAS Analysis Regional Specific Stalion Mo/Day/ Corresponding
Sample (From Low Type vativc — - Tracking Number Location Year/Time CLP Inorganic
Numbers Box 6) Med ComD
or Tag Numbers Identifier Sample Sample No
(from High Grab ox7) Collection
labels) ‘e other > ARO/
— —
5 Ice only
6 Other
(Specify in
Column 0)
preserved
N Not
J K
Sample Field OC
Initials Qualifier
D. r r S=Sn e
P R ie
D=Dr i o a: u te
PC Pplm n Ev
— OC S e
Shipment for Case Page Sarnp!e(s)to be Used for Laboratory QC Additional Sampler Signatures Chain of Custody Seal Number(s)
Complete’ (YIN) —— of I —_____________________
CHAIN OF CUSTODY RECORD
Relinquished by (Signature) Date / lime Received by (Signature) Relinquished by (Signature) Date! Time ReceiVed by (Signature)
I
Relinquished by (Signature) Date / Time Received by (Signature) Relinquished by (Signature) Date / Time Received by (Signature) —
I I
Relinquished by (Signature) Date / lime Received for Laboratory by Date / lime I Remarks Is custody seal intact 2 YIN/none
(Signature)
L --__ I
DISTRIBUTION- Blue - RegIon Copy
WhIte - Lab Copy for Return to Region
Pink. CLASS Copy EPA Form 9110.2
Yellow. Lab Copy for Return to CLASS
-------
Attachment K
Example of Contract Compliance Screening (CCS) Report
-------
U F E r A CON FRAC r LADORA FURY PRO 1’Arl
SAMPLE M I4AGErlENT OFFICE — OPERATED ICY DYIICORP VIAFc
ORGANIC CONTRACT COMPLIANCE SCREEN INC 9YS1 Eli
REC)ION COPY
KY KKKMWKK$KKI*KN IK*KKx$ KsK**W$*M$**wwKKNNflgcK$*NKK$uC*YM%3(
Y4 K$ SCRCEHINGPACKAGE
SUMMARY INFORMATION
C it MOt.8 VER 6 ==
fl W
¶3 0 1; DE IIO I
VK%N NMKK
CASE 99979
LAB DEMO
COHIRACI A9-99-9999
M X K K
REGION 0 MMXX
MM M X M MM X
MMMX Dr
-------
U S E P A CON1F( C1 LAB [ JRATUR( FROI3RAE1
SAMPLE MAHABEIIEN I OFFICE. — ORE ATFD BY DYNCE1F.J vir k
ORGANiC CON1RAC COMPLIANCE SCREENING SYSIEM
DI IEC 1 COtIH 1S BY SAMPLE AND CRITERION
EYE LAHATORY NOTES
Ii RE I 1IRI 1IUIMARIZES l i v SAMPLE I IIE TECHNICAL D [ FECT NOTE E J ON TIlL DISXETTE AND HARDCOPY DA1A PACI’AI3E THE “AN” (“ANAl p/P lY’) i
till IllS !;Hlju UlIE lItER TIlE S,ThPLE WAS CV) CR WAIJ NO I (11A AHAI.YZED. NUMBERS IN THE ‘AN” (PR “EX” ( “EX IRACTION”) CULU 1INS I HLP II A IC I
II DAYS E l WhiCh tHE EAMPLE ViOLAtED THE HOLI)INO TIME NUMBERS IN 1 1W “TECHNICALII IAHIJAL DEFECTS” CULUMNS SH(JLI FIlE HIIMUIJ: UI I
Ilhit)flF?JAHCE IJEFECIS H i l lE l ) FUR A SAMPLE UllIl REFERENCE 10 A SPECIFIC CRITERION.
CL1FIFImI:1 f’fl—99—9999 SAl utES. i i DATE RECEIVED ?9/99/Y
no s u NO S(:REEI4ER x: ixx DA1 £ SCkLLHI I)t/ ,99 ,
I I’ ) 01 111 )1 RE1i1;JH 0 MAIL DAlE (1) ‘; /99 ’
I I HOLDING tIlES I TECIIIIICAI ,tlcdluAt. rn:FECIS I
SAMPLE
1) 1 11112
DIM’ I M5
Dr 111 )211 51)
Dl 1103
jpr 11031 )1
I jlO4
DEI1O4DL
DEF1O5
1 ) 1 1 1 06
I”EMO7
V I I c I 1 ’ I P I P 1
D I S I 11 1 I i 1 1 I 1 I C I I I A I (I I F I 1 1 I
o i 14 I N I E I E 1
A I U I S 1 L I U I N I 0 I N I N I P I I A I
A I A 1 A I S I 5 1
T I R I / 1 A I N I I I N I T I I C I H S N I
I I I I IAIRIMINIEI1I IISISIFIIIUI
AILIAIEIA ! I 1611 (1 I I ITIEILI 1IAI
N IXIHIXI I4I
I 11) 1 I ICICIDIO IOIS ILI
———————.——-.———.——I————-——.
————————. ————————
Y HA HAl 1 1
P P P P 9- P + I 4 1 P I I I
‘ V Y NA I II
+ ÷ ( p + p + 4 I I 1- + -F -f I
V ‘i’ HAl II
4 F 4 + I + + 3- 4 4 F P 4- + + +
V Y HAl 1 I
-F + # + I - 4- + + 4 4 p 4- 4 I I I
V NA HAl I I
+ -I + + + + I- + 4 + + 1- 4- 4 I- I
V NA HAl II
+ + 4- + + + + 4 + 4 1 4- I- -4-
NA Y HAl I
+ + + + I 4 + 4- + + 4 I + + + I
I-IA I HAl I
+ + + + I + + 4- + + 4 + I + + I- I
V hA HAl 1 I
+ + P + I 4 + ÷ I 4 4 3- I 4 + 4 I
V hA HAl 1 I
4 + + +
I + + 1- + + + 4- I 4 F I- I
NA I NAI
2
+ 4 + +
I + + 4- + + + I F + F I
I I
+ 4- + + I + + + + -F 4 F + F + + I
I
+ + + 4 + + + + + + 4 + 4 + + I
I
F + + 4 I t + + 1 + + + 4 4 + F I
I
I- 4 + + I + + 4 F + P 4 + + 4- I
I I
-------
U S E 1’ 4 COIIIF iCT LAPURATORY PROGRArI
SAMPLE rIAHAL3EnENT OrFICE - OPERATED DY DThCURF’ V1AR
OPflAHIC CON FRAC I COMPLIANCE SCREENING SYSTEM
DEFECT COUN1S fI)P SEtit—VOLATILE FRAC1 ION
EXFLANATORY NOTES
I1I’ R1F0F l ¶ UFIr1ARTZES DY JAMIL.E THE IEcII1IJCAL DEFECTS NOTED ON 1HE DISKETTE 4110 HARDCOPY DA A PACVAr,E THE ‘AN” ( “AMALYZEI”) I
C )) IJi1I4 4 SHIIJ WhEthER 1IU (nh11Ll UAS (Y) O [ (.JA 1401 (HA) ANALYZED NUIILiERS IN TIlE “414” OR “EX” (“E tRACTIOH”) COLUMNS INDICAtE I
DAiS Fy 1111101 THE SAI1FtE VIULA1ED THE HULLUHO TIME. NU )1EIERS IN THE “TECHNICAL/MANUAL DErECTS’ COLUMNS SHOW IHE H(lrhI’FR OF I
flhI-rUI1PLIAI ICE. DEFECTS NOTED FUk A SAMr-tE .IIr1l REFERENCE w A SPECIFIC CRITERION
E 9999 CUNTRACI M i ??-9999 SAMPLES: ii DAlE RECEIVED /.‘ I99
1i)PI- 1)1 I ii) SAS HO : SCREEI hER XX/XX DAlI: SCREENED ‘ •
hit IM-:FI’ ‘I RI 010W: 0 MAIL DAlE (1) 9-”•, ?’/
I I TEcIIN)CAL/IIAIIUAL DEFECTS I
SAl IPLE
I DihlOl
DEMO2
DErIfJ IiS
I DErIO2IISD
0E1103
I DEtIO3DL
I DEMO4
DEFIO4DL
I DEMIJi
I I)ErIoe ,
I 00107
RIE
I’l I N
AIA
EIA
x I•_I I
HA
t V
+
Y
+
I
+
NA
HA
Y
I.
+
HA
I IA
I
+
0 I S I Ii I B I T I I I C I I I
AIU ISILIUIt4IOINI
TIRI/IAIN IIINITI
AIRIMIHIEITITISI
I ISII
-------
U.S E r A COH1RAC LflBORAItIRT RO6RAI1
SA IIFLE IIAHAGEIIFIIT OFFiCE -. orERnr I:D 91 DYHCORP VIAR
OR(iflHW CONTRACT CUI 1ILIAHUE SCREENiNG TEXTUAL DEFEC1 REPORT
PE IAJIED SUrillAler OF CCS REVIEU
EXPMNA JURY NOTE
1 1111’ , flI I TIRI ‘iUIJlAI:J ir ; Pill CT Ii [ 55fl6F5 INFORMATION IS ITiRENIkIE.SES Al THE END U A DEFEE 1 MES ACL REFEF¼IIIIIS THE
i ‘.‘nj r ’.i wiun:i u UIlIl& 1 1 1k I Q hJ1W1EFIIS oltJuujArED. FOLLOWiNG THE DEFICT Ill SSA’JC IS A I i T Ill ( iLL AFFEC1IM SAIffLES I
Lal , DEl hi SOS DEMOJ Fraction Semi—VaI ttle
1141 rAI:i )l I ICI
IAL S I f t II )Ai I SUI1i1A fl
II 6 1 Re—anaycts/Dilutton) is missing when (Sample/Blanks) has Internal Standard (Area) nutside the upper cmiI
lower 12-- ho ur period standard limits (9—48/0—51 SV/O—52 SV)
Samples Affected
I)EMO7
-------
U. S t r A CCThITRACf I AcKIRATORI FROGRAI1
GhMF LE MANAIWI1EW1 OFFICE — OPERATED BY DYNCORP VIAR
rJF GAN (C COWl RACt CfJl FLIANCE SCREENING MANUA l. SCREENING DElICT REPOR1
LAB DE 1O 506: OFI 1D I FRACTION VOLATILES
•q ‘:t,rIri I I)TH04 WM M
A.I I ’ Idol ] rC/I1E; INGTI.tlrlCNl FtRFORI1ANCE CHECK AND 11455 CALIBRATION (FORM 54)
I N 4 2 (Instrument 10) are missi.ng on (liar Graph Spectra). (B—tIfB—I3)
-------
Attachment L
“Guidance Document for Completing Region I Data Validation Utilizing
CADRE Data Review”, February 1995
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GUIDANCE DOCUMENT FOR COMPLETING
REGION I DATA VALIDATION
UTILIZING CADRE DATA REVIEW
CADRE RELEASE 2.10
CONTRACT LABORATORY PROGRAM
ROUTINE ANALYTICAL SERVICES
VOLATILE AND SEMIVOLATILE ORGANICS
FEBRUARY 1995
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TABLE OF CONTENTS
INTRODUCTION CADRE version 2.10 . 1
CADRE Data S ” ’” ry Tables 3
ROLES OF ESAT IN THE CADRE VALIDATION PROCESS 7
ROLES OF FIELD SAMPLING CONTRACTORS IN THE CADRE VALIDATION
PROCESS 12.
ROLES OF EPA IN THE CADRE VALIDATION PROCESS 14
REGION I TIERED APPROACH TO DATA VALIDATION 15
SECTION I DATA COMPLETflIESS 17
SECTION II QUANTITATION LIMITS 19
SECTION III HOLDING TIMES 20
SECTION IV SC/MS TUNING 24
SECTION V CALIBRATIONS 27
SECTION VI BLANKS 32
SECTION VII SMCa/5TJRROGATES 38
SECTION VIII MATRIX SPIKE/MATRIX SPIKE DUPLICATE . . 4 ].
SECTION IX FIELD DUPLICATES . . 45
SECTION X INTERNAL STANDARDS 47
SECTION XI TENTATIVELY IDENTIFIED COMPOUNDS (TICs) 50
SECTION XII COMPLETING THE DATA VALIDATION REPORT . 5 ].
LIST OF ATTACHMENTS
ATTACHMENT I COMPLETED CADRE WORKSHEETS AND REGION I DATA
VALIDATION WORKSHEETS
ATTACHMENT II BLANK REGION I DATA VALIDATION WORKSHEETS
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LIST OF ATTACBNENT (c aNt.)
ATTACfl NT III MANUAL REVIEW REQUIRED TO COMPLETE A REGION I
TIER II DATA VALIDATION
ATTAC 1T IV COMPARISON TABLE FOR GUIDELINES AND ACTIONS
USED BY CADRE, THE NATIONAL FUNCTIONAL
GUIDELINES FOR ORGANIC DATA REVIEW (DRAFT
JUNE 1991), AND THE REGION I DATA VALIDATION
FUNCTIONAL GUIDELINES FOR EVALUATING ORGANICS
ANALYSES
ATTACHMENT V REGION I COMPLETE SDG FILE RECEIPT/TRANSFER
FORM, CADRE DATA REVIEW INVENTORY SHEET,
ORGANICS COMPLETE SDG FILE (CS!) INVENTORY
SHEET
ATTACffi1EW VI CJJIRD/CADRE SEG TRACKING FORM
ATTACHMENT VII MEMORANDUM FOR QUALIFYING SOIL/SEDIMENT DATA
WITH LOW PERCENT SOLID
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INTRODUCTION CADRE version 2.10
CADRE (Computer Aided Data Review and Evaluation) version 2.10 is
a software program which is designed to aid in the validation of
volatile and semivolatile CLP RAS data packages. CADRE is
capable of interpreting the electronic deliverable which the
laboratory is required to submit to CLASS under SOWs OLMOL.9 and
OLMO3.l. CADRE performs a review of data quality by comparing
the quality control results to a preprogrammed set of criteria.
The criteria used for evaluation by CADRE are defined in the
National Functional Guidelines for Organic Data Review (Draft,
June 1991).
This document is designed to guide the validator in completion of
a Region I Tier II data validation utilizing CADRE’s findings.
For each quality control parameter reviewed, CADRE will generate
a worksheet reporting any problems found during the review.
CADRE will also provide recommendations for qualification of the
data based upon these problems. The recommendations made by
CADRE are identical to those suggested in the National Functional
Guidelines for Organic Data Review (Draft, June 1991).
In some instances, however, the recommendations of the National
Functional Guidelines (and, therefore, the recommendations made
by CADRE) may differ from those suggested in the Region I
Laboratory Data Validation Functional Guidelines for Evaluating
Organic Analyses, November 1988. The actions recommended by
CADRE on the data review worksheets should be followed unless
stated otherwise in this guidance document. In the cases where
specific actions are not stated by CADRE or included in this
guidance document, all guidelines for review and data
qualification set forth in the Region I Laboratory Data
Validation Functional Guidelines for Evaluating Organic Analyses,
November 1988, are to be followed. Any deviations in the review
process or qualifications placed on sample results must be
clearly justified in the Data Validation Memorandum as per the
Region I Laboratory Data Validation Functional Guidelines for
Evaluating Organic Analyses.
NOTE: If pesticides/PCBs were analyzed along with the
volatile and semivolatile organics for a particular
SDG, CADRE will attempt to validate the pesticide/PCB
fraction. CADRE will display its findings of the
pesticide/PCB validation on the CADRE worksheets along
with its findings of the validation of the volatile and
semivolatile fractions. Currently, CADRE validates
many pesticidefPcB parameters different than Region 1.
Any pesticide/PCE results reported by CADRE on the
CADRE worksheets should be ignored. All Region 1
pesticide/PCB analyses should be manually validated.
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Region 1 - Guidance Document Introduction
Completion of Data Validation Using CADRE Page 2 of 52
However, it should be noted that CADRE pesticide/PCB
Data Summary Tables will be generated during CADRE
validation and should be used during validation. These
Data Summary Tables will be delivered, along with the
CADRE Data Validation Report, to the Field Sampling
Contractor.
A completed set of example worksheets (CADRE and manual) is
included in Attachment I. A full set of blank Region I data
validation worksheets is included in Attachment II. A tabular
summary of the manual review necessary to complete a Region I
Tier II data validation is included in Attachment UI. The
differences between the National Functional Guidelines, CADRE,
and the Region I Functional Guidelines criteria are summarized in
a series of tables included in Attachment IV.
FEBRUARY 1995
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Region 1. - Guidance Docu tent CADRE Data Stmrm y Tables
Completion of Data Validation U aing CADRE Page 3 of 52
CADRE Data S 1Trm ry Tables
CADRE will create Data Summary Tables summarizing the results
reported by the laboratory on the Form Is. CADRE can generate
either unqualified or qualified Data Summary Tables. The CADRE
unqualified Data Summary Tables contain the Form 1 results and
qualifiers as reported by the laboratory. The CADRE qualified
Data Summary Tables contain the CADRE Form 1 results along with
any qualifiers resulting from the CADRE validation process.
CADRE, wherever possible, will recalculate sample values. On
occasion, CADRE will round values differently than the
laboratory. CADRE is programmed to round results according to
rules stated in SOWs OLMO1.9 and OLMO3.l. The differences occur
when the laboratory reporting software uses rounding rules which
vary from those stated in the SON. In these cases, the results
reported by CADRE (the CADRE Form I results) represent the true
CLP values. If, however, the CADRE results and the laboratory
Form I results differ due to slight rounding errors, the results
reported by the laboratory will be included by the ESAT CADRE
chemist on the qualified Data Summary Tables. This will insure
consistency of sample result transcription from the hardcopy to
electronic deliverables.
The CADRE qualified Data Summary Tables for the volatile and
semivolatile fractions will be provided to the Field Sampling
Contractor. These Data Summary Tables will contain qualifiers
recommended by CADRE on the CADRE worksheets generated during the
review of each QC parameter. The Field Sampling Contractor will
be required to verify that all qualifiers have been correctly
transcribed onto the Data Summary Tables by CADRE. The Field
Sampling Contractor will also be required to place any qualifiers
onto the Data Summary Tables which result from any required
manual validation.
For the pesticidefpCB fractions and in instances where major
discrepancies exist between the sample values reported on the
CADRE qualified Data Summary Tables and the laboratory Form is,
the CADRE unqualified Data Summary Tables will be sent to the
Field Sampling contractors along with a notice that the Data
Summary Tables are unqualified. The unqualified Data Summary
Tables distributed to the Field Sampling Contractors will contain
only the Form I results and qualifiers as reported by the
laboratory. The Field sampling Contractors will be required to
remove all laboratory qualifiers from the CADRE unqualified Data
Summary Tables (such as the ItDlt, and “E qualifiers), with
FEBRUARY 1995
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Region 1 - Guidance Document CADRE Data S1YT m ry Tables
Completion of Data Validation using CADRE Page 4 of 52
the exception of the “J” qua].ifier. for results detected below
the CRQL, and the “U” qualifier, for non-detect results. The
Field Sampling Contractor must then add any qualifiers resulting
from the completion of the data validation.
Along with the hardcopy Data Summary Tables, a diskette
containing the WordPerfect files for the Data Summary Tables will
be provided to the Field Sampling Contractors.
Each CADRE Data Summary Table file will be named to identify the
SDG, fraction and sample matrix. The CADRE files are created as
ASCII files and are then transformed into WordPerfect files by
the ESAT CADRE Chemist prior to being distributed to the Field
Sampling Contractor. The file naming scheme is as follows:
“SDG#XY.TXT ”.
SDG# = The SDG number for the CLP data package.
X = Fraction
B for Semivolatiles (BNA)
V for Volatiles
P for Pesticides
M for Metals
Y = Sample Matrix
A for Aqueous
S for Soil
The .TXT file extension is assigned by MSDOS, when the CADRE file
is created as an ASCII file, to designate that the file is a text
file. This extension is retained when the file is converted into
WordPerfect format.
For example - SDG AENO6 has 5 soil samples and 4 water sample for
volatiles, semivolatiles, and pesticides/PCBs analysis. The
files for the Data Summary Tables would be named as follows:
Semivolatiles
AENO6BS.TXT for the sentivolatile soil samples
AENO6BA.TXT for the semivolatile water samples
Vol at i les
AENOGVS.TXT for the volatile soil samples
AENO6VA.TXT for the volatile water samples
FEBRUARY 1995
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Region 1 - Guidance Document CADRE Data Smmnary Tables
Completion of Data Validation Using CADRE Page 5 of 52
PesticidesJPCBs
AENOGPS.TXT for the pesticide/PCB soil samples
AENO6PA.TXT for the pesticide/PCB water samples
A backup file for each Data Summary Table will also be included
on the diskette. The backup file will be named similarly to the
original file but the “.TXT” extension is replaced with a “.BKP”
extension. This backup file will be included only to serve as a
second copy of the Data Summary Tables, if for any reason the
original becomes unusable.
The Data Summary Tables will also be submitted electronically in
ASCII format. This format will be available for use in site
databases if desired. The ASCII files will be named similarly to
the original file but the “.TXT” extension will be replaced with
a “.DB”.
The CADRE Data Summary Tables have been formatted as WordPerfect
files. This formatting includes creating a defined structure for
the table boundaries.
In order to preserve the table boundaries, all edits to the
summary tables must be performed in the “typeover” mode. After
retrieving the file onto the computer screen, press the
key. To verify that you are in typeover mode, the word
“typeover” should appear on the bottom left hand corner of the
computer screen.
FEBRUARY 1995
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Region 1 - Guidance Document Completing the CADRE Report
Completion of Data Validation Using CADRE Page 6 of 52
COMPLETING TEE CADRE Data Validation Report
Upon completion of the CADRE validation, a CADRE report which
consists of the CADRE Worksheets, hardcopy and diskette CADRE
Data Summary Tables, and CADRE Data Review Inventory Sheet will
be shipped along with the CLP Data Package to the Field Sampling
Contractor. Upon receipt of the CADRE report and CL? Data
Package, the Field Sampling Contractor should complete the Region
I Complete SDG File Receipt/Transfer Form and the Organics
Complete SDG File (CSF) Inventory Sheet (Form DC-2) as usual, as
well as the CADRE Data Review Inventory Sheet to verify data
completeness. (Copies of these forms are included in Attachment
V). The completed CADRE Data Review Invenzory Sheet should be
included with the Data Validation Report.
FEBRUARY 1995
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Region 1 - Guidance Document Role8 of ESAT
Completion of Data Validation Using CADRE Page 7 of 52
ROLES OF ESAT IN THE CADRE VALIDATION PROCESS
The following section describes the roles that ESAT personnel
play in the procession of the CADRE validation.
1. Receipt of the Data Package From the EPA RSCC at ESD
The EPA RSCC at ESD will transfer custody of the data
package to the ESAT Lexington Data Preparer. The ESAT
Lexington Data Preparer will log the data package into the
CLP Sample Tracking System (CLPSTS) and will indicate on the
Region 1 Complete SDG File (CSF Receipt/Transfer Form if
the data package is for ESD/ESAT, ARCS, or TES validation.
The ESAT Data Preparer will then transfer custody of the
data package to the ESAT CADRE Chemist.
2. Initiation of CADRE SDG Tracking Process
t.Tpon receipt of the data package, the ESAT CADRE Chemist
will begin a CARD/CADRE SDG Tracking Form. (A copy of the
CARD/CADRE SDG Tracking Form is included in Attachment VI).
The purpose of this tracking form is to provide internal
assurance that all of the necessary steps for generating the
CADRE report have been completed and are documented. A copy
of the CARD/CADRE SDG Tracking Form will be included in the
CADRE report file for each SDG, which will be kept in the
EPA ESD central files.
3. Downloading of Electronic Deliverable
Upon receipt of the data package, the ESAT CADRE Chemist
will download the SDGs from the CARD database to the CADRE
PC.
4. Importing the SDG into CADRE
ESAT will import the SDG into CADRE. After successfully
importing the SDG into CADRE, ESAT will manually enter the
sampling dates, sampling preservation for volatiles,
laboratory sample numbers, and sampling locations. If any
errors are detected by CADRE during the import process, ESAT
will generate the CADRE import error reports.
FEBRUARY 1995
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Region 1 - Guidance Doc iment Roles of ESAT
Completion of Data Validation Using CADRE Page 6 of 52
5. Manual Data Entry and CADRE Data Review
The ESAT CADRE Chemist will manually enter any missing or
discrepant data. After completion of all manual data entry,
the ESAT CADRE Chemist will execute the CADRE review of the
data and generate CADRE worksheets.
6. Generating and Formatting the Data Summary Tables
The ESAT CADRE Chemist will format the Data Summary Tables
to conform to the current Region I Data Summary Table
specifications. The one exception to this format is that
currently there is no space on the CADRE Data Summary Tables
to include a column for the SOW CRQLs. However, the sample-
specific CRQLs will be listed for each compound which is not
detected. The Data Summary Tables will be exported in ASCII
format and converted into WordPerfect files. The CADRE
qualified Data Summary Tables for the volatile arid
semivolatile fractions will be provided to the Field
Sampling Contractor. These Data Summary Tables will contain
qualifiers recommended by CADRE on the CADRE worksheets
generated during’the review of each QC parameter. The Field
Sampling Contractor will be required to verify that all
qualifiers have been correctly transcribed onto the Data
Summary Tables by CADRE. The Field Sampling Contractor will
also be required to place any qualifiers onto the Data
Summary Tables which result from any required manual
validation.
For the pesticide/PCB fractions arid in instances where major
discrepancies exist between the sample values reported on
the CADRE qualified Data Summary Tables and the laboratory
Form is, the CADRE unqualified Data Summary Tables will be
sent to the Field Sampling Contractors along with a notice
that the Data Summary Tables are unqualified. The
unqualified Data Summary Tables distributed to the Field
Sampling Contractors will contain only the Form I results
and qualifiers as reported by the laboratory. The Field
Sampling Contractors will be required to remove all
laboratory qualifiers from the CADRE unqualified Data
Summary Tables (such as the UBIt, “D”, and “En qualifiers),
with the exception of the “J’ qualifier, for results
detected below the CRQL, and the “U” qualifier, for non-
detect results. The Field Sampling Contractor must then add
any qualifiers resulting from the completion of the data
validation.
FEBRUARY 1995
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Region 2. - Guidance Document Roles of ESAT
Completion of Data Validation Using CADRE Page 9 of 52
7. Delivery of CADRE report to Field Sampling Contractors
The ESAT CADRE Chemist will prepare the hardcopy CADRE
report, which consists of the CADRE worksheets and CADRE
Data Summary Tables. The ESAT CADRE Chemist will also
prepare a diskette containing three copies of the file for
the Data Summary Tables. One file is to be used as the
working file for adding qualifiers to the summary tables.
The second copy will be given a .BKP extension. This file
is included as a backup file if needed. The third copy will
be delivered in ASCII format for use in the site database if
desired.
Prior to shipping the CADRE report and CLP Data Package, the
ESAT CADRE Chemist will verify the completeness of the CADRE
report by initiating the CADRE Data Rev-jew Inventory Sheet.
This sheet will be delivered with the CADRE report to the
Field Sampling Contractor.
The ESAT CADRE Chemist will send the CLP RAS Data Package,
CADRE report, and diskette containing the files for the Data
Summary Tables simultaneously to the appropriate Field
Sampling Contractor.
8. Notification of Required Full Manual Data Validation
On some occasions, the diskette deliverable from the
laboratory will not pass the Contract Compliance Screening
(CCS), which is performed by the Contract Laboratory
Analytical Services Support (CLASS) contractor. Those SDGs
which do not pass the CCS screen will not be uploaded into
the CARD database, and subsequently, will not be available
for CADRE review.
Those SDGs must have a full manual validation performed by
the Field Sampling Contractor. The ESAT CADRE Chemist will
send those SDGs to the Field Sampling Contractor with a
notification that manual validation must be performed.
9. Notification of Required Partial Manual Validation
On some occasions, CADRE will be unable to validate a
portion of the SDG due to problems with the electronic
deliverable. These affected parameters must be manually
validated. The ESAT CADRE Chemist will send the remaining
CADRE report and data package to the Field Sampling
Contractors with a notice of which parameters must be
FEBRUARY 1995
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Region 1 - Guidance Document Roles of ESAT
Completion of Data Validation Using CADRE Page 10 of 52
manually validated.
10. Storage and Archival of CADRE Data
The ESAT Data Preparer will store a copy of all CADRE-
generated worksheets, hardcopy and diskette CADRE Data
Summary Tables, CADRE Error Reports, and the CARD/CADRE SOG
Tracking Form in the EPA ESD central files. A copy of the
CARD/CADRE SDG Tracking Form will also be kept by the ESAT
CADRE Chemist to generate the weekly CADRE Status Report for
EPA.
11. Weekly CADRE Status Reports
The ESAT CADRE Chemist will provide the EPA Data Validation
Chemist and the CLP-TPO with a weekly report summarizing the
CADRE activities for the previous week.
FE BRUARY 1995
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Region 1 - Guidance Document Roles of Field Sampling Contractors
Completion of Data Validation Tlsing CADRE Page 11 of 52
ROLES OF FIELD SANPLING CONTRACTORS IN TUE CADRE VALIDATION
PROCESS
The following section describes the roles that the Field Sampling
Contractors play in the validation of CLP RAS data utilizing
CADRE.
1. Receipt of Hardcopy Data and CADRE Report
The Field sampling Contractors shall receive the hardcopy
CLP Data Package and CADRE report, consisting of CADRE
worksheets and CADRE Data Summary Tables, simultaneously
from the ESAT CADRE Chemist. If no problems are encountered
with CADRE, the CLP Data Package and CADRE report will be
shipped by the ESAT CADRE Chemist from ESAT/ESD within 3
days of receipt of the CLP Data Package from the EPA RSCC.
A diskette containing the WordPerfect file for the Data
Summary Tables will accompany the hardcopy CADRE Data
Summary Tables and worksheets. A CADRE Data Review Inventory
Sheet which has been completed by the ESAT CADRE Chemist
will also be shipped with the CADRE report.
2. Data Completeness Check
Upon receipt of the data package, the Field Sampling
Contractor shall complete the Organics Complete SDG File
(CSF) Inventory Sheet (Form DC-2) as usual and the CADRE
Data Review Inventory Sheet to verify data completeness.
The completed CADRE Data Review Inventory Sheet should be
included with the Data Validation Report.
If any CADRE data are missing or discrepancies are detected
in the CADRE report, then the Field Sampling Contractor
should notify the Region I EPA Data Validation Chemist for
correction or clarification.
If any data are missing from the CLP Data Package, then the
Field Sampling Contractor should contact the laboratory to
obtain the missing data.
3. Completion of the Tier I Validation
If only a Tier I validation was required in the QAPjP
(Quality Assurance Project Plan) and/or SAP (Sampling and
Analysis Plan), then the Field sampling Contractor should
complete the Tier I validation as described in the Region I
FEBRUARY 1995
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Region 3. - Guidance Document Roles of Field Sampling Contractors
Completion of Data Validation Using CADRE Page 12 of 52
CSF Completeness Evidence Audit Program, dated 7/3/91. This
procedure was referenced in a memorandum titled tiRegion I
CSF Completeness Evidence Audit Program” from the Region I
CLP-TPOs to Region I Contractors, dated 7/7/91.
If a Tier II or Tier III validation was not required in the
QAPjP and/or SAP, then the CADRE report and diskette,
including the completed CADRE Data Review Inventory Sheet,
should be stored with the CLP data package.
4. Completion of the Tier II and Tier III validation
The Field Sampling Contractor shall complete the Tier II and
Tier III data validation utilizing the findings of CADRE.
The validation should be completed using the Region I Tiered
Organic and Inorganic Data Validation Guidelines, dated
7/1/93, the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organic Analyses (as modified by
Region I, 11/88) and the Guidance Document for Completing
Region I Data Validation Utilizing CADRE Data Review
(February 1995).
If CADRE review of an SDG is not possible, the Field
Sampling Contractor will be sent the CLP Data Package with a
notification that a manual validation must be performed.
Currently, manual validation must also be performed for all
CLP RAS Pesticides/PCB data. The Field Sampling Contractor
shall perform the Tier II or Tier III data validation using
the Region I Tiered Organic and Inorganic Data Validation
Guidelines, dated 7/1/93 and the Region I Laboratory Data
Validation Functional Guidelines for Evaluating Organic
Analyses (as modified by Region I, 11/88).
5. Writing of the Data Validation Report
The Field Sampling Contractor should complete the Data
Validation Memorandum, Data Summary Tables, and worksheets
as directed in the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organic Analyses (as
modified by Region I, 11/88) and the Guidance Document for
Completing Region I Data Validation Utilizing CADRE Data
Review (February 1995).
FEBRUARY 1995
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Region 1 - Guidance Document Roles o Field Sampling Contractors
Completion of Data Validation Using CADRE Page 13 of 52
6. Delivery of Final Validation Report
The final validation report, including Data Validation
Memorandum, CADRE and Region 1. Worksheets, Data Summary
Tables, CADRE Data Review Inventory Sheet, etc. should be
addressed to the appropriate EPA RSCC representative
(currently Christine Clark) at the Environmental Services
Division (ESD) in Lexington, MA. The original validation
report should be delivered to the RPM for the site ac EPA
WMD and a copy delivered to Christine Clark, EPA RSCC in
Lexington, MA.
FEBRUARY 1995
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Region 1 - Guidance Document Roles of EPA
Completion of Data Validation Using CADRE Page 14 of 52
ROLES OP EPA iN TEE CADRE VALIDATION PROCESS
The following section describes the roles that Region I EPA
personnel play in the validation of CLP RAS data utilizing CADRE.
1. Receipt of Hardcopy Data at EPA ESD
The transfer of the RSCC function from EPA Waste Management
Division (WND) to EPA Environmental Services Division (ESD}
occurred in January 1995. All CL? Data Packages are
currently supposed to be shipped to EPA ESD by the CIP
laboratories.
2. Transfer of the Data Packages From EPA WMD to EPA ESD
If any CL? Data Packages are mistakenly shipped to EPA WMD,
then EPA WMD will transfer the data package to EPA ESD via
the EPA internal mailing system.
Upon receipt of the data package by the EPA RSCC, the EPA
RSCC will initiate the custody tracking of the data package
by filling out the EPA Region 1. Complete SDG File (CSF)
Receipt/Transfer Form and will transfer custody of the data
package to the ESAT Lexington Data Preparer.
3. CADRE Support to Field Sampling Contractors
The EPA Data Validation Chemist shall provide CADRE support
to the Field Sampling Contractors. This includes tasking
ESAT to provide any CADRE resu.bmittals if necessary and/or
answering CADRE questions raised by the Field sampling
Contractors.
4. Receipt and Review of Data Validation Reports From Field
Sampling Contractors
The EPA RSCC representative (currently Christine Clark) at
the Environmental Services Division (ESD) in Lexington, MA
shall receive a copy of the Data Validation Report. The EPA
RPM for the site (located at EPA WMD) shall receive the
original validation report.
The Data Validation Report shall be reviewed by the EPA Data
Validation Chemist for use in data validation oversight and
laboratory analysis oversight activities.
PEBRT7ARY 1995
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Region 1 - Guidance Document Region I Tiered Validation
Completion of Data Validation Using CADRE Page 15 of 52
REGION I TIERED APPROACH TO DATA VALIDATION
The data validation process can be broken down into three
distinct levels: Tier I, Tier II, and Tier III.
Tier I: A Completeness Evidence Audit is performed to ensure
that all laboratory data and documentation are present.
Completeness Evidence Audits are performed in
accordance with procedures contained in the Region I
CSF Completeness Evidence Audit Program , dated 7/3/91.
(This document is the currently used procedure
referenced in the memorandum titled “Region I CSF
Evidence Audit Program” from the Region I CLP-TPOs to
Region I Contractors, dated 7/7/91.)
The validation procedures contained in this Guidance
Document for Completing Region I Data Validation
Utilizing CADRE Data Review, dated February 1995, are
not applicable for Tier I validation. The validation
procedures contained in the Region I Tiered Organic and
Inorganic Data Validation Guidelines, dated 7/1/93,
should be followed. If only a Tier I validation was
required in the QA.PJP/SA.P, then the CADRE report and
diskette should be stored with the CLP Data Package for
future use. The CADRE Data Review Inventory Sheet
should be completed by the Field Sampling Contractor
and supplied with a letter to the EPA RSCC at ESD in
Lexington, MA and the site RPM stating that the
QAPj P/SAP required only a Tier I validation. The
technical justification for performing only a Tier I
validation must also be documented in that letter.
Tier II: A Tier I Completeness Evidence Audit is performed, then
the results of all Quality Control (QC) checks and
procedures are evaluated and used to assess and qualify
sample results. Tier II data validation is performed
primarily from information contained on the tabulated
data reporting forms.
The validation procedures contained in this Guidance
Document for Completing Region I Data Validation
Utilizing CADRE Data Review, dated February 1995, and
the Region I Tiered Organic and Inorganic Data
Validation Guidelines, dated 7/1/93, are used in
conjunction with the CADRE report to complete a Tier II
validation for CLP RAS volatiles and semivolatiles.
FEBRUARY 1995
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Region 3. - Guidance Document Region I Tiered Validation
Completion of Data Validation Using CADRE Page 16 of 52
Tier III: A full validation is performed. Tier III includes Tier
I and Tier II procedures plus an in-depth examination
of all raw data to check for technical, calculation,
ana].yte identification/ana].yte quantitation, and
transcription errors.
The validation procedures contained in this Guidance
Document for Completing Region I Data Validation
Utilizing CADRE Data Review, dated February 1995, and
the Region I Tiered Organic and Inorganic Data
Validation Guidelines, dated 7/1/93, are used in
conjunction with the CADRE report to complete the Tier
II portion of the Tier III data validation. The
validation procedures contained in the Region I
Laboratory Data Validation Functional Guidelines for
Evaluating Organics Analyses, modified 11/88, are used
to complete the remainder of the Tier III data
validation.
FEBRUARY 1995
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Region 1 - Guidance Document Data Completeness
Completion of Data Validation Using CADRE Page 17 of 52
SECTION I DATA COMPLETENESS
I. INTERPRETATION OF TEE CADRE WORXSEEET AND FINDINGS
CADRE generates import error reports if it detects errors or
identifies that data are missing. All import errors are
corrected by the ESAT CADRE Chemist prior to delivery of the
CADRE report and CLIP Data Package to the Field Sampling
Contractor. Therefore, there is no interpretation required
for this parameter.
II. FtJRTEER HM UAL REVIEW REQUIRED
Verifying the Completeness of the CLP Data Package
1) The contents of the CLIP Data Package should be reviewed
for completeness by completing the Organics Complete
SDG File (CSF) Inventory Sheet (Form DC-2) as per the
Region I CSF Completeness Evidence Audit Pro ram , dated
7/3/91. This sheet is submitted by the laboratory with
the CLIP Data Package. This sheet must be signed by the
person who performed the completeness check.
2) If any data from the CLIP Data Package are missing or
incorrect, the validator must request submission of
this information from the laboratory.
3) The validator must complete the Region I Data
Completeness Worksheet. The worksheet and any Records
of Communication with the labo atory must be included
with the Data Validation Report. For completing a Tier
I validation, refer to the Roles of the Field Sampling
Contractor section for guidance.
Verifying the Completeness of the CADRE Report
1) The CADRE report and Data Summary Tables should be
reviewed for completeness and accuracy by completing
the CADRE Data Review Inventory Sheet. This sheet is
included with the CADRE report. The sheet must be
signed by the person who performed the completeness
check.
FEBRUARY 1995
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Region 1 - Guidance Document Data Completeness
Completion of Data Validation Using CADRE Page 18 of 52
2) If any CADRE report data are missing or incorrect, then
the validator must contact the Region I EPA Data
Validation Chemist for correction and/or submission of
the information.
3) The validator must complete the CADRE Data Review
Inventory Sheet. The CADRE Data Review Inventory Sheet
and any Records of Communication with the Region I EPA
Data Validation Chemist must be included with the Data
Validation Report. For completing a Tier I validation,
refer to the Roles of the Field Sampling Contractor
section for guidance.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
No action is required. All errors in electronic data
completeness will be detected by CADRE during the import
process and will be corrected by the ESAT CADRE Chemist
prior to shipping the CADRE report and CLP Data Package to
the Field Sampling Contractor.
IV. STEPS REQUIRED TO COMPLETE ThE REGION I VALIDATION
1) Complete any manual review as required in Section II.
2) Include the CADRE Data Review inventory Sheet with the
Data Validation Report. The completed photocopy of the
DC-2 form shall remain with the CLP Data Package.
3) If resubmittals were required, include any Records of
Communication requesting these resubmittals with the
Data Validation Report.
4) Include the Region I Data Completeness Worksheet after
the Region I Review of Organic Contract Laboratory Data
Package cover sheet and the CADRE Sample Listing page
in the Data Validation Report.
5) Any CLP Data Package resubmittals shall remain with the
CLP Data Package. Any CADRE resubmittals shall be
included with the Data Validation Report.
FEBRUARY 1995
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Region 1 - Guidance Document Quantitation Limits
Completion of Data Validation Using CADRE Page 19 of 52
SECTION II QUA 1TITATION LIMITS
I. INTERPRETATION OF THE CADRE WORXSHEET AND FINDINGS
CADRE produces a Quantitation Limit Report which lists any
compounds detected, below the CRQL. These results are
already qualified (J) by the laboratory on the Form is.
CADRE automatically transcribes the (J) qualifiers onto the
CADRE Data Summary Tables. No further qualification of
these results is required.
II. FURTHER MANUAL REVIEW REQUI RED
1) None.
III. REOVIRED ACTION IF ERRORS ARE DETECTED DY CADRE
1) None.
I v. STEPS REQUIRED TO COMPLETE THE REGION I VALIDATION
1) Include the CADRE Quantitation Limit Report after the
Region I Data Completeness Worksheet in the Data
Validation Report.
2) Sample result qualifiers are already placed on the Data
Summary Tables. No further action is required.
FEBRUARY 1995
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Region 1 - Guidance Document Holding Times
Completion of Data Validation Using CADRE Page 20 of 52
SECTION III HOLDING TI S
I. IN’rERPRETATION OF THE CADRE WORKSHEET AND FINDINGS
1) Holding Times
The CADRE Holding Times Report for aqueous and soil
samples displays the criteria used by CADRE for
volatiles and semivolatiles when holding times are
slightly or grossly exceeded. The criteria used by
CADRE are identical to the criteria used by Region 1.
If all holding times criteria are met, CADRE will
display the message “No problems found for this
qualification.”
If holding times are exceeded, CADRE will state which
samples exceeded holding times and the appropriate
Region I action to be taken. The CADRE qualified Data
Summary Tables will contain the correct qualifiers.
For unqualified Data Summary Tables, the validator
needs only to place the qualifiers suggested by CADRE
onto the unqualified Data Summary Tables.
It should be noted that CADRE will list any volatile
soil samples exceeding holding times twice on the
Holding Times Worksheet. This is due to a difference
in soil sample preservation designation between CADRE
and Region 1. This does not affect the validation of
holding times.
2) Percent Solids
The CADRE Percent 4oisture Report displays the criteria
used by CADRE for percent moisture (percent solid)
determination. If all percent moisture criteria are
met, CADRE will display the message “No problems found
for this qualification.” If the percent moisture
exceeds the limits specified by Region 1, CADRE will
list the samples affected and whether the percent
moisture exceeded the primary or expanded criteria.
CADRE will also list the appropriate Region 1 action to
be taken. The CADRE qualified Data Summary Tables will
contain the correct qualifiers. For unqualified Data
Summary Tables, the va].idator needs only to place the
FEBRUARY 1995
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Region 1 - Guidance Document Eolding Times
Completion of Data Validation Using CADRE Page 2]. of 52
qualifiers suggested by CADRE onto the unqualified Data
Summary Tables.
I I. FURTHER MANUAL REVIEW REQUIRED
1) If no error messages are reported, then no further
manual review is required.
2) Manual review is required if CADRE reports any of the
error messages listed in Section III. If an error is
detected by CADRE, CADRE will report this error on the
CADRE Holding Times Report or the CADRE Percent
Moisture Report. The validator should refer to Section
III to determine the extent of manual review required.
Region 1 Holding Times Worksheets must be utilized to
document the manual review.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
CADRE can display two possible error messages for Holding
Times arid one possible error message for Percent Moisture.
A. Possible Errors
Holding Times
1) Samples Missing Sampling Date.
• If CADRE does not find a sampling date, it
will perform the holding times evaluation
using the VTSR. CADRE will display an error
message on the Holding Times Report stating
that no sampling date was found.
2) Missing Holding Time Information.
• If any necessary information are missing
(other than the sampling date), CADRE will
not perform the review for this parameter.
An example of this is when there is no sample
preservation designated for volatile water
samples.
FEBRUARY 1995
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Region 1 - Guidance Document Eolding Times
Completion of Data Validation Using CADRE Page 22 of 52
Percent Moisture
1) Missing Percent Moisture Information
• If CADRE cannot find percent moisture
information, CADRE cannot perform the review
for this parameter.
B. Required Action
Holding Times
1) If either of the two holding time error messages
are reported, manual review of the sampling
paperwork and CLP Data Package must be performed
to evaluate holding times. The sampler must be
contacted to resolve discrepancies, if necessary.
Manual review of the associated holding time
information that was not reviewed by CADRE must be
performed using the criteria and actions outlined
in the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organics
Analyses. A Region I Holding Times Worksheet must
be completed to document the manual review.
Percent Moisture
1) A manual review of the percent moisture (percent
solid) information in the CLP Data Package must be
performed. The criteria and actions outlined in
the memorandum sent to Region 1 Data Validators by
the Region 1 CLP TPOs titled “Qualifying
Soil/Sediment Data With Low Percent Solid”, dated
March 29, 1990 must be used. (A copy of this
memorandum is included as Attachment VII.)
IV. STEPS REQUIRED TO COMPLETE TEE REGION I VALIDATIOJJ
1) complete any manual review as required in Section II.
2) Include the CADRE Holding Times Report and any required
Region I Holding Times Worksheets after the CADRE
Quantitation Limit Report in the Data Validation
Report. Include the CADRE Percent Moisture Report
after the CADRE Holding Times Report (and Region 1
Holding Times Worksheets, if applicable) i t t the Data
Validation Report.
FEBRUARY 2995
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Region 1 - Guidance Document Holding Times
Completion of Data Validation Using CADRE Page 23 of 52
3) Discuss any qualifications placed upon sample results
in the Data Validation Memorandum and provide
justification for sample result qualification as per
the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses.
4) Include required qualifiers in the Recommendations
Summary Table (Table I of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
5) Apply qualifiers to sample results on the Data Summary
Tables as per the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organics Analyses.
FEBRUARY 1995
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Region 2. - Guidance Document GC/MS Tuning
Completion of Data Validation Using CADRE Page 24 of 52
SECTION IV GCIMS TUNING
I. INTERPRETATION OF THE CADRE WORKSHEET AND FINDINGS
The CADRE Instrument Performance Check Report displays the
criteria used by CADRE for review of the BFB and DFTPP
instrument performance checks. The criteria used by CADRE
are identical to the criteria used by Region I. The CADRE
qualified Data Summary Tables will contain the correct
qualifiers. For unqualified Data Summary Tables, the
validator needs only to place the qualifiers suggested by
CADRE onto the unqualified Data Summary Tables. If all
criteria are met, CADRE will display the message “No
problems found for this qualification”.
II. FURTHER MANUAL REVIEW REQUIRED
1) If no error messages are reported, then no further
manual review is required.
2) Manual review is required if CADRE reports any of the
error messages listed in Section III. If an error is
detected by CADRE, CADRE will report this error on the
CADRE Instrument Performance Check Report. The
validator should refer to Section III to determine the
extent of manual review required. Region 1 GC/MS
Tuning Worksheets must be utilized to document the
manual review.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
A. Possible Errors
CADRE can display three possible error messages for
GC/MS Tuning
1) The instrument tune is missing.
• CADRE will display this message if it is
expecting to find and evaluate a BFB/DFTPP
instrument performance check sample but could
not locate one in the electronic deliverable.
FEBRUARY 1995
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Region 1 - Guidance Docunent GC/MS Tuning
Co ipletion of Data Validation Using CADRE Page 25 of 52
2) The incorrect base mass was normalized.
• During the instrument performance check, the
laboratory is required to normalize (use as
100% relative abundance) m/z 95 for BFB and
m/z 198 for DFTPP. CADRE will display this
message if it detects the base mass to be a
mass other than m/z 95 for BFB or ni/z 198 for
DFTPP.
3) The instrument tune did not meet tuning criteria.
• CADRE will display this message if the
primary BFB/DFTPP tuning criteria displayed
on the Instrument Performance Check Report
are not met.
B. Required Action
1) If any of these error messages are reported,
manual review of the CL? Data Package must be
performed to determine if the associated GC/MS
Tuning information are present and meet tuning
acceptance criteria. If the associated tuning
information are missing from the CL? Data Package,
then the laboratory must be contacted to submit
the information. Manual review of the associated
tuning information must be performed using the
criteria and actions outlined in the Region 1
Laboratory Data Validation Functional Guidelines
for Evaluating Organics Analyses. Region 1 GC/M$
Tuning Worksheets must be utilized to document the
manual review.
IV. STEPS REQUIRED TO COMPLETE THE REGION I VALIDATION
1) Complete any manual review as required in Section II.
2) Include the CADRE Instrument Performance Check Report
and any required Region 1 GC/MS Tuning Worksheets after
the CADRE Percent Moisture Report in the Data
Validation Report.
3) Discuss any qualifications placed upon sample results
in the Data Validation Memorandum and provide
justification for sample result qualification as per
the Region I Laboratory Data Validation Functional
FEBRUARY 1995
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Region 2. - Guidance Document GC/MS Tuning
Completion of Data Validation Uaing CADRE Page 26 of 52
Guidelines for Evaluating Organics Analyses.
4) Include required qualifiers in the Recommendations
Summary Table (Table I of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
5) Apply qualifiers to sample results on the Data Summary
Tables as per the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organics Analyses.
FEBRUARY 1995
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Region 1 - Guidance Document Calibrations
Completion of Data Validation Using CADRE Page 27 of 52
SECTION V CALIBRATICNS
I. INTERPRETATION OF THE CADRE WORXSHEETS AND FINDINGS
CADRE generates three reports to aid in the review of calibration
data.
1) Analytical Sequence
The report titled Analytical Sequence contains a summary of
all analyses associated with the SDG in chronological order
by instrument and fraction. This report lists the BFB/DFTPP
Instrument Performance Checks (IPCs) and calibrations, as
well as all samples which were analyzed within the 12 hour
time period following the BFB/DFTPP IPC.
2) Calibration Listing
The report titled Calibration Listing includes all the
initial and continuing calibrations which are associated
with the SDG along with the dates and times of analysis.
This report lists all samples which were associated with
each continuing calibration, and the calibrations are
reported in chronological order by instrument and fraction.
This report also lists all compounds which failed to meet
the initial calibration %RSD criteria of less than 30%
and/or the continuing calibration %D criteria of less than
25%. The actual non-compliant %RSD and/or %D values are
also reported. This report also includes a list of all
calibration compounds which failed to meet the relative
response factor (RRF) criteria of greater than 0.05. The
actual non-compliant RRFs are also reported. If the RR.F was
out in an individual standard in the initial calibration,
CADRE also identifies that individual standard.
3) Calibration Report
If all criteria are met, CADRE will display the message “No
problems found for this qualification”.
The Calibration Report displays the criteria used by CADRE
when minimum RRFs and rriaxiraum %RSDs/%Ds have been slightly
or grossly exceeded. If RRFs and/or ‘tRSD/%D criteria are
not met, CADRE will state which samples and compounds are
FEBRUARY 1995
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Region 1 - Guidance Document Calibrations
Completion of Data Validation Using CADRE Page 28 of 52
affected by non-compliant calibrations and the appropriate
Region 1 action to be taken.
The CADRE qualified Data Summary Tables will contain the
correct qualifiers. For unqualified Data Summary Tables,
the validator needs only to place the qualifiers suggested
by CADRE onto the unqualified Data Summary Tables.
I I. FURTHER MANUAL REVIEW REQUIRED
1) If no error messages are reported on the CADRE
Calibration Report, then no further manual review of
the data is required.
2) Manual review is required if CADRE reports any of the
error messages listed in Section III. If an error is
detected by CADRE, CADRE will report this error on the
CADRE Calibration Report. The validator should refer
to Section III to determine the extent of manual review
required. Region 1 Volatile Calibration Verification
and/or Semivolatile Calibration Verification Worksheets
must be utilized to document the manual review.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
CADRE can display four possible error messages for
Calibrations.
A. Possible Errors
1) Samples with no instrument performance check.
S For each sample in the SDG, CADRE will
attempt to locate the associated instrument
performance check to determine if the
instrument performance check passed the
tuning criteria. If CADRE cannot locate the
instrument performance check, it cannot
associate a calibration standard with the
instrument performance check standard. Thus,
CADRE will not evaluate the calibration
standard associated with the missing
instrument performance check. Any sample(s)
associated with the calibration standard(s)
will not be evaluated for this parameter.
FEBRUARY 1995
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Region 1 - Guidance Document Calibrations
Completion of Data Validation Using CADRE Page 29 of 52
2) Samples with no associated calibration.
• If CADRE cannot associate a calibration
standard with a sample, it cannot evaluate
calibration criteria for that sample.
3) Samples associated with a continuing calibration
for which no corresponding initial calibration is
found.
• If CADRE cannot associate a continuing
calibration with an initial calibration, it
cannot calculate a %D. Therefore, it cannot
evaluate the calibration criteria for that
sample.
4) Missing calibration information.
• If CADRE cannot locate any necessary
calibration information, other than the
information listed above, it cannot perform
an evaluation of that calibration. This may
include but is not limited to the following
information:
• Missing a response factor for one or
more compounds in the continuing
calibration.
• Missing the response factors for one or
more points in the initial calibration.
B. Required Action
1) A manual review of the CLP Data Package must be
performed to determine if the instrument
performance check associated with the
calibration(s) for the affected sample is present.
If the instrument performance check is missing
from the CLP Data Package, then the laboratory
must be contacted to submit the information.
Manual review of the instrument performance check
and the associated calibration that was not
reviewed by CADRE must be performed using the
criteria and actions outlined in the Region I
Laboratory Data Validation Functional Guidelines
for Evaluating Organics Analyses. Region 1
PEBR ARY 1995
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Region 1 - Guidance Document Calibrationa
Completion of Data Validation TYsing CADRE Page 30 of 52
Volatile Calibration Verification and/or
Sernivolatile Calibration Verification Worksheets
must be utilized to document the manual review.
2) For errors 2-4 listed in Section III above, manual
review of the CLP Data Package must be performed
to determine if the associated calibration
information are present and meet calibration
acceptance criteria. If the associated
calibration information are missing from the CLP
Data Package, then the laboratory must be
contacted to submit the information. Manual
review of the associated calibration information
must be performed using the criteria and actions
outlined in the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses. Region 1 Volatile Calibration
Verification and/or Sernivolatile Calibration
Worksheets must be utilized to document the manual
review.
IV. PS REQUIRED TO COMPLETE TEE REGION I VALIDATION
1) Complete any manual review as required in Section II.
2) Include the CADRE Analytical Sequence, Calibration
Listing, Calibration Report, and any required Region 1
Volatile Calibration Verification and/or Semivolatile
Calibration Verification Worksheets after the CADRE
Instrument Performance Check eports and any required
Region 1 GC/MS Tuning Worksheets in the Data Validation
Report.
3) Discuss any qualifications placed upon sample results
in the Data Validation Memorandum and provide
justification for sample result qualification as per
the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses (mod
11/88). Include, in the Data Validation Memorandum, a
table of compounds not meeting the calibration criteria
along with the samples associated with each
calibration.
4) Include required qualifiers in the Recommendations
Summary Table (Table I of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
FEBRUARY 1995
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Region 1 - Guidance Doci.iment Calibrations
Completion of Data Validation Using CADRE ‘age 31 of 52
Organics Analyses.
5) Apply qualifiers to sample results on the Data Summary
Tables as per the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organics Analyses.
FEBRUARY 1995
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Region 2. - Guidance Document Blanks
Completion of Data Validation Using CADRE Page 32 of 52
SECTION .VI BLANKS
I. INTERPRETATION OF THE CADRE WORKSHEET AND FINDINGS
A. Laboratory Blanks
The CADRE Laboratory Blanks Report specifies the
multipliers used for calculating action levels.
If all criteria are met, CADRE will display the message
“Mo problems found for this qualification”.
The CADRE Laboratory Blanks Report indicates which
samples and compounds have been considered as non-
detects due to method blank contamination. The CADRE
Laboratory Blanks Report will also note whether the
sample result is to be reported qualified as (U) or the
sample result is to be raised to the CRQL and qualified
as (U). The CADRE qualified Data Summary Tables will
contain the correct qualifiers. For unqualified Data
Summary Tables, the validator needs only to place the
qualifiers suggested by CADRE onto the unqualified Data
Summary Tables.
The Laboratory Blanks Report incorrectly qualifies
equipment and trip blanks due to laboratory blank
contamination. The qualification for these blanks
should be ignored as Region I does not qualify
equipment or trip blanks for laboratory blank
contamination. For qualified Data Summary Tables, the
validator needs to remove any qualifiers placed by
CADRE on equipment/trip blanks due to laboratory blank
contamination.
B. Equipment and Trip Blanks
CADRE distinguishes equipment and trip blanks from
regular field samples. CADRE has the capability to
evaluate these blank samples for contamination. This
function is currently not being used. In many
instances, the equipment and trip blank samples are not
included in the same SDGs as the field samples. CADRE
cannot evaluate these blanks if they are contained in a
separate SDG from the associated field samples.
FEBRUARY 1995
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Region 1. - Guidance Document Blanks
Completion of Data Validation Using CADRE Page 33 of 52
Manual review of the CADRE Data Summary Tables (or Form
Is) for these blanks is required to determine the
extent of contamination and to document the appropriate
qualification of the regular field samples. Region I
Blank Analysis Results Worksheets must be completed for
these blanks. The review mustbe performed using the
criteria and actions outlined in the Region I
Laboratory Data Validation Functional Guidelines for
Evaluating Organics Analyses. Actions should be
applied to all samples (except other blanks) in the
SDG. Equipment and trip blanks should not be qualified
based upon laboratory blank contamination.
II. FURTHER MANUAL REVIEW REQUIRED
A. Laboratory Blanks
If no error messages are reported, then no further
manual review of the laboratory blanks data is
required.
B. Equipment and Trip Blanks
1) The sampler or sampling paperwork must be
consulted to determine which samples, if any, are
designated as equipment or trip blanks and to
determine which regular field samples are impacted
by these equipment/trip blanks.
2) A manual review of the CADRE Data Summary Tables
(or Form Is) for these blanks must be performed.
The criteria and actions outlined in the Region I
Laboratory Data Validation Functional Guidelines
for Evaluating Organics Analyses must be used for
evaluation.
3) Sections 2 and 3 of the Region I Blank Analysis
Results Worksheets must be completed and included
in the Data Validation Report.
C. Manual Review Required Due To Errors Detected by CADRE
1) Manual review is required if CADRE reports any of
the error messages listed in Section III. If an
error is detected by CADRE, CADRE will report this
error on the CADRE Laboratory Blanks Report. The
validator should refer to Section III to determine
FEBRUARY 1995
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Region 1 - Guidance Document Blanks
Completion of Data Validation Using CADRE Page 34 of 52
the extent of manual review required. Sections 2
and 3 of the Region 1 Blanks Analysis Worksheets
must be utilized to document the manual review.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
CADRE can display six possible error messages for Laboratory
Blanks.
A. Possible Errors
1) No instrument performance check found for sample.
• CADRE will not evaluate laboratory blank
contamination for the sample if it does not
find an instrument performance check
(BFB/DFTPP) for that sample. CADRE will list
the affected sample(s).
2) No calibration found for sample.
• CADRE will not evaluate laboratory blank
contamination for the sample if it does not
find an associated initial and/or continuing
calibration far that sample. CADRE will list
the affected sample(s).
3) Samples with no associated laboratory blank.
• CADRE will display this message if there was
no laboratcry blank associated with the
sp cific sample(s) listed.
4) Invalid laboratory blank. Blank qualified CR)
during a previous qualification.
• CADRE will not evaluate a laboratory blank if
the blank has been considered as unusable for
other quality control parameters. For
instance, if the blank results have been
rejected (R) due to low surrogate recoveries.
5) Missing laboratory blank information.
• CADRE will not evaluate laboratory blank
contamination for a sample if there is
FEBRUARY 1995
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Region 2. - Gtiidance Document Blanks
Completion of Data Validation Using CADRE Page 35 of 52
information missing which is required to
associate laboratory blank contamination with
that sample (e.g., if the laboratory does not
report the weight of the blank, then CADRE
cannot calculate the 5x/lOx blank
contamination levels).
6) Mo laboratory blank samples.
S CADRE will display this error message if it
does not detect any laboratory blanks in the
whole electronic deliverable.
3. Required Action
1) A manual review of the CLP Data Package is
required to determine if the associated instrument
performance check is present. If the instrument
performance check is missing from the CLP Data
Package, then the laboratory must be contacted to
submit the information. Manual review of the
associated instrument performance check (IPC) and
laboratory blank(s) that were not reviewed by
CADRE must be performed using the criteria and
actions outlined in the Region 1 Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses (mod 11/88). The Region 1
Blanks Analysis Results Worksheets (all three
sections) must be completed to document the manual
validation.
2) A manual review of the CLP Data Package is
required to determine if the associated
calibration is present. If the associated
calibration is missing from the CLP Data Package,
then the laboratory must be contacted to submit
the information. Manual review of the associated
calibration and laboratory blank(s) that were not
reviewed by CADRE must be performed using the
criteria and actions outlined in the Region 2.
Laboratory Data Validation Functional Guidelines
for Evaluating Organics Analyses (mod 11/88). The
Region 1 Blanks Analysis Results Worksheets (all
three sections) must be completed to document the
manual validation.
FEBRUARY 1995
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Region 1 - Guidance Document Blanks
Co p1etion of Data validation Using CADRE Page 36 of 52
3) If the laboratory blank has been rejected (R)
during the review of ocher quality control
parameters? then professional judgement must be
used to determine if qualification of any positive
hits in any samples associated with the invalid
laboratory blank is necessary. The reviewer must
provide justification for sample result
qualification as per the Region 1 Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
4) For errors 4-6 listed in Section III above, a
iqanual review of the CLP Data Package is required
to determine if the associated laboratory blank
information are present and meet laboratory blank
acceptance criteria. If the associated laboratory
blank information are missing from the CLP Data
Package, then the laboratory must be contacted to
submit the information. Manual review of the
associated laboratory blank information that was
not reviewed by CADRE must be performed using the
criteria and actions outlined in the Region 1
Laboratory Data Validation Functional Guidelines
for Evaluating Organics Analyses (mod il/es). The
Region 1 Blanks Analysis Results Worksheets (all
three sections) must be completed to document the
manual validation.
IV. STEPS REQUIREDtO COMPLETE THE R!GION I VALIDATION
1) Complete any manual review as required i t t Section II.
2) Include the CADRE Laboratory Blanks Report and any
required Region I Blank Analysis Results Worksheets
after the CADRE Calibration Report and any required
Region 1 Volatile Calibration Verification and/or
Semivolatiie Calibration Verification worksheets in the
Data Validation Report.
3) Discuss any qualifications placed upon sample results
in the Data validation Memorandum and provide
justification for sample result qualification as per
the Region i Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses. Include,
in the memorandum, a table of the maximum
concentrations of contaminants found in the iaboratory,
equipment, and trip blanks.
FEBRUARY 1995
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Region 1 - Guidance Docunent Blanks
Completion of Data Validation Using CADRE Page 37 of 52
4) Include required qualifiers in the Recommendations
Summary Table (Table I of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
5) Apply qualifiers to sample results on the Data Summary
Tables as per the Region I Laboratory Data. Validation
Functional Guidelines for Evaluating Organic Analyses.
(Raise sample results to the CRQL if necessary)
FEBRUARY 2.995
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Region 1 - Guidance Docunent SMCs/Surrogates
Completion of Data Validation Using CADRE Page 38 of 52
SECTION VII 5 14Cm/SURROGATES
I. INTERPRETATION OF THE CADRE WORKSHEET AND FINDINGS
The CADRE SMC/Surrogate Report displays the criteria used
for surrogate review. The criteria used by CADRE are
identical to the criteria used by Region I. CADRE reviews
the advisory BNA surrogates but does not qualify data based
on advisory recoveries.
If all criteria are met, CADRE will display the message “No
problems found for this qualification”.
The CADRE SMC/Surrogate Report will indicate any samples
which require qualification due to poor surrogate recoveries
and will indicate the qualifiers to be placed on the sample
results. The CADRE qualified Data Summary Tables will
contain the correct qualifiers. For unqualified Data
Summary Tables, the validator needs only to place the
qualifiers suggested by CADRE onto the unqualified Data
Summary Tables.
II. FURTHER MANUAL REVIEW REQUIRED
1) If no error messages are reported 4 then no further
manual review is required.
2) Manual review is required if CADRE reports any of the
error messages listed in Section III. If an error is
detected by CADRE, CADRE will report this error on the
CADRE SMC/Surrogate Report. The validator should refer
to Section III to determine the extent of manual review
required. Region 1 Surrogate Spike Recoveries
Worksheets must be utilized to document the manual
review.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
CADRE can display three possible error messages for
SMCs/Surrogates.
FEBRUARY 1995
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Region 1 - Guidance Document SMCs/Surrogatea
completion of Data Validation Using CADRE Page 39 of 52
A. Possible Errors
1) Sample dilution factor exceeds criteria.
• This message will appear if the sample is
analyzed at greater than a 1:10 dilution.
CADRE will only review SMC/surrogate
recoveries for samples analyzed at less than
or equal to a 1:10 dilution.
2) Missing surrogate (system monitoring compound)
data.
• This message will appear if CADRE cannot
locate surrogate/SMC recoveries in the
electronic deliverable.
3) Surrogate (system monitoring compound) percent
recovery in method blank exceeds criteria.
B. Required Action
1) A manual review of the Form 2 contained in the CLP
Data Package is required for all samples analyzed
at greater than a 1:10 dilution to determine if
surrogate recoveries are within acceptance limits.
Manual review of the associated SMC/surrogate
information must be performed using the criteria
and actions outlined in the Region I Laboratory
Data Validation Functional Guidelines for
Evaluating Organics Analyses. A Region I
Surrogate Spike Recoveries Worksheet must be
utilized to document the manual review.
2) A manual review of the Form 2 contained in the CLP
Data Package must be performed to determine if the
associated SMC/surrogate information are present
and meet SMC/surrogate acceptance criteria.
Manual review of the associated SMC/surrogate
information must be performed using the criteria
and actions outlined in the Region I Laboratory
Data Validation Functional Guidelines for
Evaluating Organics Analyses. A Region I
Surrogate Spike Recoveries Worksheet must utilized
to document the manual review.
FEBRtYARY 1995
-------
Region 1 - Guidance Document SMCa/Surrogatee
Completion of Data Validation Ging CADRE Page 40 of 52
3) A manual review of SMC/surrogate data contained in
the CLP Data Package must be performed for all
samples associated with a laboratory blank
containing outlier surrogate recoveries.
Professional judgement should be used to qualify
any affected sample data due to outlier laboratory
blank surrogate recoveries as the per the Region I
Laboratory Data Validation Functional Guidelines
for Evaluating Organics Analyses. The reviewer
must provide justification for sample result
qualification as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
IV. STEPS REQUIRED TO COMPLETE THE REGION I VALIDATION
1) Complete any manual review as required in Section II.
2) Include the CADRE SMC/Surrogate Report and any required
Region I Surrogate Spike Recoveries Worksheets after
the CADRE Laboratory Blanks Report and any required
Region I Blank Analysis Results Worksheets in the Data
Validation Report.
3) Discuss any qualifications placed upon sample results
in the Data Validation Memorandum and provide
justification for sample result qualification as per
the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses. Include,
in the memorandum, a table listing any samples and
surrogates which failed to meet the acceptance
criteria.
4) Include required qualifiers in the Recommendations
Summary Table (Table 1 of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
5) Apply qualifiers to sample results on the Data Summary
Tables as per the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organics Analyses.
FEBRUARY 1995
-------
Region 1 - Guidance Document Matrix Spike
Completion of Data Validation Using CADRE Page 41 of 52
SECTION VIII MATRIX SPIKE/MATRIX SPIKE DUPLICATE
I. INTERPRETATION OF THE CADRE WORKSHEET AND FINDINGS
The CADRE Matrix Spike Report displays the criteria used for
matrix spike evaluation. The criteria used for evaluation
are identical to the criteria used by Region I.
If all matrix spike criteria are met, CADRE displays the
message “No problems were found for this qualification” on
the Matrix Spike Report.
If all criteria are not met, CADRE will indicate whether the
percent recovery or RPD criteria were not met on the Matrix
Spike Report. CADRE will also list the individual compounds
which exceeded criteria.
Where possible, CADRE will recommend specific qualifications
for MS/MSD deviations. If CADRE cannot recommend specific
qualifications, CADRE will alert the reviewer that criteria
were not met and list what manual review is necessary.
CADRE does not apply qualifiers to the qualified or
unqualified Data Summary Tables for MS/MSD percent recovery
or RPD deviations. Where possible, CADRE recommends
qualifications. For qualified and unqualified Data Summary
Tables, the validator needs to place the qualifiers
suggested by CADRE and/or resulting from any required manual
validation onto both Data Summary Tables.
II. FURTHER MANUAL REVIEW REQUIRED
1) If CADRE indicates that recovery criteria were not met,
then a manual review of Form 3 contained in the CLP
Data Package must be performed to determine if any
qualification of the data is required. The criteria
and actions outlined in the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses must be used. Region I Matrix
Spike/Matrix Spike Duplicate Worksheets must be
completed and included with the Data Validation Report.
2) CADRE does not evaluate the unspiked compounds in the
sample, MS, and MSD. This review must be performed
manually. The criteria and actions outlined in the
FEBRUARY 1995
-------
Region 1 - Guidance Docunent Matrix Spike
Coiupletion of Data Validation Using CADRE Page 42 of 52
Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses must be
used. Region I Matrix Spike/Matrix Spike Duplicate
Worksheets for unspiked compounds must be completed and
included with the Data Validation Report. A CADRE-
generated Data Summary Table which contains the sample
results for the sample, MS. and MSD is included in the
CADRE report along with the Matrix Spike Report. This
Data Summary Table may be used to aid in completing the
Region I Matrix Spike/Matrix Spike Duplicate Worksheet
for the evaluation of MS/MSD unspiked compounds.
3) Manual review is also required if CADRE detects and
reports any of the error messages listed in Section
III. If an error is detected by CADRE, CADRE will
report this error on the CADRE Matrix Spikes Report.
The validator should refer to Section 111 to determine
the extent of manual review required. Region 1 Matrix
Spike/Matrix Spike Duplicate Worksheets must be
utilized to document the manual review.
III. REQUIRED ACTIO)T IF ERRORS ARE _ DETECTED BY CADRE
CADRE can display three possible error messages for MS/MSDs.
A. Possible Errors
l Matrix spike (NS) and matrix spike duplicate (MSD)
frequency not sufficient.
• CADRE will display this message on the Matrix
Spike Report if an MS/MSD pair was not
analyzed at the required frequency of 1 per
20 samples per matrix.
2) issing matrix spike information.
• CADRE will display this message on the Matrix
Spike Report if some (or all) of the
information necessary to evaluate this
parameter is missing. This may include but
is not limited to:
• True value of matrix spike added.
• Matrix (soil or water).
FEBRUARY 1995
-------
Region 1 - Guidance Document Matrix Spike
Completion of Data Validation Using CADRE Page 43 of 52
• QC limits for % recovery and/or RPD.
3) No matrix spike data.
S CADRE will display this error message on the
Matrix Spike Report if it cannot find any
matrix spike sample(s) in the electronic
deliverable.
B. Required Action
1) As required in the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses, professional judgement must be
used to determine if there is any affect on the
data due to the insufficient frequency of MS/MSD
analysis. The, reviewer must justify, in the Data
Validation Memorandum, any action taken.
2} For errors 2 and 3 listed in Section III above,
manual review of the CLP Data Package must be
performed to determine if the associated matrix
spike information are present and meet matrix
spike acceptance criteria. If the associated
matrix spike information are missing from the CLP
Data Package, then the laboratory must be
contacted to submit the information. Manual
review of the associated matrix spike information
must be performed using the criteria and actions
outlined in the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses. Region I Matrix Spike/Matrix
Spike Duplicate Worksheets must be utilized to
document any manual review.
IV. STEPS REQUIRED TO COMPLETE THE REGION I VALIDATION
1) complete any manual review as required in Section II.
2) Include the CADRE Matrix Spike Report and any required
Region I Matrix Spike/Matrix Spike Duplicate Worksheets
after the CADRE SMC/Surrcgate Report and any required
Region I Surrogate Spike Recoveries Worksheets in the
Data Validation Report. The CADRE generated sample,
MS, and MSD Data Summary Table must be included along
with all other matrix spike worksheets.
FEBRUARY 1995
-------
Region 1 - Guidance Document Matrix Spike
Completion of Data Validation Using CADRE Page 44 of 52
3) Discuss any qualifications placed on sample results in
the Data Validation Memorandum and provide
justification for sample result qualification as per
the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses. Include,
in the memorandum, a table listing all compounds which
did not meet the matric spike acceptance criteria.
4) Include the required qualifiers in the Recommendations
Summary Table (Table 1 of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
5) Apply qualifiers to sample results on the Data Summary
Table as per the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organics Analyses.
FEBRUARY 1995
-------
Region 1. - Guidance Dccu ent Field Duplicatee
Completion of Data Validation Using CADRE Page 45 of 52
SECTION IX FIELD DUPLICATES
I. INTERPRETATION OF _ TEE CADRE WORKSHEET AND FINDINGS
CADRE does not evaluate field duplicate samples.
II. FURTHER MANUAL REVIEW REQ1YIRED
1) The reviewer must check the Organic Traffic
Report/Chain-of-Custody Form, consult the sampler, or
refer to the CL? Sample Tracking System (CLPSTS) to
determine which samples in the SDG are field duplicates
and to determine which regular field samples are
impacted by these field duplicate samples.
2) A manual review of the CADRE Data Summary Tables (or
Form is) for the field duplicates must be performed
using the criteria and actions outlined in the Region I
Laboratory Data Validation Functional Guidelines for
Evaluating Organics Analyses. Region I Field Duplicate
Precision Worksheets must be completed and included
with the Data Validation Report.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
No action is required as this parameter is not reviewed by
CADRE.
IV. STEPS REQUIRED TO COMPLETE THE REGION I VALIDATION
1) Complete any manual review required in Section II.
2) Include the Region I Field Duplicate Precision
Worksheet after the CADRE Matrix Spikes Report and any
required Region I Matrix Spike/Matrix Spike Duplicate
Worksheets in the Data Validation Report.
3) Discuss any qualifications placed on the sample results
in the Data Validation Memorandum and provide
justification for sample result qualification as per
the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses.
FEBRUARY 1995
-------
Region 1 - Guidance Document Field Duplicates
Completion of Data Validation Using CADRE Page 4 of 52
4) Include the required qualifiers in the Recommendations
Summary Table (Table I of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
5) Apply qualifiers to sample results on the
Data Summary Tables as per the Region I
Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses.
FEBRU) .RY 1995
-------
Region 1 - Guidance Document Internal Standards
Conpletion of Data Validation Using CADRE Page 47 of 52
SECTION X INTER2 AL STANDARDS
I. INTERPRETATION OF THE CADRE WOPXSHEET AND FINDINGS
The CADRE Internal Standards Report displays the
criteria used by CADRE for evaluation of internal
standards. The criteria used by CADRE are identical to
the criteria used by Region I.
If all criteria are met, CADRE will display the message
“No problems found for this qualification t.
CADRE will list, on the Internal Standards Report, the
compounds in each sample which have been qualified due
to poor internal standard recoveries or retention times
which are outside of criteria. CADRE will also list
the appropriate Region 1 action to be taken. The CADRE
qualified Data Summary Tables will contain the correct
qualifiers. For unqualified Data Summary Tables, the
validator needs only to place the qualifiers suggested
by CADRE onto the unqualified Data Summary Tables.
II. FURTHER MANUAL REVIEW REQUIRED
1) If no error messages are reported, then no further
manual review is required.
2) Manual review is required if CADRE detects and reports
any of the error messages listed in Section III. If an
error is detected by CADRE, CADRE will report this
error on the CADRE Internal Standards Report. The
validator should refer to Section III to determine the
extent of manual review required. Region 1 Internal
Standard Performance Worksheets must be utilized to
document the manual review.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY CADRE
CADRE can display three possible error messages for Internal
Standards.
FEBRUARY 1995
-------
Region 1 - Guidance Document Internal Standards
Completion of Data Validation Using CADRE Page 48 of 52
A. Possib].e Errors
1) Samples with no internal standard.
• CADRE will display this message on the
Internal Standards Report if it cannot locate
the internal standards for a sample in the
electronic deliverable.
2) Missing internal standards.
• CADRE will display this message on the
Internal Standards Report if no internal
standards for the SDG were located by CADRE
in the electronic deliverable. This may
occur if either the laboratory did not
include Form 8 in the electronic deliverable
or if CADRE failed to import Form 8.
3) Missing internal standard information.
• CADRE will display this message if a portion
of the required information for internal
standard evaluation is not present. This may
include but is not limited to the following
reasons:
• If only the internal standard area
information for the sample and/or
associated calibration standard is
missing.
• If only the retention time information
for the sample and/or associated
calibration standard is missing.
• If CADRE cannot associate the internal
standard information for a sample with a
calibration standard (i.e. either the
calibration standard information are
missing or the instrument performance
check associated with the sample or
calibration standard is missing).
FEBRUARY 1995
-------
Region 1 - Guidance Document Internal Standards
Completion of Data Validation Using CADRE Page 49 of 52
. Required Action
If any of these error messages are reported, manual
review of the CLP Data Package must be perfortned to
determine if the associated internal standard(s)
information is present in the CLP Data Package. If any
of the necessary information is missing from the CLP
Data Package, then the laboratory must be contacted to
submit the information. Manual review of the
associated internal standard information must be
performed using the criteria and actions outlined in
the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses. Region 1
Internal Standard Performance Worksheets must be
utilized to document the manual review.
IV. STEPS REQ IRED TO COMPLETE TR E REGION I VALIDATION
1) Complete any manual review as required in Section II.
2) Include the CADRE Internal Standards Report and any
required Region I Internal Standard Performance
Worksheets after the Field Duplicate Precision
Worksheets in the Data Validation Report.
3) Discuss any qualifications placed upon sample results
in the Data Validation Memorandum and provide
justification for sample result qualification as per
the Region I Laboratory Data Validation Functional
Guidelines for Evaluating Organics Analyses.
4) Include required qualifiers in the Recommendations
Summary Table (Table I of the Data Validation
Memorandum) as per the Region I Laboratory Data
Validation Functional Guidelines for Evaluating
Organics Analyses.
FEBRUARY 1995
-------
Region 1 - Guidance Document TICs
Completion of Data Validation Using CADRE Page 50 of 52
SECTION XI TENTATIVELY IDENTIFIED COMPOUNDS (TICs)
I. INTERPRETATION OF THE CADRE WORXZEEET AND FINDINGS
CADRE does not review Tentatively Identified Compound (TIC)
results. Review of TIC results is not required for Tier II
data validation. It is, however, required for Tier III data
validation.
I I. FURTHER MANUAL REVIEW REQ VIRED
For Tier III data validation, the procedure stated in the
Region I Laboratory Data Validation Functional Guidelines
for Evaluating Organics Analyses must be fàllowed to
evaluate Tentatively Identified Compounds.
For Tier II data validation, verify that target compounds
are not reported as TICS ifl another fraction. Only a
tabular summary of the detected TICS is required.
A tabular TIC summary should be included in the Data
Validation Memorandum for both Tier II and Tier III data
validations.
III. REQUIRED ACTION IF ERRORS ARE DETECTED BY, CADRE
No action is required, as this parameter is not reviewed by
CADRE.
IV. STEPS REQUIRED TO COMPLETE THE REGIO 1 I VALIDATION
1) Complete any manual review as required in Section II.
2) For Tier II data validation, summarize the TICS found
in the TIC Summary Table in the Data Validation Report.
Verify that target compounds are not reported as TICS
in another fraction. No further review of TICs is to
be performed.
3) provide an explanation of any identifications which
were changed by the reviewer or any TICS which were not
included in the TIC Summary Table. The reviewer must
justify any changes to the TIC-results in the Data
Validation Memorandum. This step is required only for
Tier III data validation.
FEBRUARY 1995
-------
Region 1 - Guidance Document Completing The Report
Completion of Data Validation eing CADRE Page 51 of 52
SECTION XII COMPLETING THE DATA VALIDATION REPORT
1) The Data Validation Memorandum must be completed as
stated in the Region I Laboratory Data Validation
Functional Guidelines for Evaluating Organics Analyses
(Section 1.5). The completed CADRE Data Review
Inventory Sheet must be included in the Data Validation
Report.
2) Any manual review of the CLP Data Package which was
performed must be documented by completing the Region I
Data Validation worksheets. These worksheets should be
included in the Data Validation Report along with the
CADRE worksheets in the order specified by this
guidance document.
3) The CADRE Data Summary Tables must be completed. The
CADRE qualified Data Summary Tables for the volatile
and semivolatile fractions will be provided to the
Field Sampling Contractor. These Data Summary Tables
will contain qualifiers recommended by CADRE on the
CADRE worksheets generated during the review of each QC
parameter. The Field Sampling Contractor will be
required to verify that all qualifiers have been
correctly transcribed onto the qualified Data Summary
Tables by CADRE. The Field Sampling Contractor will
also be required to place any qualifiers onto the Data
Summary Tables which result from any required manual
validation.
For the pesticide/PCB fractions and in instances where
major discrepancies exist between the sample values
reported on the CADRE qualified Data Summary Tables and
the laboratory Form is, the CADRE unqualified Data
Summary Tables will be sent to the Field Sampling
Contractors along with a notice that the Data Summary
Tables are unqualified. The unqualified Data Summary
Tables distributed to the Field Sampling Contractors
will contain only the Form I results and qualifiers as
reported by the laboratory. The Field Sampling
Contractors will be required to remove all laboratory
qualifiers from the CADRE unqualified Data Summary
Tables (such as the “B”, 11 D”, and “E” qualifiers), with
the exception of the “J” qualifier, for results
detected below the CRQLS and the “U” qualifier, for
non-detect results. The Field Sampling Contractor must
FEBRUARY 1995
-------
Region 3. - Guidance Docunent Completing The Report
Completion of Data Validation Using CADRE Page 52 of 52
then add any qualifiers resulting from the completion
of the data validation.
FEBRUARY 1995
-------
ATTACHMENT I
Completed CADRE and Region I Data Validation Workaheeta
-------
Region I Site Name ANDREWc ROAD LANDFiLL
Data Review Worksheets Reference Number_________________
REGION I REVIEW OF ORGANIC
CC fRACT LABORATORY DATA PACKAGE
The hardcopied(laboratory name) ENCOTEC data padcage received ax Region I has been
reviewed and the quality assurance and performance data summarized. The data review included:
Case No. 22891 SAS No. _________ Sampling date(s) 11/08/94
SDG No. AH7V5 Matrix Soil/Water Shipping date(s) 11/9/94
No. of Samples 15/5 Date(s) rec’d by lab 11/10/94
Traffic Report Nos: AETOS-AFITI6. AIIT2O-A11726. Al 1T57
Trip Blank No: AHT23
Equipment Blank No: AJITIO. Al-f T25, All T26
Field Dup Nos: WONE
Sow No. OLMOI.9 requires that specific analytical work be done and that associated reports be
provided by the laboratory to the regions, EMSL-LV, and SMO. The general criteria used to determine
the performance were based on an examination of:
-Data completeness -Matrix spike/Matrix Spike Dup
-Holding Times -Field Duplicates
-GC/MS Tuning -Internal Standard Performance
-Calibrations -Pesticide Instrument Performance
-Blanks -Compound Identification
-Surrogate Recoveries -Compound Quanrkaüori
Overall Comments: The data yackaRe was complete and well organized. Most sample results were
acceptable as reported by the laboratory.
Definitions and Qualifiers:
A - Acceptable data.
J - Approximate data due to quality control criteria.
R - reject data due to quality control data.
U - Compound not detected.
Reviewer: Thomas P. Widera Dare: 2/22L95
-------
Satçle Listthg
SE N0 22891 LABORAtVRY: RES0 A1WSYSTS . INC.
C NO: MCOS
YCA
j MaLYSIS
I EPA REGI0ZThL
SAIWLE uue spjwc.s t t c a RE IVS DATE TDC INSTR ThT
IV2LKCC / / 11/18/94 11:29 045-HP
IAfl’57 26435 11/10/94 11/18/94 13:53 045-HP
IA fl0 5— 5 5 11/12/94 11/18/94 14:28 O4SHP
AHfl9 6W-Cl 11/12/94 11/18/94 15:03 CC-HP
1A11T2 1 GW-C3 11/12/94 11/18/94 15:37 045HP
1A11T22 6 W- C t 11/12/94 11/18/94 16:13 04$-HP
JAn25 S _SD 11/12/94 11/18/94 16:41 04$-HP
AHT20 GW-02 11/12/94 11/18/94 17:22 04$-HP
NTT2O!C GW-02 11/12/94 11/18/94 17:57 045-HP
JART2CMSD GW-C2 11/12/94 11/18/94 19:32 045-HP
1MT26 5-GA l 11/ 12/94 11/18/94 19:07 CC-HP
1M4T23 1 1-Cl 11/12/94 11/18/94 19:42 045-HP
JV 5Uc03 / / 11/21/94 13:59 CC-HP
IMT0 S S 502 11/12/94 11/21/94 15:09 045-HP
5503 11/12/94 11/21/94 15:44 045-HP
JAHTO8 SS-C4 11/12/94 11/21/94 16:19 CC-HP
1A 14T09 5 5- 05 11/12/94 11/21/94 16:54 CC-HP
IAwr1 l 50-Cl 11/12/94 11/21/94 17:29 045-HP
JN Tfl2 5 3- 02 11/12/94 11/21/94 10:03 CC-HP
JM T13 50-03 11/12/94 11/21/94 18:38 045-HP
1N4T13tC SD-03 11/12/94 11/21/94 19:13 CC-HP
INfl3M5D 5D03 11/12/94 11/21/94 19:48 045-HP
J A T14 S 004 11/12/94 11/21/94 20:23 CC-HP
JAJ t15 SD—CS 11/12/94 11/21/94 20:58 CC-HP
IA}iT16 50—06 11/12/94 11/21/94 21:33 CC-HP
S5 ’C l 11/12/94 11/21/94 22:08 CC-HP
I FILE NNC; M105.StG DAtE: 83/13/95 TDC: 13:37 CORE 2.10 PIGS:
-------
Saffçle T..isting
CASE NO: 22891 LJ.BORXIVRY: RESOUR ANALYSTS. INC.
SOC O: ?44T05
SANPLE SAI4PLE Ut ER RE IV
DATE
DATE
TI?
INSTR T
IZBUOiI
I /
11/14/94
11/22/94
16:36
1*ISNP
lA T20 CW-02
11/10/94
11/14/94
11/22/94
17:45
)045•RP
IMT21 GW-03
11/10/94
11/14/94
11/22/94
18:19
)04S-)4P
IAHT22 CW-04
11/10/94
11/14/94
11/22/94
18:53
)*ISRP
MT1O E8-SS
11/10/94
11/14/94
11/22/94
19:27
1* 1 5-HP
JAXT19 CW-0t
11/10/94
11/14/94
11/22/94
20:02
IDISHP
I AHT2S £ 3- SD
11/10/94
11/14/94
11/22/94
20:36
91Mg-HP
IPM T26 £3-GAl
IS3L 1
I L 1
11/10/94
/ I
/ /
/ /
11/14/94
11/16/94
11/17/94
11/18/94
11/22/94
11/23/94
11/23/94
11/23/94
21:10
11:43
12:17
12:51
lO IS-HP
lO IS-HP
lOIS-HP
l OIS-HP
AHT13 SD03
11/12/94
11/18/94
11/23/94
14:00
l*4SHP
I AHT13M S S003
11/12/94
11/18/94
11/23/94
14:34
lOIS-HP
IAB T13MSD 50-03
11/12/94
11/18/94
11/23/94
15:08
lOIS-HP
IAHT O S SS -01
11/11/94
11/16/94
11/23/94
15:42
lOIS-HP
I A 1 T12 S 002
11/11/94
11/16/94
11/23/94
16:17
lOIS-HP
I h14 S 004
11/11/94
11/16/94
11/23/94
16:51
lOIS -HP
1AHT15 50-05
11/11/94
11/16/94
11/23/94
17:25
lO IS-HP
1MT16 5 006
11/11/94
11/16/94
11/23/94
17:59
lOIS-HP
A1iT08 SS-04
11/12/94
11/16/94
11/23/94
18:33
lOIS-HP
A$lT08MS 55-04
11/12/94
11/17/94
11/23/94
19:07
lOIS-lW
I A l T08 D 5504
11/12/94
11/17/94
11/23/94
19:42
lOIS-HP
IARfl l ED-Ol
11/11/94
11/16/94
11/23/94
20:16
lOIS-HP
1A19T09 SS-05
11/11/94
11/16/94
11/23/94
20:50
lOIS-lW
1MT06 SS-02
11/11/94
11/16/94
11/23/94
21:25
1*4 5-lW
IAHT O7 SS-03
IS3L Q
11/12/94
/ /
11/16/94
11/18/94
11/23/94
12/02/94
21:59
13:33
1*4 5-HP
lOIS-HP
Aorr2oMs GW—02
11/10/94
11/18/94
12/02/94
14:07
lOIS-lW
!AIrr2 OMSD 094-02
11/10/94
11/18/94
12/02/94
14:41
1*45-lW
! A 07RE SS—03
11/12/94
11/16/94
12/02/94
22:03
lOIS-lW
I
I FILE HAZE: ?IRTO5.SDG DArE. 03/13/95 TIIIS: 13:37 CADRE 2.10
I
-------
Region I
Data Review Worksheets
I. DATA COMPLETENESS
MISSING INFORMATION DATE LAB CONTACTED DATE REC’D
The daraj,ackaRe was complete as submitied by the 1aboraror ’.
Reviewer: TPW Date: 2/22/95
-------
Quantitatica Liait Report
SDG HO: AflO S LABGRATCRY: RESOVRCE AflL
CASE NO: 22891 GD1CY INPUT FILE: ARTO5.OAS
CONTRACT REQUTRED SMIPLE QU ZITIfl
Icy Med
Water Soil Soil
VGA 5.0 (PU..) 5.0 (C) 4.0 (C)
aza 1000.9 (Pt) 30.0 (CI 1.0 (C)
P 55 1000.0 (ML) 30.0 (C)
DC-4S: The following volatile samples have analyte concentrations below
the quantitatzon limit (QQLJ. All results below the Qt. are
qualified J.
AUTOS
Methylene chloride
A}rro C
Methylene chloride
AUTO ,
Methylene chloride
AUTOS
Methylene chloride
AUTO 9
Methylene chloride
A l4Tll
Methylene chloride
ART12
Hethylene chloride
ANT13
Methylene chloride
AMTL3MS
Methylene chloride
AUT13MSD
Methylene chloride
AE7l4
Metbylene chloride
Filename- InTO ! Date: 03/0619! Time: 02z3 6 CJWRE: 2.10 Page
-------
QuantLtati iit Z.porc
SD NO: AaTos LABORATORy: RXSOV1 i UJ.
CASE NO: AGENCY ZNPUT PZLE: AZTOS.OAB
ANTIS
P4ethylene Chloride
A&fl 16
Methylene Chloride
Afl?2 0
Methylene Chloride. Benrene
AW 2 OMS
Mechylene chloride
AHT2 OMSD
Methylene Chloride
lilcr2 3
Methylene Chloride
AHT2 6
Methylene chloride
A}iYS7
Methylene Chloride. 1,1, 2,2.Tetrach1oroetha le
VBLICCC
Methylene chloride
?4ethylene chloride
OC.66: The qua.ntitation limits of the followthg volatile 8anrples
could not be calculated, due to missing information.
Manual review of the ‘orm 1 data La required to determine if any
compounds were detected below the QQL. All compound3 reported
below the QL ahould be qualified J.
VBLX
DC-hO The followtng aemivolatile aample have analyte concentrations
below the quantitatiort limit ( QLI. All reaulta below the QL
are qualified •J.
ARTO8
Phenanthrene. Fluoranthene, Pyrene, Ben:ola)anthracene
chryeene. Eenzo(bl fluoranthene. Ben:o(k flueranthene, 8enzo(a pyTene
Indeno(l.2, 3-cd)pyrena, Renzo(g.h. i)perylane
i lename: AZTOS Date: 03/06/95 Time: 02r36 CADRE. 2.10 Page 2
-------
Quantitation Limit Ruport
SOC NO: *ZT0S tJSORAttRY; . ssona nw.
CASE NO: 3289 1 AGSNCY INPUT fl u: AST05.OAS
AW O0MS
Phenanthrene Fluora.nthene, Denzc(a)anthracene, Qtryaene
Bensolbi fKoranthene. Benzo(k lfluoranthene. 2enzo(alpyrene. Indeno(1 ,2.3-cd pyrene
Benzo(g,h, i)perylcne
A l cro BMSD
Phenanthrene, FWoranthene • Bento (a) anthracene • Chryeene
Benro Cb) fluoranthene, Benzo(k) fluoranthene, Denro(a)pyrene, Indenall, 2, 3-cdlpyrene
Bento (g. h • U perylene
AR-ri 1
Acenaphthylcne. Phenanthrene, Fluoranthene, Pyrene
Benzo(a)anthracene. Otrysene. Benro(b) fluoranthene , Benzo(k) fluoranthene
Benzo(alpyrcne. Indenoll2.3-cd)wrene , Benro(g,h.i)perylene
AIF r20
1,4 -Dithlorcbenzene
DC-Ill: The quantitation limits of the following gemuvolatile samples
could not be calculated due to missing information.
Manual rev .ew of the Form 1 is required to determine if any
compounds were reported below the QId. All compounds reported
below the CtQL should be qualified 3.
snuafJ, SBZJGDC, satiaa
DC-iS O : The following pesttc lde samples have e.nalyte concentrat&ona below
the quancitacion limit (CRQL). All results below the CRQL, are
qualified ¶J•.
INTO B
Aroclor-l254
ANT i)
1,4’-ODE, 4,4-DOT
DC-lS9: The quancitation limits of the following pesticide samples could
not be calculated due to missing information.
Manual review of Form 1 is required to determine if any compounds
were reported below the CRQL. All results reported below the
act should be qualified J.
P 2tX17
rilename: A lto ! Date: 03/06/95 time: 02:36 CADRE: 2.10 Paqe 3
-------
VOLAT ILES
- - - - Aromatic - . - -
Primary Expanded
7 14
14 28
-• Won-aromatic
Pr imary Expanded
14 28
14 28
S 4IVOLATILES
- - - Extraction - - -
Primary Expandec
7 14
7 14
Analysis
Primary Expanded
40 60
40 60
PEST IC I DES
- - -- Analysis - - - -
Primary Expanded
40 60
7 14 40 60
DC-74. The followtng semivolatile water samples are outside primary
extraction holding time criteria. Hits are qualified P and
non-detects are qualified U3.
AXT2OMS. AHT2OMSD
DC- 106. The following semivolatile soil samples are outside primary
extraction holding time criteria.
Hits are qualified J” and non-detects are qualified ZL1’.
ARTOSI AJ4TO6. A}C107. AHTO7RZ ABTO8. AHIOSMS
AHTOBMSO. AKIO9. ABT11. AHT12. JQifl3. ART13MS
AHTI3MSD. A5T14 • AHT1S. AHT16
fold ing IS a. Report
SOC NO. £2103 LABORAtORY: RZSOU* SI lOS
CASE NO. 22891 AGENCY INPUT F ILE: AWrO3.OAS
HOLDING TIIC CAITERIA
Primary Expanded
14 28
Preserved
Water
Unpreserved
Water
Soil
Water
Soil
- - - Extraction - - -
Primary Expanded
7 14
Water
Soil
FLlename: A2703 Date: 03/06/93 Time: 02:36 CADRE. 3.10 Page 1
-------
Eoldieq na. Rspcrt
SOC NO: ABTO S L.ADORATORY: &ZSCOBn M L
CASE NO- 22 191 AG CY INPUT FILE: AZTO5.QA3
DC- 161: The following pesticide water samples are outside primary
extraction holding time criteria.
Kits are qualif ted ‘3” and non-detects are qualified UJ’.
M uONS . AHT2ONSD
DC-163: The following pesticide soil samples are outside primary
extraction holding time criteria.
Hits are qualified J and non-detects are qualified ‘03’.
AICOS. AMTO6. M{TO1. ABTOS. A11t09. AHTll
ABT12. Aafl3. ABTL3NS. AHT13NSO. A11tl4. ABT1S
ANTi S
Filename: ARIaS Date: 03f06 9S time: 02:36 CADRE: 2.10 Page 2
-------
P.rcsnt Xaiittx. Raport
sr &o: C.ASORATQRY: &ZSCVRa MaX.
CASE MO: 22391 ACfliCT IMPUT FILE. ABTOS.OAS
PERCZYT MOIS7VRE LIMITS
Primary Expanded
VOA 70% 90 %
ENA 70% 90%
PCS 70% 90%
No prcblees found for this qualification.
F dename AETOS Date: 03/06(93 Time: 02 36 CADRE: 2.10 Page
-------
Xmatx .ant P.rfoe.aaes sck Rsport
SOC NO: XZ05 LA3ORATOR : USO0R .L
CASE NO: 22891 AG (CY INPUT FILE: 1.2705.0 1.3
The complete primary criteria for 8Th are as follows:
Bromofluorobenzene (OFO)
m/z ION AflUNW.N ITtRIA (Vol&tile)
SO 8.0 - 40.0% of m/z 95
75 30.0 - 66.0% of rn/S 95
95 base peak. 100.0% relative abundance
96 5.0 - 9.0% of rn/a 95
173 lees than 2.0% of rn/Z 174
174 50.0 - 120.0% of rn/a 95
175 4.0 - 9.0% of n/a 174
176 93,0 - 101.0% of rn/a 174
177 5.0 9.0% of ca/a 176
The complete primary criteria for OFI’PP are as followrn:
Decafluorotriphenyiphosphine (DFTPP)
rn/z ION ABUNDANcE CRITERIA (Seruvolatile)
51 30.0 60.0% of ce/S 199
68 less than 2.0% of rn/a 69
69 present
70 less than 2.0% of rn/a 69
127 25.0 - 75.0% of rn/S 190
197 less than 1.0% of rn/a 198
198 base peak. 100.0% relative abundance
199 5.0 - 9 0% of rn/S 198
275 10.0 30.0% of rn/z 198
365 greater than 0.75% of rn/a 196
441 present, but less than rn/S 443
442 40.0 110.0% of cal: 198
443 15.0 - 24.0% of n/a 442
No problems found for this qualification.
? j.ename: 3 .3705 Date: 03/06/95 Time: 02:37 CABRE: 3.10 Page
-------
N .IxrICAL SEQV
CASE HO: 22891 IJ.BCRA7ORY: RESOVR A .LYSTS. INC.
StG NO: )J T05 LHSRLD 2 T: OtS4
# I1lOD: VOA
SAIWL2 HD LAB FILE ID/CC COL 1 DATE TI?
C6020 xrc C6020 10/25/94 16:19
Initial Calibration C6024 10/25/94 18 :48
C64 17 x c C6417 11/18/94 09:45
Continuing Calibration C6419 11/18/94 10:93
VBLXCC Method Blank C6420 11/18/94 11:29
ANYS7 Routine Sawple C6424 11/18/94 13:53
?.HT1O Equipment Blank C6425 11/10/94 14:28
AKT19 Routine Sai Le C6426 11/10/94 15:03
AHT21 Routine Saxi 1e C6427 11/18/94 15:37
AIiT22 Routine Sanple C6429 11/18/94 16:13
AH T25 Equipment Blank C6429 11/18/94 16:47
MT20 P.autthe Sanpie C6430 11/10/94 17:22
AiIT2OM .S Matrix Spike C6431 11/18/94 17:57
MT209 D Matrix Spike Dup C6432 11/18/94 18:32
AWI26 Equ .pment Blank C6433 11/10/94 19:07
AW 23 Trip Blank C 6434 11/18/94 19:42
FILE NAZ : AJITOS DATE 0)113195 TI1 . 13:37 CAERE 2.10 PACE:
-------
ANATdflICAL SEQU ( (X
CASE NO: 22891 £J 2ORATORY: RXSCCR A LYS7S. INC.
I . ... NO: ANTOS INSflQ T: OiS.RP
00: VGA
SAMPLE Nt2G t t n t LAD FILE ID/CC COL *1 DATE TDC
C464 1 I NC C4641 09/27194 11:11
Initial Calibration C465 1 09/27/94 16:54
C6439 I NC C6439 11/21/94 11: 16
Continuing Calibration C6441 11 /21/94 12:41
VBLXC Method Blank C6443 11/21/94 13:59
Mt06 Routine Sample C 644S 11/21/94 15:09
A}{t07 Routine Sample C6446 11/21/94 15:44
A 1C08 Routine Sample C6447 11/21 )94 16:19
A1f 109 Routine Sample CG448 11/21/94 16:54
A lffl l Routine Sample C6449 11/21/94 17:29
MCfl2 Routine Sample C54 50 11/21/94 13:03
A 14113 Routine Sample C64 5 1 11/21/94 18:38
ARfl3MS Matrix Spike C 5452 11/21/94 19:13
AJffl3MSD Matrix Spike Dip C 54 53 11/21/94 19:48
AWfl4 Routsne Sample C6454 11/21/94 20:23
ART1S Routine Sample C 5455 11/21/94 20:58
ANTIS Routine Sample CE4SS 11/21/94 21:33
ASiTOS Routj.ne San’le C64 57 11/21/94 22:08
FILE NAJC: ANTOS DATE: 03/13/95 tDC: 13:37 CADRE 2.10 PAcE: 2
-------
ABALrrx .L SEQUU
QSE NO: 22891 LABORATORY: R!SOUR ANALYSTS. INC.
SOC NO: ANTO5 LflSTR T: IBIS -NP
E0OD: ONA
SAMPLE NtB TYPE LAB FILE ID/CC CVIAR’Ql DATE TD
1 (6929 1(6929 .1/22/94 12:42
Initial Calibration 06932 11/22/94 13:34
58U 04 1 Method 9jjjaJ 1 (6936 11/22/94 16:36
Routine Sample 1(6938 11/22/94 17:45
AKI2 1 Routine Sample 1(6939 11/22/94 18:19
A 0T22 Routine Sample 1(6940 11/22/94 18:53
AHT IO Equipment Blank 06941 11/22/94 19:27
A 0719 Routine Sample H6942 11/22/94 20:02
AXT2S Equipment Blank 1(6943 11/22/94 20:36
)J4T26 Equipment B18 .M 06944 11/22/94 21:10
06947 IPC 1(6947 11/23/94 10:38
Continuing Calibration 1(6949 11/23/94 10:59
SBUO J Method Blank 1(6950 11/23194 11:43
SBLIOQ ( Method Blank 06951 11/23/94 12:17
9LIO (L Method Blank 1 (6952 11/23/94 12:51
AK 713 Routine Sample 1(6954 11/23/94 14:00
AHT13MS Matrix Spike 06955 11/23/94 14:34
AXT13MSD Matrix Spike Dup 06956 11/23/94 15:08
AWIOS Routine Sample 06957 11/23/94 15:42
AI IT12 Routine Sample H6958 11/23/94 15:17
?1 1T14 Routine Sample 06959 11/23/94 16:51
AET 1S Routine Sample 06960 11/23/94 17:25
A 0T16 Routine Sample 1(6961 11/23/94 17:59
AHTOO Routine Sample 06962 11/23/94 18:33
AXTO8MS Matrix Spike 1(6963 11/23/94 19:07
MTO8MSD Matrix Spike Dup 1(6964 11/23/94 19:42
Awr l l Routine Sample 06965 11/23/94 20:16
ABT O9 Routine Sample 1(6966 11/23/94 20:50
A OTO6 Routine Sample 06967 11/23/94 21:25
AI4T O7 Routine Sample 1(6968 11/23/94 21:59
1(7032 IPC 07032 12/02/94 10:50
Continui.ng Calibration 07034 12/02/94 11:09
SBLJO(Q Method Blank 01038 12/02/94 13:33
A OT2 OMS Matrix Spike 1(7039 12/02/94 14:07
AET2 OMSD Matrix Spike Dup 01040 12/02/94 14:41
A OT O7RE Routine Sample 07053 12/02/94 22:03
FILE NAI . AXTOS DATE: 03/13/95 TD : 13:37 cADRE 2.10 PAGE: 3
-------
Calthrarion £ isttng
I CP.S NO; 22091 LABDRAIVR : RESOUR MU L’tS , INC.
NO; ?JiTOS
LAB FILE 10/ %RSD
- 2ION 1NSTRT .B T TIPE GC COID9 0? IE TD COMPOUND P R? (%D/P.PD1
VOp Q -HP INITIAL C6024 10/25/94 18:40
Q 1or necbane 34.7
Acetone 30.3
Carbon Disultide 45.2
VOA 4S-I P CorrNtnnO C6419 11/10/94 10:53
Carbon Disulfide -74.5
2-Butanone 37.7
4-Methy l-2-Peritanone 34.0
2-Hexanone 43.2
Aesoc. Saaçle(s7 : VBUCCC 11/18/94 11:29
AKYS7 11/10/94 13:53
MT1 O 11/10/94 14:28
AflT19 11/18/94 15:03
A16F21 11/18/94 15:37
3J I22 1.1.110/94 16:13
xr25 11/10/94 16:47
1iT20 11/10/94 17:22
AHT2OI4S 11/10/94 17 57
T2QMSO 11/1.0194 2 .8 32
.HT26 11/18194 19:07
AHT23 11/18/94 19:42
A Q S-MP LNITI.P.L C4651 09/27/94 16:54
VOA C1S- co rrINUIx C6441 . 11/21/94 12.41
2-Butanone 30.2
Asnoc. Sa1rç1e(5 : VBLECO 11/21/94 13.59
A24T06 11/21/94 15:09
A 14T07 11121/94 23:44
AHTO8 1.2./21/94 2.6:19
AN T U9 11/21/94 16:54
11/21/94 17:29
A&fl’12 11121/94 18:03
AMT13 11/21/94 18:30
ART 13KS 11/21/94 19:13
M 13MSD 11/21/94 19.48
Mi 114 11/21/94 20:23
11121/94 2C58
1J T16 11/21/94 21:33
MTO5 11/21/94 22:08
FILE 7W E: A1iT05.S1 3 OPilt: 03/13/95 TIl B: 13:37 CAORE 2.10 PPGE:
Only RRP and %R.SD C%D/P.PD) values which exceed cr ter1a are Listed.
-------
CASE NO:
S NO:
CAlibratiou Lioting
22891 LAaORAT W: RESOUR AZCALYSTS. INC.
AHTOS
LAB PILE !D/ %RSO
F9.ACrICN INS R 2 I ‘19E CC COU2 .0 ORTE IJ RPS I%D/RP
804S4W 1N171).L U6932 3 .1/22/94 13:34
Benza(k)f luoranthene 37.9
A eoc. .nç1eCs : S3U0 Z 11/22/94 16:36
pgr2a 11/22/94 17:45
21T21 11/22/94 18:19
AKT22 11/22/94 18:53
11/22/94 19:27
?JtT19 11/22/94 20:02
1{T2S 11/22/94 20:36
AHTZ6 11/22/94 21:10
W 1C45XP cONTINUINC 146949 11/23/94 10:59
2.4-Dthitrcphcnol 32.8
Ass c. Saiiple(s) : 501.104? 11/23/94 11:43
SBI.JOUC 11/23/94 12:17
SDtJOfl. 11/23/94 12:51
AHT I3 11/23/94 14:00
AHTI3MS 11/23/94 14:34
?.&IT13MSD 11/23/94 15:08
A}LT O S 11/23/94 15:42
MT12 11/23/94 16:11
A 4T14 11/23/94 16:51
A 4T1S 11/23/94 17:25
AWfl6 11/23/94 17:59
AXTOB 11/23/94 18:33
A XT0BMS 11/23/94 19:07
A I1T OBMSD 11123/94 19:42
MT11 12/23/94 20:16
AXTO9 11/23/94 20:50
11/23/94 21:25
A I 1T O7 11/23/94 21:59
I* -}CP 147034 12/02/94 11:09
Benzo(k)f luorantherie -25.3,
Msoe. Sar 1e(s4: S2L Q 12/02/94 13:33
MT2OMS 12/02/94 14:07
A I4T2OMSD 12/02/94 14:41
A I4T O7RE 12/02/94 22:03
I.
PILE KAt : AHTO5.SDG DATE: 03/13/95 T : 13:38 CABRE 2.10 PACE: 1
• Only PR? azd %R.SD t%D/RPDI values which exceed criteria are listed.
-------
Calibratiae Rport
SOC ND: AZTOS LAB0RATOR : R O R A L
CASE NO: 22891 AS CY INP F FILE: A 0S.O*3
CALIBRATION C t IA
VOLATILES
Prinary Expanded
Mini.ntum RAP 0.05 0.05
Max jm %R.SD (Lru.tial calibration) 30 so
Maxiraim ‘ .0 (corlt3.nutng calibration) 25 50
Calibration time period 12
S 1IVOLATILES
Primary Expanded
Minimum RR 0.05 0.05
Maxtenim %RSD (initial calibration) 30 SO
Maximum ‘.0 (continuing calibration) 25 50
Calibration time period 12
PESTICIDES
Maximum %RSD (initial calibration) - T analyte! 20
- surrogatea 30
Mximum RPD (continuing calibration) 25
Continuing calibration sequence time 12
DC•22: The following volatile samples are associated with a continuing
calibration whose correspond.tng initial calibration ha., percent
relative stan4ard deviation (%RSD) outside primary criteria.
Hits are qualified J and non-detects are not qualified.
O loromethane
A1C r10 • AHT 19 • ABT2 0 • ART2 OMS • AHT2OMSD • ART2L
ADT22. AHT23. ABT2S. )JtT26 • JHY57 • VBLXCC
Acetone
?J (T10. AKT19. PIFF2O. AXT2OMS, MF2OMSD. ?.HT2 I
A}(T22, RET23 • ABT25 • AW 126 • AHY57 • VBL.XCC
Carbon Disulfide
A}1T10. AHT I9 • ABT2 C • AMT2 OMS • P,1 (T2 OMSD • 7 BT2l
AHT22, AHT2 3 • AHT2 S • ? 1 H726 • AHYS 7 • VBLXCC
Filename: AET0S Date: 03/06/95 Time: 02,37 CADRE: 2.3.0 Page
-------
Calibnticn Zapørt
SOC tO : AUTOS tAaoItATOfl: azsona *zw.
CASE NO: 22691 ACDCY INPUT PILE: A OS.OL9
DC-23: The following volatile samples are associated with a continuing
calibration percent difference (tO) outside primary criteria.
Hits are qualified J and non-detects are not qualified.
2 .But5j . ne
ARTOS, ARTOG AHTO7, ARTOO, fl1T09, ANTIO
AliTfl, A14fl2, AHTI3, AHTI3MS, AHT13NSD. AETI4
MITtS, ANTIS, N1fl9, ABTZO, PIBT2OMS, ABT2OMSD
A11121, MT22, A1iT23. AET2S, MT26, AHYS7
v9LxCC, vDwco
4-MethyL -2- Pentanone
ANflO, N1fl9, AKflO, AHT2OMS. AXT2CMSD. AIIT21
AHT22, MiT23, A11T25, AMT26, AHYS7, VDLXCC
2 -Hexanone
ANT1O, AETI9, AHT2O. AJiT2OMS. AMT2OMSDS AMT21
AMT22, AflT23, AHT2S, MlflG. Alit’S ?. VELZCC
DC-fl: The following setnivolatile samples are associated with an initial
calibration percent relative standard deviation (%RSD) outside
primary criteria.
Hits are qualified ¶J and non-detects are not qualified.
Eenzo(k( fluoranthene
ANTLO. AWfl9 A11T20, A}it2l, AXT22, A&IT2S
AHT2G. SDL)O4I
DC-SO: The following semivolatile samples are associated with a
continuing calibration whose corresponding initial calibration
has percent relative standard deviation (%RSD) outside primary
criteria -
Hits are qualified ‘J and non-detects are not qualified.
Benro fit) f luoranthene
A lTOS. AKT06. AlTO ?. AJ4TO7RE. AlTOS, A&OTOSIC
ARTOOKSD, AXT09, ANTS1, A$lTl2, AUT13. AMTL3MS
ABT23MSD. ANTI4. ART1S, ARTI6, ANT2OMS. AJIT2OMSD
SOLJOCJ. S2LICOC, EDUCE.. SBLIDIQ
DC-tOO: The following sem ivolatile samples are associated vith a
continusng calibration percent difference ( ID) outside primary
FilenameS AUTOS Date: 03/06 ( 95 Time: Olifl CANRE: 2.10 Page 2
-------
Calibration Import
SOC NO: AETOS LABORATORX: RxsCVRa AflL
C74.SE NO: 22891 AG (CY INPUT FILE: AZTO!.OIS
criteria.
Hits are qualified J and non-detects are not qualified.
2, 4-Dinttrophenol
SiWIOS, MTO6, MITO7, AUTOS, ?4tTOOMS. ARTOSMSD
?JITO9, Aflfll, A11T12. AHT13, AHfl3MP, AHT13MSD
MTL4, A}{T1S, AHT16. SDLIO4J. SDU0 K. SDLJPC.
Benzo (k I luoranthene
AJfTD7RE, AHT2OMS. AHT2OMSD, SPLIOtO
DC-l94: The at of the analyte in the midpoint ENDAIINDD fell outside the
R I ’ window established during the initial calibration.
Manual review of the chrosatograma for the associated sasiples is
required to determine if false positiveslnegatives exist.
Qualification is left to professional Judgement.
AJ F IO7
4,4 ’ -ODD, Endosulfan sulfate. 4,4’ - CD ?, Methoxychlor
Endrin aldehyde
AKID B
4,4’-DDD, Endosulfan sulfate, 4,4’-DDT, Metftoxychlor
Endrin aldehyde
4,4’-DDD, Endosulfsn sulfate. 4,4’-DOT. Methoxychlor
Endrtn aldehyde
M n ]
4.4’ -COD. Endosulfan sulfate. 4,4’ -PD?. Methoxychior
Endri.n aldehyde
A NT 1 INS
4,4’ -DOD, Endosulfan sulfate, 4,4’-DDT, Methoxychlor
Endrin aldehyde
AJ4T13MSD
4,4’ -ODD, Endosulfan sulfate, 4,4’ -DOt, Methoxychlor
Endrin aldehyda
A I IT I9
4,4’-DDD, Endosulfan sulfate, 4,4’ -DOT, Mathoxychior
Endrin aldehyde
AJt 120
Filename: AETOS Date: 03/58/95 time: 02,31 CORE: 2.10 Page 3
-------
Calibration Report
500 NO: AZTOS L.ABORA’IVRY: RZ5OU2 arni.
CASt NO: 2 389 3 . AGDCCT INPUT FILE: AUT0S.CU
4,4’ -ODD, Endosulfan sulfate. 4,4’ -DOT, MethoxychiOr
Endrin aldehyde
AHT2OMS
4.4’ -ODD, Endosulfan sulfate, 4,4 ’ -DOT, Methoxycttlor
Endrin aldehyde
AWT2 01430
4.4’ -000, Endosulfan sulfate, 4,4-DOT. Methoxychlor
Endrin aldehyde
A}F1’2 1
4,4’ -DOD. Endosulfsn sulfate, 4,4-DOT, KethoxychlOr
Endrin aldehyde
4,4’-DDD, Dtdosulfan sulfste, 4,4’-DDT, l4ethoxychlor
Endrin aldehyde
AHT25
4,4’ -ODD, Endosuif an sulfate, Endrin ketone, Endrin aldehyde
pscn 9
4,4’ -ODD, Endosulfan sulfate, 4,4’-DDT. Methoxychlor
Endrin aldehyde
POLC I
4,4’ -DOD, Endosulfan sulfate, 4,4’-DDT, Methoxychlor
Endrin aldehyde
P OLC2
4,4’-DDD, Endosulfan sulfate, 4,4’-DDT, Methoxychl*r
Endrin aldehyde
DC-341: The following volatile samples are associated with a continuing
calibration percent difference (tO) outside expanded criteria,
Hits are qualified J and non-detects are qualified ‘UJ’.
Carbon Disulfide
A}tTlO. AXT19, MT2O. AHT2OMS, flITIOMSD. W it
ARfl2, AX’T23, AI4T2S, Mil lS. A11Y57, VBLTCC
Filename: AUTOS Date: 01/06/93 Tim :: 02:37 ODRS: 2.10 Page 4
-------
L.bontozy Blanks flpcrt
SDG NO: &ros LABORATORY: RZS00R AflI.
CASE NO: ACENCY INPUT FILE: ARTO5.OSS
LABORATORY BUNKS CRITER IA
VCtJC L IES
Method Blank Contamination Threshold Multipliers
First Expanded
Coimtn contaminant compounds 10.00 10.00
Other compounds 5.00 5.00
SD ILVOLI¼TILES
Method Blank Contamination Threshold Multipliers
First Expanded
Cosrtn contaminant compounds 10.00 10.00
Other compounds 5.00 5.00
PESTICIDES
Method Blank Contamination Threshold Multipliers
First Expanded
All compounds 5.00 5.00
DC-ZOO: The following volatile samples have analyte concentrations
reported below the CRQL and less than or equal to ten times (lOX)
the associated method blank concentration. Reported sample
concentrations have been elevated to the CRQL.
Hits are qualified U and non-detects are not flagged.
MTO S
Hethylene thloride
AWt0
Methylene Chloride
Filename: SKTOS Date: 03F06/95 Tine: 02s40 CADRE: 2.10 Page
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L&boratoxy 21 nka Ruport
$00 NO AETO5 LMORATORY: R!SOU AWL
CASE O: 22191 AG CY N tIr FILE. 1. ?OS.CAS
Methylene 1oride
AK OB
Methylene t1oride
AKTO9
MethyLenc auorido
AT1I
MethyLene 1oride
AWt 2
MethyLcne 1oride
ART13
Methylene chloride
ANT 13MS
NethyLene chloride
ARr 13MSD
Methylene chloride
AWLI4
Methylene chloride
A}rrls
Mcthylene chloride
)Jrrl6
Methyl e r ie chlor de
3ixT20
Methylene chloride
AMT2 OMS
Methylerie chloride
T2OMSO
Methylene chloride
?JfI23
Methylene chloride
AWD2S
Methylene chloride
ilename; A TO5 Date: 03/06195 Time: 02:40 CADRE: 2.10 Page 2
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T..boratøy Bha ka .port
SDG NO: A TO5 LABORATOPX: IZSCVP. 29L
C.SE NO: 22 9L G CY INPOT FILE: AETQ5.Q&3
A1 (51
M thy1ene Q Lcride
DC-233: The fo11owi q pea:icide mep1e5 are not qualified for laboratory
blank., because of eiaatn laboratory blank 1nforu ation.
Manual reviev of the d Ca La cequLred for this parameter.
PBLX I9
F 1enatne : A ?O5 Date: O3/O f9S Tjf e: 02z40 C?DAE: 2.10 Page 3 -
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Region I
Data Review Worksheet
V A. BLANK ANALYSiS RESULTS (Sections 1 & 2)
List the contamination in the blanks below Level: Tj,w
I. Laboratory Blanks
DATE LAB ID FRACTION/ COMPOUND CONCENTRATION/
MATRIX UNITS
2. Equipment and Trip Blanks
DATE TR # FRACTION/ COMPOUND CONCENTRATIONI
MATRIX tTh!ITS
12-7 AffT26 VOA Metfrvlene chloride 1 u /L
12/7 AHT26 VO4 Acetone _ 8 ugIL
12/10 AFJT26 BNA bis(2-Ez/rvlheiy!)j,hthalate 10 u ’fL
A separate worksheet should be used for low and medium level blanks.
Reviewer: TPW Date: 2122195
-------
Region I
Data Review Worksheet
V B. BLANK ANALYSiS RESULTS (Section 3)
3. Blank Actions
Action levels should be based upon the highest concentration of contaminant determined in any blank.
The action level for samples which have been concentrated or diluted should be multiplied by the
concentration/dilution fictor. No positive sample result should be reported unless the concentration of
the compound in the sample exceeds the action level of lOX the amount in the blank for the common
contaminants, or SX the amount for any other compound. Specific actions are as follows:
1. The concentration is less than the CRQL, report the CRQL qualified with a 13.
2. The concentration is greater than the CRQL, but less than the action level, report the
concentration found with a U.
3. The concentration is greater than the action level, report the concentration unqualified.
For examples refer to the Regional Guidelines.
Common contaminants: Methylene chloride, Acetone, 2-Butanone, Toluene, and Phthalates.
LEVEL: frw
COMPOUND MAXIMUM CONC./ ACTION LEVEL! CROL
UNiTS UN iTS
? vfethylene chloride . 7 ugiL 10 ug/Kg 10
Acetone 8u2 1L 80 t ic/KR 10 -
_________________________________________________________ JO ug/L 100 t sR / I C R 330 _
A separate worksheet should be filled out for low and medium level blanks.
Reviewer: TPW Date:_2/22/9 5
-------
Ocfsurrogtts Report
soc io saros L a BOR A TOR Y Usovza a.nz.
CASE NO: 22832 AGDtCY INPUT FILE: AZ?05.QA3
SMC/SURRcGATE OtItEttA
votaTtLES
Percent Recovery Limits
Tolutne-d8
Brotnof luorobentene
1. 2-D lchlorcet iuxte-d4
- - - Water - - -
Lower Upper
80.0 110.0
86.0 115.0
76.0 114.0
----Soi l---
Lower Upper
84.0 138.0
59.0 113.0
70.0 121.0
gmlwotaTu2s
Percent Recovery Limits
Nitrobenzene-65
2- Fluorobipheny l
Terpheny l-d 14
Phenn l-d S
2-F luorophenol
2, 4 6-Tribro pheno1
2 -chlorophenol-44
1. 2-Oichlorobenzene-44
Water - . -
tower Upper
35.0 114.0
43.0 116.0
33.0 141.0
10.0 110.0
21..0 110.0
10.0 123.0
33.0 110.0
16.0 110.0
--—-S oi l-- -
tower Upper
23.0 120.0
30.0 115.0
18.0 137.0
24.0 113.0
25.0 121.0
19.0 122.0
20.0 130.0
20.0 130.0
PEST IC IDES
Percent Recovery Limits
Tetrachioro -m-xylene
Water
Lower Upper
60.0 150.0
60.0 150.0
-———soi l--—
tower Upper
60.0 150.0
60.0 150.0
DC- 173: The follcvLng pest Icide samp les have surrogate aT ’s ctttszde the
Filename- 3.fl05 Date: 03/06/95 Time: 02.38 CADRE: 2.20 Page 5.
-------
/3urrogat. g.pOre
SOC NO: £ 05 LAEORATORY: SO 5 L2øiL
CP.S NO: 22 591 ? G CY INPVT FILE: AZTOS.OAS
RT window established during the initial calibration.
Manual review of the chrcfflatogtatfl iS required to determine if the
possibility of false positives or negatives exist. Qualification
is left to the professional ud enent of the validator.
AI rl3MS. AI r13MED
DC-177: The following pesticide samples have surrogate percent recoveries
outside the Lower limit of the criteria window, but greater than
10%. Hits are qualified J and non-detects are qualified
AJ4TOS. AMTO7, )J T09, ANTLO. ARfll. AHT12
• AET I3KS • ARTL3MSO. ).ETL4 PJFtIS. ANT1
PJ4T]. 9. AET2 0, ? .lcr2 OMS • AHT2OMSD • ANT2 1, ?.11T22
ARr2s
DC-1e2 The following pesticide nethod blanks have surrogate percent
recoveries outside criteria. A visual inspection is required
to determine the validity of the sample data.
Qualificatiort is left to the profes LonaL udgement of the
valjdstor.
PBLXI7. PELX2L. PBL1 2
Filename: A r05 Oate: o3/O6/ Tine: 02 35 Cm P.E: 2.10 Page 2
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Xatriz Opik. Paport
SOC NO: 2 05 LABORATORY: RES0O* ).10.X.
CASE NO: 3 993 AG C1’ INPUT FILE: A2105.0A3
MATRIX SP lICE CRITERIA
VOLATILES
Percent Recovery Limits & RPD
Water Soil
Lower Upper P.PD Lower Upper ROD
1,1-Dichioroethene 61.0 145.0 14.0 59.0 172.0 22.0
Trichloroethene 71.0 120.0 14.0 62.0 137.0 24.0
flen2ene 76.0 127.0 11.0 66.0 142.0 21.0
Toluene 76.0 125.0 13.0 S9.0 139.0 21.0
Q 1orobexi.zen e 75.0 130.0 13.0 60.0 133.0 21.0
SD4IVOLATILES
Percent Recovery Limits & RPD
W&t Soil
Lover Upper P.PO tower Upper RPD
Phenol 12.0 110.0 42.0 26.0 90.0 35.0
2-C loropheno 1 27.0 123.0 40.0 25.0 102.0 50.0
1.4-Dichlorobenzerte 36.0 97.0 28.0 28.0 104.0 27.0
N-Nitroso-di-n-propylamine 41.0 116.0 38.0 41.0 126.0 38.0
..2,4-Tricb1orobenzene 39.0 98.0 28.0 38.0 107.0 23.&
4-C 1oro-3-methy1phenol 23.0 97.0 42.0 26.0 103.0 33.0
Acenaphthene 46.0 118.0 31.0 31.0 137.0 19.0
4-Nitrophenol 10.0 80.0 50.0 11.0 114.0 50.0
2.4-Dinitrotoluene 24.0 96.0 30.0 28.0 89.0 47.0
Pentachlorophenol 9.0 103.0 50.0 17.0 109.0 47.0
Pyrene 26.0 127.0 31.0 35.0 142.0 36.0
PESTICIDES
Percett Recovery Limits & ROD
water Soil
Lower Upper RPD Lower Upper RPD
Filename: BT05 Date: 03/06/95 Time: 02i37 CADRE: 2.3.0 Page
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Xatz iz Spik. P ..pcrt
SOC NO: aZrOS USORATORY: US00P. Iz J.
CASE NO: 22091. AG CZ INPUT FILE: AETOS.CA5
gaeera-BNC (T4ndane) 56.0 123.0 1.5.0 46.0 1.27.0 50.0
Heptach lor 40.0 131.0 20.0 35.0 130.0 31.0
Aidrin 40.0 120.0 22.0 34.0 132.0 43.0
Die ldrin 52.0 126.0 1.0.0 31.0 134.0 30.0
Endrin 56.0 121.0 21.0 42.0 139.0 45.0
4.0 -DOT 38.0 1.27.0 27.0 23.0 134.0 50.0
DC-SI.: The following ,em volati1e natrix 3pUce/matrix spike duplicate
samplea have percent recovery outside criteria. Manual review of
FOri , 3 is required to determine if recoveries are high or lOw.
Hits axe qualified J. Non-detect, are qualified cnly if
recoveries are Low. Action app1i only to the un.,piked san 1e.
A1412 0 143
4 -Nitrophenol. Pentachioropherwi
AR12 QMSD
4-Nitrophenol
Filename: A.gros Date: 03/06/95 Time: 02:37 CADRE: 2.1.0 Page 2
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Region I
Data Review Worksheet
VU A. MATRIX SPIKE/MATRIX SPIKE DUPLICATE
1. Matrix SpikeIMatrix Spike Duplicate Recoveries and Precision
TR Nos. I4HT20 ,___________ Level: Low Matrix: Soil
List the percent recoveries and RPD’s of compounds which did not meet the criteria stated on Form 3.
FRACTION COMPOUND %REC/ OC LIMITS
MS OR MSD RPD
BNA/MS 4-nit rophenol 10 11-114
BWA/MS pentachlorophenol 115 1 7-109
BNA/MSD 4-nitrophenol 9 11-114
SQUALIFICATION IS LIMITED TO THE UNSPIKED SAMPLE ONLY
1. If any compound does not meet the Contract Required Recoveiy Range (CRR) follow the actions
stated below:
PERCENT RECOVERY
CRR
Positive Sample Results I I I
Non-detected Results R A A
2. If any compound does not meet the RPD criteria, flag positive results for that compound as
estimated (3).
A separate worksheet should be used for each MSIMSD pair.
Reviewer: TPW
Date: 2/22/95
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Region I
Data Review Worksheet
VII B. MATRIX SPlICE/MATRIX SPIKE DUPLICATE
3. Matrix Spike/Matrix Spike Duplicate - Unspiked Compounds
TR t4os. AR720
List the concentrations of the unspiked compounds and determine the percent RSD’s of the unspiked
sample, matrix spike, and matrix spike duplicate. No limits have been developed for the RSD values of
the unspiked compounds.
FRACTION COMPOUND SAMPLE.MS.MSD CONC %RSD
DNA Acenaphthylene 251. 231. U 87
DNA Phenanthrene 2001. 2701. 1001 45
DNA Anthracene 231. 291. U 88
DNA Carbazole 26 1, U. U 173
BNA Di-n-but’ ’lphtha1are 23 1. U. U 173
DNA Fluoranthene 3201. 3401. 280J 10
DNA Bulvlbenr9t ahzhalare 41 1. U. U 173
BNA Benzo(a)anthracene 170 L190 J. 140 J 15
BNI4 Chr,’sene 2101. 2201. 1701 13
BNA bis(2-Ethvlhexvl)phthalate 871. 601. 581 24
BNA Benzo(b)fluoranthene 320 J .320 1. 2701 10
BNA Benzo(a)pyrene 1401. 1701. 1201 18
BNA Indeno(1,2,3-cd)yyrene 1001. 37J. 26) 73
BWA Benzo(R .h,i)per9lene 801. 301. U 110
The reviewer must use professional judgement to determine if there is a need to qualify any of the
unspiked compounds in the sample.
A separate worksheet should be filled out for each matrix spike/matrix spike duplicate.
Reviewer: TPW Date: 2/22/95
-------
r
l t d OIThLIFIW SPREAZS}CT
)
QSE NO: 22891
S ITE:
—
NO: JUl05
LASORAItRY: RESOUR ANALYSTS.
SA?QLE u l9 :
.......IO1 L SAMPLE Nt3C t:
SI mPLE t.CCATION:
IAHT13 IMT13MS IflCT13MSD
l SO- 0 3 150 -03 15003
I I
SAJ’W12 TYPE:
09.TR U/J. laLy5I5:
taotatine Sample Matrix Spike IMatr ix Spike Ott
(SOIL/LOW [ SO IL/LOW ISOIL/LOW I
DILUTION FACtOR:
1.0
1.0 I 1.0
2fl 1T ICISTURE:
48
48 I 48
Hu&
th lorome t ha n a 19 UI 20 UI 19 U )
Eroexxiethane 19 UI 20 UI 19 UI
I Vinyl Otloride 19 UI 20 UI 19 UI
F th loroethane 19 UI 20 UI 19 UI
Plethyiene thioride 19 UI 20 UI 19 UI
‘Acetone S9 I 32 I 31 I
earboxt Oisultidt 19 UI 20 UI 19 UI
1.1-Dich loroethtne 19 UI 11.0 I 113 I
1.1- Dichjoroeth.j.ne 19 UI 20 UI 19 UI
1.2-Dlchlcroethsne (total) 19 UI 20 UI 19 UI
th loroforn I 19 UI 20 UI 19 UI
1,2- Oichloroethane 19 UI 20 UI 19 UI
2-Butajione 19 UI 20 Ut 19 UI
1 .1 . 1 -trjch 1oroetJta 19 UI 20 UI 19 UI
Carbon Tetrachlorjde 19 UI 20 UI 19 UI
Brotnad.ich 1or thana 19 UI 20 UI 19 UI
1.2-Dichioropropane 19 Ut 20 UI 19 UI
Ci 3-1.3-Dichloroprvpene 19 UI 20 UI 19 UI
Trich loroethene II 19 UI 110 I 1 00 I
Dthrchloromethane II 19 UI 20 UI 19 UI
1 . 1 .2 - Tr ich loroe t ha na II 19 UI 20 UI 19 UI
Benzene II 19 UI 1 10 I 110 I
tran.s-1.3-Dichloropropene II 19 UI 20 UI 19 UI
Ermectorm II 19 UI 20 UI 19 UI
4-Metby l-2-Pentanone II 19 UI 20 UI 19 UI
— “txanone II 19 UI 20 UI 19 UI
-ach loroethene II 19 UI 20 UI 19 UI
2.2-Tetnchjoroethana II 19 UI 20 UI 19 UI
i e e e II 19 UI 98 I 98 I
Otlorobenrene I 21 I 100 I 110 I
Ethy lbcnzene I 19 UI 20 UI 19 UI
Styrene II 19 UI 20 Ut 19 Ut
Xylene (total) II 19 UI 20 UI 19 UI
FILENAME: ANT05.SDQ DflE: 03/13195 IDE: 13:40 CADRE 2.10 PA GE:
Water units are reported in ug/L.
Soil uatts axe reported in ug/Kg.
-------
TCL 0RIGU AL SPBZA SH!ET
CASE NO: 22091 SITE:
S NO: AHTOS LABoRA OP.Y: RES0UR AW.LYSTS.
EPA SAMPLE NER:
R.ECIc?tAL S.MPLE N ER:
SAMPLE LO TI0N:
SAMPLE TYPE:
MA T EXX/ANAL YSIS:
DILUTION FACIOR:
PERT t4 ISTURE: I
I
IAXT2O l A1 20MS lAHD20
ICW-02 IcW .02 IG ’-02
I I
IRoutine Sample jMatrix Spike IMatrix Spike D
WATER/LOW I WATER/LOW t W&TER/L0W
1.0 1.0 1.0
I
I
O 1orechana 10 VI 10 VI 10 V
Bro mcthane 10 UI 10 UI 10 UI
Vinyl QLloride 10 UI 10 UI 10 UI
iloroethane 10 UI 10 UI 10 UI
Methylene thloride 4 8 .71 I
Acetone 10 UI 10 UI 10 UI
Carbon Disulfide 10 UI 10 U 10 UI
1.1-Dichiotoethene 10 UI 45 46 I
1.1-Dich loroethane 10 UI 10 UI 10 UI
1.2-Dichioroethene (tor.al) 10 UI 10 UI 10 UI
iloroform 10 VI 10 UI 10 U,
1.2-Dich loroethane 10 UI 10 UI 10 UI
2-3utanone 10 UI 10 UI 10 UI
1.1.2 .-Trichloroethane 10 UI 10 UI 10 UI
Carbon Tetrachloride 10 UI 10 UI 10 UI
Br dichloromethane 10 UI 10 UI 10 DI
1.2-Dichioropropana 10 UI 10 UI 10 3I
cis-1.3-Dichioroprcpene 10 UI 10 UI 10 UI
Trichioroethene 10 UI 47 I 48 I
Dibro chlor ethane 10 UI 10 UI 10 UI
1.1.2-Trichioroethane 10 UI 10 UI 10 DI
Benzene 3 .71 49 I I
tran.e-1.3-Dich loropropene 10 UI 10 UI 10 UI
Dr forn 10 UI 10 UI 10 UI
4-Methyl-2-Pentan one 10 UI 10 UI 10 DI
2- ( a none 10 VI 10 UI 10 UI
Tetrach loroethene 10 UI 10 UI 10 U
1. 1.2,2-Tetrachioroetb .ane 10 UI 10 UI 10 DI
Toluene 10 UI 46 I 46 I
C, . lorobenzene 19 I 69 70 I
tthylbenzene 10 UI 10 UI 10 UI
Styreno 10 UI 10 UI 10 UI
Xylene (total) 10 UI 10 U, 10 DI
FIL Z : AJ4TOS.SDG DATE: 03/13/95 TI? : 13:41 CADRE 2.10 PAGE:
Water uiuts arc reported in ugIL.
So 1 units are reported in ug/Eg.
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1 . ORIGflQIL SpREADS1 r
l0 22891 SITE:
: pjrros LABORATORY: R SOOR AMAL iSTS. INC.
SAMPLE NU 8 :
RECI L SAMPLE 1flGER:
SAMPLE 1 TIQN:
SAMPLE T (PE:
M ’IX/ANPiLYSIS:
UILUTICN F L ’OR :
? ‘ ISTUP.E :
IM I13 I AHT13MS 1AHT13M D
ISD-03 I 5 003 ISo-03
I I
I Rotitine Sançle I Mar.xix Spike I Matrix Spike
IS0IL/, ’ D ,SOtL/ ISOXt ./t
1.0 1.0 1.0
49 49 49
I
I
f
I
E1
Phenol
bia )2-Q loroethy1) ether
2-Qilorophenol
1. 3-Dichiorobenrene
I • 4 -DicKlorobenzcne
1, 2-Dichiorobeniene
2-Methyiphenoi
2.2 ’ -oxybLe (1-Chieropropane
4 -Methylphenol
N-Nitre3o-d.i -n-propy1am ne
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
49000
20000
49000
20000
20000
20000
49000
20000
49000
49000
20000
20000
20000
20000
20000
49000
49000
20000
20000
20000
49000
20000
20000
20000
20000
20000
20000
20000
20000
20000
20000
28000
20000
20000
20000
20000
20000
20000
20000
UI 82000
UI 20000
UI 95000
UI 20000
UI 56000
DI 20000
20000
UI 20000
UI 20000
UI 70000
Ut 20000
UI 20000
UI 20000
UI 20000
UI 20000
UI 20000
UI 20000
UI 61000
UI 20000
20000
UI 20000
UI 100000
U 20000
UI 20000
DI 20000
49000
VI 20000
UI 49000
UI 20000
UI 20000
VI 20000
UI 49000
UI 65000
Ut 49000
110000
20000
UI 70000
UI 20000
20000
UI 20000
UI 49000
DI 49000
DI 20000
20000
DI 20000
DI 120000
UI 20000
DI 20000
UI 20000
UI 20000
VI 20000
UI 68000
VI 20000
20000
UI 20000
UI 20000
I 29000
20000
UI 20000
UI 20000
UI 20000
20000
UI 20000
DI 20000
Ni trobenzene
I ophorone
2 -Nitrophenøl
2 • 4 -DLeiethylpheno].
bLe (2-Chloroethoxy) methane
2 • 4 -Dich].orophenoi
1 2 • 4 -Trichloroben.zene
Naphtha lene
4-c3 iloroani line
1 exach1orobutadiene
4- Chic ro-3-methy lphe no l
2-Methy1na htha1ene
exachlorocyc1opentadiene
- • 6-Drich lorophenol .
5 -Tr ch1oropheno1
i lor onaphth a iene
Ltroan. i linc
Dia ethy1phtha1ate
Acenaphthy lene
2. 6-DLn.ttrocoluene
3-Nitroanfline
Acenaphthene
2. 4-Dinitrophenol
4 -Nitrophenol
Diberz.rofuran
2, 4-Dinitrotoluene
Diethylphtha1a e
4- 1oropheny1 -phenyl ether
Fluore ne
4-Nit oani1ine
4,6 -Dinitro-2-rnethylphenol
N-nitrosodipheny lanine
4-Br phenyL-pheny1ether
flexachiorobenrene
Pentachiorophenol
Phenanthrene
Mthracene
Carbazole
Di-n-butylphtha late
Fluoranthene
Pyrene
Dutythenzy lphtha iate
3.3’ - Dichiorcbenzidina
Benao (a) anthracene
Chxy cne
bia (2-Ethylbexyllphthalate
Di -n-oceylphthaiate
Benro (b) flue ranthene
“- ro Ut) flucranthene
zo (a) pyrci e
eno (1, 2 • 3-cd) pyrene
enr (a.h) anthracene
Benro ( , h. i )perylene
DI
Ut
DI
UI
UI
Di
DI
D
CI
CI
UI
U!
UI
UI
CI
UI
UI
UI
UI
UI
ul
UI
UI
CI
UI
UI
UI
UI
UI
UI
V i
UI
UI
UI
UI
UI
UI
UI
82000
18000
95000
18000
59000
18000
18000
18000
18000
68000
18000
18000
18000
18000
18000
18000
18000
65000
18000
18000
18000
100000
18000
18000
10000
45000
18000
45000
18000
18000
18000
45000
65000
45000
100000
18000
67000
18000
18000
18000
45000
4S000
18000
18000
16000
110000
18000
18000
18000
18000
18000
72000
10000
18000
18000
18000
39000
18000
18000
18000
18000
18000
18000
10000
Ut
UI
UI
U I
U’
UI
UI
DI
UI
UI
UI
UI
UI
UI
U’
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
UI
U’
Ut
UI
UI
UI
UI
UI
UI
UI
UI
Ill
UI
U’
II
PIL Q .? : AWEOS.SDG 07 ,30: 03/13/95 tD : 13:41 CADRE 2.10 PAGE: 1
Water units are reported in ug/t.
Soil un.ics are reported i.n u5/K .
-------
T . OaIGIZ L SP S1 U?
QS NO: 2299 . srr
570 NO: AXTOS OR RY . RESOU M LYSTS.
EPA £PJ4PLE Ntfl :
R70XON?.L .10 tE NW :
S3Z4PLE L TION:
S7i WLE TYPE:
MRIX/ Z ALYSIS :
DILUTION FAC’IO :
P T ISIVRE:
1AXT20 IAMT2OMS fANT2 OMSD
IG 4-02 IGw-o2 iCW-02
I I I
IRoutine Saeçle IMatrix Spike lMAtriX Spike Du
IwAr /Lcw I WAT c/WW IWAT JLG14
1.0 1 • 0 1.0
P1 enoi I 11 U 55 58
bie(2-Oiloroethyl) ether fI 11 0 1 12. UI 10 UI
2 1oropheno1 . I 3.1 UI 59 I 62 I
i.3-Dichlorobenzene U UI 11 UI 10 U
1.4-Dichiorobenrene 4 Sf 34 I 38 I
1.2-Dich iorvbenzene ti U i1 UI 10 UI
2-Methy lpheno l 3.1 UI 11 U 10 Uf
2.2-o ,cybie(i- loropropane U UI 11 UI 10 UI
4-Mathyiphenol. 11 UI 11. UI 10 UI
N-Nitro3o-di-rt-propylaeu.ne U UI 42 I 45 I
exach1orcethane ii 01 11 UI 10 UI
Nitrobenzene Li Of 11 UI 10 UI
Isophorone Li U 11 UI 10 UI
2-Nitrophenol U Of 11 Of 10 U
2.4-Dimethy lphenol ii. o ii UI 10 UI
bis(2-Qtloroethoxy) methane ii UI 11 Uf 10 UI
2.4 -Dich loropheno l U UI ii UI 10 UI
i .2 .4-Trich lorcbenxenc 11 UI 37 I 39 I
Naphtha lene 3.3. U 11 UI 10 UI
4-Qi loroaittiine I 11 UI 11 UI 10 UI
Hexach1or atadiene I 11 0 11 UI 10 UI
4. 1oro-3-methylphenoL I U 01 70 I 72 I
2-I4ethy ln.aphtha lene I U UI 11 ul 10 UI
Ke ch1orocyc1epentad.iene 11 UI 11 UI 10 UI
2,4 .6-Trich loropheno l ii U 11 UI 10 UI
2.4.S-TriC1tLOropheno l 26 01 27 UI 26 UI
2- 1oronaphtha1ene ii U ii UI 10 UI
2-Nitroaai lthe 26 Uf 27 UI 26 UI
Dieiethy lphtha late 11 Of 11 UI 10 UI
Acenaphthy lene U UI 11 UI 10 UI
2.6-Dinitrotoluene U UI 11 UI 10 UI
3-Nitro&ni lthe . 26 UI 27 UI 26 UI
Acenaphthene I U U 40 I 42 I
2.4-Dinitrophenol 26 UI 27 UI 26 UI
4-Nitrophev .01 26 UI 69 71 I
Dibenzofu a n Li Of 11 UI 10 UI
2.4-DinitrotOluene i of 39 I 41 I
Oiethy lphth.a late 11 UI U UI 10 UI
4- t1orOphenyi-phefly1 ether Li UI U UI 10 UI
Fluorene Li U U UI 10 UI
4-Nitroaniiifle 26 Of 27 UI 26 UI
4 .6-DinitrO-2r thY1PhenO1 26 UI 27 UI 26 UI
N.nir .ro odipheny1a1nine Li UI it UI 10 UI
4-Broe phefly1-pheny1ether U UI ii UI 10 UI
Hexachieroben:efle 11 Of 11 UI 10 UI
Pentacbiorophenoi 26 01 86 I 79 I
Phcnanthrene II U UI 12. UI 10 UI
Mth acena I ii UI U UI 10 UI
Carbazole 11 UI 11 UI 10 UI
t -n-butyiphtha1ate 11 U ii UI 10 UI
Fluoranthefle 11 UI U UI 10 UI
Pyrene 11 UI 43 44 I
Buty lbenzy lphthaiate 11 UI ii UI 10 UI
3 .3-Dichloroben zidlne 11 UI 11 UI 10 DI
nz o(a anchraceno 11 UI ii UI 10 UI
Ciryeene U U i 10 UI
bis(2 -Ethy lhexy l)phtha late 11 UI 11 UI 10
D -n-octy1phtha1ate 11 UI 11 UI 10 UI
Benzo(b)fluoran thene I 1]. UI 11 Uf 10 UI
Benzo(k)fiuoranthefle 3j. o 11 UI 10 UI
BenzoCa)pyrene I 11 UI 12. UI 10 UI
IndenoU.2.3-cdlpYrerte II 13. UI 13. UI 10 UI
I Dibenz(a.hlanthracerte II U UI 11 UI 10 UI
Denzo(g.h.i)peryte n e II 11 Uf 11 UI to u
FIL. W : J4T05.SOG DATE: 03/13/95 TI)C: 13:42 CAERE 2.10 P? E: 3.
Water urUt3 arc reported in u /L..
So 1 urut are reported in ug/Kg.
-------
Int.mnl S tanñards Rapofl
SOC NO: AET OS LABORATORY: nsovaa AWL
CASt NO: 22&9 1 ADfl4CY iNPUT P it t: A 05.OU
INrrRr L STANDARD aITERIA
VOLATILES
Retention Time & Area Count Units
Retencton time
Area count
— — Pr imary — -
Lower tipper
- 0.5 • 0.5
/ 2 • 2
- Eiçanded - -
Lover Upper
0.5 • 0.5
5 2
s 4IvOlaTtLES
Retention Time & Area Count Limits
Retention time
Area count
- - Primary - -
Lover Upper
0.5 • O.S
2 2
- Expanded - .
Lover Upper
- 0.5 • 0.5
f 5• 2
DC-77: The following semivolatile samples have internal standard area
counts that are outside the lower limit of primary criteria.
Hits are qualified 3 and non-detects are qualified ‘03 ’.
AX 07
DL-n-octylphthalate. Bencoib) fluoranthene. Benzo(k) flucranthene, Benzo(alpyrene
todeno (1.2.3-cd) pyrene. Dibent (a • tO anthracene, Benzo (g. h. i i perylene
AHT07RS
Di-n-octylphthalate, Benro ItO f luoranthene, Benzo{k) fluoranthene, Benzo(a)pyrene
tndeng(1,2, 3-cd)pyrene, Dibenz(a.b)anthxacene, Senzotg,h.i)perylene
Filename- Azx:05
Date: 03/06 /95 time: 02*37 CADRE: 2.10
Page 1
-------
Regionj. . ...
ORGANIC REGIONAL DATA ASSESSMENT
CASE NO. 22891 SITE Andrews Road Landfill BarrinRron, CT
LABORATORY ENCO7EC NO OF SAMPLESIMATRJX 15 Soil/S Water
SDG NO. ABTO5 REVIEWER (IF NOT ESD) _ Lockheed/ESAT
SOW NO. OLMO I.9 REVIEWER’S NAME Thomas P. Widera
DPO:ACTION FYI X COMPLETION DATE 2/22/95
DATA ASSESSMENT SUMMARY
VOA BNA PEST OTHER
1. HOLDING TIMES 0 0 NA NA
2. GCIMS TUNE/INSTR. PERFORM. 0 0 NA NA
3. CALIBRATIONS 0’ 0 NA NA
4. BLANKS 02 02 NA NA
5. SURROGATES 0 0 NA NA
6. MATRIX SPIKE/MATRIX SPIKE DUP 0 0 NA NA
7. OTHERQC 0 ____ NA NA
8. INTERNAL STANDARDS 0 0 NA NA
9. COMPOUND IDENTIFICATION 0 0 NA NA
10. SYSTEM PERFORMANCE 0 0 NA NA
11. OVERALL ASSESSMENT 0 0 NA NA
0 Data had no problems or was qualified due to minor problems.
M Data qualified due to major problems.
Z = Data unacceptable.
X = Problems, but do not affect data.
ACTION ITEMS:_________
AREAS OF CONCERN: (Y - Several compounds did not meet calibration criteria. 2 - Low level acetone.
merlr,’lene chloride, 2-butanone, and bis(2-etlr,’lhexyl)yhthalare contamination .
NOTABLE PERFORMANCE:________________________________________________
Reviewer: Thomas P. Widera Date: 2/22/95
-------
VOLATILE AQUEOUS
ANALYSIS
CASE NO: 22891
SOC NO: AHTO5
SITE: ANOREI1S ROAD LANDFILL BARRINGTON,
LABORATORY: RESOURCE ANALYSTS, INC.
CT
SANPLE N SER:
AHT1O
AHT I9
AHT2O
AHT2 I
AH122
‘I.E LOCATION:
EBSS
GW01
G 1J02
GW03
GW04
)RATORY SAMPLE NUNBER:
42161-12
42161-13
4216117
4216114
42161-15
‘LE TYPE:
MATRIX/ANALYSIS:
Equipeent
WATER/LOW
Blank
Routine Seaple
WATER/LOW
Routine Sanpie
WATER/LOW
Routine San te
WATER/LOW
Routine Sarrpte
WATER/LOW
DILUTION FACTOR:
1.0
1.0
1.0
1.0
1.0
DATE SAMPlED:
11/08/94
11/08/94
11/08/94
11/08/94
11/08/94
DATE ANALYZED:
11/18/94
11/18/94
11/18/94
11/18/94
11/18/94
VOA
Chloromethane
10 U
10
U
10 U
10 U
10
U
Bromomethane
10 U
10
U
10 U
10 U
10
U
Vinyl ChLoride
Chtoroethane
10 U
10 U
10
10
U
U
10 U
10 U
10 U
10 U
10
10
U
U
MethyLene Chloride
Acetone
10 U
10 U
10
10
U
U
4 BJ
10 U
10 U
10 U
10
10
U
U
Carbon Oi utfide
10 U
10
U
10 U
10 U
10
U
1 ,1-Oichtoroethene
1,1-Oichtcroethane
1,2-Oichteroethene (total)
Chloroform
10 U
10 U
10 U
10 U
10
10
10
10
U
U
U
U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10
10
10
10
U
U
U
U
1,2-Dichtoroethane
2-Butanone
10 U
33
10
10
U
U
10 U
10 U
10 U
10 U
10
10
U
U
1 ,1,1-Tr lch loroethane
Carbon Tetrachloride
10 U
10 U
10
10
U
U
10 U
10 U
10 U
10 U
10
10
U
U
Bromodichtoromethane
10 U
10
U
10 U
10 U
10
U
1.2-DIchLoropropar e
cis-1 ,3-D ichtoropropene
Trichtoroethene
10 U
10 U
10 U
10
10
10
U
U
U
10 U
10 U
10 U
10 U
10 U
10 U
10
10
10
U
U
U
DibromochLoromethane
10 U
10
U
10 U
10 U
10
U
1 1 ,2-Trichloroethane
Berizene
10 U
10 U
10
10
U
U
10 U
3 J
10 U
10 U
10
10
U
U
trans-1,3-Dichloropropene
Bromoform
10 U
10 U
10
10
U
U
10 U
10 U
10 U
10 U
10
10
U
U
4-Methyt-2-Pentanone
2-Hexanone
10 U
10 U
10
10
U
U
10 U
10 U
10 U
10 U
10
10
U
U
Tetrachtoroethene
10 U
10
U
10 U
10 U
10
U
1 ,1,2,2-TetrachLoroethane
10 U
10
U
10 U
10 U
10
U
icne
10 U
10
U
10 U
10 U
10
U
robenzene
10 U
10
U
19
10 U
10
U
yLbenzene
10 U
10
U
10 U
10 U
10
U
rene
10 U
10
U
10 U
10 U
10
U
(total)
10 U
10
U
10 U
10 U
10
U
FILENAME: AHTO5SDC DATE: 02/17/95 TINE: 09:34 CADRE 2.10
PAGE:
1
Water ntits are reported in ug/L.
Soil w its are reported in ug/Kg.
-------
VOLATILE AOUEWS ANALYSIS
CASE O: 22891 SITE: ANDIEWS ROAD LANDFILL 8ARRINGTON, CT
G NO: AHTOS LABORATORY: RESOJRCE ANALYSTS, INC.
EPA SAMPLE kl O(8ER:
SAMPLE LOCATION:
LABORATORY SAMPLE NUMBER:
SAMPLE TYPE:
MATR IX/ANALYS 1S:
DILUTION FACTOR:
DATE SAMPLED:
DATE ANALYZED:
ANT23
TB -01
42161-19
Trip BLank
WATER/LOW
1.0
11/08/94
11/18/94
AHT25
EBSO
42161-16
EquIpi ent Blank
WATER/LOW
1.0
11/08/94
11/18/94
AHTZ6
£8-GAl
42161-18
Equi nent Blank
WATER/LOW
1.0
11/08/94
11/18/94
AHY5T
26435
42161-20
Routine Saaiple
MATER/LOW
1.0
11/08/94
11/18/94
VGA
ChLoroti thane
8ra u ethane
Vinyt Chloride
Chlorvethane
Nethytene ChLoride
Acetone
Carbon Disutflde
1,1 -Dichtoroethene
1,1-O lchloroethene
1 ,2-Dichloroethene (totaL)
chloroform
1 ,2•Dlchtoroethane
2-Butanone
1 ,1,1 -Trichtoroethane
Carbon Tetrachloride
Bro dich(oromethane
1 ,2-Dich loropropane
cis- 1 ,3-D chtoropropene
Tr lchtoroethene
Oibronoth loromethane
1,1,2-Trichtoroethane
Benzene
trans-1 ,3-D lchLoropropene
Brx form
4•Methyl-2-Pentanone
2-Hexanone
Tetrathloroethene
1 ,1 ,2 ,2•Tetrachtoroethane
Totuene
chLorobenzene
Ethytbenzene
Styrene
Xytene (total)
10 U
10 U
10 U
10 U
4 BJ
10 U
10 U
10 U
10 U
10 U
10 U
10 U
36
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
24
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
ID U
10 U
10 U
10 U
10 U
10 U
10 U
4 8.1
10 U
10 U
10 U
10 U
10 U
10 U
10 U
38
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
¶0 U
10 U
10 U
10 U
10 U
10 U
10 U
10 1?
10 U
10 U
10 U
10 U
10 U
10 U
4 8.1
10 U
10 U
10 U
10 U
10 U
92
10 U
78
10 U
10 U
10 U
10 U
89
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
9 .1
10 U
35
10 U
100
110
FILENAME: AHTOSSDG DATE: 02/17/95 TIME: 09:34 CADRE 2.10 PAGE: 2
Water iaiits are reported in ug/L.
Soil I its are reported in ug/Kg.
-------
VOLATILE SOIL ANALYSIS
CASE NO: 22891 SITE: ANOREWS ROAD LANDFILL BARRINGTON,
SOG NO: AHTO5 LABORATORY: RESOURCE ANALYSTS. INC.
CT
SAMPLE NUMBER:
AHT O S
ANTO6
AHTOT
AHT O8
AHTO9
PLE LOCATION:
SS-O1
SS-02
SS03
SS 04
5 5 -05
ORATORY SAMPLE NUMBER:
42161-1
421612
421613
42161-4
4a1615
PLE TYPE:
ru .RIX/AMALYSIS:
DILUTION FACTOR:
Routine Saa Le
SOIL/LOW
1.0
Routine Sanpte
SOIL/LOW
1.0
Routine
SOIL/LOW
1.0
Sanpie
Routine Sanpte
SOIL/LOW
1.0
Routine Sar te
SOIL/LOW
1.0
DATE SAMPLED:
DATE ANALYZED:
PERCENT MOISTURE:
11/08/94
11/21/94
32
11/08/94
11/21/94
36
11/08/94
11/21/94
30
11/08/94
11/21/94
10
11/08/94
11/21/94
18
VGA
Chtoromethane
15 U
16 U
14 U
10 U
12
U
Brc methane
15 U
16 U
14 U
10 U
12
U
Vinyl ChLoride
Chtoroethane
15 U
15 U
16 U
16 U
14 U
14 U
10 U
10 U
12
12
U
U
Methylene Chloride
Acetone
13 BJ
120
11 Li
28
13 Li
33
8 Li
18
11
23
8.1
Carbon Disutfide
15 U
16 U
14 U
10 U
12
U
1,1-Dichloroethe n e
15 U
16 U
14 U
10 U
12
U
1,1- Oichtoroethane
15 U
16 U
14 U
10 U
12
U
1 2-DichLoroetherie (totaL)
15 U
16 U
14 U
10 U
12
U
ChLoro1orn
15 U
16 U
14 U
10 U
12
U
1,2-Dichtoroethane
15 U
16 U
14 U
10 U
12
U
2sutanane
17
16 I)
14 U
10 U
12
U
1,1,1-Trichtoroethane
15 U
16 U
14 U
10 U
12
U
Carbon Tetrachloride
15 U
16 U
14 U
10 U
12
U
Bronodtchtoromethane
15 U
16 U
14 U
10 U
12
U
1 1 2-Dichloropropane
cis-1,3-Dichtoropropene
Trichloroethene
15 U
15 U
15 U
16 U
16 U
16 U
14 U
14 U
14 U
10 U
10 U
10 U
12
12
12
U
U
U
Dibrm ch(oron thane
15 U
16 U
14 U
10 U
12
U
1 ,1 2-TrichLoroethane
15 U
16 U
16 U
10 U
ia
u
Benzene
15 U
16 U
14 U
10 U
12
U
trans -1 .3-Dichtoropropene
Bromoform
15 U
15 U
16 U
16 U
14 U
14 U
10 U
10 U
ia
12
u
U
4-Methy(-2-Pentanone
15 U
16 U
14 U
10 U
12
U
2-Hexanone
15 U
16 U
14 U
10 U
12
U
Tetrachtoroeth a ne
15 U
16 U
14 U
10 U
12
U
l .1 .2,2-Tetrachtoroethane
15 U
16 U
14 U
10 U
12
U
Luene
15 U
16 U
14 U
10 U
12
U
orobenzene
15 U
16 U
14 U
10 U
12
U
iytbenzene
15 U
16 U
14 U
10 U
12
U
/rene
15 U
16 U
14 U
10 U
12
U
Xytene (totaL)
15 U
16 U
14 U
10 U
12
U
FILENAME: AHTO5.SVG DATE: 02/17/95 TIME: 09:32 CADRE 2.10
PAGE:
1
Water u its are reported In ug/%..
Soil u its are reported in ug/Kg.
-------
VOLATILE SOIL ANALYSIS
CASE NO: 22891 SITE: ANDREjJS RoAn LAjIOFILL BARRINGTON, CT
— SOG HO: AIITO5 LABORATORY: RESQJRCE ANALYSTS, INC.
EPA SAMPLE NUMBER:
SAMPLE LOCATION:
LABORATORY SAMPLE NUMBER:
SAMPLE TYPE:
MATRIX/ANALYSIS:
DILUTION FACTOR:
DATE SAMPLED:
DATE ANALYZED:
PERCENT MOISTURE:
AHT I1
SO-Ol
421616
Routine Sarrple
SOIL/LOW
1.0
11/08194
11/21/94
32
AHT12
S 002
42t61 7
Routine Safple
SOIL/LOW
1.0
11/08/94
11/21/94
14
AHT13
S003
421618
Routine Su te
5011/LOW
1.0
11/08/94
11/21/94
48
AHTI4
WO4
42161-9
Routine Sanple
SOIL/LOW
1.0
11/08/94
11/21/94
28
AHT I S
So .05
42 1611 0
Routine Sarple
SOIL/LOW
1.0
11/08/94
11/21/94
22
VOA
cMoromethane
Oron nethane
VinyL thloride
Chtoroethane
Methy ene ChLoride
Acetone
Carbon DisuUfde
1,1-D ich taroothene
1 ,1’OichLoroethane
1 2-DlchLoroethene (total)
C hLoroforn
1 Z-O chLoroethane
2-Butanone
1 1 ,1 -TrichLoroethane
Carbon TetrachLor de
Bromodfthloromethane
1(2-Dichtoropropane
cis-1 ,3-OichLorcpropene
Trichtoroethene
DibrcmochLoronothane
1 1,2 -TrichLoroethane
Benzene
trana -1,3-Dichlorcpropene
8r fona
4-Methyt-2-Pentanone
2-Hexanone
Tetrachloroethene
1 1,2,2 -retrach1oroethane
Totuene
CMorobenzene
Ethytbenzene
Styrene
XyLene (total)
16 U
16 U
16 U
16 U
15 84
47
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
16 U
11 U
11 U
11 U
11 U
9 BJ
23
11 U
11 U
11 U
11 (1
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
19 U
19 U
19 U
19 U
15 8.1
59
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
19 U
21
19 U
19 U
19 U
13 U
13 U
13 U
13 U
12 84
14
13 U
13 U
13 U
13 Ii
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
13 U
12 U
12 U
12 U
12 U
11 84
14
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
12 U
FILENAME: AHTOS.SDG DATE: 02/17(95 TIME: 09:32 CADRE 2.10 PAGE: 2
Water iwiits are re rted in ug/L.
Soil units are reported In ug/K9.
-------
VOLATILE
SOIL ANALYSIS
CASE NO: 22891
SITE: ANDREWS ROAD LANDFILL
BARRINGTON,
CT
SDG NO: AHTO5
LABORATORY: RESWRCE ANALYSTS, INC.
EPA SAMPLE NLD48ER:
AHT16
PLE LOCATION:
S0 06
ORATORY SAIIPLE NLP4BER:
4216111
LPLE TYPE:
Routine
Swt ,te
._..RIX/ANALYSIS:
SOIL/LOW
DILUTION FACTOR:
1.0
DATE SAMPLED:
11/08/94
DATE ANALYZED:
11/21/94
PERCENT MOISTURE:
19
-
VQA
Chtoromethane
12 U
Bromomethane
12 U
Vinyl ChLoride
Ch loroethane
12 U
12 U
Methytene ChLoride
Acetone
11 BJ
12 U
Carbon Disulfide
12 U
1 ,1-OfchLoroethene
12 U
1 ,1-DhchLoroethane
12 U
1,2DichLoroechene (totaL)
12 U
ChLoroform
12 U
1 ,2-D lchtoroethane
12 U
2-Sutanone
12 U
1,1,1-Tr ichtoroethane
12 U
Carbon Tetrachloride
12 U
8ror dich(oromethane
12 U
1 ZDichloropropane
cs-1 ,3-Dich toropropene
TrichLoroethene
12 U
12 U
12 U
•
Oibromochtor o methane
12 U
1 ,1 ,2-Trichtoroethane
12 U
Benzene
12 U
tran -1,3-DhchLoropropene
Bromoforte
12 U
12 U
4-Nethyt-2-Pentanone
12 U
2-Nexanone
12 U
Tetrachtoroethene
12 U
l,1.2,2-TetrachLoroethane
12 U
uene
12 U
orobenzene
‘Lbenzene
12 U
12 U
rene
12 U
Xytene (total)
12 U
FILENAME; AHTOS.SDG DATE: 02/17/95 TIME: 09:32 CADRE
2.10
PAGE:
3
hater a its are reported in ugh.
Soil wtits are reported in ug/Kg.
-------
EPA SAMPLE I UM6ER:
AHT I O
SAIIPLE LOCATION:
EBSS
LABORATORY SAMPLE NUMBER:
421549
SAJ4PLE TYPE:
Equipi ertc
BLank
MATRZX/AI IALYS IS:
WATER/LOW
DILUTION FACTOR:
1.0
DATE SAMPLED:
11/08/94
DATE EXTRACTED:
11/14/94
DATE ANALYZED:
11/22/Vt.
SEMIVOL.ATILE AQUEOUS ANALYSIS
CASE NO: 22891 SITE: ANDREIJS ROAD LANDFILL BARRINGTON, CT
SOC NO: AHTC5 LABORATORY: RESOURCE ANALYSTS, INC.
AHT19
Ow-al
42154-10
Routine Saapte
WATER/LOW
1.0
11/08194
11/14/94
11/22194
ANT Z O
Gu-02
42154-11
Routine Sanpte
WATER/LOW
1.0
11(08/94
11/14/94
11(22/94
AHT21
GV-03
42154-12
Routine Sairpte
WATER/LOW
1.0
11/08(94
11/14/94
11/22/94
AHT2Z
0W 04
42154-13
RoutIne Sarpte
WATER/LOW
1.0
11/08/94
11/14/94
11/22/94
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
Li
U
U
U
U
U
U
U
U
U
E l lA
Phenot
bis(2 -Chtoroethyt) ether
2-ChtoraØienot
1,3 -Dichtorobenzene
l4-Dichtorobenzene
1,2 -Dichtorobenzene
2l1ethyLpheno t
2,2’-oxybis( l-chtoropropane
4-Methy tplienot
N-Nitroso -di-n-propy lamine
HexechLoroethane
Ni trobenzene
I sophororie
2 -NitrcphenoL
2,4-Oirnethy tphenot
bis(2-Chtoroethoxy) methane
2,4-O lchtoropflenoL
I ,2 ,4-Trichtorobenzene
NaphthaLene
4 -Chtoroanit ine
Hexachtorob.itadiene
4-ChLoro-3 rnethyLplienoL
2-Methy1na theLene
Hexachi orocyct opentadi ene
2,4,6-Trich torcphenoL
2 ,4,5-TrichtoroØieno(
2-Ch tcronaphchatene
2-Ilitroanl Line
Dimethytphthatate
Acenaphthytene
2,6-Dinitrototuene
3-Nitroanit Inc
Acenaph thene
2,4-Dlnitraphenot
4-Nitrophenot
Di benzofuran
2 4-Dinitratotuene
D ethytphth Late
4-ChLoroplienyt-phenyL ether
Flucrene
4-Nitroanit In c
4 ,6-Dini tro-Z-methytphenol
N-ni tro odiphenyLamine
4-Brai phenyt -phenytether
Hexachtorobenzene
Pentach LorophenoL
Phenanthrene
Anthracenc
Carbazot e
Of -n-butytphtha Late
Ft uoranthene
Pyrene
ButytbenzyLphthaLate
3•3’ -DichLorobenzidine
Benzo(a) arithracene
Chrysene
bis(2-Ethylhexyl )phtha(ate
Di -n-octytphthalate
Benzo(b)f tuoronthene
BenzoCk)ftuaranthene
Benzo(a)pyrene
IndenoCi ,2 .3-cd pyrene
Dibenz(a ,h)anthracene
Benzo(g.t1, I )perylene
ID
ID
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
25
10
26
10
10
10
26
10
26
26
10
10
10
10
10
26
26
10
10
10
26
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
25 U
10 U
25 U
10 U
10 U
10 U
25 U
10 U
25 U
25 U
10 U
10 U
10 U
10 U
10 U
25 U
25 U
10 U
10 U
10 U
25U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 LI
10 U
10 U
10 U
11
11
11
11
4
11
11
1 1
11
11
11
11
11
11
11
p
11
11
11
11
26
11
26
11
11
11
26
11
26
26
11
11
11
11
11
26
26
11
11
11
26
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
11
U
U
U
U
J
U
U
U
U
U
U
LI
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
U
LI
U
U
U
U
U
U
10 U
10 U
IC U
10 U
Ia U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 LI
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
26 U
10 U
26 U
10 U
10 U
10 U
26 U
10 U
26 U
26 U
10 U
10 U
10 U
10 U
10 U
26 U
26 U
10 U
10 U
10 U
26 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
10 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
Ii U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
26 U
11 U
26 U
11 U
ii U
11 U
26 U
11 U
26 U
26 U
11 U
11 U
11 U
11 U
11 U
26 U
26 U
11 U
11 U
11 U
26 U
11 U
11 U
11 U
11 U
It U
11 U
11 U
11 U
11 U
11 U
11 U
11 U
Ii U
11 U
II U
11 U
11 U
11 U
FILENAME: AHTO5.SDG DATE: 02/17195 TINE: 09:40 CADRE 2.10 PACE: 1
Water units are reported in ugh.
SoiL units are reported in ug/Kg.
-------
CASE NC: 22891
SDG NO: ANTOS
SEMI VOLATILE
AQUEOUS ANALYSIS
SITE: ANDREWS ROAD LANDFILL EARRIN TON, CT
LABORATORY: RESOURCE ANALYSTS 1 INC.
DA SAMPLE NUMBER:
AHT25
AHT26
NPLE tOCATION:
EB-SO
ES-GAl
BORATORT SAMPLE
NUMBER:
42154-14
42154-15
NPLE TYPE:
Equip7lent
Stank
Equlpnent
Stank
. .TRIX/AMALTSIS:
I1ATERILOW
VATER/LOW
DILUTION FACTOR:
1.0
1 .0
DATE SAMPLED:
11/08/94
11/08/94
DATE EXTRACTED:
11/16/94
11116/94
DATE ANALYZED:
11/22/94
11/22/94
10 U 10 U
bis(2-ChLoroethyL) ether 10 U 10 U
Z-chLoro enoL 10 U 10 U
1,3 -Dichtcrobenzene 10 U 10 U
1 4-DIchtorobenzene 10 U 10 U
1 2-Dichtorobenzene 10 U 10 U
2-Nethytphenot 10 U 10 U
2.2’-ozybis( l-ChLoropropane 10 U 10 U
4-Nethytplienot 10 U Ia u
N-Nttrc o-di-n-propytamine 10 U 10 U
Hexachtoroethane 10 U 10 U
Nitrobenzene 10 U 10 U
IsoØ ,orone 10 U 10 U
2-Nitrcphenot 10 U 10 U
2 .4-DfnethyLphenot 10 U 10 U
bia(2-Chtoroethoxy) methane 10 U 10 U
2,4-Dfchtoroplienut 10 U 10 U
1,2 1 4-Tr lchtorobenzene 10 U 10 U
Waphthatene 10 U 10 U
4-Chioroanitlrte 10 U 10 U
HexachIoro itadIene 10 U 10 U
4-Ch toro-3-methy lphenot 10 U 10 U
2-MethyLr apl thaLene 10 U 10 U
Hexachtorocyctcpentadlene 10 U 10 U
2.4 6-Trichtorophenot 10 U 10 U
24,5-Tr lch torophenot 26 U 28 U
2-thtoronaphtha tene 10 U 10 U
2-NitroaniLine 26 U 26 U
thyLpl thatate 10 U 10 U
napMhyLene 10 U 10 U
-D lnltrotoLuene 10 U 10 U
I ltrcan lL lne 26 U 26 U
Acenapi thene 10 U 10 U
2.4-D nitropl enot 26 U 26 U
4-Nitrcphenot 26 U 26 U
Dibentofuran 10 U 10 U
2,4-DIn ltrototuene 10 U 10 U
DIethy phthaLate 10 U 10 U
4-Chtorophenyt-phenyt ether 10 U 10 U
F tuorene 10 U 10 U
4-Nitroan itlne 26 U 26 U
4,6-Oin ltro-2 -methytphenot 26 U 26 U
N-n ltrosodiphenytam lre 10 U 10 U
4-BromopllenyL-phenytether 10 U 10 U
KexacNtorobenzene 10 U 10 U
PentacblorophenoL 26 U 26 U
Phenonthrene 10 U 10 U
Arithracene 10 U 10 U
CarbaLoLe 10 U 10 U
Dt-n-buty tphthatate 10 U 10 U
FLuoranthene 10 U IC U
Pyrene 10 U 10 U
Butytbenzytphthatate 10 U 10 U
3,3’-Dichtorobenzidine 10 U 10 U
Benzo(a)anrhracene 10 U 10 U
Chryserie 10 U 10 U
bis(2-Ethy thexyt)phthatate 10 U 10 U
Di-n-octytphthalate 10 U 10 U
Benzo(b)ftuoranthene 10 U 10 U
Benzo(k)ftuoranthene 10 U 10 U
Benzo(a)pyrene 10 U 10 U
Indeno(1.2.3-cd)pyrene 10 U 10 U
Dibenz(a,h)arithracene 10 U 10 U
Benzocg 4 h,i)pery te r te 10 U 10 U
NAJIE: AHTDS.SDG DATE: 02/17/95 TINE: 09:40 CADRE 2.10 PAGE: 2
er unite are reported In ug/L.
L units are reported in ug/Kg.
-------
SEMIVOLATILE SOIL ANALYSIS
CASE NO: 22891 SITE: ANDREUS ROAD LANDFILL BARRINGTON, CT
G NO: Afl105 L.ABORAIORY: RESWR ANALYSTS, INC.
EPA SAMPLE NUMBER:
SAMPLE LOCATION:
U.BORATCRY SAMPLE NUMBER:
SAMPLE TYPE:
MATRIX/ANAITSIS:
DILUTION FACTOR:
DATE SAMPLED:
DATE EXTRACTED:
DATE ANALYZED:
PERCENT MOISTURE:
AIITO5
5 5-01
42154-1
Routine Sa pLe
SOIL/LOW
1.0
11/8/96
11/16/94
11/23/94
30
AHTO6
$S 02
42154-2
Routine Saaple
SOIL/LOW
1.0
1118/94
11/16194
11)23/94
29
ANTO?
S 5 03
42172-1
Routine 5az Le
SOIL/LOW
1.0
1118/94
11/16/94
11/23/%
33
ANTO8
SS 04
42172 -2
Routine Saaçte
SOIL/LOW
1.0
11(8194
11(16/94
11/23)94
9
AHTO9
5 5-05
42154-3
Routine SapLe
S OIL/t.OU
1.0
11/8/94
11/16(94
11/23/94
16
ENA
PhenoL 470 U 460 U 490 U 360 U 390 U
bic(2-thloroethyt) ether 470 U 460 U 490 U 360 U 390 U
2-CMorcphenoL 470 U 460 U 490 U 360 U 390 U
1,3-D lchtorcbenzene 470 Li 460 U 490 U 360 U 390 U
1,6 -Dich lorobenzene 470 U 460 U 490 U 360 U 390 U
1 ,2-Dichtorobenzerte 470 U 460 U 490 U 360 LI 390 U
2Methytphenot 470 U 460 U 490 U 360 U 390 U
2,2 ’-oxybis( l-Chloroprcpane 470 U 460 U 490 U 360 U 390 U
4-Methytpflenot 473 U 460 U 490 U 360 U 390 U
N-Nltroso-dI-n-propytanline 470 U 460 U 490 U 360 U 390 U
HexachLoroetharte 470 U 460 U 490 U 360 U 390 U
N Itrobeniei e 673 U 460 U 490 U 360 U 390 U
Isophorone 470 U 460 U 490 U 360 U 390 U
2-Ni trophenot 470 U 460 U 490 U 360 U 390 U
2 1 6-Oimethytphenot 470 U 460 U 490 U 368 U 390 U
b :s(2-Chtoroethozy) methane 470 U 460 U 490 U 360 U 390 U
2,’.- O ichtorcphenot 470 U 460 U 490 U 360 U 390 U
1 ,2,4-Trichlorobenzene 470 U 460 U 490 U 360 U 390 U
Naphthatene 470 U 460 U 490 U 360 U 390 U
4-ChLoroanitine 470 Li 460 U 490 U 360 U 390 U
Ke, achLorobutadiene 470 U 460 U 490 U 360 U 390 U
4-Chloro-3-methy lphenot 470 U 660 U 490 U 360 U 390 U
2-MethylnaplithaLene 470 U 460 U 490 U 360 U 390 U
Hexachtorocyc(opentadfene 470 U 460 U 490 U 360 U 390 U
2.L ,6-Tr lthLoro i*enol 470 U 460 U 490 U 360 U 390 U
2,4,S-Tr ichLoropl ,enoL 1100 U 1100 U 1200 U 880 U 950 U
2-Chtoronaphthatene 470 U 460 U 490 U 360 U 390 U
2-Nltroanitine 1100 U 1100 U 1200 U 880 U 950 U
Dimethytphthatate 470 U 460 U 490 U 360 U 390 U
Acenaplithylene 470 U 460 U 490 U 360 U 390 U
2 ,6-DinitrotoLuene 470 U 460 U 490 U 360 U 390 U
3- Il ltroan lline 1103 U 1100 U 1200 U 880 U 950 U
Acenaphthene 470 U 460 U 490 U 360 U 390 U
2,4-Olnitroplienot 1103 U 1100 U 1200 U 880 U 950 U
4-NitrephenoL 1100 U 1100 U 1200 U 880 U 950 U
Oibe nzofuran 470 U 460 U 490 U 360 U 390 U
2 ,6-Othitrototuene 470 U 460 U 490 U 360 U 390 U
D iethytphthotate 470 U 460 U 490 U 360 U 390 U
6-Chtorophenyk-phenyL ether 470 U 460 U 490 U 360 U 390 U
Fluorene 470 U 460 U 690 U 360 U 390 U
4-M itroan lline 1100 U 1100 U 1200 U 880 U 950 U
4.6- O lnitro-2methytphenoL 1100 U 1100 U 1200 U 880 U 950 U
N-nitrosodipheny(amine 470 U 460 U 490 U 360 U 390 U
4-Bromophenyt-phenyLether 470 U 460 U 490 U 360 U 390 U
HexachLorobenzene 470 U 460 U 690 U 360 U 390 U
Pentachtorophenot 1100 U 1100 U ¶200 U 880 U 950 U
Phenanthrene 470 U 460 U 490 U 220 J 390 U
Anthracene 470 U 460 U 490 U 360 U 390 U
Carbazote 470 U 460 U 490 U 360 U 390 U
DI-n-buty(p*ithatate 470 U 460 U 490 U 360 U 390 U
Ftuoranthene 470 U 460 U 490 U 320 J 390 U
Pyrene 470 U 460 U 490 U 270 J 390 U
Buty lben zy lphthotate 470 U 460 U 490 U 360 U 390 U
3 ,3’-D chLorobenzidIne 470 U 460 U 490 U 360 U 390 U
BcnzoCa)anthra cene 470 U 460 U 490 U 160 J 390 U
Chrysene 470 U 460 U 490 U 170 J 390 U
bisC2-Ethythe yL)phthaLate 470 U 460 U 490 U 360 U 390 U
Di.n-octytphthatate 470 U 463 U 490 U 360 U 390 Ii
Benzo(b)ftu orafltherle 470 U 460 U 490 U 150 J 390 U
Benzo(k)ftuoranthefle 470 U 460 U 490 U 160 J 390 U
Benza(a)pyrefle 470 U 460 U 490 U 150 .1 390 U
Indeno(1,2 ,3-cd)p yrene 470 U 460 U 490 U 76 .1 390 U
Dibenz(a.h)anthracefle 470 U 460 U 490 U 360 U 390 U
Benzocg, li ,i)perytene 470 U 460 U 690 U 83 .1 390 U
FILENAME: AHTO5.SDO DATE: 02(17/95 TIME: 09:39 CADRE 2.10 PACE: 1
Water LantS are reported in ug/%..
SoiL t iIts are reported in ug/IC9.
-------
SEMIVOLATILE SOIL ANALYSIS
CASE NO: 22891
500 NO: AHIOS
SITE: ANDREIJS ROAD LANDFILL BARRINGTON, CT
LABORATORY: RESOURCE ANALYSTS, INC.
- SAI4PLE NUMBER:
AHT1I
AHT12
ANTI3
AHTI4
ANTIS
4PLE LOCATION:
0RATORY SAMPLE
PLE TYPE:
rui (RIX/AIJALYSI5:
DILUTION FACTOR:
NUMBER:
50-01
42154-4
Routine Sar Le
SOIL/LOW
1.0
50-02
42154-5
Routine SaITpIe
SOIL/LOW
1.0
50-03
42172-3
Routine
SOIL/MED
1.0
San te
50-04
42154-6
Routine San te
SOIL/LW
1.0
so-os
42154-7
RoutIne Saaçte
SOIL/LOW
1.0
DATE SAMPLED:
DATE EXTRACTED:
DATE ANALYZED:
PERCENT MOISTURE:
11/08/96
11/16/94
11/23/96
37
11/08/94
11/16/94
11/23/94
18
11/08/94
11/16/94
11/23/94
49
11/08196
11/16/94
11/23/94
25
11/08/94
11/16/94
11/23/94
25
BNA
PhenoL 520 U 400 U 20000 U 440 U 640 U
bis(2-Chtoroethyt) ether 520 U 400 U 20000 U 440 U 640 U
2-Chiorophenot 520 U 400 U 20000 U 640 U 440 U
1 3-OichLorobenzene 520 U 400 U 20000 U 440 U 440 U
1 4-Ojch(orobenzene 520 U 400 U 20000 U 440 U 440 U
1,2-Dfchtcrobenzene 520 U 400 U 20000 U 460 U 440 U
2-MethytphenoL 520 U 400 U 20000 U 440 U 440 U
2,2’-oxyDis(l-Chtoropropane 520 U 400 U 20000 U 440 U 640 U
4-MethyLplienot 520 U 400 U 20000 U 440 U 440 U
N-Nitroso-di-n-propytamine 520 U 400 U 20000 U 440 U 440 U
Hexachtoroethane 520 U 400 U 20000 U 440 U 4-40 U
Nitrobenzene 520 U 400 U 20000 U 440 U 440— U
Isophorone 520 U 400 U 20000 U 440 U 440 U
2-Nisrophenot 520 U 400 U 20000 U 440 U 440 U
2 1 4-Dimethytpheno( 520 U 400 U 20000 U 440 U 440 U
bis(2-Chtoroethoxy) methane 520 U 400 U 20000 U 440 U 440 U
2 .4-OichLorophenot 520 U 400 U 20000 U 440 U 440 U
1.2,4-Trichtorobenzene 520 U 400 U 20000 U 440 U 440 U
NaphtheLene 520 U 400 U 20000 U 440 U 440 U
4-Ch toroani(fne 520 U 400 U 20000 U 440 U 440 U
Hexachtorobutadiene 520 U 400 U 20000 U 440 U 640 U
4-Ch(oro-3-methy lpnenct 520 U 400 U 20000 U 440 U 640 U
2-Methytnaphthatene 520 U 400 U 20000 U 440 U 440 U
HexachlorocycLopentadiene 520 U 400 U 20000 U 440 U 640 U
2.4,6-Tr ichtorophenot 520 U 400 U 20000 U 440 U 440 U
2,4,5 -Tr ichtoropheno( 1300 U 970 U 49000 U 1100 U 1100 U
-‘ hLoronaphthaLene 520 U 400 U 20000 U 440 U 440 U
litroanitine 1300 U 970 U 49000 U 1100 U 1100 U
ethyLphthaLate 520 U 400 U 20000 U 440 U 440 U
naphthyLene 120 J 400 U 20000 U 440 U 440 U
_,j-Din ltrototuene 520 U 400 U 20300 U 440 U 440 U
3-Nitrcanitine 1300 U 970 U 49000 U 1100 U 1100 U
Acenaphthene 520 U 400 U 20000 U 440 U 440 U
2,4-Dinitrophenot 1300 U 970 U 49000 U 1100 U 1100 U
4-Nitrophenot 1300 U 970 U 49000 U 1100 U 11O U
Dibenzefuran 520 U 400 U 20000 U 440 U 640 U
2,4-Dinitrototuene 520 U 400 U 20000 U 4-40 U 440 U
Diethytphthatate 520 U 400 U 20000 U 440 U 440 U
4-Chtoropheny(-pheny( ether 520 U 400 U 20000 U 440 U 640 U
Ftuorene 520 U 400 U 20000 U 440 U 440 U
4-N itroanil. Ine 1300 U 970 U 49000 U 1100 U 1100 U
4 ,6-O initro-2-methyLphenot 1300 U 970 U 49000 U 1100 U 1100 U
N-nitrcsodip lieriylamjne 520 U 400 U 20000 U 440 U 440 U
6-Brcxnop henyt-phenytether 520 U 400 U 20000 U 440 U 440 U
Xexachtorobenzene 520 U 400 U 20000 U 440 U 440 U
PentachLorophenol 1300 U 970 U 49000 U 1100 U 1100 U
Phenanthrene 180 J 400 U 20000 U 440 U 640 U
Anthracene 520 U 400 U 20000 U 440 U 440 U
Carbazote 520 U 400 U 20000 U 440 U 640 U
Oi-n-butyLphthatate 520 U 400 U 20000 U 440 U 640 U
Ftuoranthene 470 J 400 U 20000 U 440 U 440 U
Pyrene 460 J 400 U 20000 U 440 U 440 U
ButytbenzyLphthaLate 520 U 400 U 20000 U 440 U 440 U
3,3’-D lchtorobenzidine 520 U 400 U 20000 U 440 U 440 U
Benzo(a)anthracene 200 J 400 U 20000 U 440 U 640 U
Chrysene 330 J 400 U 20000 U 440 U 440 U
bisc2-Ethythexyt)phth atate 520 U 400 U 28000 440 U 440 U
Di-n-octytphthatate 520 U 400 U 20000 U 440 U 4-40 U
Benzo(b)ftuoranthene 370 J 400 U 20000 U 440 U 440 U
Benzo(k)f tuoranthene 350 J 400 U 20000 U 640 U 640 U
Benzo(a)pyrene 260 J 400 U 20000 U 440 U 640 U
Indeno(1,2,3-cd)pyrene 140 J 400 U 20000 U 440 U 640 U
Dibenz(a,h)anthracene 520 U 400 U 20000 U 440 U 640 U
Benzo(g ,h,i)pery lene 130 J 400 U 20000 U 440 U 440 U
NAME: AHTOS.SOG DATE: 02/17/95 TIME: 09:39 CADRE 2.10 PAGE: 2
_er Louts are reported in Ugh.
SoiL units are reported in ug/Kg.
-------
SEMIVOLATILE SOIL ANALYSIS
CASE NO: 22891 SITE: ANDREIJS ROAD LANDFILL BARRINGTON. CT
SOD NO: AHTOS LABORATORY: RESWRCE ANALYSTS, INC.
EPA SAMPLE NUMBER:
SAMPLE LOCATION:
LABORATORY SAMPLE NUMBER:
SAMPLE TYPE:
kATRIX/ANALYSIS:
DILUTION FACTOR:
DATE SAMPLED:
BATE EXTRACTED:
BATE ANALYZED:
PERCENT MOISTURE:
AHT16
50-06
42154-8
Routine San te
SOIL/LO u
1.0
11/08/96
11/16/94
11/23/94
19
•
Phenot 600 U
bis(2-Chloroethyt) ether 600 U
2-Ctitorophenot 400 U
1,3-D lchtorobenzene 600 U
1,4-Ofchtorobenzene 400 U
1,2-D lchLorobenzene 400 U
2-Hethytphenøt 600 U
2 ,2’-oxyb ls( l-ChLoroprepane 400 U
4-Methylphenot 400 U
NNItroso-dIn-propy(a iine 400 U
Nexechtoroethane 400 U
Nltrobcnzene 400 U
Isophorone 400 U
2-Ni trophenot 400 U
2,4-Dimethyt p henot 400 U
bis(2-ChLoroethoxy) methane 600 U
2,4-Dichtorophenot 400 U
1 ,2 ,4-TrichLorobenzene 400 U
Naphthatene 400 U
4-Chtoroanitine 400 U
HexachLorobutadiene 400 U
4-Chtoro -3-methy(phenot 400 U
2-NethyLnaphthatene 600 U
Hexathtorocyctopentad iene 400 U
2 ,4,6-TrichLoroØ enoL 400 U
2,4 ,5-Tr ichtorophenot 980 U
2-thtoronaphthaLene 400 U
2-N itroenitine 980 U
D lmethytplflha(ate 400 U
Acenaphthy tene 400 U
2 ,6-Dinitrototuene 400 U
3-Nitroanitine 980 U
Acenaphthene 400 U
2,4-Dinitrophenot 980 U
4-NitrophenoL 980 U
D lbenzofuran 400 U
2,4-Oln itrototuene 400 U
DiethytphthaLate 400 U
4-ChtorophenyL-pheny( ether 400 U
Ftuorene 400 U
4-Nitroanit ine 980 U
4,6- O initro-2- inethy tphenoL 980 U
N-nitrosod lpheny(amine 400 U
4-Bromophenyt-phenytether 400 U
Nexachtorobenzene 400 U
Pentachtorophenol. 980 U
Phenanthrene 400 U
Anthracene 400 U
Carbazote 400 U
Di-n-butylphthatate 400 U
Ftuoranthene 400 U
Pyrene 400 U
ButyLbenzytphthatate 400 U
3,3’-Dich torobenzidine 400 U
Senzo(a)anthracene 400 U
Chrysene 400 U
bis(2-Ethythexyt)phtha tate 400 U
Ot-n-octy(phthatatc 400 u
Benzo(b)f(uoranthene 600 U
Benzo(k)ftuorar%thefle 400 U
Benzo(a)pyrene 400 U
!ndeno(1,2,3-cd)pyrefle 400 U
Dibenz(a,h)anthracefle 400 U
eenzog,h ,i)perytene 400 U ______________
FILENAME: AHTO5.SDG DATE: 02/17/95 TIME: 09:39 CADRE 2.10 PAGE: 3
Uater units are reported In ug/L.
SoiL units are reported in ug/Kg.
-------
CASE NO: 12891
SOG NO: ANTOS
PESTICIDE/PC8 AQUE( JS ANALYSIS
SITE: ANOREWS ROAD LANDFILL BARRINGTON, CT
LABORATORY: RESOURCE ANALYSTS, INC.
— SAMPLE N.R4BER:
PLE LOCATION:
BORATORY SAMPLE
PLE TYPE:
MTRIX/ANALYSIS:
DILUTION FACTOR:
DATE SAMPLED:
DATE EXTRACTED:
DATE ANALYZED:
NUMBER:
ANTIO
EB-SS
42154-9
Equipnent BLank
WATER!
1.0
11/08/96
11/15/94
12/01/94
AKT19
G’J.O l
42154-10
Routine S8IT9LC
WATER/
1.0
11/08/94
11/15/94
12/02/94
AHT2 O
Gw02
42154-11
Routine SalTp(e
WATER/
1.0
11/08/96
11/15/94
12/02194
ART2 I
GW-03
42154-12
Routine Sa pIe
WATER!
1.0
11/08/94
11/15/94
12/02194
AHT2Z
GW-06
4215413
Routine
WATER/
1.0
11/08/94
11/15/94
12/02/94
Sanpte
PES
atp %a-BHC 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
beta-BHC 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
detta-GHC 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
g ria-BHC (Lir ane) 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
Ileptachlor 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
Atdrin 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
HeptachLor epoxlde 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
EndotuLfan 1 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
Dietdrin 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
4,4’-DOE 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
Endrln 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
Endosutfan II 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
4 ,4’- 00 0 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
EndosuLfan suLfate 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
4 ,4’-ODT 0.10 U 0.10 U 0.10 U 0.10 .ll 0.11 U
Mcthoxychtor 0.50 U 0.51 U 0.50 U 0.50 U 0.53 U
Endrin ketone 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
Endrin aLdehyde 0.10 U 0.10 U 0.10 U 0.10 U 0.11 U
atpha-Chtordane 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
gai -ChLordar%e 0.05 U 0.05 U 0.05 U 0.05 U 0.05 U
Toxaphene 5.0 U 5.1 U 5.0 U 5.0 U 5.3 U
ArocLor-1 016 1.0 U 1.0 U 1.0 U 1.0 U 1.1 U
Aroctor-1221 2.0 U 2.0 U 2.0 U 2.0 U 2.1 U
Aroctor-1232 1.0 U 1.0 U 1.0 U 1.0 U 1.1 U
ArocLcr -1242 1.0 U 1.0 U 1.0 U 1.0 U 1.1 U
ArocLor•1248 1.0 U 1.0 U 1.0 U 1.0 U 1.1 U
ArocLor-1254 1.0 U 1.0 U 1.0 U 1.0 U 1.1 U
ocLor-126O 1.0 U 1.0 U 1.0 U 1.0 U 1.1 U
ENAME: AHTOS.SOG DATE: 02/17/95 TIME: 09:49 CADRE 2.10 PAGE: 1
_ter units are reported in ug/L.
SoiL units are reported in ug/Kg.
-------
PESTICIOEIPCS AQUEQJS ANALYSIS
CASE NO: 22891 SITE: ANDREWS ROAD LANDFILL BARRINGTON 1 CT
- 500 NO: AHTOS LABORATORY: RESWRCE Aw*trsrs, iatc.
EPA SAMPLE NWIBER:
SAMPLE LOCATION:
LABORATORY SAMPLE NLD(BER:
SAMPLE TYPE:
MATRIX/ANALYSIS:
DILUTION FACTOR:
OATE SAMPLED:
DATE EXTRACTED:
- DATE ANALYZED:
AIIT25
EB-SO
4215614
Equfpient Stank
WATERF
1.0
11 i08f94
11 /15/94
12/02/94
PES
at ia-BMC
beta-BHC
del ta-BHC
gwmta—BHC (Lindane)
}Ieptachtor
Atdrfn
Ileptathtor epox lde
Endosutfan I
Dietdrin
4,4’-DDE
E n dr In
Endosutfan II
4 ,4 ’ - C D ]
Endosulfan sulfate
4,4 ’-DDT
Methoxych(or
Endrin ketone
Endrlrr atdeliyde
a lpha-Ch tordanc
gam -ChLordane
Toxaphene
Aroctor-1016
Aroctor- IZZ i
Aroctor-1232
Aroclor-1242
Aroctor-1268
Aroctor-1254
Aroctor-1260
0.05 U
0.05 U
0.05 U
0.05 U
0.05 U
0.05 U
0.05 U
0.05 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.10 U
0.50 U
0.10 U
0.10 U
0.05 0
0.05 U
5 ,0 U
1.0 U
2.0 U
1,0 U
1.0 U
1.0 U
1.0 i i
1.0 U
FILENAME: AKT0S.SOG DATE: 02 /17/95 TIME: 09:49 CADRE 2.10 PAGE: 2
Water units are reported In t ag/I.
SoiL units are reported in tag/Kg.
-------
CASE NO: 22891
SOC NO: AIITO5
PESTICDE/PCB SOIl. ANALYSIS
SITE: ANOREWS ROAD LANDFILL BARRINGTON. CT
LABORATORY: RESOURCE ANALYSTS, INC.
e SAMPLE NUMBER:
AHTC S
AHTO6
AHTO7
AHT08
AHTO9
.MPLE LOCATION:
SS -01
SS-OZ
SS-03
SS-04
5$-OS
8ORAT0RY SAMPLE
NUMBER:
42161-1
42161-2
42161 .3
42161-4
42161-5
UIPLE TYPE:
Routftie
San Le
Routine
Sat7pLe
Routine
S&r9te
Routine San te
Routine
Soaple
riATRIX/ANALYSIS:
SOIL/
SO IL/
SO IL/
SOIL!
5011/
DILUT ICN FACTOR:
1.0
1.0
1.0
l.a
1.0
DATE SAJ4PLEO:
11/08194
11/08/94
11/08/94
11/08/94
11/03/94
DATE EXTRACTED:
11/17/94
11/17/94
11/17/94
11/17/94
11/17/94
DATE ANALYZED:
PERCENT MOISTURE:
11/24/94
30
11/24/94
29
11/24/94
33
11/24/94
9
11/24/94
16
PES
aLpha-SHC 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
beta•BHC 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
deLt.-BNC 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
g me-8HC (Lindarte) 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
Heptachlor 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
ALdrln 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
Heptbchtor epoxide 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
Endosulfon 1 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
DfeLdr in 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
44’O DE 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
Endrin 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
Erdosutfan II 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
4,4’-COD 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
Endosu(fan sulfate 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
4 ,4’-ODT 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
Methoxychtor 24 U 24 U 25 U 18 U 20 U
Endrin ketone 4.7 U 4.6 U 4.9 U 3.6 U 3.9 U
Endrin atdehyde 4,7 U 4.6 U 4.9 U 3.6 U 3.9 U
at ia-Chtcrdane 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
ga ma-C I (ordane 2.4 U 2.4 U 2.5 U 1.8 U 2.0 U
TCXOF*iene 240 U 240 U 250 U 180 Li 200 U
Aroclor -1016 47 U 46 U 49 U 36 U 39 U
Aroctor -122 1 94 U 94 U 99 U 73 U 79 U
ArocLor -1232 47 U 46 U 49 U 36 U 39 U
Aroctor-1242 47 U 46 U 49 U 36 U 39 U
Aroctor -1248 47 U 46 U 49 U 36 U 39 U
£r Lor.1254 47 U 46 U 49 U 24 39 U
octor -126O 47 U 46 U 49 U 36 U 39 U
.EI4AME: ANTO5.SCG DATE: 02j17 /95 TINE: 11:36 CADRE 2.10 PAGE: 1
water u its are reported in u9/L.
SoIL in its are reported in ug/Kg.
-------
CASE HO: 22591
SOG HO: AuTOS
PESTICIDE/PCB SOIL ANALYSIS
SITE: ANDREWS ROAD LANDFILL BARRINGTON, CT
— LABORATORY: RESOURCE ANALYSTS 1 INC.
EPA SAMPLE NL 4BER:
AHT16
PIE LOCATION:
50-06
ORATORY SAMPLE
NUMBER:
42161-11
PIE TYPE:
Routine
Sanpte
• RIX/ANALYSIS:
SOIL!
DILUTION FACTOR:
1.0
DATE SAMPLED:
11/08/94
DATE EXTRACTED:
11/17/94
DATE ANALYZED:
11/24/96
PERCENT MOISTURE:
19
PES
aL a-BHC 2.1 U
beta-BHC 2.1 U
de(ta-BHC 2.1 U
g -BHC (Lindane) 2.1 U
Heptacldor 2.1 U
AIdr in 2.1 U
Heptachior epoxide 2.1 U
Endosutfan 1 2.1 U
D leldrin 4.1 U
4,4’-DDE 4.1 U
Endrin 4.1 U
Endosutfan II 4.1 U
4,4’-DDD 4.1 U
Endosutfan sulfate 4.1 U
4,4’-DDT 4.1 U
Methoxych lor 21 U
Endrin ketone 4.1 U
Endrin atdehyde 4.1 U
aL ia-ChLordane 2.1 U
g t -Chtordane 2.1 U
Toxaphene 210 U
Aroc lor-1016 41 U
Aroc lor-1221 82 U
Aroc lor-1232 41 U
Aroclor-124 2 41 U
Aroctor-1248 41 U
Aroctor-1254 41 U
clor-1260 41 U
NA1lE: AHTO5.SDG DATE: 02/17/95 TIME: 11:36 CADRE 2.10 PAGE: 3
uater tn its are reported in ug/L.
Soil uiits are reported in ug/tg.
-------
ATTACHMENT II
Blank Region I IData Validation Workaheets
-------
Region I Site Name_____________________
Data Review Worksheets Reference Numoer_____________
REGION I REVIEW OF ORGANIC
CONTRACT LABORATORY DATA PACKAGE
The hardcopied(laborazory name) data pack 2ge received at Region I has been
reviewed and the quality assurance and perrorrnance data summarized. The data review included:
Case No. ______ SAS No. _______ Sampling daze(s) _______________
SDG No. Matrix _________ Shipping daze(s) ___________________
No. of Samples Daze s) rec’d by lab ____________________
Traffic Report Nos: _____________________________________
Trip Blank No: __________________________________
Equipment Blank No: __________________________________________________
Field Dup Nos: ________________________________________________
Sow No.__________ requires that specitic analytical work be done and that associated reports be
provided by the laboratory to the regions. EMSL-LV. and SMO. The general criteria u.sea to determine
the perrormance were based on an examination or:
-Data completeness -Matrix spikelMatrix Spike Dup
-Holding Times -Field Duplicates
-GC/MS Tuning -Internal Standard Performance
-Calibrations -Pesticide Instrument Perrormance
-Blanks -Compound Identiticanon
-Surrogate Recoveries -Comoound Quaziutauon
Overazi Comments:
Definitions and Qualifiers:
A - Acceptable data.
J - Approximate data due to quality control criteria.
R - reject data due to quality control data.
U - Compound not detected.
Reviewer: - -______________________________________________________ Date: ________________
-------
Region I
Data Review Workst eetS
I. DATA COXPLETE ZSS
MISSING !NFO MATIOM DATE LAB CONThCTED DATE REC’D
Reviewer: ___________ Date:
-------
Region I
Data Review Worksheets
II. HOLDING TIMES
Complete table for all samples and circle the fractions which are
not within criteria.
SwçIo
ID
Due
Sampled
Data
ASIIIYLCd
(VOA)
BNA
PE S’r/pcn
Due
£mid ed
i
Data Data
Analyzed Extziued
Data
yze
I
I
I..
I
Unpreserved: Aromatic within 7 days. non-aromatic within [ 4 days oi sample
collection.
Preserved: Both within 14 days of sample collection.
Soils: Both within 14 days oi sample collection.
B 4A & PEST Extracted within 7 days. analyzed within 40 days of extraction for waters
and soils.
ACTION: 1. If holding times are exceeded. all positive results are estimated (1) anu all non-detects
are estimated (113).
2. If holding times are grossly exceeded, the reviewer may determine u’iaz non-detects
are unusable.
VOA
-------
Region I
Data Review Worksheets
III. GC/XS T iI ZG
The DFTPP perfornance results were reviewed and found to
be within the specified criteria.
If no, samples affected: _____________________________
The BFB performance results were reviewed and found to be
within the specified criteria.
If no, samples affected: _____________________________
If mass calibration is in error, refer to the Reaional Guidelines
for expanded criteria. If necessary, qualify all assoc:atad data
as unusable (R).
Reviewer: DATE:
-------
Region I
DaLI Review Worksheeu
IV A. VOLATILE CALIBRATION VERIFICATION
Data of lniual Calibranon
Dates) of Coaunuing Calibrznocs:
In.suatmcnt ID:
Maxnv Level:
DATE CRITERIA OUT COMPOUND ( VALTJEI
RF. %RSD,RF. %D
Samples Arf :
Samples Aff ted:
Samples Affected
Samples Affecsed:
Samptes Atfecied:
Samples Affected:
Sampies Atfected:
Samptes Affected:
Sampies Affected:
I. All RFs. and RF’s must be> 0.05
2. All %RSDs must be < 30.
3. All%Dsmustbe<25.
ACTION:
I. If any compound ha.s an initial R.For a conunuing RF of < 0.05:
a. Flag positive results for that compound as estimated (I).
b. Flag eon-detects for that compound as unusable (R).
2. Ifanvcoxxipoundhasa%RSD> 30ora%D>25:
a. Flag positive results for that compound as estimated (J .
b. FlaQ nondetects for that compound as esuma”4 (Ui) if the %RSD or %D is> 50.
A separate worksheet should be tilled out for each initial curve.
Reviewer: - - _______ Date:__________
-------
Regton!
DaL* Review Wcthh
IV 8. SEMIVOL.ATILE CALLBRATION VERIFICATION
Dazc of fl iüaI Ca1ibrzucu
D s) 01 Coocwwng CaI bnuons
Iasirumaii ID:
DATE CRITERIAJ)UT COMPOUND ( YALUE )
RF, %RSD.RF. %D
Samplea Atf ted:
Sa les Atfuted:
Samplea Alf ted:
Saxnplea Atf ted:
Samples Atf ed:
Sampi Atfected:
Sampies Mf ted:
Sampies Afected:
Samptes Alt ectcd:
I. All RF’s. asd RF’ must be> 0.05
2. All %RSD’s must be < 30.
3. .AJ1%D’s inuscbe 30 or a %D > 25:
a. Flag positive results for that compound as e5tim21 d (i).
b. F1a nocdet ts for that concund as est irn (W i(the %RSD or %D is > 50.
A separate worKsheet should be tilled out tor each in.iual curve.
Reviewer
-------
Regton I
Data Review Worksheet
V A. BLANK ANALYSIS RESULTS (Sections 1 & 2’)
List the C0n12mtnatiOfl in the blanks below Level:_______
1. Laboratory Blanks
DATE LAB ID FRACTION! COMPOUND CONCENTRATIO
MATRIX
Equipment and Trip Blanks
DATE TR FRACTION! COMPOUND CONCENTRATION’
MATRIX UNITS
A seDarare worksheet should be used for tow and medium level blanks.
Reviewer:_______________________ Dare:___________
-------
Region I
Data Review Worksheet
V B. BLANK ANALYSIS RESULTS (Section 3
3. Blank Actions
Action leveis should be based upon the highest concentration oi conr2mimlnr determined in any blank.
The action level for samples which have been concentrated or diluted should be multiplied by the
concentration/dilution factor. No positive sample result should be reported unless the concentration of
the compound in the sample exceeds the action level of lOX the amount itt the blank for the common
cont2mIrt nt . or 5X the amount for any other compound. Specific actions are as follows:
1. The concentration is less than the CRQL, report the CRQL qualified with a U.
2. The concentration is greater than the CRQL. but less than the action level, report the
concentration found with a U.
3. ‘the concentration is greater than the action level, report the concentration unqualified.
For examples refer to the Regional Guidelines.
C xnmo conr2min2n : Methylene chloride. Acetone. 2-Butanone. Toluene. and Phthalates.
LEVEL:__________
COMPOUND MAXIMUM CO 4C.I ACTTON LEVEL,’ CR01,.
UNITS UNITS
A separate worksheet should be tilled our for low and medium level blanks.
Reviewer:______________________ Date:___________
-------
egioa I
Data Review Workaheez
vi. SURROGATE SPIKE RECOVERIES
List the percent recoveries which do not meet the crzteria for surrogate recovery.
Matrix:__________
VOA ACTD PEST’
TR #‘5 IQJ j Z lEff DBC
QCLirnits — — — — — — —
to to to to to to to to to to
Surro are Actions: Advisory oniy
PERCENT RECOVERY
< 10% 10%-CRR > CRR
Positive sample results I I I
Non-detected results R UI A
CRR = Conrract Required Recovery Range.
Surrogate acuon should be açplied if:
1. At least two surrogates in a B/N or Acid fraction or one surrogate in the VOA fraction are out or the
specified CRR. but have recoveries which are > 10%.
Any one surrogate in a fraction shows < 10% recovery.
Reviewer:________________________ Date: ____________
-------
PERCENT RECOVERY
< tO% IO%.CRR CRR
.1 .1 i
R A A
2. If any compound does not meet the RPD criteria. flag positive results for that compound as
eaumated U).
A separate worksheet should be used for each MS/MSD pair.
Region I
Data Review Worksheet
VrI A. MATRIX SPIKE/MATRIX SPIKE DUPUCATE
L. MazrL SpikesMarrix Spike Duplicate Recoveri and Precision
TR Nos._ L vei:__________
Ust the percent recoveries and RPD’s of compounds which did not me the
FRACTION COMPOUND REC/
MSCRMSD
Ma ix:______
criteria stated on Form 3.
OCJJMITS
‘QUALIFICATION IS LIMITED TO THE UNSPIKED SAMPLE ONLY’
1. If any compound does not meet the Contract Required Recovery Range (CRR) follow the actions
stated below:
Positive Sample Results
Non-detected Results
Reviewer:
Date:
-------
Region I
Data Review Work he
VII B. MATRIX SPIKEIMATRIX SPIKE DUPLICATE
3. Matrix SpikeiMaxnx Spike Duplicate- Unspiked Compounds
TR Nos.____________________
List the concentrations of the unspiked compounds and determine the percent RSD’s of the unspiked
sample, matrix spike 1 and matrix spike duplicate. No limits have b n developed for the RSD vaIu of
the unspiked compounds.
ELACT ON COMPOUND SAMPLE.MS..MSD CONC ° RSD
The reviewer must use prof sional judgernent to determine if there is a need to qualify any of the
unspiked compounds in the sample.
A separate worksheet should be tilled out for each matrix spikeimatrix spike duplicate.
Reviewer:_______________________ Date:___________
-------
Region L
Data Review Worksheet
VU!. FIF1I ) DUPLICATE PRECISION
Sample TR No. Duplicate TR No.___________ Matria:________
List the concen ations of the mpountc which did not meet the following RPD criceria
I. An RID of <30% for waxer duplicates.
2. An RPDof <50% for soils.
SAMPLE DUPLICATE
FRACTION COMPOUND CONC CONC
ACTIONS:
I. If the results of any comoounds do not meet the RPD criteria. flag the positive results for that
compound as estimated.
. f one value is nondetected. aiid one is above the CRQL:
a. Flag the positive resuLt as estimated (J).
b. Flag the non-detect as estimated (U I).
QTJALIFTERS APPLY TO THE DUPLICATE PAIR ONLY
NOTE: Professional judgement may be used to qualify au samples of a similar matrix.
A separate worksheet should be tilled out for each duplicate pair.
Reviewer: Date:
-------
Region I
Data Review Worksheet
IX. Ir TERNAL STANDARD PERFORMANCE
List the internal sr i i rd areas of samples which did not meet criteria of 4 100% or -50% of the internal
standard area in the associated continuing calibration standard.
RT OR
SAMPLE ID DATE IS 0111 IS AREA ACt±.1’TABLERANG ACTION
ACTION:
1. If an associated area count is outside the criteria -50% or + 100% of the associated standard:
a. Positive results for compounds quantitated using that IS are ilagged as estimated (J) for that
sample traction.
b. Non-detects for compounds quantitared using that IS are tlagged as estimated (US) for that
sample traction.
. If extremely low area counts are reported, or if performance exhibits a major dropotf. then
a severe loss at sensiüviw is indicated. Non-detects should then be dagged as unusable ER).
2. 11 an IS retention time varies by more than 30 seconds, the chromatography pmriie for that sample
must be examined io determine if any false positives or negatives exist. For shifts of a large
magnitude. the reviewer may consider partial or total rejection oi the data ror that sanapie fraction.
Reviewer:_____________________ Date:___________
-------
Region
Daza Review Worktheet
X I I. SAMPLE QUANTITATION
fo the space below, please show a mini utn of one sample calculation per fraction:
VO :
BNA:
PEST/PCB :
Reviewer:______________________ Date:___________
-------
Region____
ORGANIC REGIONAL DATA ASSESSMENT
CASE NO.____________________ SITE________________________________
LABORATORY________________ N0OF SAMPLESIMATR1X________________
SOC NO.____________________ REVIEWER (IF NOT ESD)__________________
SOW NO.___________________ REVIEWER’S NAME____________________
DPO:ACTION FYI________ COMPLETION DATE___________________
DATA ASSESSMENT S JMMARY
VOA BNA PEST OTHER
1. HOLD [ NG TIMES
CC/MS TUNE!tNSTR. PERFORM.
3. CALIBRATIONS
4. BLANKS
5. SURROGATES
6. MATRIX SPIKEIMATRIX SPIKE DUP
7. OTHERQC
8. INTERNAL STANDARDS
9. COMPOUND IDENTIFICATION
10. SYSTEM PERFORMANCE
11. OVERALL ASSESSM ENT
0 - Osia hid o probMnia or wes qualiüsd due io mu proClcma.
M — Di i. . qiuiifi.d due o misor proolemi.
Z — Diii unmcccp ao1o.
X Pn,bk u. bui do nd .l(cct diii.
ACTION ITEMS
AREAS OF CONCERN:
NOTABLE PERFORMANCE:__________________________________________
Reviewer:___________________ Date:_________
-------
ATTACHMENT III
Manual Review NeceaBary to Complete a Tier II Data Validation
-------
SUMMARY OF CADRE DATA REVIEW - REQUIRED MANUAL REVIEW NECESSARY TO COMPLETE A REGION I TIER II DATA
VALIDATION
QC CRITERIA ]
DATA
COMPLETENESS
REVIEW PERFORMED BY CADRE
REQUIRED MANUAL REVIEW
• CADRE lists any errors or omissions which were
de ccted in the electronic deliverable. These errors arc
corrected prior to data review,
• CADRE does not delect errors or omissions in the raw
data.
• The Complete SDG File (CSF) form must be completed and
signed by the rcvicwer. All supporting documentation must be
present in the data package. The reviewer must request from
the laboratory any data missing from the data package (For
cAamptc if a hardcopy Form us missing). The Region I Data
Completeness Worksheet must be completed and included in
the Data Va1ida ion Report along with any records of
communication.
• The CADRE Data Review Inventory Sheet must be
completed and signed by the reviewer. The reviewer must
request from the EPA Data Validation Chemist any information
missing from the CADRE report sent by ESAT. The CADRE
Data Review Inventory Sheet must be included in the Data
Validation Report.
HOLDING TIMES
• CADRE reviews holding times for waters and soils as
per Region I guidelincs.
• If CADRE detects no errors, no further manual review is
required.
• Manual review is required if CADRE reports any errors
during data review. Required review is stated in Section III of
Guidance Document.
PERCENT SOLID
• CADRE evaluates percent solid content as per Region
1 Guidelines,
• If CADRE detects no errors, no funher manual review is
required.
• Manual review is required if CADRE reports arty errors
during data review. Required review is stated in Section Ill of
Guidance Document.
-------
SUMMARY OF CADRE DATA REVIEW - REQUIRED MANUAL REVIEW NECESSARY TO COMPLETE A REGION I TIER II DATA
VALIDATION
QC CRITERIA
REVIEW PERFORMED BY CADRE
REQUIRED MANUAL REVIEW
GC/MS TUNING
• CADRE evaluates GCIMS tunes based on current
Region I guidelines,
• If CADRE detects no errors, no further manual review is
required.
• Manual review is required if CADRE reports any errors
during data review, Required review is stated in Section III of
Guidance Document.
CALIBRATIONS
• CADRE reviews calibration criteria based on current
Region I Guidelines,
• If CADRE detects no errors, no further manual review is
required.
• Manual review is required if CADRE reports any errors
during data review. Required review is stated in Section III of
Guidance Document.
BLANKS
• CADRE reviews and qualifies results for laboratory
blanks based on current Region I guidelines,
• CADRE capability to review equipment or trip blanks
is currently not being used.
.
• If CADRE detects no errors, no further manual review is
required.
• A manual review of all equipment and trip blanks is
necessary to assess contamination.
• Manual review is required If CADRE reports any errors
during data review. Required review Is stated in Section II I of
Guidance Document.
-------
SUMMARY OF CADRE DATA REVIEW - REQUIRED MANUAL REViEW NECESSARY TO COMPLETE A REGION I TiER H DATA
VALIDATION
QC CRITERIA
REVIEW PERFORMED BY CADRE
REQUIRED MANUAL REVIEW
SURROGATES
• CADRE reviews and qualifies surrogate data based on
current Region I guidelines. CADRE reviews the
advisory surrogates for DNA but does not qualify data
for outlier advisory surrogate recoveries.
• CADRE does not review surrogate recoveries if
samples were analyzed at a dilution greater than 1: 10.
• If CADRE detects no errors or if samples were analyzed at a
dilution less than or equal to 1:10, no further manual review is
required.
S A manual review of Form 2 is necessary for all samples
analyzed at a dilution greater than 1:10.
• Manual review is required if CADRE rcports any errors
during data review. Required review is stated in Section III of
Guidance Document.
MATRIX SPIKE
• CADRE reviews matrix spike data based on Current
Region I guidelines,
S CADRE does not quality data for matrix spikes, but
indicates which compounds did not meet matrix spike
acceptance criteria.
• If all criteria were met for %R and RPD or if CADRE
detects no errors, no further manual review is required (or %R
and RPD.
S If recovery criteria were exceeded, a manual review of Form
3 is necessary to determine if qualification of the data is
required
• Manual review of the CADRE sample, MS. MSD Summary
Table is required to assess the %RSD of unspiked compounds.
• Manual review is required if CADRE reports any errors
during data review. Required review is stated in Section III of
Guidance Document.
• CADRE does not qualify results for MS/MSD deviations on
the CADRE qualified Data Summary Tables. The validator
needs to apply qualifiers to both the qualified and unqualified
Data Summary Tables for any MS/MSD deviations.
-------
SUMMARY OF CADRE DATA REVIEW - REQUIRED MANUAL REVIEW NECESSARY TO COMPLETE A REGION I TIER II DATA
VALIDATION
QC CRITERIA
REVIEW PERFORMED BY CADRE
REQUIRED MANUAL REVIEW
FIELD DUPLICATES
• CADRE does not evaluate field duplicates.
• A manual review of the CADRE Data Summary Tables (or
Form Is) for the field duplicates is required to assess precision.
INTERNAL
STANDARDS
• CADRE evaluates primary internal standard criteria
based on the current Region I guidelines. For the
criteria of cxtremely low areas counts, CADRE assigns
a defined value of less than 20% of the internal standard
area of the associated calibration,
• If CADRE detected no errors, no further manual review is
required.
• Manual review is required if CADRE reports any errors
during data review. Required review is stated in Section HI of
Guidance Document.
TENTATIVELY
IDENTIFIED
COMPOUNDS
• CADRE does not evaluate this criterion.
• No manual review for TICs is required for Tier 11. A table
summarizing the TICs detected must be completed. The
rcvicwer must verify that target Compounds are not reported as
TICs in another fraction.
COMPOUND
iDENTIFICATION
AND
QUANTITATION
• CADRE does not check any raw data but where
possible does check and verify calculations and rounding
procedures.
• If CADRE detects errors in calculations and rounding.
CADRE will generate an error form and suggest its
correct result. However, for consistency between the
hardcopy and electronic data deliverables 1 the laboratory
Form I result will be reported by the ESAT CADRE
Chemist if the error Is due to rounding.
• CADRE produces a worksheet which lists all
compounds detected less than the CRQL.
• No manual review is required. Evaluation of compound
Idernificatlon and Quantitation is not required for Tier II data
validation.
-------
SUMMARY OF CADRE DATA REVIEW - REQUIRED MANUAL REVIEW NECESSARY TO COMPLETE A REGION I TIER II DATA
VALIDATION
QC CRITERIA
REVIEW PERFORMED BY CADRE I
REQUIRED MANUAL REVIEW
OVERALL
ASSESSMENT OF
DATA FOR A CASE
• CADRE reviews each parameter independent of other
parameters.
• No manual review is required. An overall summaly of data
qualifications should be included at the end of the Data
Validation Memorandum as outlined in the Region I Laboratory
Data Validation Functional Guidelines for Evaluating Organic
Analyses.
-------
ATTACHMENT IV
Criteria Comparison Between CADRE,
National Functional Guidelines and
Region Functional Guidelines
-------
HOLDING
liMES
CC/MS
TUNING
Evth iaxndby
Tier II?
Revonl FwscnomiGudehnm
Modified 11/88
• Unpreat vedw,ter Aromanc within 7
days. non-aromaucwithu I4 days of sample
collection.
• Preserved water and soul : both within 14
days of wnpte coll on.
• Action: (I) positive ruuuci assd (U I) non.
dctecu. Usc pro(csslona ljudgaTucntwben(R)
rvj ang dais for grossly caccoded holding
wuco.
Brornoftuorobentene
mit Ion AbundaoccCnterss
50 8.0-400%ofbasepeak
75 30.0-66 O%of base peak
95 base peak. 100% relative abundance
96 5.0-9.0% of base peak
173 < 2.0% otto/c 174
174 50.120% of mit 95
1754.0-9.0% of mix 174
176> 93.0% but < 101 0% of mix 174
177 5.0-9.0% of m/x 176
• I2houroanepeaaod.
• ActionS (It) all data it tosas calibranon is in
error.
• If ion abundance catena not cod. use
professional jialgmuceiw determine if
qualification is usecesanty.
CADRE
Vcrsso 2.10
• Urrrreservod waters : Prfcoary: within 7
days of coU ion for ammanca and 14 days
of colleciaoo for non-aromaZics. Expanded:
within 14 days of colleoson for aromacce and
28 days of collection for non-atomancs.
• Preserved waters and soils : PrImary:
wWun 14 days of collemon br all
compounds. Expandedi within 28 days of
collection for all compounds.
• ActionS (3) posiuve ronsits and (W) non-
dctectz outside pnmary cntcna. (I) positive
rcnslts and (It) non-desecu ouuale expanded
Brctnofluorob cnxene
m/x Ion AbundanceCruena
50 80-400%ofm/x95
7530.0-660% of m/t 95
95 base peak. 100% relative abundance
96 5.0-9.0%oI,nlz9S
173 <2.0% of m /t 174
174 >50 0%-120 O%of mit 95
175 4.0-9 0% of mix 174
176 >93 0%-lOt 0%of mit 174
177 5.0-90% of ct/c 176
• llhournincpcnod.
• a i ssa l review QidSil is rw sy
to ddermune umbility of dais if ma
calibration is in error or ion abundaxcciizcria
ate Dot cots.
• Will alert vslsds ior to perform manual
review of the data it it cannot associate
umplcaw th a nine file.
Nusorul FuncoonalGuddinea
Draft, 6/91
• Unproseroed& Preseyvof : Bcthwaier
and soil within 14 days of sample
coll xon.
• ( I) positive ressilts. (W) non-
detects. Use profcusanalpadguncntwttcn
(It) rejecosig dais.
Bromofluorobciuene
m/x Ion AbuMinetCnterta
50 8.0-40.0% of mix 95
75 300-660%o(co/z95
95 base peak. 100% relative abundance
96 5.0-90% of m/x 95
173 <2.0% of rn/c 174
174 >50.0%- 1200%ofm/x95
175 4 0-9 0% of m/x 174
176 >93.0%-l01.0%of m/z 174
1775.0.9.0% of nut 176
• I2houtasncpenod.
• Acuon:(R) all dais if mass calibration ii
in a or. Use expanded crusna if
lwp ,y .
CADRE METHOD COMPARISON
VOLAT ILES
Yes
Yea
• ton abundance cncersa used should reflect
the morr current vernon of the SOW.
-------
INrnAL
CAL IBRAflON
Eva1u*co
by r in
Rq ool FuocooeaIGu31thn
Mod t1o I /U
• All avaijc RJth muabe 0.05.
• All %RSDi rnu bc 30%.
• ii RKF <005. (1)311 poiuivc
r lts for thai compound in n plca
usocaaznd wuth f tc iiutsjl and oabscqu 1
connciuingcalibrvzou. (R) iaonde*eom(o:
h2z coripowaSin iplei a w r,iIM an
inconored. l(%P .SD >30%. U) posauavc
romics (or tha i coanpoundrn usocsaief
samplan. I1%R D > 50%.alao(UJ)aon-
deteers.
CADRE
Vthaon2. 10
• All avenge RP$s mua be 0.05.
• ALl %RSDzmunbe O%.
• Acalon: If RRF <0.05. (3) all poainve
rcoaLta (or due compound in samples
azocaased with the isaual and eibscquenz
conwauuigcaiibranons. (R) aon .desecu (or
thai coinpoundin samples uiociawi U
sacouonnd. If %RSD >30%. U) porurve
resu1 (or tha i compound in asaociaznd
samples. if %RSD > 50%, alao (W) non-
d cW.
NanorW Funcoonal Gudduica
Draft. 6/91
• M1n, mum P.P.F cñwiii omflth per
compound.
• %RSDamugbe S 20.3%.
• Accuine. 2•Buunonc. Caiton D Llfidc.
atloroethane. CbJo oin hane. li-
Drocthan iouiUuvcoo %RSD
cbtgRRPsmusabe 0.01.
• :RRFcmcruajudgndim
conjwucszon with the RSD. Professional
in qualify da wtten RRF
50. dan (U I) t n-
dinoms (or thai pound in usocaat i
temples.
S I( RRF <0.05.0) posadvermults
ind (R) nO del 5 for thai coinpowidin
aamptea assoesated with the cthbrsssoa. If
%D> 25.U)posiaveromha (Ord lai
compoundin aaaccaaxnd samples. If %D>
50. also (UI) aca-dereom for thai compound in
aaiociaied samples.
• :ifRRP isbetwecnOOl and
aerepunec cruena. or above 0.01 (or the
selcctnd ccmpowafi.(J) ponuve renilis
izid(UJ) non4utomt atu. I(RRF <
0.0I. (R) c cc etecesand (1) pounve
tesaisa with amepsabic oman putrwn. It
%D > SO. (1) ponnve resaiks. Use
pzofomwnaljudgunau (or ren.dci .
-------
• One method blank per rnausi per
concesoauon level per Ii bout nine per
syncsn.
• Equipmcni and ulp blanks are ireatod as
mcthod blanks.
• One method blank per mama per
conceniratlon level per 12 hour nine per
sy mn.
• Equipmmt and trip blank contaminanon is
not validated by CADRE.
National Fumoaonal Guidclmes
Draft. 6191
• No coowiooconumusa ibouId be
pre u .
• One m odbLank per esamz per
ccncescanoo level pa Ii hour nine per
• FirM blanks arc ireund as method blanks.
• No TCL couipcundiabove5x CRQL
• No conspousidmuat not have pesk
r > l0%olthenmrcsiuutemalstasalsid.
• l cornasntnans also dewcied in
sample, qualify data (U) at the CRQL. if
conccamat ionl3 < Si blank level (lOt for
common lab coniansusazua(CLCa) and cia
than CRQL Qualify (U) at raised detection
Wiut fcaoccntrauoois < $ablanklcvcl(l0z
for CLCs) tod greater than CRQL Actions
apply to any blank conumtnauon(mcthod.
equipment, or trip).
• Action: If contasnussietUo detected its
sample, qualify data (U) at the CRQL if
coecauranonhs <5 i bLank level (10* for
common Lab contaminants (CLCi) and less
than CRQL Qualify (U) at raised detection
hnsui(cooc anooi* lO%. bus
CRR (1)
positive results only.
Analyse QC Limits QC Limits
toil waler
Tolucne-d. 84-138 88-ItO
Bromofluorobensene 59.113 86.115
l.2-Dichloroethane.d. 70.121 76.114
S All blanks and astriples muse mna surrogate
recovery criteria,
• If any nirsugaxea arc> 10%, bus
CRA (3)
positive renilis only.
Analyte QC Licuts QC Limits
water soil
Toluene-d. 84-138 88-110
Broinofluorobcnzene 59.113 86.115
l.2-D,duloroethane .d. 70.121 76.114
• All blanks and somples muse meet
surrogate recovery criteria.
• II surrogate recovery is < 10%
(R) noa-det saed (J) poastavereuzlm. If
recoveries are l0%-CRR(UJ) non-detects
aid (I) positive results, If recoveries arc>
CRA (A) non-detects and (3) positive renalts,
MSIMSD
Yes
% Recovery Soil RPD Water RID
l,l.DichlorocthaneS9-l72 22 61-145 14
Trichlorocthcne 62-137 24 71-hO 14
Sat iate 66-142 21 76-127 II
Toluctie 59.139 21 76-l2S 13
Chlorobuazene 60-133 21 75-130 13
• One MSIMSD analysed per SDG. per
mania,
• Action- Itrecoveryis C l0%(R) non-
desecia and (3) posuuvc results inunspikod
sample. Ifrccovenesarc I0%-CRR(U3) non-
detects and (I) positive results in the unspiked
sample. If recoveries arc > CRR (A) ron-
dc t ecua n d(3)posiuvere sulumthew ’sp lked
sample. If RID > CRR (3) positive results.
Use professional judgemetu to qualify
compoundafor high RSD between sample.
MS. and MSD for non.spikecoinpowsds.
% Recovery Soil RID Water RID
l,I-Dithlorocthasie59 -lfl 22 61-145 14
Tnchloroethcne 62-137 24 71.120 14
Betizene 66-142 21 76.127 II
Toluene 59.139 21 76-125 13
CIiIOrObCIIZCS 1C 60.133 2! 75-130 IS
I One MS/MSD analyzed per SDC. pa
mama.
• Acxion:CADR!perforiT%sthltev aluataon
but does not qualify sample retsilts Iiith did
rsosmcmcnrcrsl. CADREdocalisethe
ccmpoundswtiich failed criteria,
% Recovery Soil RID Water RID
l.l.D,chtoroetlianei9-172 22 61-145 14
Tricliloroethere 62-137 24 71.120 14
Benzene 66-142 21 76.127 II
Toluase 59.139 21 76.125 13
Cblorcbetesene 60.133 21 75-130 13
• One MSIMSD analyzed per SDG. pa
ITUO1 S.
• Ifrscoveiyis C lO%(R ) non-
daccu arid (33 positive renills. If recoveries
arc l0%-CRR(Ul) non-detecuand(3)
positive rcualti If recoveries are > CRR
(A) noo-dctccu and (I) posiovc results. If
RID> CRRU)poszssvcrcsis!ts. U sc
pro(enssooaljudgcnait for RSD in wsspikod
samples and only for the MS/MSD sainplc.
-------
FIELD
DUPLICATES
INTERNAL
STANDARDS
TCL COMPOUND
IDENT IFICA11ON
Evaluated
by Tier I I ?
Region I FmlGuIdelI
ModiDed 1 1/88
•RPD(orwaxeris <30%;RPDfarsoilb
CSO%.
• For duplicate sempica. RED fOr
water is > 30% (1) posiuve resultS. Alio. if
RPD for soil is > SO%(l) possuvercsealu.
Use pmfmua gomcinto qualify all
tart pIes of the woe mama.
• Area counts may not vary by more than a
(actor o(2 from the associated calibranon
sousdard. The RTs may not shift more than
30 seconds.
• If area counts are ow. (I) positive
results and (UI) non-dotow rmulu for
compour4iquannwed using that weroal
standard. If area couma are extrmsidy tow.
rion-dotcesa should be rejected (R). Usc
professional judgcnec ltf RT ihxfts by more
than 30 seconds.
S Compound muse be within j006 (RR1)
units of the standard (RAT).
• M w spccea muse mow cruerw
1. All ions prescrein the inndardala
relative intensity> 10% muse be presoti in
the wopic spccoima.
2. Relative intenaines of ions specified above
naustagrec ± 20%.
3. Ions> 10% mthcsamplespcctrwobuz
not present io the siandard muse be accounted
(or.
4 Technical judganeni may be used if all
cntefla ate not mu.
• Ariion Use professional judsanent
CADRE
Vcn io 2.1O
• Presently. CADRE does not evaluate fldd
duplicates.
• Prtsnary: Area countS may not vary by
more than a (actor o(2 from the associated
calibration standard. The Ris may act shift
more than 30 seconds. Expanded: arms
counts may not dectesse by more than a
(actor of 5.
• Action: If area counnare outof primary
cruena low. (I) posiave rcntlu and (UI) non-
detect results for coxnpowid.squantiwed using
that uisetnsl standard. If areas counts are out
high. (I) pontave rmulto associatod with dial
incenul standard. U area cousin are outside
expandulcnsena (I) positive renilia and (R)
non-detects usocaazrd with that ictesnal
standard. Manual validation is ra uxred to
qualify data (or receenon tone shifts of more
than 30 seconds.
• CADRE does not evaluate this cnscnon.
Nsisonal Functional Guidelines
Draft. 6/91
• Criteria determined by mdi Region.
• Action Action musebe its accordance
with Regional specifications.
• Ares counts may not vary by more than a
(actor or 2 (root the associated calibration
intalard. The Ris may not shift mare than
30 seconds.
• Action: It area counts are ow. (I) positive
results arid (UI) ncti-dctcci rciulcs (or
compounitsqssan titated using that intend
standard. 11 area counts are cxwmnely low.
non-dctntts should be rejected (R). Use
pro(cenoealjudganaui( RT thitia by more
than 30 seconds.
• Compound muse be within ± 0.06 (RET)
units of the standasd(RRT).
• Mw speeaa muse meet entena:
I. All ionsprcscsizinthean iidarda xa
relative itssty >10% musebepresenztn
the sample specenun.
2. Relative inansiaca of ions specified
above muse agree ±20%.
3. Ions >10% in the wnplc spectrum but
not presast in the ndard muse be
accounted for.
4 T nscal judgenseni may be used if all
minis ate not roes.
• Vie pm(csasonaljudganais.
CADRE METHOD COMPARISON Continued
VOLA .TILES
Yes
No
COMPOUND
CRQLs Yes
• See anached CRQL list for ciarrent
• CADRE prepanna report listing all
• Sec CRQL list.
QUANT ITATTO It
compound list and CRQL5 (or waxer and soil.
cornpouniswluch were reported bcl w the
AND CRQLs
Quanutsuan
No
• REF must be calculated based on intesnol
gtandstd specified in SOW OLMOI.
• Quartuutsoo muse be based on the specific
quanutation ion listed in the SOW.
• Quaiuxcuson is performed wing the REF
obiaused from the daily calibration standard.
• 1 e Pro(esatorul judgan u is used to
dctctmine if reported compowatsate (use
positives or if false negatives ate reported.
CRQL. arid flags all those results as (I).
S CADRE does not evaluate raw data.
therefore, cannot verify spectra.
• REF muse be calculated based on
standard specified in SOW OLMOL.
• Quannuazion muse be baaed on the specific
quanuntion ioti listed in the SOW.
• Quamutanoa is performed using the REF
obtained from the daily cslibnnon siandaid.
• Actiow Professional judguncr itis used to
determine if reported compoundiare false
positives or if false negatives arc reported.
-------
1ThTA11V Y
ID flflED
COMPOUNDS
Evi!uazoi Regiori I Fwsoooos Gwdclthea
byrierir ? ModdIcd II(&8
• The zorymu mndUaa mass
spcco I scardi of the PIES libriry and
rcportthcbY (Orth 10
lasgeas VGA fiiwori peaks. Rcporw
peaks ate sos mzTOgUc. uizeii .I
sundards or itt. compoW 3. bui have
ar he gh1> 10% of the sac of the
itc ar essiS.
• Action: AU liCe arc flaggnd U). TICs
are suzwnar in iabutar format
CADRE
Vermon 2.10
S CADRE does not CYSIIISIC nor li st a
ainimary of the reportcd TICs even
though they vs includnd on a rcpomng
form.
Nadorul FuemonalGu4etinea
Dnft. 6 191
• The labonsory must cosdussa mass
sp sl ecardi of the PIES library and
rq,ortthcpoasblcidaiu iy for the 10
largen VOA fraeaion peaks. Rcportnd
peaks are not amy gase ineemal
sus tatdaor iti. compounds. but have
arcaheigha> l0%ofthesrzcofthc
neatest IS.
• AU TICs axe flaggnd 0).
CADRE METHOD COMPARISON Continued
VOLATI LES
SYSTEM
PERFORMANCE
No
• Use pmfesstonaljudgancottto eva1ua e
effects of poor thmntstography.abrupt
shifts so buchne peak ushng or splining,
etc.
• CADRE doci not evaluate thu
ntetson. CADRE reports the findings of
each parameter ualepetalcteof other OC
p a rameters.
• Use professional udgemcnz to
evaluate cfieus of poor daromasogrophy.
abrupt shifti in baseline peak failing or
splitting. etc.
OVERALL
ASSESSMENT OF
DATA
Yea
• Use prc(esasonal judgetncnzwttm
aasomng data.
• CADRE doc not tvaluatc this
cnterton. CADRE reports the fualings of
each parameter tndcpcndestof other QC
parameters.
• Usc pro(csaional judgcmcnswhcn
assomang data.
-------
CON’IRACT REQUIRED QUANTITATION LIMITS (CRQLa)
VOIaATILES ____ -
II
Regm
II
CADRE II NatzonaJ Fw ocil Gu4din
Analyte
Wazc •
pg/L
Sod •
pg/Kg
Watcr
pgIL
Soil
pg/Kg
W at
pgiL
Soil
pg/Kg
l.l.l.TncMoroethane
10
10
10
10
10
10
l.I.2. .Te tIoroctha
10
10
10
10
10
10
l.l.2-Tnth lorocthanc
ID
tO
10
10
10
10
I.I.DichI rocthanc
10
I D
10
tO
tO
10
I.I-Dkh lorocthene
10
ID
10
10
10
10
t.2-D thIoroethane
to
ID
10
10
10
10
t.2.Dich lorocthcnc(To t a I)
IC
ID
10
10
10
10
l.2-Dichloropropane
10
10
10
10
10
10
2.Bu iaz oi
IC
10
10
10
10
10
2-Heunonc
10
ID
10
10
10
10
4. -Mcthy l-2-Pcnunonc
10
10
10
10
10
tO
Ac one
10
ID
10
10
10
10
Ben2ene
10
ID
10
10
10
10
Sromodrchloromcthanc
10
ID
10
tO
10
10
Bronso(onn
10
ID
10
10
10
10
Broniorn 1unc
10
ID
10
10
10
10
Carbon Duultidc
10
ID
10
10
10
tO
Carbon Tctr achiondc
10
ID
10
10
10
10
Qiloroba2ate
10
ID
10
tO
10
tO
Q lorocthane
10
tO
10
10
10
10
O tloroIorrn
10
tO
tO
10
10
10
C t Ioromcthanc
10
10
10
10
10
10
c u-I .3-D ithlompropenc
10
10
10
10
10
10
Dibr ornochloromethanc
10
ID
10
10
10
10
Ethyl Bcnzene
10
10
10
10
10
10
McthylcncCh londc
10
10
10
10
10
10
S iyrcnc
10
tO
10
10
10
10
TcuicMorocthene
10
10
10
10
lO
tO
Totuenc
10
tO
10
10
10
lO
trazu-I.3-Dtthloropropcne
10
10
10
tO
10
tO
Tnchloroethcne
10
tO
tO
10
10
10
V nytC?iIondc
tO
tO
tO
10
10
10
Xylcnc (Total)
10
lO
ID
10
10
10
Indicates that currently Region I uses CRQLs (rem SOW 3/90.
-------
INmA I.
CALIBRA11ON
Evaluassdby
L ‘ t 1 LJ
Rc otsI Fu oiaa1Gu’detlnes
modified 11/88
• Estnci on : toil and water simpIta
within 7 days of collection.
• Atulyciral . Both within 40 days c i
ete iction.
• Action: (1) positive results said
(UJ)non.dcineri. liboWtngumcia
grossly exceeded. ouy n in (R)
nets-detects.
DFTPP
rn/a Ion Abundance Criteria
SI 30.0-80 O%of rn/a 198
68 Ices than 2.0% olm/z 69
69 presart
70 len than 2.0% of rn/i 69
1272 .50 -75.0% of rn/a 198
197 len than 1.0% of rn/i 198
198 base peak. 100% reLative
abundance
19950-90% of rn/c 198
275 10 0-30 0% of rn/a 198
363 greater than0.75% of rn/i 198
441 present, but less than 443
442 40 0-l10%of rn/a 198
443 15.0-24.0% of rn/a 442
S I hourusne period
• SB2!L (R) all data if mass
calibration is in crier.
• It Ion abundsncecruena not met.
use professional judganait to
deterrnuac ii qualification is
nec .
• Ion abundance criteria used should
reflect the moo current veteran of
the SOW.
• All avesege RRFs muat be
003.
• All %RSDsmuatbe 30%.
• Actron If RRF <005. (1) all
posiuve reaslls for that conipoundun
samples associated with the initial
and subsequent continuing
calibrasion (R) non-detects (or that
compound in aamplct associated ii
mrnuoned. If %RSD >30%. (1)
positive results (or that compound in
associated santplcs. Ii %RSD >
50%. also (Ufl non-detects.
CADRE
Version 2.10
• Exmicn : Prisuary: waler and
sod samples within 7 days of
coUxtson. Expassded water and
soil samples within 14 days of
coU ron.
• Analytical PrImary: both within
40 days of extraction. Expanded:
both within 60 days of extracoon.
• Acoon: (I) positive results and
(W) non-detects outside primary
criteria. (I) positive results and (It)
non-detects outside expanded
cr ite t•aI .
DF PP
r n/i Ion Abundance Criteria
51 30.0. 800% olin/a 198
68 Iessthanl.0%ofznlz69
69 present
70 less than 2.0% of rn/i 69
12725.0-750% of rn/c 198
197 lcasdaan 1.0% of rn/a 198
198 base peak. 100% relative
1995 0-9.0% of rn/a 198
275 I0.0-30.0%otrn/z 198
365 greater than 0.75% of mix 198
441 preaesu. but Icti than 443
442 40.0-1 10% of rn/i 198
443 1S.0 -240%ofna/x442
• 12 bourssne period.
• Action- Ma review oldata ta
neccatasy to determine usability of
data if mass calibration is in error,
ton abundance criteria are not met.
or if rn/c 198 is not base peak.
• Will alert valsdalor to perform
miawal review if it cannot associate
samples with a tune fIle.
• Action: Ii RAP <0 03. (3) all
positive results for that compound in
samples associated with the initial
and subsequent continuing
calibr inons. (It) non-detects for that
compound in samples associated as
mentioned. If %RSD >30%. (1)
positive results (or that compound in
aswciazctd samples. If %RSD >
50%. also (WI non-detects.
Nasionat FunctrontlGwdcluies
Dafl. 6/91
• Extraction wiser samples within
7 days of Collection. Soil samples
recommended within 14 days of
collection.
• Analytical Both within 40 days
of extraction.
• Action: (I ) possuve results and
(WI quawsianonlunses. If MT
grossly exceeded. may need to (It)
non-detects.
DFTPP
tn/i Ion AbundanccCnteria
51 30.0- 80 0% of rn/i 198
68 len than 2.0% of rn/i 69
69 present
70 less than 2.0% of rn/i 69
127250-750% of rn/c 198
l97lcss dun 1.0% of tn/a 198
198 base peak. 100% relative
abundance
1995.0-9 0% of m/x 198
275 10.0-30 0%of mix 198
365 greaser thanO7S% of rn/c 198
441 present, but Ic s than 443
d .4240.0-IlO%o(rn/z 198
44315 0-24.0%of rn/a 442
• l2hourn aneperiod
• Action (It) all data if mass
calibration is in error. Use
judgetnent if ion abundance criteria
ate oo( met.
• Minimum REF cntcna spotifled
per compound.
• %RSDsmustbe 20.3%.
• 19 selected cornpoundahave no
%RSD criteria, but RAPs mum be
001.
• Action: RAP criteria Judged its
conjusicuonwith the RSD.
Professional judgetnettt used to
qualify data whoa RAP <
minimwn criteria. Data ant
qualified due to non-compliant
%RSDcrucna based onif the high.
low or middle part of muse is out.
CADRE METHOD COMPARISON
SEMI -VOL ATtLES
NG ‘liMES
Yc i
CC/MS TUNING
Yes
• All avcragc RAPs mug be
003.
‘All %RSDs mum be 30%.
-------
CADRE METHOD COMPARISON Continued
SEMI -VOLATILES
CONT INUING
CALIBRATION
Region! FunoaonalGuidellnes
modit ied Il/U
..l(RRF <0.05.(J)
positive r ilis and (R) con-dinects
(or thai compound in tsmptct
ano ” with the eslabrauon. If
%D ) 25. (1) ponuverut ii for
that compound n astscaaied
ssmpks. l(%D>50.also(Ui)
non-detects (or that compound in
assocused iampks.
• No oonri iiunsn rishould be
• One blank per m im i.
ccncatainoo level and extraction
batch.
• EquipinctitbiajikS arc tressed at
method blanks.
• I(conwnutanzalso
detected in stmple. quaUy dais (U)
at the CRQL if conccnuatlon is <
S i blank level (lOs (or common lab
con n,n ntt(CLCS) and less than
CRQL Quulify(U)atraasoS
detection limit if ccxno aIaon Is <
Sc blank level (lOs (or CLCs) and
grmeer than CRQL Actions apply
to any blank conmnunanon(mctbod
at equipinctu).
CADRE
Version 2.10
• RRFs muat be ZOOS.
• %Dsniuaibc 2S.
• Action: I(RP.F < 0.05,(J)
pouuvc results and CR) non-dcieces
for that compound in samples
associated with the calibration. l(
%D> iS. (1) positive resulu (or
that compound in associated
samples. If SD > 50. also (U I)
ntin-dct (or thai compound in
asao” ’ p(
• No cossarsinasun should be
pres .
• One blank pci ma.
concentration level and extraction
baick.
• Equipineniblanks arc not
validated by CADRE.
• S!! If collt am lnanl also
detected in sample, qualify data (U)
utheCRQLWccncaunaisonis <
S i blank level (lOx (or commonbb
conwmnanin(CLCs) and tom than
CRQL Qualify (U) at taited
descoson hai ti if coocciunnon is <
Si blank level (lOx (or CICa) and
than CRQL Actions apply
onlyto wnplcsassociaccd with the
conuminased blank (from Form 4).
Na onaJ FoncuoaaiGuidduies
Draft. 6/91
• RRF cntena specified per
compound.
• SOs muatbe 2.5%.
• Selected cornpoundshave no SD
crucnabulRRFsmuubc Z 001.
• Action: If RRF is bctwccis0.0l
acid acceptance criteria, or above
001 (or the icheced compounds.
(I) positive rctsil*i and (UI) non.
det rom1ss. l(RRP < 00l.(R)
non-detects and (I) pounve rcsaslu
with acceptable mass spcen mi. l(
SD> 10. (1) posiuvc romlis.
Use proIonaljudganent(or
non-detects.
• No contaminanesthouldbc
present.
• One blank pci mains.
concesunanon level and cw cnon
batdt.
• Field blanksarc treated as
method blanks.
• Lab Blank Action : l(conuounanz
also detected in sample. qualify
data (U) at the CRQL. if
concenoanonis ( Sxblanklevd
(lOx for common lab conuminasun
(CLCs) and less than CRQL
Qualify (U) at raised detcenori limit
if eonceslzranonhz < 3 * blank level
(lOx for CLCs) and greater than
CRQL
• Field blanks should riot contain
any TCI. above its CRQL. and
should oct contain the cosesnon
phthalase coruamuwimat
concentrations> 2* CRQL
• Should not contain TICs.
• Field Blank Action : Qualify the
writ as (or Region I Funcoonal
Gucdchnes except use only Sc level.
II Eviiuazedby
TIer II ?
Yes
• RRFs muat be Z 0.05.
• %Ds muatbe 25.0%.
BLANKS
Yea
-------
Evil
U
Region I FóonoJGusithnes
modified 11/88
CADRE METHOD COMPARISON Continued
SEMI-VOLATILES -
— SURRO-
GATES
Yci
CADRE
Va ioa2.10
% Recovery
Niuobcnzcnc-d,
2.Fluorobiph yl
Teopha iy l-4 1 .
Ptia iot-
2 -Fluorophenal
2.4.6-Tnbromophasol
Soil Aqueous
23.120 35-114
30.115 43-116
18-137 33-141
24-113 10-94
2.5.121 21.100
19.122 10-123
National Functional Guwid ici
Draft. 6/91
% Recovery
Soil Aqueous
l4u iroba izaec -d,
23-120 35-114
2-Fluorobiphasyl
30.115 43.116
Tcrpt iu iyl-d 1 .
18-137 33-141
Phencl-d 1
24-113 10-110
2-Ruoropheon l
25.121 21-110
2.4 .6-Tnbromophcnol
19.122 10.123
2.Ciloropbenol-d.
20-130 33-110
I.2-Dichlorobcnzenc -d.
20-130 16-110
% Recovery
Nuuobaizate-d,
2-Flucrob iphenyl
Terpben l ..d,.
Phaiol-d,
2-Fluor ophonol
2.4.6-Tnbromophcnol
2 l cr ophcnoI .d,
l.2-Duthlorobon’ece--d ,
• Action: If at leasi 2 siurogaaea in a hue/neutral
or aCid (raCUOr IUC> 10%. but CRR (I) positive tesults only.
Soil Aqueous
23-120 35.114
30-115 43.116
18-137 33.141
24-113 10-ItO
25-121 21.110
19-122 10-123
20-130 33-110
20-130 16-110
• Action: If at Ieait 2 surrogates in a base/neutral
or acid fraction are> 10%. but CRR (I) positive results only.
• CADRE does not take uuo consideration
idvusory surrogate recoveries when quatil img
dies. (i.e does n04 include thon as one of the iwo
owluer surrogazes required for quahficanon).
• CADRE will not cealuate siatiogate eccovetics
on a Sample u i dilution greater than lIOwu
performed on that sample. -
MS/MSD
• If at least 2 surrogates in a
base/neutral or acid fraction are ohs, but> 10%.
(I) positive results for that traction (8/N. or A)
said (W) quanunnon limits (or that (action. If
< 10%. Ci) positive results for that fraction and
(R) or ( I) non-detect results (or that fraction.
Yea.
S R vry
S R veiy
Soul RPD
Aqu
RPO
26.09 33
12.89
42
2.Cb loi 9 i nl
25.102 50
77.123
40
I.4-0.c$iloi.
21.104 27
36.97
28
N-Nac di.o.ç.v .
41.126 38
4 1-I 16
38
31-107 23
39-9*
28
26.102 33
23 .41
42
Ac nth u
31.137 19
46-Its
31
4-N u i O. ..,l
11-114 50
i0-
50
niw iucvi
28.89 47
24-96
33
Pcmth1 ephci l
11-109 47
9-102
50
P vivc
35-142 36
26-127
31
Sod 8.10 Aqi s RID
Soil R IO Aq oio RPO
PIr l 26-09 25 12-89 42
2 . loi $rod 35.102 50 77-123 40
2*-lOt 27 36-97 28
NNu o.da .n .pvcp. 41.126 31 41-116 38
I .24-Tnduloi u eiw 38-I C? 23 39-9* 28
,ceju Ip&ml 26.102 33 23-91 42
31-137 (9 46-Ill 31
((-114 50 I0- 50
24-Danauu ue 28-89 47 24-96 31
Per loivpiimel 17-109 47 9.102 50
35.142 36 26.127 31
• Acusor CADRE pafoieo dun c.iiu.oor h a
niify unavilc r uJ wh d4 , me
CADRE iso wh uçuonh hiha
I4-D
N -P t nuo di-opr ep
U.4-Tr ITh eecrc
.,-..-
• tr r u,m Ste v xr dtaai luuuim tJ) punitive
roiidui in wopiha iaepk. If uv . .i au lois dna
iumuu b un a lOS. (1) mve rciuuiu in wapiked uncle.
If rwovv- .rc < 10%. (1) punsiuc rosin s (R) r
&wo tcivlu us wnpi d un 4c. (Sic pseumeni
jistgnaucri in qiahfy mml i ( high RSD boiv a ianuie.
MS. iuil MSD run-ipebu unnaunu
24-90 35
25-102 50
28. 104 27
41-126 38
38-107 23
26. 102 33
31-137 19
11-114 50
28-89 47
17.109 47
12.89
27-125
36.97
41-116
39.98
33.97
46-I IS
lO
24.96
9-103
42
4°
23
3*
2*
42
31
50
3$
50
31
35.142 36 26-127
• ACtuni ( iso penimivawl judlcoicre in &.rtruuuli sacd
C.r q.uiuI uios of the dsoi.
-------
CADRE METHOD COMPARISON (Continued)
SEMI -VOLATILES ____
Ev ahm n dBy
T&ctI I?
RcVon I Fuacesonsi Guidelines
modIfied 11/88
CADRE
Version 2.10
Nasional OWGU CCIoea
Draft 6/91
FIELD
DUPUCATES
Yes
• RPD toriquno plcautuatbe
<30%. For soils. RED stun be
<50%.
• :IfRPDl imiUare
exctod . (I) positive resulli for that
compound in both saniples. Use
professional judg au to quality all
samples of the same mains.
• Presently. CADRE does not
evaluate Ileld dupliesnes. CADRE
does rmogntee field duplicote pairs
but does not have an evaluation
parannerer. Thuopuonisschedulnd
for unplmocnWlOnIC ftinirc
releases.
• Criteria detcrminndby each
Region.
• :Acuonmunbem
accordance with Regional
spec stics uons.
INTERNAL
STANDARDS
Yes
• Area counts may not vaiy by
snore than a factor of 2 from the
issociased calibranosi standard. The
RTs may not shift more than 30
seconds.
• Action: II area muon are out. (I)
positive remiss and (W) non-deson
rcsiulcs (or mmpowiquaaniased
usuig that internal standard. If area
cou nts are extremely low. non-
dctccta should bc rcjuted (R). U sc
proC onaljudgunentif RT shifts
by snore thin 30 semeda.
• Frt ry: Area couzm may me
viny by more dun a factor of 2
(tom the associated calibranoms
standard. ilie RTs may not shift
more than 30 seconds. Erpsnded
areas counts may not decrease by
more than a (aceor of S.
• If area counts are oisi of
prinnasy criteria low. ( I) positive
remiss and (LU) non-detect results
for conspoundaq” ” using that
izsnernai nsndard. If areas counts
are out high. (I) positive results
associated with dint internal
siandard. If area counts arc outside
espanded criteria Ci) poslove rondes
and (P.) sin-detects j 15 .. .rM with
that laicmal stazida Manual
validation is required to ejiald ’ date
(or retention tone hiha of more than
30 seconds.
• Area counts may riot vary by
more than a factor of 2 from the
associated calibration eandard.
The RTa may not shift more than
30 seconds.
• If arcs comm are out.
(I) positive results and (UI) non-
doted results for compounds
quannutoS using that internal
standard. If arcs muon ate
extremely low. non-dceocu should
be rejected CR). Use professional
judgctnntsi if RI shifts by more
than 30 seconds.
TCL
COMPOUND
IDENTIFICATION
.
‘
Ho
• Cornpouodmuot be within 0.06
RRT units of the standard RRT.
• Mass spears of the sample
compound sod a current lab
geotratod standard must match
according w spcciIlc ion cotena.
• n: Use professional
judgen init.
• CADRE does sot evaluate thu
criterion.
S Compound moat be within ±
0.06 RRT units of the nsndasd
RRT.
S Mass spectra of die sample
compound and a current lab
geneestini standard mutt snatch
according to specsIlc lo criteria.
These criteria are the same as those
llttctilndscRegiosl Functional
Guiddlin
• Use pro(essional
j u d!ciT sei iL
-------
bMPOUND
.C. . .ANTITA11ON
AND CRQLI
Evaluaxoil by
Th U?
RC1On1 FtmcoondGui m..
toodiilaj [ 1188
• Se c seached CRQL list (or Qirrens soil
arid ware CRQLS (or each compound.
• RRFmustbcclcaslawibuedon
io2ernaI smndard 9ec1Iied in appropruoc
Sow.
• Qusmitasson mu bc based on the
tpccsflc qualthi2lIon Ion listed in the
Sow.
• Quannisnon Is performed using the
REF ob soed from the duly calibranon
• Profeanocal judg enLts used
to determine If reported compowadsaze
(abc ponnvcn or if (alac negasavea are
reported.
CADRE
Version 2.10
• CADRE prcpara a report liinng all
compounds which were reported below the
CRQL and flags ill those resialti as 0).
• CADRE doc not evalusie raw dam.
thcrc(orc . cannot vcnfy apeena.
Nauoiag PuncnottelGuaddlioco
Draft 6 191
•S e cCRQL I i s t.
• RRF must be calcataind based on
inlental swsdajd wecified in SOW
OLM OI.
• Qusniunnon must be based on the
spotific quazuusason ion listed in the
Sow.
• Qusiususion u performed umsg the
RRF obtained train the daily calabranon
• PrafcsssonaJjudgcrnauu used
us determine if reported compounds are
false possorea or if false ncgwvcs arc
reported.
CADRE METHOD COMPARISON (Continued)
SEMI -VOLATILES
CRQLS Yes
Ctmpound
Quar non
No
TENTATIVELY
IDENTIFIED
COMPOUNDS
.
. Yes
• Must report pOssible denory if ihi 20
lazgen oos-TCL. or nurrogase peaks wthch
havcazcacoussi> lO%ofncar lS.
• S!i2ii Use professional jWgcmcnzw
determine if proper idmnflcanoascr
claisifimusons bate been made. TICs
nsmznanzed in inbular formas.
• CADRE does not c,sluaic nor list a
nimmary of the reported flCs c en
thougbthcyarcimc ludedonarcporung
form.
S Must report poinble idenuty if the 20
largest ron-TCL or sorrogaic peaks
wluchhaveareaccunu> IO%of
ne azcstLS.
• Use pro(esstonaijudgetnenico
detconune if paper idas fieassoni or
cliasifiesnona have been made.
SYSTEM
PERFORMANCE
No
• Use pmfc onal judgeminno eraluaze
cifecis of poor chrov asograplty.abnjpo
shifts in baseline peak tailing or lmsng,
etc.
• CADRE doca not cvalua ic this
criterion. CADRE reporm the findings of
m di pasainmer irdcpcndauot other QC
parameters.
• Usc pro(muoitaijudgcmmztocvaluase
effects of poor chromazography. abrupt
shifts in biockne peak tailing or lhnng.
etc.
-------
CON’TRACT REQUIRED QUANTITATION LIMITS CRQLB)
SEMI -VOLATILE S
II
Rq IonI
II
CADRE II Nioo a2 m o jGrnd In,.
Anaiycc
Wijg
,glL
Soil
u JKg
W& a
pgIL
Sod
g/K
Wgz r
pgIL
Soil
1 igiKg
l.2.4-Tnddorvbau c
10
330
10
330
10
330
l.2-DicftIoxoba zcnc
10
330
10
330
10
330
l.3-DichIotob e
10
330
10
330
10
330
I.4-D.chlomba z
10
330
I D
330
10
330
2.2.o ybi I.ChIoropropuic)
ID
330
10
330
10
330
2.4.5-Tñcb orvphemI
23
800
25
800
25
800
2.4.6-Tnchloro8hcnol
10
330
tO
330
10
330
2.4.Dschtor phaioI
tO
330
10
330
10
330
2,4-Dimcthylphmo l
10
330
10
330
10
330
2.4.Di iwropha iol
25
800
25
800
23
800
2 4-Di uirowtu ie
tO
330
10
330
10
330
2.6-Dinzo tucuc
10
330
10
330
10
330
2. 1oronaphdu1ene
10
330
10
330
10
330
2h loropheno l
10
330
10
330
tO
330
2-Mcthylnapbthaicoe
10
330
tO
330
tO
330
2-Me ihyiphenol
IC
330
10
330
tO
330
2.Nicroanilino
25
800
25
800
25
800
2.N iuuph 1
10
330
tO
330
10
330
3.3-Dithlorobeizidunc
10
330
tO
330
tO
330
3-NIao2n,Itne
25
800
25
800
25
800
4.6.Dinitro-2.McthyIp hc ol
25
800
25
800
25
800
4-Brvmoph nyI-PhcnyIc ier
tO
330
10
330
tO
330
4-Ch lom-3-Methylpheno l
I C
330
tO
330
tO
330
4—Chlorovulgne
tO
330
tO
330
10
330
4-Chlorophmyl.Phe iiylether
tO
330
I C
330
10
330
4.Mcthy lphenol
10
330
10
330
tO
330
4-Ntuoinj l inc
23
800
25
800
25
800
4—Ntcroph oI
25
800
25
800
25
800
AC UPhth Ie
tO
330
tO
330
10
330
Accnaphthylene
10
330
- tO
330
10
330
A,uhr ccnc
10
330
10
330
10
330
Ret xc(l) nthr2ceI1e
10
330
10
330
10
330
Berixc(a)pyrei c
10
330
- 10
330
10
330
Bcnzo(blfluorinthcne
10
330
10
330
tO
330
(g.h.1)PctYl
tO
330
tO
330
tO
330
&zo kU1uorinth ic
tO
330
10
330
10
330
bu 2-ChIorocthoxy 1mc isnc
10
330
10
330
10
330
-------
CONTRACT REQUIRED QUAN’IITATION LIMITS (CRQLs) Continued
S I-VOLATILES
CM3R.E II Naoow.1 Ftmcoonal G iidehnes
Analyse
W 1XCT
pgIL
Soil
pg/Kg
Wa&ct
p g/L
Soul
jig/Kg
WaLCt
pg/L
Soil
pg/Kg
bt 2.C l lorocthyl)cthet
tO
330
10
330
10
330
bu 2-ethylhczyl)phthalaIe
tO
330
10
330
10
330
Buty lbvylphth i la ic
10
330
tO
330
10
330
Caxba.!otc
tO
330
I D
330
tO
330
Chryscne
10
330
10
330
tO
330
Du-n-buty lphthala&e
10
330
10
330
tO
330
Di. i-oczyIphtha1 ic
10
330
10
330
10
330
Diba o h)antlu2ccnc
10
330
10
330
10
330
Dub zofwa
10
330
10
330
10
330
Di hytphtha1axe
10
330
tO
330
10
330
Duncthy lphthztate
tO
330
tO
330
tO
330
Fluorantha e
10
330
tO
330
tO
330
Ruor c
tO
330
tO
330
10
330
Hez2th lorobatzene
tO
330
10
330
tO
330
Hcz.athtorobu dicnr
tO
330
10
330
tO
330
Hcxic l itorucycIopau dic c
10
330
tO
330
tO
- 330
Mcucltioructhai
10
330
ID
330
10
330
ti a o(I.2.3.c4)pyrcne
10
330
tO
330
10
330
lsophronc
tO
330
tO
330
10
330
N.M i oso-du.n.prvpytamrnc
10
330
ID
330
tO
330
N.Nitrosodiphenytasrnn l)
tO
330
tO
330
10
330
Naphthatcne
tO
330
tO
330
ID
330
Ni obenw e
tO
330
10
330
ID
330
Pcnuchtorophcnol
23
800
23
800
23
800
P? i unthrene
tO
330
ID
330
tO
330
Pbcto l
tO
330
tO
330
tO
330
Pyrei e
I I )
330
tO
330
tO
330
II
-------
ATTACI E V
Organics Complete SDG File (CSF) Inventory Sheet
CADRE Data Review Inventory Sheet
Region I Complete SDG File Receipt/Tranafer For -
-------
RG .NIC Cc LE S C T (CSfl fl vu rOR!
LECRACRY TAME _________________________________
c’Y’srArz _____
c z : o. ____________ G O. ____________ SEC ioS. :o FOLLC ___________
____________ __________ SAS NO.
ccNrRAc :ro. -
SOW t O. __________________________________
A.L]. c ocumsnc c.aiizeceø j . the coiece SEC file i.s e or’- - i. ocugnc
4iere poss .b1e. (R CZ I3IT 3. SEC ON II a.n.d SEC ON 1:1.)
PAGE NOs
FROM 0
I ror-, S he t (Tor DC-2) (Do t oc =car)
SEC ease litir
SEC Cover S e c/T rf 9 ayort
Vo .pc les Data ,
a. QC S” ’7
Svsce Monicori Co caund S” ”- 7
(Form II IOA)
M.acr .x Soika/Macrix p±ke D zoL1caca 5itt
(To III VQAY
Method Bti k St? nty (Fort IV VOA)
CC/ 1S I st !,,.I1c Pa o ’ ca Cl ac c
(Yor V VGA)
:n u S dard p ____
(Porn VIII VGA)
b. Sa.1a Data
:c. 0A)
anc.atLveLy Ider:.: -. . Copound.s
(Torn I 7OA-i IC
Racotst’. :ad :otai. .on chro aco rams (RIC
for eacn saole
or eac saia:
3a,w s eera and. bac rott d- su caczad.
.ass s ecv .a of tar ec c cuno.s
Lda tc fie
Quanc tacjon revorts
Mass specta of all. :eporred TICs vtt three
best Librarr .actnas
c. S noards Data (ALl. Iost encs)
tnitiai. Calibration Data (Por V I VGA) ____ _______
alcs and Qu.an Raoorts if or all. S and.ard.i ____ _______
Conc1 -ting C.alibratiori Data (Form VII VGA,) _____ _______
RICs an Qu ncitat .on Reçortz for all. Standards _____ ________
Law CC 3aca
3 F3
3laxt Data
tatrix Soikei ac j x SQika Du l.icaca Data
_I . 1 %,
:v a
-------
:ac.& Ic c i t_ !: ccz i t .LV -CHX S’ T (C t.
z :;o. a :o. sac :OS. :3 FOL.L t1
j LAS NO.
?ACZ NOs
LA Z!
Sj7oLptil s Data
a. CC 5Itf?H .r
Surrogate Percent Recoiier9 5ii r (Form El LV) ____ _______
j/ 5 Sti,.w7 (Form III LV) ____ ___ ____ _______
‘.ecbo 51 ” (Form IV LV) ____ ____ ____ _______
CC/ In..it.enr P Chec
(Form V LV)
: erm.ai. S an aro . Area a A
(Form ‘/111 LV)
S. Said Dac.z -
:. uit. (F0t I SV-L, SV-2)
aricaciveiy Idanrifiea Co ou oi (Form I SV-TC)
Raccns ur:eo. ocaJ. ion c x icograms ( ..IC)
r esc sa D1a
7or eacà za zi :
L iv sp.crra and back rct d . su crmcted
razz spccra oi target caatlnd3 _____ ________
QuincitaciQu retorc3 _____ ________
ttlz svscra of TCa wt three beic Library acchas ____ _______
C2C cbroacog a (Lf GPC .r ormsd) ____ ______
c. S 2 ft2?d .1 Data (All
C- 1i racton Data (Form VI 57-1, 57-2) _______
and Quan ae crta for all L - rd., _______
Conc ii in C 1ibracion Data. (Form VII $7.1. SV-Z) _______
IC.c acd Qu citation Keporta for a.U. S miard. _______
vo .acjLa PC C.alibrac .on Da.ca-UV
ecac: r ::ace
d. Liv QC Data
31an Data
ac x S ikaiMa . Spike Du ii aca Data
a. C Sir’r
!uzrogace Percent R.ecov ry Stm.i .i-y (Form LI PEST) ________
.5/MSD Du Licaca Suarr (Form LII PEST) ________
cno 31an Sur. (Form IV PEST) _______
FORM DC.2-2
tMr 1 — —
-------
:acA JIC CC cPLE G LZ (C Z) T7E!?TCR! (C flC.
sz Q. _________ DC C. _________ DG : oS. FOLL Z
_________ ________ AS O. __________________
PAGE NOs C E
i. cone.;
b. !a1 ie aca
CL aasui - •Dr ani Anaiv3L. Daca Sheec
(Form I PEST
ro zv.o!ra s (Pr .. arv Colu) _____ ________
Cram&ca ra 3 from econ CC co . con c on ____ _______
cc :Acfl Ci0fl a orc or daca svsc r c uc _____ ________
Anhim1 .JOr. sneecs _____ ________
For 3tcidu/Arociors ccn.fied by CC/MS. pias
o :av specc a and coutes o &c ro11nd- w3cracr d ass
suecca o r sc oimd (samules & sr rcs)
c. Daca
.ic a1 Calibracion o Single Co uonenc
Aualvtas (Form VI PE ST- i and PEST -2)
:nici.a.]. C.alibractoa oj Mu.i:jcoon.nc An.LLvce.s
( or VI PEST-3) ______
Ac.a.iyra Sttii”v ry (For Vt PEST-”) ________
Calibration VerifLcarion StT?!!I .?y (Fo VII PEST4) _______
C lthrartau ‘Ieri.ficacjon S’—’.’-y (Fo VII P!ST-Z) ________
An.üycica.l Seauaucs ( ‘or VIII PEST) _______
flori. il Carridge Checic (Form PEST-I) _______
Pesctcida CPC CaIThranjon (Form P!ST-Z) ________
sicide td.anti.fLcation Si ry for S!T le C onanc
Ai’rces ( or I PEST-I)
?esd.cida d.ancificac on Sttr’ r!I.r7 for con nt
Analytas (Yorm I PEST-Z)
an data s•ysce ntout
A pr: .tc o :ecantion :ies ana c ..esuanrti pea
area3 or a& c heights
P .da CPC calibration d.aca V dacacor aces
d. Raw CC aca
31axa Data
ac .x ike,l’.ac . Spike Dupi .caca Data
FORM C-Z .
— — /01
,,J_
-------
aa1 % MIc3 c L=Z SDG F Z ( ,. I1WITCaY 571 (C nc.)
m SZ JO.
[
SDC NO. SDC SOS. 0 FOL U
s .s io.
PACE NO ____
TO
i ceL1aneo is Data
Ori;{m i rep*xactcn and. 1t 1yzi.3 for i or capic Ct
Pr5VIZZCLOn an4 1o boo pa. s
Incarv .&i. umpls and. samaLe exacc cazifer
G fl•O C1 3COUT record3
5cr ei,i i record3
All ii snc ouc uc, s ip c * t3
f m sceafti ac .vj e.a (ducribe or
ZPA Thi oin JRecej’rth Doe’ nrs
AirbilL (no. at s ipe t. ) ____ ____ ____ _______
C .ain-of-Cu . ro4y R.acor z ____ ____ _____ ________
Sample tags
Sample Lh3g.tn Sheet (Lab & DC1) ____ ____ ____ _______
MLs eiLan.oui Shippinzjbceivlng aacord.s
(daicrib. or hit)
Inrer L tab S le T nster ! eecr js At d Th cki z Sheets
(da crthe or Li.st)
). Other ?.ecord ! (descr.he or li.2c)
Taleghone C r icacthn L
)16ced by: _________________________
(CL Lab) (Sig acure) (Pri cad Iaa. TLtLa) (Oata
&thttad by: _____________________ ______________________________ __________
VA) (5L nac xe) (Prt aa a.ma TLtLe) (Datni
FORM DC.Z-4
OL Ol.7 7/91
-------
CADRE DATA REVIEW
INVENTORY SHEET
The following items are required to be delivered from ESD to the Field
Sampling Contractor in the CADRE data review report. Please verify
delivery and receipt of each item by checkin the appropriate column. This
form is to be included with the Data Validation Report.
Case No:_________ SDG No:_________
Field Samplinq
Contractor
1) Sample Listing _____ _____
2) Quantitation Limit Report _____ _____
3) Holding Time Report _____ _____
4) Percent Moisture _____ _____
5) Instrument Performance Check Report _____ _____
6) Analytical Sequence
7) Calibration Listing _____ _____
8) Calibration Report _____ _____
Laboratory Blanks Report _____ _____
b SMC/Surrogate Report
1].) Matrix Spike Report _____ _____
11) MS/MSD Non-Spike Compounds Tables _____ _____
12) Internal Standards Report _____ _____
13) Volatile Data Summary Table _____ _____
14) Semivolatile Data Summary Table _____ _____
15) Pesticide/PCB Data Summary Table _____ _____
16) Diskette with Data Summary Table Files _____ _____
CADRE Report
Prepared by:______________ Affiliation:_______________ Date:
PIDRE Report
pproved by:______________ Affiliation:_______________ Date:
Received and
Audited by:_________________ Affiliation: Date:
-------
EPA REGION I
COHPLETh DD VILE
RECEIPT/ RM18FER FORM
Ikase I: SDG: Data Package 1:
Receipt
Date
.
Received by:
Name mit. Affiliation
-.
CSF
Activity
.
Custody Seals:
Present / intact
(On Receipt)
-
IN V N
111 IN
IN V N
V H I N
V N I N
V N I N
I N Y N
• IN V N
I N V H
V N V N
IN — IN
IN IN
Released:
To Date
.
-------
ATTACH EN’r VI
CARD/CADRE SDG Tracking Form
-------
CARD/CADRE SDG TRACKING FORM
SDG:_________ NO. SAMPLES:________ MATRIX:_____
J. ORATORY:__________________ FIELD SAMPLING CONTRACTOR:_____________
SITE:____________________ PARAMETERS:___________
= = = = = = = = == = == = = = = = = = = = = = == = = = = = = = = = = = = = ========= = = = = = = = = = = = = = = = = = = = = = == = =
DATE PKG. RECD AT ESD RSCC:_________ DATE PKG.RECD BY ESAT:__________
DATE DOWNLOAD ATTEMPTED:________ WAS EXTRACT AVAILABLE?:__________
IF NOT AVAILABLE, WHY?_______________________________________________
DATE DOWNLOADED:_________________ CARD DOWNLOAD FILE NAME:_________
DOWNLOAD FORMAT: (ASF OR CARD) _________________
DATE IMPORTED INTO CADRE:_______ CADRE IMPORT FILE NAME:_________
= = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = =
DATE IMPORTED INTO CADRE:__________ NO. FORMS (RECORDS) IMPORTED:________
IMPORT TIME: _______ NO. ERRORS DETECTED:_____ ERROR REPORT PRINTED:_
EXPLANATION OF MANUAL ENTRY REQUIRED:____________________________________
TIME REQUIRED FOR MANUAL ENTRY:_______________
= = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = == = = = = = = = = = = =
____ SUMMARY TABLES GENERATED FILENAME(S): BNA (S) __________ (W) _________
VOA (S) __________ (W) _________
PEST (5) ___________ (W) __________
____ FORMATTED ____ CONVERTED TO WP ____ FLOPPIED
____ BACKUP MADE BACKUP FILENAME(S) : BNA (3) __________ (W) __________
VOA (S)__________ (W) __________
PEST CS) ___________ (W) __________
= = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = = =
_____ ALL WORKSHEETS GENERATED
____ SAMPLE LISTING ____ ANALYTICAL SEQUENCE ____ HOLDING TIMES
____ CALIBRATION REPORT ____ CALIBRATION LISTING ____ IPC ____ s MOISTURE
____ QIJANTITATION LIMIT ____ BLANKS ____ SMC/SURROGATES ____ MS/MSD
____ INTERNAL STANDARD ____ MS/MSD NON-SPIKE TABLES ____ SUMMARY TABLES
CADRE REPORT ____ DISKETTE OF DATA SUMMARY TABLES _____ DATABASE FILES
INCLUDED: ____ HARDCOPY REPORT ____ HARDCOPY DATA SUMMARY TABLES
E CADRE REPORT AND DATA PACKAGE PREPARED FOR SHIPPING:________
CADRE REPORT AND DATA PACKAGE SENT TO FIELD SAMPLING CONTRACTOR BY:__________
DATE CADRE REPORT AND DATA PACKAGE SENT TO FIELD SAMPLING CONTRACTOR:________
-------
ATTACHMENT VII
Me .orandum for Qualifying Soil/Sediment Data with Low Percent Solid
-------
I 4 J - - -
RZGION I
Environ enta]. Ser Vices Division
60 Westviev Street, Lexington, MA 02173—3185
ORANDVX
DATE: March 29, 1990
ST B7: Qualifying Soil/S9diment Data with lou Percent Solids
PROM: Moira Lataille/CLP—TPO
Deborah Szaro/CLP-TPO
TO: Data Validators
The PAZ Inorganic and Organic SOWs may be used to analyze
water and soil/sediment samples. However, what constitutes
a soil/sediment sample is not addressed in either of the SOWS
or the current CLP User’s guide.
To maintain consistency in the validation of soil/sediment
data, Region I will adhere to the definition of soil sample
used by the Office of Water Regulations and Standards
Industrial Technology Division.
Soil Samples——Soils, sediments and sludge samples containing
more than 30% solids. (1)
Therefore, all soil data may be accepted when the percent solids
are greater than 30%.
All positive results are to be approximated (J’d) when % solids
are 10% or greater and less than or equal to 30%.
All positive results are to be rejected when % solids are less
than 10%.
All non—detected results are to be rejected when % solids are
less than or equal to 30%.
Summary
% Solids >30%
A = All results
% Solids 30% 10%
J = All positive results
R = All non-detects
% Solids < 10%
R = All results
Reference:
1. Method 1620: Metals by Inductively Coupled Plasma Atomic
Emmissionspectroscopy and Atomic Absorption Spectr scopy-Draft
-------
Attachment M
Example Tier I Validation Cover Letter
-------
Example Tier I Validation Cover Letter for
VOA/SV Soil Samples Analyzed under CLP OLMO3 .2
-------
Christine Clark June 1, 1997
Regional Sample Control Center B-97-06-FF-05
U.S. EPA Region I
60 Westview Street
Lexington, Massachusetts 02173
RE: WA No. 03-718
SDG SAAO9, Case No. 1011
Fine Analytical Labs
Lou’s Landfill
Tier I Organic Data Validation
Volatiles: 6/Soils! SAAO9, SAAb, SAA11, SAA12, SAA13,
SAAb 4
(Soil Field Duplicate Pair/SAA13 and SAA14)
1/Aqueous Trip Blank/SAA15
1/Aqueous PES/SAA25
Semivolatiles: 6/Soils! SAAO9, SAAb, SAA11, SAA12, SAA13,
SAAb 4
(Soil Field Duplicate Pair/SAA13 and SAA14)
1/Aqueous Equipment Blank/SAA16
1/Aqueous PES/SAA23
Dear Ms. Clark:
A Tier I data validation, in accordance with the Region I. EPA-NE
Data Validation Functional Guidelines for Evaluatinc Environmental
Analyses , December 1996 criteria, was performed on the organic
analytical data for six low/medium level soil samples, two aqueous
blanks (semivolatile equipment and volatile trip), and 2 aqueous PE
samples collected by U.S. EPA Region I, from Lou’s Landfill site.
The volatile and semivolatile soil samples, blanks, and PESs were
analyzed under the CLP RAS prcgram using the OLMO3.2 Statement of
Work. A Tier I data validation was deemed sufficient at this time.
A follow up Tier II validation will be performed at the end of the
six month monitoring period.
A Tier I data validation is based only on the following parameter:
* S Data Completeness (CSF Audit - Tier I)
* All criteria were met for this parameter.
EX.ANPLE - 12/96
-------
The PE sample results were evaluated for this Sample Delivery
Group. All criteria were not met. Carbon Tetrachioride and
tetrachioroethane received “Action High” and “Action Low” scores,
respectively. If a Tier II or Tier II I validation were performed
the following actions would be applied to the sample data: all
carbon tetrachioride positive detects would be biased high and
therefore 1 estimated (J) and all carbon tetrachioride non-detects
would be accepted. Due to the “Action Low” score 1 the
tetrachioroethane non-detects would be rejected (R) and the
positive detects would be potentially biased low and therefore,
estimated ( 3) . All sernivolatile PES results were within criteria.
Plaase contact M. Howard at (999) 232-7000 should you have any
questions or comments regarding this information.
Very truly yours,
HOWARD ENVIRONMENTAL
‘fr W u)cz- - J
M. Howard
Data Validator
S. Howard
Senior Validator
Attachments: 1.. Data Summary Tables
2. Accuracy Check/PES Score Report
3. Field Sampling Notes
4. CSF Audit (DC-2 Form)
5. DQO Summary Form
CC: Victor Hernon, EPA Site Manager
EXAMPLE - 12/96
-------
DATA SUMMARY TABLE
Volatile Soil Analysts
uglkg
NOT VALIDATED
SITE Lou s Landflhl - Anywhere. MA
CASE No. 1011 SDGNO. S A09
SAMPLE NUMBER SM O9 SM1D SMI 1 SAA12 SM13 SAA14
STATION LOCATION NW1 NW2 SE1 SE2 Ni NI
LABORATORY NUMBER LAB O9 LAB 1O LAB 1 1 LA1312 LAB13 LABI4
COMPOUND CROL
Chloromelt iane 10 11 U 50 U 130 U 12 U 12 U 13 U
Bromomethane 10 11 U 50 U 130 U 12 U 12 U 13 U
Viny lChloride 10 11 U 50 U 130 U 12 U 12 U 13 U
Chloroethane 10 11 U 50 U 130 U 12 U 12 U 13 U
MethyleneChloride 10 11 U 50 U 130 U 12 U 12 U 13 U
Acetone 10 11 U 50 U 130 U 12 U 12 U 13 U
Carbon Disullude 10 11 U 50 U 130 U 12 U 12 U 13 U
1 .1-Dithloroethene 10 11 U 50 U 130 U 12 U 12 U 13 U
1 1-Dichloroethane 10 11 U 50 U 130 U 12 U 12 U 13 U
1.2-Duchtoroethene(total) 10 11 U 50 U 130 U 12 U 12 U 13 U
Chloroform 10 11 U 50 U 130 U 12 U 12 U 13 U
1.2-Dich!oroethane 10 5 J 8 J 3 J 12 U 12 U 13 U
2-Butanone 10 11 U 50 U 130 U 12 U 12 U 13 U
1,1 1-TrichIoroethane 10 11 U 50 U 130 U 12 U 29 140
Carbon Tetrachloride 10 11 U 50 U 130 U 20 12 U 13 U
Bromodich loromethane 10 11 U 50 U 130 U 12 U 12 U 13 U
1.2-Duchloropropane 10 11 U 50 U 130 U 12 U 12 U 13 U
cis-1.3 -O lchloropropene 10 11 U 50 U 130 U 12 U 12 U 13 U
Trich loroelhene 10 11 U 75 130 U 82 12 133
Dibromochloromethane 10 11 U 50 U 130 U 12 U 12 U 13 U
1 .1 .2-Trithloroethane 10 11 U 50 U 130 U 12 U 12 U 13 U
Benzene 10 16 100 130 U 12 U 29 167
trans-1,3-Dichloropropene 10 11 U 50 U 130 U 12 U 12 U 13 U
Bromoforru 10 ii U 50 U 130 U 12 U 12 U 13 U
4.Melhyl-2-Pentanone 10 11 U 50 U 130 U 12 U 12 U 13 U
2-Hexanone 10 11 U 50 U 130 U 16 12 U 13 U
Tetrachloroethene 10 22 50 U 130 I .) 12 U 12 U 19
Toluene 10 11 U 50 U 130 U 12 U 12 U 13 U
1.1.2.2-Tetrach loroethane 10 11 U 50 U 130 U 12 U 12 U 13 U
1.2-Dubromoethane 10 11 U 50 U 130 U 12 U 12 U 13 U
Chlorobenzene 10 11 U 50 U 130 U 12 U 12 U 13 U
Ethy lbenzene 10 11 U 50 U 130 U 12 U 12 U 13 U
Slyrene 10 11 U 50 U 130 U 12 U 12 U 13 U
TotaiXylenes 10 11 U 50 U 130 U 13 12 U 13 U —
DILUTION FACTOR: 1 0 1.0 1 0 1 0 1 0 1 0
DATE SAMPLED: 03/23/97 03/23/97 03/23/97 03/23/97 03/23/97 03/23/97
DATE ANALYZED 03/29/97 03129197 03/29/97 03/29/97 03129197 03/29/97
% SOLIDS 95 20 8 85 80 75
-------
SITE Lou’s landfill - Anywhere. MA
CASE NO 1011 SDGNO: S 4A09
SAMPLE NUMBER SAA15
STATION LOCATION TB
LABORATORY NUMBER LAB15
COMPOUND CROL
Ch loromethane 10 10 U
Brornomethane 10 10 U
Vinyl Chloride 10 10 U
Ch loroethane 10 10 U
Meihylene Chloride 10 10 U
Acetone 10 10 U
Carbon Dusullide 10 10 U
1.1-Dichloroethene 10 10 U
1.1-Dich loroethane 10 10 U
1.2-Dichloroethene((otaI) 10 10 U
Chloroform 10 68
1,2-Dich loroethane 10 35
2-Butanone 10 15
1,1,1-Trichloroethane 10 10 U
Carbon Tetrachloride 10 10 U
Bromoduch loromethane 10 10 Ii
1,2-Dichloropropane 10 10 U
cis-1.3-Dichloropropene 10 10 U
Trlchloroethene 10 10 U
Dubromochloromethane 10 10 U
1,1,2-Trichloroethane 10 10 U
Benzene 10 10 U
trans-1.3-Dichloropropene 10 10 U
Bromoform 10 10 U
4-Methyl-2-Pentarione 10 10 U
2-Hexanone 10 10 U
Tetrachloroethene 10 10 U
Toluene 10 10 U
1,1,2.2-Tetrachforoet hane 10 10 U
1.2-Dibromoethane 10 10 U
Chlorobenzene 10 10 U
Ethylbenzene 10 10 U
Styrene 10 10 U
Total Xylenes 10 10 U
r rn =rr
DILUTION FACTOR: 1 0
DATE SAMPLED: 03123/97
ATE ANALYZED. 03/29/97
DATA SUMMARY TABLE
Volatile Aqueous Analysis
ugIL
NOT VALIDATED
-------
DATA SUMMARY TABLE
Semivolalule SoIl Analysis
uglKg
NOT VALIDATED
SITE Lou’s Landfill - Anywhere. MA
CASENO: loll SOGNO SAAO9
SAMPLE NUMBER SAA O9 SN 10 SAAI1 SAAI2 SA/\13 SM14
SAMPLE LOCAl ION NW1 NW2 SE1 SE2 NI Ni
LABORATORY NUMBER IAB O9 LABI O LAB1I LAB12 LAB13 LAB I4
COMPOUND CRQ
Phenol 330 350 U 1050 U 4125 U 350 U 410 U 440 U
bls(2 -Chloroethyl) ether 330 350 U 1650 U 4125 U 390 U 410 U 440 U
2-Ch lorophenol 330 350 U 1650 U 5000 390 U 410 U 440 U
l.3-D lclutorobenzene 330 350 U 1650 Ii 4125 U 390 U 410 U 440 U
1.4-D lc l u lorobenzene 330 360 1650 U 4125 U 390 U 750 4700
1.2.Dich lorobenzene 330 350 U 1650 U 4125 U 390 U 410 U 410 U
2-Methy lphenol 330 350 U 560 4125 U 390 U 410 U 440 U
2.2-oxybls(1-Ch loropropane) 330 350 U 1650 U 4125 U 390 U 410 U 440 U
4-Meihy lphenol 330 350 U 1650 U 412’; U 390 U 410 U 440 U
N-Ni lroso-dI-n-propy lainiuie 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Hexathloroe lhane 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Nltrobenzene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Isophorone 330 350 U 1650 U 4125 U 390 U 410 U 440 U
2-Nitrophenol 330 350 U 810 4125 U 390 U 411) U 440 U
2.4-Dirnethylphenol 330 350 U 1650 U 4125 U 300 U 410 U 440 U
b ls(2-Chtoroethoxy)me lhane 330 350 U 1650 U 4125 U 390 U 410 U 440 U
2,4-Dichlorophenol 330 350 U 1650 U 4125 U 390 U 410 U 440 U
1 ,2.4-Trlch!otobenzene 330 350 U 420 4125 U 390 U 660 670
Naphthatene 330 350 U 1650 U 4125 U 480 480 2100
4Chloroanj ljne 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Hexach lorobuladlene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
4 .Chloro-3-Melhylphenol 330 350 U 1650 U 4125 U 390 U 410 U 440 U
2-Methylnaphlhalene 330 350 U 1650 U 4300 390 U 410 U 440 U
Hexachlorocyc lopentadiene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
2.4.6.Tr lchloropheno l 330 350 U 1650 U 4125 U 390 U 410 U 440 U
2,4.5-Trlchlo ,opl uenol 800 810 U 4000 U 10000 U 940 U 1000 U 1100 U
2-Chloronaphthatene 330 350 U 680 4125 U 390 U 410 U 440 U
2-Nutroan lhne 800 840 U 4000 U 10000 U 940 U 1000 U 1100 U
Dimethylphthalate 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Acenaphlhylene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
2 ,6-Dlnutrotoluene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
3-Nitroanhlune 800 840 U 4000 U 10000 U 940 U 1000 U 1 l JU U
Acenaph lhene 330 620 1650 U 4125 U 580 560 1300
2,4-Olnltrophenol 800 840 U 4000 U 10000 U 940 U 1000 U 1100 U
4-Nutrophenol 800 840 U 4000 U 10000 U 940 U 1000 U 1100 U
Dubenzofuran 330 630 1650 U 4125 U 530 410 U 440 U
2,4-Dlnutrotoluene 330 350 U 1650 U 4500 300 U 410 U 440 U
Olethyiphthalale 330 350 U 1650 U 4125 U 390 U 410 U 440 U
4-Clulorophenyl-Pheny lelher 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Fluorene 330 350 U 1650 U 4125 U 420 410 U 440 U
4-Nitroanhl lne 800 840 U 4000 U 10000 U 940 U 1000 U 1100 U
4,6-DlnI lro-2-Methytpheno l 800 840 U 4000 U 10000 U 940 U 1000 U 1100 U
N-n llrosod ipheny lanilne 3.30 350 U 1650 U 4125 U 390 U 410 U 440 U
4-Bromophenyl-Phenylether 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Hexach louobenzene 330 350 U 550 4125 U 390 U 410 U 440 U
-------
DATA SUMMARY TABLE
Semivolatule Soil Analysis
uglKg
NOT VALIDATED
SITE: Lous Landrull - Anywhere, MA
CASENO.: 1011 SDGNO. SAAO9
SAMPLE NUMBER SAAO9 SAA1O SAA11 SAA12 SAA13 SAA14
SAMPLE LOCATION NW1 NW2 SE1 SE2 Ni Ni
LABORATORY NUMBER: LABO9 LAB1O LAB 1 1 LAB12 LAB13 LAB14
COMPOUND CR0
Pentach lorophenol 800 840 U 4000 U 10000 U 940 U 1000 U 1100 U
Phenanthrene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Anthracene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Carbazo le 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Di-n-butylphlha lale 330 350 U 1650 U 4125 U 390 U 410 U 440 U
F luoranthene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Pyrene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Bu ly lbenzy lphthalate 330 350 Li 1650 U 4125 U 390 U 410 U 440 U
3,3’-Dich lorobenz ldine 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Benzo(a)anthracene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Chrysene 330 350 U 1GSO U 4125 U 390 U 410 U 440 U
Bis(2-elhylhexyl)ptithalate 330 350 U 1650 U 4125 U 390 U 2000 2000
Di-n-octy lphthalate 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Benzo(b)fluoranthene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Benzo(k)Iluoranthene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Benzo(a)pyrene 330 350 U 2200 4125 U 390 U 500 530
lndeno(1.2,3.cd)pyrene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Dibenz(a,h)an lhracene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
Oenzo(g,h,u)perylene 330 350 U 1650 U 4125 U 390 U 410 U 440 U
DILUTION FACTOR: 1.0 1.0 1.0 10 1.0 10
DATE SAMPLED: 03/23/97 03/23/97 03/23/97 03/23/97 03/23/97 03/23/97
DATE EXTRACTED: 03/29197 03/29/97 03/29/97 03/29/97 03/29/97 03/29/97
DATE ANALYZED: 04/13/97 04/13/97 04/13/97 04/13/97 04/13/97 04/13/ J1
% SOLID: 95 20 8 85 80 75
-------
SITE Lou’s L8ndfuII - Anywhere. MA
CASE NO: loll SOG NO’ SPAO9
SAMPLE NUMBER SAA16
SAMPLE LOCATION EB
LABORATORY NUMBER LABIG
COMPOUND CR0
Phenol 10 10 U
bls(2-Chloroethyl) ether 10 10 U
2-Chloropheno l 10 10 U
1.3-D lc li torobenzene 10 10 U
1.4-Dichto robenzene tO 10 U
l.2.D lchtorobenzene 10 10 U
2-Me thytphenol 10 10 U
2.2 ’-oxybls( l-C li loropropane) 10 10 U
4-Methylphenol 10 10 U
N-Nutroso-dI-n-propylamlne 10 10 U
Hexac lrloroethane 10 10 U
Nitrobenzene 10 10 U
lsopl;orone 10 10 U
2-Nitrophenol 10 10 U
2.4-Dimethy lphenol 10 10 U
bls(2-Chloroethoxy)methane 10 10 U
2.4-Dichlorophenot 10 10 U
1.2.4-T ,Ichlorobenzene 10 10 U
Naphlhalene 10 10 U
4-Chioroanlllne 10 10 U
Hexachlorobutadlene 10 10 U
4-Ch loro.3-Methylphenol 10 10 U
2-Methylnaph thalene 10 10 U
Hexachtorocyclopenthdiene 10 10 U
2.4.6-Tr lchiorophenol 10 10 U
2.4.5 -Trich lorophenol 25 25 U
2-Ch loronaphtha lene 10 10 U
2-Nutroaniline 25 25 U
Dimethylphihatate 10 10 U
Acenaph thylene 10 10 U
2.6Dtn ltrotoluene 10 10 U
3-Nutroanhtine 25 25 U
Acenaphthene 10 10 U
2.4 -Dinttropheno l 25 25 U
4-Nitrophenol 25 25 U
Dubenzofuran 10 50
2.4-D lu ultrototuene tO 10 U
Diethy lptuthalale 10 10 U
4-Chlorophe uuyl-Pheny lelher 10 10 U
Fluorene 10 10 U
4-Nutroanhline 25 25 U
4.6-Dinltro-2-Methy lp lienol 25 25 U
N-nu lrosodiphenylainlne 10 10 U
4-Bromophenyl-Phenylether 10 10 U
Hexach u lorobenzene 10 10 U
DATA SUt BLE
Senulvolatile Aqueous Analysis
ugIL
NOT VALIDATED
-------
SITE Lous Landfill - Anyv here, MA
CASE NO.: 1011 SDG NO. SAAO9
SAMPLE NUMBER. SAA16
SAMPLE LOCATION EB
LABORATORY NUMBER: LAB1S
COMPOUND CR0
Penlach lorophenol 25 25 U
Phenarithiene 10 10 U
Anthracene 10 10 U
Carbazole 10 10 U
Di-n-bulylphlhalate 10 10 U
Fluoranthene 10 10 U
Pyrene 10 10 U
Butylbenzylphthalate 10 10 U
3.Y-Dichtorobenzidine 10 10 U
Benzo(a)anthracene 10 10 U
Chrysene 10 10 U
Bis(2 -ethylhexy l)phLh2late 10 10 U
Di -n-octylphthalate 10 10 U
Benzo(b)fluoranthene 10 10 U
Benzo(k)fluoranthene 10 10 U
Benzo(a)pyrene 10 10 U
lndeno(1.2.3-cd)pyrene 10 10 U
Dibenz(a.h)anthracene 10 10 U
Benzo(g.h.i)perylene 10 10 U
DILUTION FACTOR. 1 0
0/VIE SAMPLED: 03/23/97
DATE EXTRACTED: 03/29/97
DATE ANALYZED: 04/13197
DATA SUMMARY TABLE
Senuvolatile Aqueous Analysis
ug/L
NOT VALIDATED
-------
EI’A-Nii -vala Validation Wozkshcct
VOAISV - l’cs(/l’CB-XI
X I. ACCURACY CIIECIC
(l’erfurinaiice Evaluation Results) — List all analytes [ hat ate outside ci itci ia.
SDGNo: Sm-t301
CASE: / 0/1
Are niore Luau one-half of the I’ES analyles witluiui c i itet Ia for cacti pal anicter. V ) N
I’E
Saii j te
Aiiij;ulc
Nusiibcr
I’ai aiiic(cr
Type uf
I’ES
l Ia(a 1c
i%isaly(e
Cuiic.
l vgloii I E A
I’ES Scui cs ’
Nuii—I i A PES
Scm cs’
Saunhiles I lhectcil
Acfluii
Niiiiibcr
s s
‘
rrüo I
‘
yprt
-
4,
P Q
‘ ‘
Cøtb (ruCMar-iic
fQd(4 Jl
3(zj/L-
A J(L.
/1cJ n 1 ’ 1 L
/1-cJ r . Lou)
w, ì
W / ’
5n9-W1 S
cr 5flg/5-
‘Y f\
jZ.
Scoic Report Result: Action high; Action Low; TCL MISS; TCL CONTAMINANT; TIC
to
** For Non-EPA PESs indicate [ lie non-EI’A PES Score: PES COMPOUNI) MiSS; I’ES COMPOUND CONTAMINANT; l’ES COMI’OUNI
III ’!’ (% Recovery Limits)
Validator: IV\• f ’(OL42 d Date: 3 3/ 7
For Region I PESs indicate the Region I I’ES
lilT; TIC MISS; TIC CONTAMINANT
12/96
-------
RAS ORGANIC
PE SAMPLE NUMBER: TT00851
Lab
Lab
Lab
Lab
Name: Fine
Code: FAL
Sample ID:
File ID: NA
Analytical Labs
JJAS No.: NA
9503005-25
TCL HITS
Carbon Tetrachioride
Tetrachioroetherie
TCL MISSES
TCL CONTAMINANTS
TIC HITS
TIC MISSES
TIC CONTAMINANTS
NOT SCORED
Contract: 68-D555
SDG No.: SAAO9
Date Received: 03/25/97
Date Analyzed: / /
Action High
Action Low
73 ugiL
22 ug/L
EXANPLE- 12/96
-------
RAS ORGANIC
PE SAMPLE NUMBER: TT00855
TCL HITS
Analytical Labs
DAS No.: NA
9503005-23
Contract: 68-D555
SDG No.: SAAO9
Date Received:
Date Analyzed:
TCL MISSES
TCL CONTAMINANTS
TIC HITS
TIC MISSES
TIC CONTAMINANTS
NOT SCORED
Lab
Lab
Lab
Lab
Name: Fine
Code: FAL
Sample ID:
File ID: NA
2 -Methyiphenol
Fluorene
Eenzo [ b] fluroanthene
Benzo (k] fluroanthene
03/25 / 97
/-
32 ug/L
22 ug/L
19 ug/L
39 ug/L
In Window
In Window
In Window
In Window
EXAMPLE- 12/9 6
-------
3 ?3i - (e +. M-C A pr ° P j
31 LOL 4 .’S LL L/1d LL, / L o S L-’ A IL
S’k Ie/&iJi?z-cde 1 s ’ 4O ?3’MJ
oc’ - lot I — Vo (‘ -h - -‘ ‘ “ f t(iL i& ii - - ‘oo
L ) pd L-1 (j L’ 4, .’,i : —
I e.
WI — S’IA’3- ,ooo( -/
i1- P h - ‘ /0
r 4e U5e . o I 3 CM-Q 4S K ASSeSS,% .€JL# I - i 7f11SI/bro ’t
pU-i 5p ,n z-. tpL ty r co1L
Ls r oJ r -
o & j j Te l P. /1
C X i - 1 o- -c 6UOI k E . ( i ’M
1 ottIe (a i* -y u+ 35
10:00 / SAAOR m (es NW
i p. ?0
SCtr4 so/C — 1 et b ri -J- ’e — - a’t - -’ — ‘- do &f-
13 c t i S L c4i - Me ,6o le ‘Cs c
NUJ ft’c’-1O -f. ? i f’ - NW
[ )(t A W -pb I Th tP. “C NO Lr 1 z’tth( c or ôbvk
1 e, : ic y, so,L ( jfJ - ,vi.ed. br j u, 7 ,,‘ 5D C
S 1- S t( /00 E 5ft I
V J - r sffre4 ; Uc ( - Sf fli b - e t)
-
-------
Evidence Audit Photocopy
O2 rIC2 CO1Qt S G F.Z (027)
LA ORATcR NAME
c: r/ v r!
CASE NO.
O O Rr c
t’i L-4 ti &
.
La
DG NO.
SA.
&D
cj. pcocI
SDG
NOS.
TO
FOL.OW
MO.
C NT AC MO.
SOW NO.
iivent t-r Sheet ( c DC—2) (Do r ot nu er)
S G Case ar atjve
SDG C er Sheet/ fic ! e e t ____ ____ ___________
4. Vojat . e Da
a. QC SLI ’*’ y
Sy3ta Mcnit ring c= c nd ii VOA} ____ ____ _____ _________
Maz .x 5piJ a/Mar_tix Spijca D p1itata S”t’ 7
(Pc II: VOA)
Method Blank Su’ a 7 (Porm I v VOA) ____ ____ ______ __________
Ot/MS Itmant Per tr anca CS ack (7O V VOA) ____ ____ _____ _________
Intarna]. Standard Area and RT 5Ua.y
( o VIII VOA)
b. Sale Data ____ ____ ______ __________
T . Ree .il.t — (Yoz I VOA)
T9ntatively IdentifLed c mçcux d ar t vth—T:c) ______ __________
Rectn tt ctad t tai. ict c trc nat:gram1 (R.ZC) fcr
each zampla
For each sale:
Raw ec :a and backgr nd— trac ed ase
s ectra of ta.;ac c tcund identLf Led ______
Quantltation re c s ______
1 ase s ef all. raccrted 1103 with three
best 1ibra atthes
C. Standards Data (All. tast mentS)
Initial Ca . ratjcn Data (F0r Vt VOA)
RICa and Quan Retorts for all. Stan .r ______
C ttjflUr.g Cali ratisn Data (?cr VI VCA) ______
RIca and antitaticn e crt3 for all .ndards ______ __________
d. Raw QC Data
4 8 ________
3lank Data
“arrix ike/Mat ..x Soj. e Dwolicata Data ____ ____ _________
All. dccusi.nt delivered i.i the Ca=Leta SCG File uwt be original. dccuent3
where pose le.
cac
EPA
,
‘—
‘,
V
V
b/
v,
,
VI
v,
v/
v,
VI
PAGZ NOe
?RCM TO LAB
I I +
I D I )- ____
r I.S ____
1(1 I • ____
L • __
t? - ____
‘ -I
VI
a,
•;T.3 %
J
V —
a,, —
EXAMPLE-12/96
FORM DC-2-2.
cr O.
-------
Evidence Audit F’notocop
ORGXNICS CO LETE SOC FILE (CSF) INE TOR SaE : (C t.)
cAs: O. 10 ( 1 s No. q -i 9 5CC NOS. TO FO .O —
SAS NO.
PAGE NOs c ec:<
FRCM O EPA
5. Se iy 1ati1ei at
a. QC Swt rnary
Sur: gate Pe:cent Rec ve:y Sumna7 (Fcr i II 57) IOD __________
M5/MSO S a:y (Fc III SV) 101 tO ? _________
Met d 2Lar k Swr. tary (Fcr IV SV) 101 V I
CC/MS I str rnent p f r ar ce Check (FC V S’J) tO ic V I ’
Inter a1. Star dar Area ar d R Su . iary
(1C v::I 5 0’ IO’ — /
b. Samcle Da:a (D t 9
TCE. Results (F r I SV—l, 51-2)
Te i:a:.velv Ide :i ie C: S I 5V- C) h” VI ’
Rer s::.c:e :a. ra: ;ra S (R:C) f
each garn 1e
Fcr ac.’ sa. Le:
Raw ssec::a ar basker r.d—Sut aCed mass
ssec:ra Cf tar e : C? !
Qua:i:at. : re : s “ ___________
Ma ec : cf Cs t C- E
G C c r :: :a -: ( .f GPO per )
C. aar a:a : :e :s LtPC) I .
: .: a: Ca:a: . : Da:a = v: s —, SV—)
R:cs a R ::s f : a . E:aa::E V ’ ___________
c:: .._ c : :_- oa i:::— v: S ’ SV )
R C ar. Q:.:a:: Re :! f a.1 £:a- _: ! ______
±. Rae . C Ca:a
____ / __________
ELa:-. : a:a I’IS . ‘ —
Ma:r.x £:.. c s _c :a:e Ca:a N’ ? ______ V I
e. Raw C C C a: a c0 OS I ’ V I ’
6. Pes ic.de
a. C’ 5•—— -
:: a:e ?e::s : Pe:: e:y S ra:y (F I: t ‘ P-)A . —
/ ‘.5 D e ar’: PES) ) — —
5 z-. a:y (T; :? PEE ____ ‘ ______ —
:=. ‘ ::-: : c C:..
EXAMPLE 12/96
-------
Evidence Au n rnotocupy
ORG NICS CO LZTE SOC FILE (CSF) INENTOR SSEE (Cc t.)
c. sz rio. jQti . ___________ s c sos. TO Fo .O —
S S NO. _________
PP GZ NOs C ZC(
FRCM TO EPA
Pe t .c d i (Cent.)
b. Sam 1e Data
TC. Results — Orçar ic Analysis Data Sheet
(For I PEST)
Ch smat gra nz (P .rzia_y CO].UI?Ifl)
Chrc agra £ cm aecond CC column c .rsatjcn
CC Integratio t :c:t or data 5y5t
flanual work sheets
For pes: cidesfArc lcrs snfLr ted y CC/)4S
c ies c raw s ec::a and c pies o backqroun —
subt:acted mass ect:a cf taraet c .mpnunds
(6a s les & s:anda: E)
C. Standards Data
Initial Cali raticn of Sinçle c c er Ana1y es
(Fort Vt PEST—i and PEST—2)
I?.i:ial Cali ra:i n of M:icp r ent Ana .yteS
(?c VI PEE—S)
rtal rte Resoli.:itn Sun a:y (FC: v: ?E =- )
Perfsr anee a tisn M..x:ure (F:r v: :— )
Individual Standard Mixture V ?: - )
:ndi’.’i al Stan r: V E :—)
Caii :a:j Ve:j a ary
(Fc:n v:: P!S—l)
Calj :a;j n Ve: fjc :j Su .a
(Fcr v:: PZS—2)
a -i al Se enoc (T - v:::
F..c: ..s...l Ca:::..o e C-e ’ ( c? I’
Pes:i ide G?C Ca_i a:.c (FC X
P: .:i a :da : i:a:_: s z:y f:: S.;.a
C; e : v:e (F r X
Pea:i:. . a : e :ifi i: S a:y f
ne : A ay:eE (F::— X 2)
C ra: :a.n and da:a svae
p .nt : cf tinas an
a:eas C: ea,. e..; :s
B QC a:a pJPr jp
_an. ata ____
S ke! ’:::,: S:..ke _ :a-_a _aa ____ ____
:z—2- CtXC2.
EXi 4PLE12/ 9 S
-------
vi ez1
ORGANICS CO LZTE SDG FILE (CSF) INEN OR f S EE (Coat.)
C:
o1l
5 , 0 q s C NOs. TO FCL.LOW
L;s no.
P CZ NOs
FRC. TO
LA3
Pe ttc±d s (Cent.)
e. Raw GPC Da:a
f. aw fl.cr .siL Data
j JI: r iJA
. 19 . 1 ’
—
• }4i celi nei us Data
Origina . p para: .on and ana1y is f r s c c ies ef
eparation and aria1ys .s logbook pages
Inter ia1. aan ple and asn le axtracz t ans er chain—
of-c z cdy reco: s
Scr ening r c rds
Mi ins . en: tt : St f
20:eening ac: .vi:ies (cescr.be ot list)
3. EP Shiin /Receiv .ria ie ts
A i:ls (NC. of s ip er.:s _)
C ai —cf-C s:: y Rec :
Sa.z le Tacs
s lo L —:n &
IB ..; Re
(desc: 9 or list)
r te- 31 tab 5a l Tra s ? R Os ! a d
Sb. et ! (es::_ 9
Ot e (das: i:a or
aD ___
‘ 3o
f,J, ( ‘ip,
_ 4 . ___
. Zc-I ac ____
9 / ____
a j
4..
T 1r: a C:: t-
T Jej L’ne Corn t o i L - i ki I 43L 4
k,ie — +./ nF J “ 4
‘k ’c- ra-
-------
Evidence Audit Photoccpy
ORC 21ICZ C MPL Z G ?LZ (C 7) OR (C t.)
DG M C. 5P r SCG &OS. rO Ot..CW __________
SAS Na. _________
C Lat3d by:
cc:p :a.b)
Ver ..figd by:
(c7 t. )
AudLt2d by:
( P.;)
(5igr1at )
(Sig a .U )
(Sig a 9)
L- (n 1 \ 12 / 1’. C & 4 +
(Pr 9d Na e/’i .e)
J j I s+. L&
(Prin d Naa/T!..t )
. rc / flcr - thJJdaJVr
(?ri ed aa/TLtLa)
4•i& 9
(Da )
4 i-i’. (i—’
17
( ata)
5 1 8 ’. 7
(Da 2)
L:.
c .sz
NO. 1
C .uti:
EXANPLE-12/96
CC-2E
CL2 C
-------
EPA Program: TSCA ( ) RCRA OW NPDES CAA
Other
Projeced Date(s of Sampling 3 . O —
EPA Site Manager V c 4u tr a’ ’
EPA Case learn Members C\ci. a .¼,r” iv1 3
r o
t t
Site Name
Site Location m
Assigned Site LaotudetLongiuidc a ‘ 3’ ic, 4 t • ) 3’ iv
CERCT A StwJSptU tdeneifier No. 01 .j Ito Unchide Operable Unit)
Phase: ERA SAISI pee-Ri ( j )Cphase I. cta. FS RD PA pcu-RA
(circle one) Other.
Drat) DQO Sumjn ri Farm 11/96
EPA-NE - DQO SUMMARY FORM Page f of
A separate Poem houtd be completed for each samptiog e’fcI t. Refer m Attac.hmesst A 3c emets O t Completing this form. AnactuTtent for a complete list
[ the parameter codes and Ar chment C for an example of a completed form.
2. QAPjP Title and Revision Date ( u.a .Q.44 . 1SU.r& LL c. CLf% r Lo L&i c 1(c .
Approved by_N I t n 4 (‘ -h.4. Date of Approvai: (. J .
Tide of Approvmg Official: Lo ./ Lak4 - 1 ’t1 & ject IY 4l4 1 Organizatiari _________________________
U other than EPA. record date approval authorily was delegated:__________________________________________________________
EPA Over ighe Project (cccl : one) Y ‘4 Type of EPA Oversight (circle one) PRP or FF Othert .J A
Conuinnawt? Analysis for Field Screer cg y It EPA Oversight or Contirenatory: % splits__________________
Are cosnoarabtlity cncena documented? Y
3. a.
b.
C.
4.
C.
Marni Code’
I
ParsmererCode
O J i tO.ty’ OtMO3.2.S
Preservation Code’
5
6
1
Anaivuc ervtces Mechanism
(..LP PJ’
L?4AS
No. of Sarnole Locations
S
6
I
Field QC:
(. Otinuicate Pairs I /
g. Blanks I
I i. VOA Trio Blanks —
Cooler Tcrnoeeaa.irc Blanks I 1
j. Boide Blanks LO 3 (o LdJ tII t S6_ A
k. Other______________
I sent to Laboratory ii /
Labarceary QC:
in. Reanent Blank 1 — I
fl- Duclicare 1 1
0. Macu Soike / I
p. Matrix Soike Dunlicate I
Other_____
4. Site liwjmiaeion
Site Dunensions 500 4 . X SOC ’ Ft .
List sit potentially contaminated macices -
Range of Depth to Groundwater /1 — I
Sod Types: Suthce Subsurface Other ‘ - ad.( 4 U
Sediment Types: Stream Pond euarv wetland O¾her ________________ Expected Soil/Sediment Moisture Contenc High
Whefl mulop c macices will be sampled during a sampling eveflt. complete Sections 5 W for each malsix. Macis Code SO
S. Data Use (circle all dim apply) Site lnvescganowAsscssinect PRP Decennination Removal Actions
i4arur and Extent of Contamination Human aM/or( oeical Pisit Remedianon Alternaovcs
Enginnerina Design Remedial Action
Posc.Remediai Action (quarterly monitonng) Other S j ’e..i. XD
EXA24PLE-12/96
-------
DQOs: V() Sii) *q4; 4. ° ’ y)s4L b 7 7 & *
4efrg(A,/ar ’e -fh qrie 3? &i) L4 , - D( i -D 4-, l . 9. -
.? c 4 q ( .ivi i ’i Th4 ’P W . CO ,
0
Comolete_Table_if_aoouic ble
Action Levels
Analytical Method.Quanriratton Limits
‘o
Ie,roe k,e,,e
Io y/k cy
I C C k 24e.
(cirde technique) Bailer Low flow pump (Region I method: .Ycs No) Perisulde Pump
Positive DisolacemenC Pump Faucet or Spigot Other_______________________
EI Sp ) Dredge Trowel Other________________
Procedures (SOP name. No.. Rev. II, and date) 5p1i t S cr ( .wP’3 ) 12ev. 3/’1
Sample Locations ThLIJ LO4J ?4 Uç r 4ie. .-t’ (.s) r 1 a.,- ’4 4. Unc’frea...i
Composite ‘
6 ) No
(cirtle) ORP pH Specific Conductance DissoLved O Turbidisy
Other____________________________________________________________
Methods and Paraxnetera
cirlcJSOP nama MethodJSOP
Identification number
Revision Date Target Paeaxtieeers I
(VOA. SV. Pe zfPCB. Metals. eec.Lj
Criteria (circle one) 1. Recion 1. EP .-NE Data Validation Functional Guidelines for valuathie Environmental Analvses. Ill
or IV
2. Other Approved V daoon Cntcna:___________________________________________
(circle one) I II I Partial Tier Ill.
Performing Data Validation 1 S -.
4os .je .,-d Grni ia.P Conetact Number SS
(e.g. START. RACS. etc.) AQ.CS Work Assignment No. O - ?1
Forrnrrit!eJo cfl , 1 ea-M#4 tj Date of DQO Summasy Form Complenon_ •/ - 7 —
Matrix Codes t - Refer to Attachment B, Part I
Parameter Codes- - Refer to Attachment B, Part II
Preservation Codes 3
I. HCI to pH 2 7. K Cr 0 7
2. HNO. 8. Freeze
3. NaHSO 4 9. Room Temperature (avoid e cezsive heat)
4 H.SO. 10. Other (Specify)
5. Cool @ 4C (± 2) N. Not preserved
6. NaOH
- To supplement Matrix Codes and/or Parameter Codes contact the QA Unit
Draft DQO Summary Form 11196
-------
Attachment N
Example Tier III Data Validation Reports
-------
Example Tier III Data Validation Report for
VOA/SV Low Concentration Surface Water Samples
Analyzed under DAS OLCO2.1
-------
REGION I, EPA-NE ORGANIC REGIONAL DATA ASSESS [ ENT (ORDA)*
CASE #: O6 3 SITE NAME: rr1 ‘ I ,
LAB NAME: 050 R ’i 1 4cJLa g II OF SAMPLES/MATRIX: ( oSt , L,2 P8
SDG #: S,44 ) / VALIDATION CONTRACTOR: TTS
SOW f /CONTRACT #: ‘kS OLe4 . i VALIDATOR’S NAME: t 4 -ci
EPA-NE DV TIER LEVEL: ______ DATE DP RECD BY EPA-NE: f
TPO/PO: **ACTION ii ____ DV COMPLETION DATE: G 2.0
ANALYTICAL DATA OUALITY SUMMARY
VOA SV PestIPCB
1. Preservation and Contractual Holding Times C ________
2. GC/MS I GCIECD Instrumen Performance Check 0 ’ _______
3. initial Calibration ______ ( ) _________
4. Continuing Calibration _______ _______ ___________
5. Blanks ______ ______ _________
6. Surrogate Compounds ________ ___________
7. Internal Standards 0 0
3. Matrix Spikeflvlatrix Spike Duplicate _______ L)A ___________
9. Sensitivity Check ! JP _______ ___________
10. PE Samples-Accuracy Check Z . ___________
11. Target Compound Identification ________ ________
12. Compound Quantiration and Reported QLs ________ — 0 ___________
13. Tentatively Identified Compounds 0 0 ____________
14. Semivolatile CleanupfPesticide/PCB Cleanup — ____________
15. Data Completeness 0 ________ ____________
16. Overall Evaluation of Data _______ — __________
o = Data had no problems or were qualified due to minor contractual problems.
m = Data were qualified due to major contractual problems.
z = Data were rejected as unusable due major contractual problems.
ACTION ITEMS: (z items) -?- LJ’ - ’ re
÷ p ’ ‘ -c -i - c -r -c -.
a - i-ce rcto ’eri c d. c &c d -i ( v i &+ rr e r
S J d po 4 j d...td.. p SI .) L .5 cLPI t .fj ( .
AREAS OF
l . -PdJ a
CONCERN: (m items) w ‘- ô’ c - ipL!. &
-jrc .
c-)
COrVIMENTS: d - /°t
I4 r.
—
p.. . ” - 1 -d /&1c - /€. C ,cot . d.
*This form assesses the analytical data quality in terms of contractual compliance only. It does not assess sampling
errors andior non-contractual analytical issues that affect data quality.
* Check ACTION” only if contractual defects resulted in reduced payment/data rejection recommendations.
Va [ jdacor: rv . Date: 6 2o 1
INSTRUCTIONS ON REVERSE SIDE
12/96
EXAHPLE-12/96
-------
GUIDANCE FOR COMPLET1I (G THE ORDA
The ORDA form provides the laboratory’s CLP-TPO and other contract management personnel with an overview
of the contractual analysis and reporting deficiencies found in an analytical data package and identifies those
contractual deficiencies that resulted in reduced payment/data rejection recommendations/actions. The ORDA form
is used to summarize analytical data quality only in terms of contractual compliance. Sampling errors and non-
contractual analytical errors that affect data quality are not summarized on this form, but rather are documented in
the Tier I Validation Cover Letter and Tier 11/Ill Data Validation Reports. For instance, if the sampler did not ship
the samples until after the holding time had expired, a notation would not be made on the ORDA form since the
laboratory is not responsible for the sampler’s actions.
The ORDA form should be completed as follows:
1. Fill in all of the header information (with the exception of the TPO Action/FYI field): Case Number, Site
Name, Laboratory Name, number and matrix of samples in the data package, SDG Number, Validation
Contractor, SOW#/Contract#, Data Vaiidator’s Name, EPA-NE Data Validation Tier Level (i.e., I, II, Ill
or partial 1 1111 1), Date the Data Package was received by EPA-NE, and the Data Validation Completion
Date.
2. Summarize the contractual problems discovered during data Validation by fraction and by evaluation criteria
in the “Analytical Data Summary - table, and in the Action Items” and “Areas of Concern” sections as
described in items 3 through 6 below. Use the Data Validation Memoranda as a guide when completing
the ORDA form.
3. The following qualifiers must be utilized to document contractual problems on the ORDA forms.
0 = Data had no problems or were qualified due to minor contractual problems
m = Data were qualified due to major contractual problems
z = Data were rejected as unusable due to major contractual problems
4. If the data were acceptable, or were qualified due to minor contractual problems, enter the qualifier “o
into the appropriate column (fraction) and row (evaluation criteria). No further documentation is necessary
on the ORDA form. An example of a minor problem would be a semivolatile compound that slightly
exceeded the SOW-specified %RSD initial calibration criterion.
5. If the data were qualified due to major contractual problems, enter the qualifier “m” into the appropriate
column (fraction) and row (evaluation criteria). Use a different superscnpt (m’, &, etc.) for each major
contractual problem identified and provide a brief description of each major problem in the “Areas of
Concern” section. An example of a major contractual problem resulting in data qualification would be a
sernivolatile internal standard that had extremely low area counts (below the lower limit of the SOW-
specified acceptance criterion) and reanalysis was not performed.
6. If the data were rejected as unusable due to major contractual problems, enter the qualifier “z ” in the
appropriate column (fraction) and row (evaluation criteria). Use a different superscript (z’, z 2 , etc.) for
each major contractual problem identified and provide a brief description of each major problem in the
“Action Items” section. An example of a major contractual problem resulting in data rejection would be
contractual holding time criteria that were exceeded for volatiles.
7. Complete the TPO Action/FYI field using the information contained in the “Action Items” and “Areas of
Concern” sections. TPO Action should be indicated with a check mark (V’) in the space following “Action”
only if the contractual defects resulted in reduced payment or data rejection. If no TPO Actions are
indicated, then a check mark (V) should be placed in the space following “FYI”.
8. The validator who completed the ORDA form must sign his/her name in the “Validator” field and enter
the ORDA completion date in the “Date” field.
-------
Christine Clark May 20, 1997
Regional Sample Control Center B-97-05-FF-01
U.S. EPA Region I
60 Westview Street
Lexington, Massachusetts 02173
RE: WA No. 03-718
SDG SAAO1, Case No. 5063
OSO Fine Analytical Labs
Mac’s Marsh
Organic Data Validation
Volatiles: 6/Surface Waters! SAAO1, SAAO2, SAAO3,
SAAO4, SAAO5,SAAO6
(SW Field Duplicate Pair/SAAO5 and SAAOG)
1/Aqueous Trip Blank/SAAO7
1/Aqueous PES/SAA19
Sernivolatiles: 6/Surface Waters! SAAO1, SAAO2, SAAO3,
SAAO4, SAAO5, SAAO6
(SW Field Duplicate Pair/SAAO5 and SAAO6)
1/Aqueous Equipment Blank/SAAO8
1/Aqueous PES/SAA2O
Dear Ms. Clark:
A Tier III data validation was performed on the organic analytical
data for six low level surface water samples, two aqueous blanks
(one volatile trip blank and one semivolatile equipment blank) and
2 aqueous PE samples, collected by U.S. EPA Region I, from the
Mac’s Marsh site. The data validation was performed using the
Region I, EPA-NE Data Validation Functional Guidelines for
Evaluating Environmental Analyses , December 1996 criteria. One
approved modification was used to assess the continuing calibration
low concentration VOA aqueous data. An expanded D of 30 rather
than 25! was used to validate the VOA aqueous data. The volatile
and sernjvolatjle surface water samples, blanks, and PESs were
analyzed under the ARCS DAS program using the low concentration
water Statement of Work OLCO2.1.
EXANPLE-.12/96
-------
Christine Clark
Page 2
The data were evaluated based on the following parameters:
• Overall Evaluation of Data and Potential Usability Issues
* • Data Completeness (CSF Audit - Tier I)
• Preservation and Technical Holding Times
• GC/MS Instrument Performance Check (Tuning)
• Initial and Continuing Calibrations
• Blanks
• Surrogate compounds
* S Internal Standards
NA I Matrix Spike/Matrix Spike Duplicate
* Field Duplicates
NA S Sensitivity Check
• PE Samples/Accuracy Check
• Target Compound Identification
* Compound Quantitation and Reported Quantitation Limits
* Tentatively Identified Compounds
NA • Semivolatile Cleanup
• System Performance
* - All criteria were met for this parameter.
Note: Worksheets, except for Worksheet XIII-Sample
Quantitation, are not included for parameters that
have met criteria or for criteria that are not
applicable (NA) to the method.
The following information was used to generate the Data Validation
Memorandum attachments :
Table I: Recommendation Summary Table - summarizes
validation recommendations
Table II: Overall Evaluation of Data - summarizes Site DQO5
and potential usability issues
Table III: Tentatively Identified Compounds - summarizes
volatile and semivolatile compounds tentatively
identified by GC/MS
Data Summary Tables - summarize accepted, qualified, and rejected
data
EXANPLE- 12/96
-------
Christine Clark
Page 3
Overall Evaluation of Data and Potential Usability Issues
Following is a summary of the site DQOs:
I Data Use - Ecological Risk Assessment for the following
compounds: benzene, trichioroethene, phenol
pentachloropheriol, and naphthalene.
Volatile
Volatile sample results were qualified as a result of both
analytical error and sampling error, it is important to distinguish
between the two because the laboratory does not have control of
sampling error. The following list summarizes the error associated
with sampling: improper sample preservation resulting in missed
analytical holding times.
• Due to a failure to properly preserve samples SAAO]. and SAAO3,
aromatic holding times were not met, therefore, all aromatic
positive detects in samples SAAO1 and SAAO3 were estimated (J)
to indicate potential low bias and all aromatic non-detects in
samples SAAO1 and SAP O3 were rejected (P.) as unusable due to
the possibility of false negatives. This may potentially
impact the assessment of ecological risk.
The following list summarizes the measurement error associated with
analysis: highest point of the calibration curve eliminated for
trichioroethene to meet the RSD criteria, instrument calibration
variability, high surrogate recoveries, and unacceptable PES
results.
• In all samples, SAAO1-SAAO7, positive detects for benzene were
estimated (J) due to a high bias PE sample result and a high
LCS recovery. This may potentially impact the assessment of
ecological risk.
• In all samples, SAAO1-SAAO7, non-detects for trichioroethene,
a contaminant of concern at the site, were rejected (P.) as
unusable due to the possibility of false negatives and all
positive detects for trichioroethene were estimated (J) due to
a low bias PE sample result and a low LCS recovery. As a
result of the rejected trichioroethene non-detects, no
determination of ecological risk can be made. Since the
positive trichioroethene results are estimated (J), any
ecological risk calculated using qualified trichloroethene
data should take into account the uncertainty associated with
the measurement error. It is recommended that these samples
be resampled and reanalyzed to obtain unqualified sample
results.
EX . NPLE-l2/96
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Christine Clark
Page 4
Semivolatile
Semivolatile sample results were qualified as a result of
analytical error. The following list summarizes the measurement
error associated with analysis: missed extraction holding time and
poor acid surrogate and LCS recoveries. Data validation did not
identify any sampling errors.
• In samples SAAQ3 and SAAO4, all acid compound non-detects were
rejected (R) due to low acid surrogate recoveries and low acid
recoveries in the LCS resulting from extraction problems.
Since the non-detects for all acid compounds are rejected (R)
as unusable due to the possibility of false negatives, no
ecological risk determinations can be made for the acid
compounds, specifically for phenol and pentachiorophenol, site
contaminants of concern. It is recommended that these samples
be resampled, re-extracted, and reanalyzed to obtain usable
results.
• In sample SAAO2, the positive detects were estimated (J) and
the non-detects were estimated (UJ) due to a missed extraction
holding time. This may potentially impact the assessment of
ecological risk.
Preservation and Technical Holding Times
Volatile
The following table summarizes the volatile samples which failed to
meet the technical holding time criteria:
Problem
Action
Affected
Samples
Positive
Detects
NDa
Samples not properly preserved
with acid and exceeded aromatic
technical holding time
J - aromatics
A - a].]. non-
aromatics
R - aromatics
A - all non-
aromatics
SAAO1 & SAAO3
Note that for sample SAAO]. there were no positive aromatic detects
and, therefore, all aromatic compound results were rejected CR) as
unusable due to the possibility of false negatives.
EXANPLE- 12/96
-------
Christine Clark
Page 5
Semivolatile
The following table summarizes the serrtivolatile samples which
failed to meet the technical holding tic e criteria:
Problem
Action
Affected
Sainpi es
positive
DetectS
NDs
Extraction technical holding
time exceeded
J
V .1
SA .O2
cc/MS Instrument performance Check (Tuning )
‘0]. a tile
The following table summarizes the volatile samples which failed to
meet the tuning criteria:
Problem
Action
Affected
Samples
Positive
Detects
NDs
The BFB tunes were performed at
14 hr intervals instead of the
contr ctually required 12 hours.
A*
A*
SAAOL-07
* Professional judgment was used to assess the impact on the
data. Since the BFB tunes met the ion abundance criteria; the
internal standards recovered within criteria and there was no
loss of internal standard sensitivity; the data associated
with the non-compliant tunes were considered acceptable.
Semivolatile
All semivolatile tuning criteria were met.
Initial and Continuing Calibrations
‘lola tile
The OLCO2.l continuing calibration %D criteria is 30%; therefore,
an approved expanded data validation %D criteria was used to
evaluate data as per the site QAPjP.
EXANPLE- 12/96
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Christine Clark
Page 6
The following table surnrrtarizes the volatile initial calibration
(IC) and continuing calibration (CC) compounds which failed to meet
the calibration criteria of %D < 30% and %RSD < 30%:
I Instrument
M
14 Action
Affected
Samples
Compound
IC
2/27/97
j
CC Positive
3/29/97 detects [
NDo
Tetrachioroethene
%RSD = 60%*
A - s lOug/L
J - > lOugfL
A
SAAO3.-07
].,2-Dibromoethane
%D 38%
.3
UJ
SAAO1 & SAAO3
* The percent RSD for tetrachioroethene was 60% and the average
RRF was 0.07. When the highest calibration point was
eliminated and a four point calibration curve was used, the
%RSD was 18%. Therefore, since linearity was established, all
positive detects and non-detects for the associated samples
with tetrachioroethene results at the highest linear point (10
ug/L) or below were accepted. The positive results for
tetrachioroethene reported above 10 ug/L samples in SAAO2 and
SAAO3 were estimated (J).
Note that for samples SAAO1 and SAAO3 there were no positive
detects for dibrornoethane.
The continuing calibrations for the volatile low concentration
waters were performed at 14 hour intervals instead of the
contractually required 12 hour interval. However, the continuing
calibration met criteria, therefore, professional judgment was used
to accept the data.
Sexnivolati le
All criteria were met for semivolatile surface water calibrations.
Blanks
The following table summarizes the level of volatile and
semivolatile blank contamination detected in the laboratory,
equipment, and trip blanks:
Compound
Type of
Blank
Max
Conc.
g/L
Action
Level
ug/L
CRQL
ug/L
Chloroform
Trip
15
75
1
Di-n-butylphtha late
Method
12
120
5
EXANPLE-12/96
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Christine Clark
Page 7
Volatile
Chloroform was detected in the trip blank at a concentration of 15
ug/L with an action level of 75 ug/L. The source of chloroform,
which was not detected in any of the samples, is unknown. Either
another source for the trip blank water should be used, or
additional testing of the trip blank water prior to use should be
performed. The sampler was notified. (See Phone Log). Chloroform
was not detected in any field samples, therefore, no qualifications
were necessary.
All volatile laboratory blanks were free of contamination.
Semivolatile
Di-n-butylphthalate was detected in a laboratory method blank at a
concentration of 12 ug/L. Since di-n-but.ylphthalate is a common
laboratory contaminant, the lOx rule applies. Sample results less
than 10 times the blank contaminant concentration but greater than
the CRQL are qualified U. Di-n-butylphthalate was not detected in
any of the samples, therefore, no action was taken.
Surroq’ate Compounds
Volatile
The following samples had surrogate spike recoveries outside of the
recovery limits:
Surrogate
% Rec
QC Liznit
Action
Sa. p1e
Number
[ -
Positive NDs
Detects
BFB
132
80-120
J A
SAA03
BFB
142
80-120
Data not reported
SAA O3RE
The surrogate brornofluorobenzene recovered outside of the QC limits
in volatile surface water sample SAA03. The sample was reanalyzed
within the analytical holding time, and again the BFB recovered
high. The results for sample SAAO3 were reported from the original
analysis and all positive detects were estimated (J) . The
reanalysis was submitted to verify that a possible matrix
interference was the cause of the high surrogate recovery and not
laboratory error.
EXANPLE-12/96
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Christine Clark
Page 8
Semivolatile
The following samples had surrogate spike recoveries outside of the
recovery limits:
Sa iple
Nuaber
Surrogate
% Rec
QC
Limits
Action I
.
Positive
Detects
NDs
S AD3
Phenol-dS
S
15-115
J - all acids
R - all acids
2,4,6-Tribromophenol
12
15-130
J - all acids
R - all acids
SAA O4
Phenol-d5
3
15-115
J - all acids
R - all acids
2-Fluorophenol
10
15-110
J - all acids
R - all acids
Samples S A03 and SAAO4 both reported two out of three acid
surrogates below the QC acceptance limits. In addition, Phenol-d5
recovered at less than 10% in both samples. These two samples and
the LCS were prepared separately from the other samples in the SDG.
The laboratory did not provide an explanation for preparing the
samples in different batches. It appears as if there was a problem
with the extraction and/or concentration of the sample extracts for
acid compounds and acid surrogates for samples SA.A03 and SAP 04. As
a result of the low acid surrogate recoveries in samples SA.A03 and
SAP 04, all acid non-detects were rejected (R) as unusable due to
the possibility of false negatives. There were no positive acid
detects. The laboratory failed to re-extract and reanalyze the
samples as required in the DAS analytical specification. It is
recommended that these samples be collected again, re-extracted,
and reanalyzed if warranted to achieve site DQOs.
PE Samples - Accuracy Check
Volatile - LCS and PES
The following table summarizes the volatile compounds that failed
to meet the LCS recovery limits:
Copouad
% Roe
QC
Limits
Action J
Affected
Samples
Positive
Detects
j
NDs
Benzene
180
60-140
J
A
SAAO1-07
Trichioroethene
28
60-140
J
UJ
SP A0107
EXANPLE- 12/96
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Christine Clark
Page 9
An aqueous low concentration volatile PEG was obtained from Region
I OEME-QA. The results of the performance evaluation sample, EPA
number SAA19, did not meet the required criteria for the following
compounds. The following table notes the score and corresponding
action.
Compound
Score
Action
Affected
Samples
Positive
Detects
NDs
Benzene
Action High
J
A
SAAO 1-07
[ Trichioroethene
Action Low
J
R
SAA O1O7
The laboratory has demonstrated an inability to accurately recover
benzene and trichioroethene through poor LCS recoveries and poor
PES results. Since benzene recoveries, in both the LCS and the
PES, were above the QC acceptance limits, the sample results for
benzene are potentially biased high. Since trichloroethene
recoveries, a contaminant of concern at the site, in both the LCS
and the PES, were below the QC acceptance limits, the sample
results for trichioroethene are potentially biased low. The
results of the performance evaluation sample EPA number SAA1S met
all criteria for the following compounds: 1,2-dichloroethane,
toluene, 2-butanone, ethylbenzene, and tetrachioroethene.
Semivolatile - LCS and PEG
The following table summarizes the semivolatile compounds that
failed to meet the specified LCS recovery limits:
Compound
% ec
QC
Limits
Action
Affected
Samples
Positive
Detects
NDs
Phenol.
10
40-120
J all acids
R all acids
S .A03, SAAO4
2-Chiorophenol
22
50110
SAAO3, SAAO4
AAO3. SAAO4
2,4,6-Tribrornophenol
19
40-120
The low recoveries of the acid compounds in the LCS coupled with
the low acid surrogate recoveries in samples SAAO3 and SAAO4
indicate a possible laboratory accuracy problem since the samples
were extracted with the LCS. It appears as if the acid compounds
might have been lost in the extraction and/or concentration phase.
The fact that the acid PES compounds were recovered within the QC
acceptance limits and that the PES was extracted in a different
batch from samples SAAO3 and SAAO4 also leads the validator to
conclude that the extraction/concentration problem was limited to
samples SAAO3 and SAAO4 and the LCS. As a result of the poor
EXANPLE-12/96
-------
Christine Clark
Page 10
laboratory accuracy, all acid non-detects in samples SAAO3 and
SAAO4 were rejected (R) as unusable due to the possibility of false
negatives. There were no positive acid detects in samples SAAO3
and SAAO4. Since ecological risk cannot be determined for either
phenol or pentachiorophenol for samples SA 03 and SAAO4, it is
recommended that these samples be resampled, re-extracted, and
reanalyzed to obtain usable results.
An aqueous low concentration sernivolatile PES was obtained from
Region I OEME-QA. The results of the performance evaluation
sample, EPA sample number SAA2O met all criteria for the following
compounds: bis (2-chioroethyl) ether, hexachioroethane, fluorene,
pentachiorophenol, 2,4-dimethyiphenol, 3-nitroaniline,
benzo (b] fluoranthene, and benzo Ek] fluoranthene.
Tarqet Compound Identification
In sample SAAO4, the laboratory identified the peak with molecular
ion 128 as 2-chiorophenol. Retention time comparison suggests that
naphthalene would be a more accurate identification of this peak.
The laboratory was contacted on 5/8/97, but did not respond.
Therefore, the validator used professional judgment to report
naphthalene as detected on the Data Summary Table, and 2-
chiorophenol was reported as ND at the CRQL.
System Performance
Volatile
The results for the volatile surface water samples indicate major
analytical data quality problems in the analysis of trichioroethene
and benzene, which are contaminants of concern at the site. The
“Action Low” PE score for trichioroethene and “Action High” PE
score for benzene was substantiated by the low LCS recovery for
trichioroethene and high LCS recovery for benzene.
Semivolatile
The results of the semivolatile surface water samples indicate a
laboratory problem. The acid surrogates in two samples recovered
low. The LCS prepared with those two samples recovered all acid
compounds below the QC limits with some < l0 . Furthermore, the
PES sample extracted in a different batch recovered the acid
compounds and surrogates without any problems. It appears as if
the laboratory had a problem in the extraction/concentration phase
for the extraction batch associated with these two samples.
EX.AMPLE-12/96
-------
Christine Clark
Page 11
Please contact M. Howard at (999) 232-7000 if you have any
questions regarding this information.
Very truly yours,
HOWARD ENVIRONMENTAL
2. HCtc,’CL
M. Howard
Data Validator
S. / /ôiua, L
S. Howard
Senior Validator
cc: Victor Hernon, EPA Site Manager
Attachments: Table I: Recommendation Summary Table
Table II: Overall Evaluation of Data
Table III: TIC Summary Table
Data Summary Tables
Data Validation Worksheets
PES Score Reports
Communication/Phone Logs
Field Sampling Notes
Reduced Payment Letter
EPA-approved QAPjP amendment
CSF Audit (DC-2 Form)
DQO Summary Form
EXAMPLE- 12/9 6
-------
TABLE I
RecomntendatiOfl Summary Table for Volatiles
Mac’s Marsh
SDG SAAO1
TABLE I: RECOMMENDATION SUMMARY TABLE
[ Sample Number
Matrix
Qualifiers
SAAO1
SW
J’ 3 1 R’
SAAO2
SW
J 2 . 5
SAAO3
SW
J 12345 1 R 1
SAAO4
SW
R 2
SAAO5
SW
R 2
SAAO6
SW
R 2
SAAO7
SW
R 2
- Aromatic analytical holding times: J aromatic detects
(Potential low bias)
- Highest point of the initial calibration curve for
tetrachioroethene eliminated to meet the %RSD criteria: J
tetrachioroethene detects above 10 ug/L
- D criteria ( D > 30’d: UJ 1,2-dibromoethane non-detects
- High surrogate spike recovery for BFB: J detects (Potential
high bias)
- Unacceptable PES and LCS results: J benzene (Potential high
bias) and trjchloroethene detects (Potential low bias)
- Aromatic analytical holding times; R aromatic non-detects
(Possibility of false negatives)
R 2 - Unacceptable PES result: R trichioroethene non-detects
(Possibility of false negatives)
EXAMPLE-12/96
-------
TABLE I
Recommendation Summary Table for Semivolatileg
Mac’s Marsh
SDG SAAO].
I TABLE I: RECOMMENDATION StJT 4MARY TABLE
Sample Number
Matrix
Qualifiers
Acid
B/N
SAAO1
SW
A
A
SAAO2
SW
J
J 1
SAAO3
SW
R” 2
A
SAAO4
SW
R’ 2
A
SAAO5
SW
A
A
SAAO6
SW
A
A
SAAO8
SW
A
A
J 1 - Extraction holding times: J detects, UJ non-detects
(Potential low bias)
R 1 - Low acid surrogate recoveries (some < 10 9 d: R all acid non-
detects (Possibility of false negatives)
R 2 - Low acid compound recoveries in the LCS (one 1O ): R all
acid non-detects (Possibility of false negatives)
A - Accept all data
EXA}IPLE-l2/96
-------
EPA-NE - Data Validation Worksheet
Overall Evaluation of Data - Data Validatloit Memoranduiti - Table 11
VOLATILE ORGAN ICS
DQO (list all DQOs)
Sain ,ling* and/or
Analytical Method
Appropriate
Yes or No
Measurement Error
Smnpliiig
Variabili ty
I’otciiiinl
Usability
Issucs
Analytical Error
Sampling Errort
•Determiiie the presence of
ecological risk iii surface waters -
compounds of interest are:
Trichioroetliene
Dcnzcne
Analytical method:
Yes, CLP SOW
OL O2.1
Sampling method:
Unknown
Refer to qualifications
in RIS Key:
J 4
R 2
Refer to qualiuicatioiis
iii RIS Key:
i’
R’
•Rcjcct all tricliloroctlicne non-
deiccis in all volaiilc surface water
samples due to low bias of P13
result and the possibility of false
negatives. All tricliloroethene
positive iletcets ate potentially
biased low.
•Aromatic i,on-delccts are rejected
in volatile samples SAAOI &
SAAO3 due to Ircserva(iolt
violations.
•AIl bcn7culc positive (1dec15 for
all samples arc potentially biased
high due to high bias of PES
results.
* The evaluation of “sampling error” cannot be completely assessed in data validation.
Sampling variability is not assessed iii data validation.
Validator: “ ‘ -
Date:
0
(‘1
r;1
M
12/96
-------
EPA-NE - Data Validation Woikshcet
Overall Evaluation of Data - Data Validation Meinorauduni - Table 11
SEMIVOLATILE ORGANICS
DQO (list all DQOs)
Sampling and/or
Analytical Method
Appropriate
Ycs or No
Measurement Error
Sampling
Variability**
Polenlial
Usabilily
Issucs
Analytical Error
Sampling Errort
•Determine the presence of
ecological risk in surface waters -
compounds of inreresi are:
Phenol
Pcnlacliloropliciiul
Naptithalene
Analyiical method:
Yes. CLP SOW
OLcU2.1
Samnpliuig iiicthod:
Unknown
Refer to qualifications
in R/S Key:
ji
Rta
Refer to qualifications
iii k/S Key:
•All acid compound mioii-dclccts
arc rcjcclcd in seuimivolatilc samples
SAAO3 & SAAO4 due lo exractioII
problems. Time phenol and
j ciilacliloropliciiol iiwi-deiccts lot
SAAU3 & SAAO4 arc uiiusablc due
to the possibility of false negatives.
• MI scioLvotatite positive detects
m md quaulila lion limits (iiicludimig
those for phenol,
pciitacliIoroplmeimol, and
naplitlialcuc) are estimated in
SAAO2 due 10 mimisscd extraction
holding time.
* The evaluation of sampliiig error ’ t cannot be completely assessed iii data validation.
** Sampling variability is not assessed in data validation.
Validator: • ii1. )L/ )L(JCCL .e
Date: ____________
0
a’
r-i
____ r
12/96
-------
TABLE III: VOLATILE TENTATtVELY IDENTIFIED COMPOUND SUMMARY
There were no reported volatile tentatively identified compounds.
EXAMPLE- 12/96
-------
TABLE III: SEMIVOLATILE TENTATIVELY IDENTIFIED COMPOUND SUMMARY
Classification/isomer
SAAOi.
SkP 1 O2
SAAO3
SAAO4
SAAO5
SAAO6 I
Dodecarioic acid
1
1
Unknown hydrocarbon
1
1
1
1
Saturated hydrocarbon
1
1
1
Meptacosane
1
1
1
Dimethyiphenanthrene
1
1
ulH-Benzo (a] fluorene
1
Perylene
1
1
1
The number indicated in the above table represents the number of compounds
of that classification identified in the sample.
EXAMPLE-12/96
-------
DATA Su1vevvu Y lADLE
Volatile Aqueous Analysis
ugIL
SITE Macs Marsh - Debsvilie. MA
CASE NO.. 5063 SOC NO• SA A O1
SAMPLE NUMBER. SAA O I SAAO2 SIV 03 SAAO4 SAA0 SAAOG SAA O7
STATION LOCATION. US OSI 0 52 DS Cs CS DUP TO
LABORATORY NUMBER. LABO 1 LABO2 LABO3 LAB O4 LAB O5 LAB O6 LAOO7
FIELD DUP FIELD DUP TRIP BLANK
COMPOUND CRQL
Chloromethane 1 1 U 1 U 1 U I U 1 U I U I U
Bromomelhane 1 1 U 4 1 U 3 1 U 1 U 1 U
Vinyl Chloride 1 1 U I U 1 U 1 U 1 U I U 1 U
Chioroethane I 1 U I U I U 1 U I U 1 U 1 U
Methylene Chloride 2 2 U 6 2 U 2 U 2 U 2 U 2 U
Acetone 5 5U 5 1J 5U 5U 5U 5U 5U
Carbon Disullide 1 1 U 1 U 1 U 1 U 1 U 1 U 1 U
1,1-Dich loroelhene 1 1 U I U 1 U 1 U 7 9 1 U
1.1.Dich loroeihane 1 1 U 1 U 1 U I U 1 U 1 U 1 U
cls.1,2-D lchloroethene I I U I U 1 U I U 1 U I U I U
trans.1,2-Dlchtoroethene I I U I U I U I U I U 1 U 1 U
Chloroform 1 1 U I U 1 U I U 1 U 1 U 15
1.2 -Dichioroethane I I U 1 U I U 1 U I U 1 U I U
2-Butanone 5 5 U 5 U 5 U 5 U 5 U 5 U 5 U
Bromothtoronielhai e I I U 1 U I U 1 U I U I U I U
1.1.1-Tr lch ioroethane 1 1 U I U 1 U 1 U 13 15 1 U
Carbon Tetrachioride I 1 U I U I U 1 U 1 U 1 U 1 U
Bromodich ioron ,ethane 1 1 U I Li 1 U 1 U 1 U I U 1 U
1.2.D lchloropropane I I U I U I U I U 1 U 1 U 1 U
cis-1.3-Dlchloropropene I I U 1 U I U I U 1 U 1 U 1 U
Trithioroethene I R 9 J 4 J R ii R R
Dibromochloromethane 1 1 U 1 U 1 U I U I U I U I U
L12-Trlth loroethane 1 I U I U 1 U I U 6 6 1 U
Benzene I R 8 J 9 J I U 1 U 1 U 1 U
trans-1,3 .D lth loropropene 1 13 1 U 1 U I U 1 U 1 U I U
Bromolorm I I U I U 1 U 1 U 1 U I U 1 U
4-Melhyl-2.Pen tanone 5 5 U 5 U 5 U 5 U 5 U 5 U 5 U
2-Hexanone 5 5 U 5 U 5 U 5 U 5 U 5 U 5 U
Tetcachloroethene 1 1 U 11 J 12 J 1 U 1 U 1 U 1 U
To luene 1 18 J 10 21 J I U 1 U I U I U
1.1.2.2-Tetrach loroethane 1 I U I U 1 U I U 1 U I U I U
1.2-Dibromoethane 1 1 UJ I U 1 UJ 1 U 1 U I U 1 U
Ch lorobenzene 1 R 1 U R 1 U 1 U 1 U 1 U
Ethylbenzene I R 1 U R I U 1 U 1 U I U
Slyrene I R 1 U Il 1 U I U 1 U 1 U
Tolal Xylenes 1 R I U R 1 U 1 Ii I U I U
1.3-Dlchi orobenrene I R I U R 1 U I U 1 U I U
1.4 -Dich lorobenzene I R 1 U R 1 U I U 1 U I U
1.2 -Oichlorobenzene I R I U R I U I U 1 U I U
1.2 -D ibromo-3.chloropropane 1 1 U 1 U 1 U I U I U 1 U 1 U
1.2.4.Trlchtorobenzene I R I U R 1 U 1 U I U I U
nnnrcerrr eetn=r=r=ee====flt
D 1LUTIONFACTOR: 10 10 10 10 10 10 10
DATE SAMPLED: 03123197 03123/97 03123197 03123197 03/23197 03 /23/97 03/23/97
DATE ANALYZED• 04/04/97 03129197 04/04/97 03/29/97 03/29/97 03/29/97 03/29/97
-------
D MA SUMMARY lADLE
Seinivolalula Aqueous Analysis
ugfl.
SITE Macs Marsh - Debsvulle. MA
CASE NO: 5063 SDCNO SAAOI
SAMPLE NUMBER- SAAO1 SAAO2 SAAO3 SM O4 SAAO S 5ftA06 SAAOB
SAMPLE LOCA IION US 0 51 052 DS CS Cs DUP l EG
LABORAtORY NUMBER LABO I LABO2 LABO3 LA1304 L A G O S 1/WOO I ABOB
FIELD OUP FIELD DUP EQUIP. BLANK
COMPOUND CR0
Phenol 5 5 % ) SU ) R A 10 12 5U
bls(2-Chloroelhyl) elher 5 5 U S Ui S U S U 5 U 5 U S U
2 -Chloropluenol 5 SU 5Ui I i A SU 5U SU
2 -MelhyIplu noI 5 14 5 Ui A A 5 U 5 U 5 U
2 ,2-oxybls(1-Chloropropane) S 5 U 5 Ui 5 U S U 5 U S U S U
4-Me lhyiphenol 5 SU SUi A A 5U 5U SU
N-Nilioso .dI .n .propylamlne 5 5 U S Ui S U 5 U 5 U 5 U 5 U
Hexath loroelbane 5 5U 5Ui 5U SU 5U SU 5U
Nutrobenzene 5 SU SUi SU SU SU SU 5U
Isophocone 5 5 % ) S W 5%) 5%) SU SU SU
2-Niltoplienol 5 5U 5Ui A A SU 5U SU
2 .4 -D lmethy lphenol 5 5 U 5 Ui A A 6 B 5 U
bls(2-Chloroelhoxy jmelhane 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
2 .4-Dich lorophenol 5 5 U 5 UJ A A S U 5 U 5 U
Naph lha lene 5 5U 12J 5U 12 42 47 SU
4-Ch loroan irune 5 5U 5UJ 5U SU SU SU SU
Hexac l u lorobutad lene 5 5U SUi 5U 5U SU 5U 5U
4-Chloro-3-Melhylphenol 5 5 U 5 Ui A A 5 U 5 U 5 U
2-Methylnaphll ;aleite 5 5 U S Ui 5 U S U S U S U S U
Hexachlorocyclopenladlene 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
2 .4 .6-Tr lth lo rophenol 5 5 U 5 Ui A A 5 U 5 U 5 U
2 .4.5 -Trich lorophenol 20 20 U 20 Ui A A 20 U 20 U 20 U
2-Chloronaphthalene 5 SU SUi SU SU 5 % ) 5% ) SU
2-Nu lroani line - 20 20 % ) 2 OUJ 20U 20U 20 % ) 20U 20U
Olmethy iph lhalate 5 SU 5Ui 5U 5U 5%) 5U 5%)
Acen apl u lhylene 5 SU 5Ui SU SU 5U 5U SU
2 .6-D l nitrotoluene 5 5U 5UJ 5U 5U SU SU SU
3-NIlroanIIine 20 20 U 20 UJ 20 U 20 U 20 U 20 U 20 U
Acenaplithene 5 5 U 5 Ui 15 5 U 22 27 5 U
2.4-Dlnllrophenol 20 20 U 20 Ui A R 20 U 20 U 20 U
4-N u lrophenol 20 20 U 20 Ui B B 20 U 20 U 20 U
Otenzoturan 5 SU 5UJ SU SU 5U 5U SU
2,4-tjlnltrotoluene 5 SU SUJ 5U 5U SU 5 % ) 5U
Qlethylphthalate 5 SU SUJ 5U SU 5U 5%) SU
4-Ch lorophenyl-Phenyletl ier 5 5 U 5 Ui 5 U S U S U 5 U 5 U
Fluorene 5 SU 19) 5U 5 % ) SU 5U 5U
4-N utroanuflne 20 20 U 20 Ui 20 U 20 U 20 U 20 U 20 U
4 ,6-QInIlro -2-Me lhylphenol 20 20 U 20 Ui R A 20 U 20 U 20 U
N-nitrosodlpheny lamlne 5 5 U 5 Ui 5 U S U 5 U 5 U 5 U
4-Bromophenyi.Phenylether 5 5 U 5 Ui S U 5 U 5 U 5 U 5 U
Hexachlorobenzene 5 15 5 % ) ) 5U 5U 5U SU SU
Penlach lo rophenol 20 20 U 20 Ui A A 20 U 20 U 20 U
Phenanlhrene 5 5%) SUi SU SU 33 34 SU
Anthracene 5 5U 5Ui 5U SU 5U 5U SU
DI-n-bulylphthatate 5 5U 5Ui 5U SU SU SU 5%)
-------
DATA .. ._. . ..RY TABLE
Sernivolalile Aqueous Analysis
ug/L
SITE Macs Marsh - Debsville. MA
CASE NO• 5063 SDG NO: SA.A01
SAMPLE NUMBER. SAAO1 Sf%A02 SAAO3 SAAO4 SMO5 SAAO6 SAAO8
SAMPLE LOCATION. US OS1 0S2 Os G5 GS OUP EB
LABORATORY NUMBER LABOl LABO2 LABO3 LABO4 LAB05 LAB O6 LABO8
FIELD DUP FIELD DUP EQUIP. BLANK
COMPOUND CR0
Fluoran lhene 5 5 U 5 Ui 5 U 5 U 5 U 5 U S U
Pyrene 5 SU S W 5U 5U 50 5U 5U
Butylbenzy lphtha late 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
3,3’•D lchtorobenzidine 5 5 U 5 UJ 5 U 5 U 5 U 5 U 5 U
Benzo(a)anthracene 5 5 U 5 Ui 5 U 5 U 5 U S U 5 U
Chrysene 5 5 U 5 Ui 5 U 5 U 21 17 5 U
Bis(2-elhy lhexy l)phlha la le 5 5 U 5 UJ 5 U 5 U 5 U 5 U 5 U
Di-n-octy lphthalate 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
Benzo(b)fluoranthene 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
Benzo(kjfluoran lhene 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
Benzo(a)pyrene 5 5 U 5 UJ 5 U 5 U 5 U 5 U 5 U
Indeno(1.2.3-cd)pyrene 5 5 U 5 UJ 5 U 5 U 5 U 5 U 5 U
Dibenz(a.h)anthracene 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
Benzo g.h.s)peiytene 5 5 U 5 Ui 5 U 5 U 5 U 5 U 5 U
DILUTION FACTOR. 1 0 1 0 1 0 1 0 1 0 1 0 1 0
DATE SAMPLED 03/23/97 03 (23197 03/23/97 03/23/97 03/23/97 03/23/97 03123/97
DATE EXTRACTED. 03(29/97 04/04/97 03130197 03/30197 03/29/97 03129197 03/29/97
DATEANALYZED 04113197 04113197 04(13197 04/13(97 04113/97 04/13(97 04113197
to
H
-------
EPA-NE
Data Validation Worksheet Cover Page - Page 1
Site Name mo ..c ’ s
Reference No. rv \
REGION I ORGANIC DATA VALIDATION
The following data package has been validated:
Lab Name OSO a 1’ c. .i-O U-bs
Case/Project No. cpC 3
SDG No. 5 i°rOi
No. of Samples/Matrix SL - 1 L
Trip Blank No. 54I’ O?-
Equipment Blank No. 5 1 4b&
Botle Blank No. , VOA/C -& / k Lot / ,..c) pr ./itI- /y t J ck d / 196
Field Duplicate Nos. __ S4. 9t c
PES Nos.
The Re2ion 1. EPA-NE Data Validation Functional Guidelines for Evaluatin2 Environmental Analyses,
revision J?4 (, was used to evaluate the data or 1 ov drnodifications to the 1 PA:N
( iionai were ii ë to evaluate the data and are attach d to this cover page: (attach modified
criteria from EPA approvedQAPjP or amendment to QAPJP). 4 e v (&C4ed p 9 Z.
A Tier II or6j evaluation was used to validate the data (circle one). If a Tier U validation with a
partial Tier Ill was used, then identify samples, parameters, etc. that received partial Tier III validation
The data were evaluated based upon the following parameters:
- Overall Evaluation of Data
- Data Completeness (CSF Audit - Tier I)
- Preservation & Technical Holding Times
- GC/MS & GC/ECD Instrument Performance Check
- Initial & Continuing Calibrations
- Blanks
- Surrogate Compounds
- Internal Standards
- Matrix Spike/Matrix Spike Duplicate
Region I Definitions and Qualifiers:
- Field Duplicates
- Sensitivity Check
- PE Samples/Accuracy Check
- Target Compound Identification
- Compound Quantitation and Reported
Quancitacion Limits
- TICs
- Setnivolatile and Pesticide/PCB Cleanup
- System Performance
A - Acceptable Data
J - Numerical value associated with compound is an estimated quantity.
R - The data are rejected as unusable. The R replaces the numerical value or sample quantitarion limit.
U - Compound not detected at that numerical sample quanticarion limit.
UJ - The sample quantication limit is an estimated quantity.
TB, BB, EB - Compound detected in aqueous trip blank, aqueous bottle blank, or aqueous equipment
blank associated with soil/sediment samples.
Validator’s Name P A .
Date Validation Started __________
•Company Name 113 Phone Number 73 000
Date Validation Completed ‘ ?O
SOW/Method No.
Sampling Date(s)
Shipping Date(s)
Date Rec’d by lab
Traffic Report Sample Nos. ) I .- 5/ I O( ,
- D4S
3. ç.
EXANPLE-.].2/96
12/96
-------
EPA-NE
Data Validation Worksheet Cover Page - Page 2
Check if all criteria are met and no hard copy worksheet provided. Indicate NA if worksheet is not applica 1e
to analytical method. Note: there is no standard worksheet for System Performance, however, the vali
must document all system performance issues in the Data Validation Memorandum.
VOA/SV worksheets :
VOA/SV-Pest/PCB COMPLETE SDG FILE (CSF) AUDIT V
VOA/SV-PesdPCB-I PRESERVATION AND HOLDING TIMES ____
VOA/SV-II GC/MS INSTRUMENT PERFORMANCE CHECK (TUNING) ____
VOA/S V-Il l INITIAL CALIBRATION _____
VOAJSV-IV CONTINUING CALIBRATION ____
VOA/SV-Pest/PCB-V-A BLANK ANALYSIS _____
VOA/SV-Pes tJPCfl-V-B BLANK ANALYSIS _____
VOA-VI VOA SURROGATE SPIKE RECOVERIES ____
SV-VI SV SURROGATE SPIKE RECOVERIES ____
VOAJSV-VU INTERNAL STANDARD PERFORMANCE ____
VOA/SV-PesUPCB -VJII MATRIX SPIKE/MATRIX SPIKE DUPLICATE _____
VOAJSV-PestJPCB-JX FIELD DUPLICATE PRECISION ____
VOA/SV-Pe /PC3 -X SENSITIVITY CHECK I JA
VOA/SV-PestJPCB-XI ACCURACY CHECK ____
VOA/SV-PestJPCB -X1J TARGET COMPOUND IDENTIFICATION ____
VOAJSV-PesUPCB -XjII SAMPLE QUANTITATION ____
VOA/SV-XW TENTATIVELY IDENTIFIED COMPOUNDS ____
VOAJSV-XV SEMI VOLATILE CLEANUP ____
TABLE Il-WORKSHEET OVERALL EVALUATION OF DATA ____
PestIPCB worksheets :
VOAJSV-PestJPCB COMPLETE SDG FILE (CSF) AUDIT
VOA/SV-Pest1PCB-I PRESERVATION AND HOLDING TIMES
Pes t/PCB-IIA GC/ECD INSTRUMENT PERFORMANCE CHECK-
RESOLUTION
Pest/PCB-UB GC/ECD INSTRUMENT PERFORMANCE CHECK-
RETENTION TIMES
Pest/PCB-IIC GC/ECD INSTRUMENT PERFORMANCE CHECK-
ACCURACY CHECK OF INITIAL CALIBRATION
PestJPCB-IID GC/ECD INSTRUMENT PERFORMANCE CHECK-
PESTICIDE DEGRADATION
Pest/PCB-III INITIAL CALIBRATION
Pest/PCB-IV CONTINUING CALIBRATION
VOA/SV-PestJPCB-V-A BLANK ANALYSIS
VOA/SV-PesUPCB-V.B BLANK ANALYSIS
Pest/PCB-VI SURROGATE COMPOUNDS:
SPIKE RECOVERIES AND RETENTION TIME SHIFT
Pest/PCB-VII PESTICIDE CLEANUP
VOAISV-Pest/PCB -VIII MATRIX SPIKE/MATRIX SPIKE DUPLICATE
VOA/SV-PesijPCB-IX FIELD DUPLICATE PRECISION
VOA/SV-Pest/PCB-X SENSITIVITY CHECK
VOAJSV-PescJPCB.XI ACCURACY CHECK
Pest/PCB-XII COMPOUND IDENTIFICATION
VOAISV-PestjPCB-XJII SAMPLE QUANTITATION
TABLE 11-WORKSHEET OVERALL EVALUATION OF DATA
I certify that all criteria were met for the worksheets checked above.
Signature: fl . Name: ( Y1Oe /ô Ja c
Date:
12/96
-------
The data validator generates a Data Validation Report, applicable to Data Validation Tiers II and III, that consists
of the following components in the order specified below: (Refer to Section 11 for a description of each of the
Data Validation Report components).
1. Organic Regional Data Assessment/Inorganic Regional Data Assessment
(ORDA/IRDA) Form
2. Data Validation Memorandum
a. Narrative
b. Table I-Qualifier Recommendation Summary Table
c. Table Il-Overall Evaluation of Data
d. Table Ill-Tentatively Identified Compounds
e. Data Summary Tables
3. Standard Data Validation Worksheets
a. Manual
b. Automated Data Review Reports (i.e., CADRE)
4. Support Documentation
a. Copy of non-CLP analytical method, e.g., DAS methods, modified EPA methods
b. Copies of PES Score Reports/Vendor PES QC Acceptance Limits
c. Copies of Telephone Logs/Communication Forms for:
• RSCC communications
• Requests for laboratory data resubmissions/clarifications
• Communications with samplers resolving sampling problems
• Communications with TPO/Lead Chemist to report contractually-deficient data
for rejection/reduced payment
• Communications with EPA Site Manager concerning possible data rejection
• EPA Site Manager authorization for alternate DV tier
d. Copies of data supporting recommendations for reduced payment resulting from CSF
Audit and/or PE sample result evaluation
e. Original data to support recommendations for data rejection/non-payment identified from
Tier II or Tier HI data validation
f. Copies of field sampling notes andlor field report supplied by field sampler
g. Copies of EPA-approved amendments to QAPjP andlor SAP describing modified criteria
to be used for validating site data
5. CSF Completeness Evidence Audit
6. DQO Summary Form
The data validator is responsible for implementing all corrective actions required by the contractor Lead Chemist
in response to EPA-NE data validation oversight findings.
12196
EXAMPLE-12/96
-------
12/96
Ssnu t Mo
iit Ho
M,t,j
nc,
Code
I)aic
Sm, 1 led
VOA I
DfIA
I
“I_Sil l C_Il
Date
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ham S iip.
to U ,aI
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trim, Saint.
to Late /( )
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I ‘-‘ar’
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to Anal
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J t•i ac
I a( L ay
(r,nhI Sati .p
to I_au I( )
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( ,Irnl L lr
to An,I.
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ot
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— —
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Pr ervn(lo,i Code:
1. Cuul@4°C(±2°)
2. Preserve with llCl to at least p 11 2
3. Protect froni light
4. Freeze
5. Room Temperature (Avoid excessive heat)
(Extrnc(lun Code:)
UL - Liquid/Liquid
SON - Soimication
SEP - Separatory Funnel
SOX - Soxhmlet
SPE - Solid Phase Extraction
Action Coile:
J - Estimate (J) Dctcctcd Valucs
Ui - Estimate (Ui) Non-Detected Values
R - Rcjcct (R) Non-Detected Values
EPA-NE - Dal latioii
VOA/SV - Vesl/I’C [ l-I
Sampler: oe rt;f; i
Company: 4 0 u,O1 c [ Eiwiconni j An.O Contacted: No
PRESERVATION AND 1IOLDlN 3 TIMES - Circle sauiiplc imumnbcrs with cxcccdcd icchuiical holding times or oiuiltcd l)fCSCrVatiUtm.
List all required jmreservat oit codcs mul circle oimmittcd l)Ieservahiomm codes.
Circle all exceeded technical hmoldimig times.
Identify extraction technique after “ft of Days”/( t Extraction Code).
D.ttc: S.(.o Zl
(s
H
r
Validator: fl ”\. -&cti.) -
Date: ________
-------
EPA-Nfl - Data Validatioti Woikslicct
VOA/SV-I!
11. C C/MS INSTIWMENT 1’ElUrOIth’IANCE C11U CK (TU IN C)
List all Instrument Perluniiaiicc Cheeks that flLC outside method QC Luililig acceptance c i itet ia.
Volatile
liis(ruiiient l’erfuriiiniucc Check
(Coitliwiuliti Name)
Aiiaiy fs
Dnte mid ‘lime
lush uunent
loii(c)
Alfected
Percent
Relative
Ab iri ui laiiec
QC
Lliiiits
Samples All ecteil
Action
1?
TY\
Soj-Sfl, Q -
I
Coinmenis: j& 11- &c L1 &* t.to.Q r 4 e& c 1 -I(-g. S
r ’sjo.J c -‘ S - - -Q Crt 41’ . - -‘ - ‘ - ‘ - ‘d a -Q.Q j ’ w- rc 0 -R- . : t
So c - + p c , - 4 L& v-4. Prt-( C n4r t)s’I v- rc c -tp .-ble .. -A. ,-/A -t.
a-e ’h ’ü s rc’ iccct.
Seuii I rolal He
liislri inent l’ei lonnance Check
(Coniputmd Name)
Auui iysis
liMe nud ‘lime
liistriuiiicuit
l ou(s) I
Miected I
l’erceuut
Relative
Mn mntlmice
QC [
Lhuul(s
Sai.ijulcs AFFected
Actiuui
4L-(
tTh _-4
Comments:
t O
C l
P 1
r
r
If tuning compounds and criteria arc different from those specified in CLI’ SOW OLMO3. 1, then the validator should include a COPY of the niethod-
specific tuning criteria with this worksheet.
VaIidator. fI\.
Datc:_ Lr .9
171Y6
-------
EPA-NE - Data Validation Wotksliecl.
VOA/S V-HI
111. INITIAL CALIBRATiON - List all analytcs dial a e outside calibration criteria.
J) iIe of
ICi%L
lush uiuiciit
I’m autucter
1 Jnhu I x
Cwiii iniiid
%
flSD
1UtF
Si tii pies
/tlFectcd
Achiou
l-
ç(\
JO”t
4 teoe. Ri e
I
-
sr f\O%—A(Y
tQ.
(on.
. ( D:At -1 -E cCJkL - -‘°- CL - S IP O dt(. .C z r - ci
b -kt : r’ Q - 4 C & ( A +s. A o - c Qf c t —l A (- I)o ,i J-e
4 ,r -ti -rc c 1 - I ,,toe4L ‘ i & - ( po r cd o i - lo IL ‘( C -)•
0
r;i
Validator: -ffl . J.JO4 UAtC(
Date: Lq ./O.cIçL
12/96
-------
EPA-NE - Data Validation Woikslicct
VOAISV-IV
IV. CONTINUING CALIBRAI’ION - List all analytes that arc outside calibiatkm ciitciia.
hate of
Dale of
lush uiiuent
Paraiuictcr
I\1a rL
Cwiiiuuuinl
%I)
ItRF
Snuuupks MIccleil
Achiwi
ICAL
CCAL
2 .9R
voA
St.J
-
S P’O), CS
t o3
3 .
tAY’
Couiiinents: p%a CA Q.i bv 4i - s wei e a- - L. 2(J i 1 s ,-,LeC .c 1 ‘ d o-( Ji
c o r 4-r&c #t.& o Q ç re I çç - j cJ .. Att Q nkV1 L I \. C4- -’ hr t1 ‘- C & 4 rQC,& L 4 J 1Q
ç - ; d ry 4 & L jt - 4 — ct°J .
VaHdator:
fW.
Date: £io. ?
16
-------
E PA-NE - Data Validation Wotksliec [
VOA/SV - I’cs(/I’CB-V-A
V. BLANK ANALYSIS
List the blank contamination below.
Saiiipher: J ’e ¶: M; 1 -1- . .
Con paI y: ‘ o E ’i iv-o
Concentration
Contacted: No
Level: L.OI.4-
L)ate:- e: , . 9
1. Laboratory: Method, Storage and Iustru nciit Blanks
Date Dale
l!.xtrncted Analyzed
l’ni niiietcr/ Saitipic No.
M:it,ix (IJiniuk Type)
lush IUhICtl(/
Column
Compuusnl
Colic.
(u.uulis)
. -
.v/AG
uLDI (we ..-kiod)
y 1 - g ph-H-aJaJc
D - ’- -/1-
2. Field: Equipment (Riiisate , Trip and Bottle Blaiiks
l)ate
Extracted
l Jl
Date
A iinIr rI
3.zel.(r? .
VoF M
Vahidator: rYL kpLD1e
Date:
J’arniueter/
Matrix
Satiiple No.
(Blank l’vnc
c t - (-r? ,)
lust ruuiienh/
Culunin --
,w
Cotnpouiid
Cu i
Coiic. (units)
/ -it_
‘ -I
0
H
12/96
-------
EI’A-Nt - Data Validation Woikshect
VOAIS ’ - l’esl/I’CB-V-B
3. Blank /ictioiis — List the niaxitnulu conceifli ations of blaiik compounds.
Validatur: m
Date: 5•iO ?
Conipoond
‘1y ie of lilank
J)atc hank 1 la c.
Sainp led/Ozigitinted I Cone.
(wilts)
Actluii
Level
(units)
Saiiiple
QL
S;iniplcs
Affected
Ai.i uti
Pn-bA pkIaJ
C1 ’ Ioo pr,u
r4 t’ .oa
ii
3.zf.i L
;
i? t jIL
ic 1 IL-
i c A Ij/L
i ç jJL
5 i1’-
livgIL
Oi’ O O(s’, O
S 4O!_ Si1r1o
MTh - Z#I
D
Jbii ctL 1
re is V1?
G
-------
EPA-NE - Data Validatioti Woikshcet
VOA-VI
VI. VOA SURROGATE SPIKE RECOVERIES - List all sunogac coiiipouiid iccovetics that ate outside iiic(liod QC acceptance c&i(cria.
Mc(Iwd
Volnille Isleiliod QC Accepliutice Cuiteila
Tolucuc-d 8
[ 1113
DCi -d 4
Oilier:
OLMOJ.2
Watcr Soil
88-110 84-138
Water Soil
80-115 59-113
Vaicr Soil
76-114 70-121
OLCO2.1
NA
80-120
NA
Oilier:
Sauuiple NuuuibcrfISJntrL
% Recovery
% Recovery
% l(ccoveiy
% Recuvety
Aitioii
SP p O .:!,
)4
Zr 1 k
Valklalor: Ifl.
Date: s.io.7q
0 i
r-1
r
JM(AFI’ 12/96
-------
E1’A-N13 - Data Validation Wwksheet
sy-VI
VI. SV SUJUtOGATE SI’IKE RECOVERIES - List all suiroguic coinpoutid iccoverics that ate outside itictitod QC acccptatiee ciitcria.
2-FP
Watcr Suit
21-110 25-121
15-110
Acid MetiwdOC
;ccutflhice Ci itci In
2-CP-d 1 ’
Oilier:
? lc(Iiod
lluise/Ncuti il f Ietliud QC ACCCpIIUICC Ci itci In
N IJZ-d 1
2-1 I31’
TPlI-tl -
1,2-DCI3-d 4
Oilier:
OLM O31
Water PJ1
35-11423-120
Water Suit
43-I1630-1 15
Waict J1
33.141 18-137
i c! JI
10-11020-130
OLCO2.i
40-110
30.110
20-140
NA
Oilier:
Saniple
NwiiberThln(iix
% JAccoveiy
% Recovery
% Recovery
% Recovery
%
Recovery
Action
OLMU3.2
OLCUZ. 1
Oilier:
i Iethod
Saniple NuinberlMattix
cet-p-cD -
f -o1--
i’licnul -d 1
Water
Soil
10- 1 10
24-113
15-115
% ltccoverv
s
% Recovery
It
A
2.4.6- 1 1W
\Vater Soil
10-123 19-122
15- 130
% Recovery
I ?.
Water Soil
33-110 20-130
NA
% Recuv cay
% itecoycay
Action
* Advisory Surrogates - OLM O3.2
VaLidator: 01.
Date: 5id
12/96
-------
PE
Saiiiple
Ampule
Number
Parameter Type or
J’ES
Matrix
Atinlyte
Cuiic.
Region I EPA
I’ES Scuics’
Nun-EPA L’ES
Scorcs**
S2tuIples AUccied
Action
Nuniber
-
Sv’ c t°l
.1.
LC.S
1.
L-C.S
I
4,
1iio 1o
w”
L
TIJI ’
I
,
..jipft
1
4
,____
..JPJP.
—
1’
Th I
1’
Lt
J ’
L. s
... __
— —
—
— —
—
‘ -“e
Trl Oe’ 4 n
1 -,troe4 ,en ,
The , ipP
4 cJ,la2Jp1 e?1e’f
,4L..-T P
Ia /L
(p)bjIt.
ujft-
4 !t
3 /L.
L1, tjII
,tcJIa, Th
J C4 ’n LOu)
gg ,( o-lio)
( -i’W)
)O(fo-/.2o)
WA
P
o(-Jift1-O
SO?’,r 5FW*
r
3 (‘t
ZF.UJ
(O 4 iJdfj
TCL CONTAMINANT; TIC
* For Region I PESs indicate (lie Region I PES Score Report Result: Action High; Action Low; TCL MISS;
HIT; TIC MISS; TIC CONTAMINANT
** For Non-EPA PESs indicate the non-EPA PES Score: PES COMPOUND MISS; PES COMPOUND CONTAMINANT; PES COMPOUND
HIT (% Recovery Limits)
Validator: Th. /c c,c rd Date:
EPA-NE - Daia Validation Wozkshect
VOA/SY - I’est/PCB-XI
XI. ACCURACY CIIECI( (Performance Evaluation Results) - List all analytes that are outside criteria.
SDG No: s ol CASE: 5V
Are more than one-half of (lie PES analytes within criteria for each parameter.
12/96
-------
RAS ORGANIC
PE SAMPLE NUMBER: TT00840
Analytical Labs
DAS No.: NA
9503006-19
Contract: 68-D555
SDG No.: SA AO1
Date Received:
Date Analyzed:
TCL HITS
Benzene
Trichioroethene
1,2 -dichioroethane
Toluene
2 -butanone
Ethy lbenzene
Tetrachloroe thane
Action High
Action Low
In Window
In Window
In Window
In Window
In Window
12 ug/L
6 ug/L
9 ug/L
10 ug/L
6 ug/L
11 ug/L
8 ug/L
Lab
Lab
Lab
Lab
r’Tame: Fine
Code: FAL
Sample ID:
File ID: NA
03/25/97
II
TCL MISSES
TCL CONTAMINANTS
TIC HITS
TIC MISSES
TIC CONTAMINANTS
NOT SCORED
EXANPLE-12/96
-------
RAS ORGANIC
PE SAMPLE NUMBER: TT00842
Lab
Lab
Lab
Lab
Name: Fine
Code: FAL
Sample ID:
File ID: NA
Analytical Labs
DAS No.: NA
9503006 -20
TCL HITS
Contract: 68-D555
SDG No.: SAAO1
Date Received: 03/25/97
Date Analyzed: / I
In
In
In
In
In
In
In
In
Window
Window
Window
Window
Window
Window
Window
Window
bis (2-chloroethyl)ether
Hexachloroe thane
Fluorene
Pentachiorophenol
2,4 -dime thyl henol
3 -nitroaniline
Benzo (b] fluoranthene
Benzo [ k] fluoranthene
TCL MISSES
TCL CONTAMINANTS
TIC HITS
TIC MISSES
TIC CONTAMINANTS
NOT SCORED
12 ugiL
15 ug/L
9 ug/L
29 ug/L
8 ug/L
32 ug/L
11 ug/L
15 ug/L
EX.AMPLE- 12/96
-------
EPA-NE - Data Validatiwi Woikslicct
VOA/SV - l’es(/I’CB-XJI
XII. TARGET COP ll’OUfND iDENTIFiCATION — List lie analytes that ate outside the acceptance ci ltd in.
Stiiijiic Nuuiiber
Cuiiiimuiid J i\ IS 10115
I(i 1
Acl luii
5r y%O’f -
?- cbtoroptie t
ano e c,ia.eJrd
3 Mi 7 L
170 1 P/,7’fia(eIlC ei t 5: ‘• ? 6 -1-
djd. t pa;td. P ( 1 e 1 4ilO r1a0
ciç ivic i t v 6 ( pP/-
‘f(.’ _ ba -9cL StML
aA .d 10
-cJiiIyophe -P a4
0
0 i
N
H
l x i
Vatidator: ________________ Date: /O?
12/96
-------
I3PA-NE - Data Va!ithLIiOU Wurkshcct
VOA/SV - l’est/I’Cll-XIIl
Xlii. SAAII’LE QUANTI ’fA ’I’ION
Recalculate, froni the raw data, the concentratiotis for one positive detect and one reported sample qualititatioti limit for a un—dctect i ii a diluted sailmitle or uil saiiijtlc
per fraction. (Note: Although Section XIII, C. 1.i, requires that one calculation for each frnctiuii in each sample be pci formed, ihc validator is only icquiicd to
rcproduce aim example, br each fraction, of one positive detect and onc sample quatititation limit calculation on this vom kshcct.)
Do all suil(scdiincait saitiplcs have % solids greater than 30%? iV4 V N
If ito, list sample miutmibers
Frict lo,i
CnIc it tti ,t,
V(JA
(/3900D)CE)CI)
__— . /0. 34- /o-’- -g-( i_
(Iidco)O,?)(5)
S iiiple No:
5A 4Qc2
Rejwt med Culltiwund:
-,
(01 IA.d.rI€.
Rc 1 .wtcd Value:
/Q 1-/I•-
Nut Detected Cotnpuuiid:
Repotmed Quamuitalkimi Limit:
I . .Lç E .f 1—
IINA
( oX 2o)&oao) /3.( ,4 -=-)
c’R ’99) (i.i) (W0& Ci)
SanipleNo.
•SñiQo/
Reputted Compound:
Repofled Value:
—fl1cIhJ2pheJiD
/f4tt/L.
Nut Detected Comnpouitd
Repouled Quauititatiun Limitit:
‘ fL_
l’estkkle!rCB
Sattiple No
Rcpottcd_Coinpuund:
Repoited Value:
Not_Detected_Coitipoumid.
Rc oited Quauitimamkii, Lhnit:
Validator: in. Date: ‘ /0 ‘7
0
c i
(‘4
r
,-1
12/96
-------
EPA-NB - Data Validation Woiksliee(
VOA/S V-XI V
Xl v. TENTATIVI LY IDENTIFIEI) CO1\lI’OUNDS (liCs)
List (lie 5 TICs having the highest conccii(iation for each sample pai amctcr.
Sample Nuiiibcr
l’arnimmctcr
Comimputimad j IU(’F J Est. Comic. j
Action
3A-hz,
ØpJPt
ot in 4roc, q’ &’n
/ . a,
S/ wj/L
r
5 o1
5AA-O
,q o’J-
v o4
I
4’
P- ’
TXw cj fphni lirCil
T)O CCD OI ,4cJ L
?ctyIer
/ 3. (4
i 4.0?-
!5.S 5
3I 1/1
t fL4
4 iO VD 4 77& .
Valiiia(or: *7. Hok)ZrcL
Date: _________
0
( -4
r
N
12196
-------
‘ t — Lab w7
32 1 o d for foL1aw i. .):
6 ) ‘to&-
to Refez c to C3se so(s):
5 J( , 7 St,6ikJO.St 1O !
Su xy oI Qu w ’1 Dir ia 4 :
( -ie - ______
-k. tL uiO b .d\lC.. ed.:-
/L.
-r - c.
-*- ç q c &‘ (cs.
e e l - o 1 R 4 ’
Z , ot
(p &4 fl I J
_____.t ii 6 Z- Ls
( ) S& pLe c
-;t: v\ C t \ cc r e
‘I P -r
a \’ \ b-
Y .
(1) Lin Coav, C i ) Reço (3) MO C.
D &a
Coou c L. bor2LCrY Progr m
REGIONAL/LABCRATOR’ ’ COMMUNTC. TION SYSTEM
Ti!e Oo0 P rd Log
D aoiCa&
I.b ,r.w.y t. :
Ho ,&rd b, I;( Ofl 4±4
‘3 - -
EX !PLE-12/96
-------
DEL, o C 11:
L bon. c.7 Ha :
L b C rn
C U Tnj rd — L&b i&oc7
In r • to f th fcUo u a (i):
(_ ) cD4- J)¼ _____
La Rdct c to Case ?1o(5):
ço P i $, t JI
01 r,. II*3ca Dir’
( ) - -l I YI-O p h tA CLA i is i -WJ -d fn - SWD4-
Jk n b t l uia & k 1L J-eJ1 ..
( ) Lc k cdZ (’1 - J - L & ( t 4o
1-
5 A v ro
i’ I - t J o r ü - 4 çe 4 Jnr-
Di r o
USA. +tô d
(I) I.ib C. v, Cl ) eg 0o C. oy. ( .3) MO C y
DiLl
Cc cr et Labor crY Froga m
RECIONALJLABORAT0RY COMMUNICATION
SYSTEM
TdepàOi1 R ord Log
oso 1 c P t4 O
L.a%s
L . P’
•1
m.
EXA PLE-12/96
-------
I—
Dcek
t bs j c, yfl
5 +L
Lon j1 4c((p( ft dc krô c . s° O /QLJ
V ( irfiL qi. ,voeaJY(
Wcck / .S w-9/c4
U E *Q- C hcLt .
5°
S,1 B k Rt p/ia IE
t:&-zt L : E e 105 , P ê- ’sk 4 , ie i
Or G r’t.b vvtpti f ljjc,d& EA kd
VOft 7ô 5 V .eijdo Cd/ceJ cj e f
4 1 L( -f.
1 k 73 / t Lo
iS 5- c°” .ccx)yd
? -s m . io.o’c.
g o Q 1 5 t - SJ 74O 1 S 7-
ec -1-: Al / (9 t °c:
- 5ni o3 m - - -—- çz dr
ftLCtK —
iW—c.’ Feii tp. /O.0 ’c
‘7D 0 V S - rcc - 5OO yds
M_tct-r 1 :i-,
• TH5.3
• c/j - c 7 .c 9c 7 S s i &cnec /t.14c. c
• Mc xcL
• Te,. p /c .o C_
s p- 5 i4t)4’ c ne’-
oe-’S jL c rA
‘p 1 -i-- S 2 1e. ip ic °
Jo --r -
1po5
} pli’cit- 5. 5m?- 1c - __
jo rc / .e s I 1 S
r i
-------
May 1, 1997
Dr. Sydney Black
0S0 Fine Analytical Labs
MacKenzie, CT 04321
RE: Contract No: DAS OLCO2.1
Case No. 5063, SDG No. SAAO1
Dear Dr. Black:
090 Fine Analytical Labs failed to comply with the following
contractual requirements when analyzing CASE No. 5063, SDG No.
SAAO1 under DAS contract-DAS OLCO2.l. A reduced payment has been
assessed for each contractual deficiency as noted.
1) Trichioroethene PES recovery results were outside the
contract required QC acceptance limits. Reduced payment:
10% per sample; SAAO1-SAAO8.
2) Benzene PES recovery results were outside the contract
required QC acceptance limits. Reduced payment: l0 per
sample; SAAO1-SAAO8.
3) The laboratory failed to perform contract required
reanalysis on samples SAAO3 and SAAO4 that had surrogate
recoveries outside the contract QC acceptance limits.
Reduced payment: 50% per sample; SAA03 and SAAO4.
Please contact Moe Howard at the Howard Environmental office (617)
232-7000 should you have any questions regarding this reduced
payment notification.
Sincerely,
HOWARD ENVI RONMENTAL
Moe Howard
Data Validator
C :Sydblack .597
EXANPLE-12/96
-------
QUALITY ASSURANCE PROJECT PLAN AMENDMENT
(QAPjP)
MAC’S MARSH - DEBSVILL E, MASSACHUSETTS
SITE INVESTIGATION
5.5.1 Data Validation Modifications
The Region I, EPA-NE Data Validation Functional Guidelines for
Evaluatina Environmental Analyses, December 1996 will be used
to validate all surface water data with the following
modification: The %D continuing calibration criteria to
evaluate volatile organic data will be expanded from 25% to
30%. The validation criteria has been expanded to reflect the
contractual acceptance criteria for OLCO2.1 analytical
specification utilized under the DAS mechanism for obtaining
analytical services. The expanded criteria will not impact
the achievement of DQOs.
EPA Site Manager Approval Signature
EXAMPLE-12/95
-------
Uk(IgAZ4IC t .J. (CS?) IXVNOP
flORATOR ’ NAIIE OSo 1te . 4) L 2J
C SZ NO. O( .o! . ____________ S G NOS. TO FOLLOW —
___________ ___________ SAS NO. ________
C NTRAC NO. ( - S55
SCW NO. — - —
AU C fl t3 delivered in the c npLeca S G Pile mu z be original c ma t3
where pcsoible.
PAGE NOe c cx
PROM TO
7 t I-7 sb t (T oc-2) (Do r.ct n er ____ ____ ______ _________
2. s I _ 3 ______ I . ,
3. S C. #e t/ .3ff:c R crt ____ ( . 0 . . _________
4. Valati! D e3
a. QC Surr naay
System cnii : ir g C pcund i: cn _
La c:a rv C t : L £acn le Rec te:y
(Fcr II! LC 1) _ 1 J ? _________
Method 3La 5 ar i (7 r I V ..CV) 14 _________
GCJMS I 5 me perfc: ance Check ( rn V LCV) ____ ____ 1. ’
Inte:nal S ar.dard ?%:e a. c W Se nay
(Zc::: V I LCV)
b. Sa. le Ca a
TCL Results - ( ‘C: I LCV)
Ter a:i ;ely Ider :ifie f C urnd (To:— z r ..cv— :cj ______
Fc eaoh sar nle:
Reco zz: o:ed c a1 ic c o a:oc:ar S (P.IC) , .
Raw spec :a and bac: ds :raC rnass
of tar e: c our.d ide :ifie f
Quan: a jcn re cr:s ______ “
Maz5 s .eo::a of all. : c::ed
li :ary ma es ______
C. S anda Data (Ai.]. Ie ; )
In . .al Cal :a on Data (TCr v: LC ) —
RC and Q ia e crzs fc all. S andar S ___________
C nt i g CaLth :a:icr. Daa (Fo v:: E .C/) __________
RICE a d Qwar. jtatjcn Re c s for all a da:ds /
d. Raw QC Da:a
813 ______ _________
3larik Data ______ _________
Labcrato:y C n :o1 Sam 1e Data ______
Evidence Audit Photocopy
flc—:-: CLC .
EX? fPLE- 12f96
-------
ORG?JJICS CO) LZS S G FILE (CSF) INVtNTORY EE (Cat t.)
L ASZ NO. c
—
NO.
S S
•gA-r -OI SDG NOS. TO FOt.L w I J
No.
PACZ NCe
FROM
5. ? i’el2tL1ss Oata
a. cc Sumzsa y
Zur: gate Percent Rectve:y s =ary (For i II LCSV) ____ ____ _____
La crat ry CQnt:ol Sample Recovery (Form III
LCSV)
)4ethcd Blank Sun ary (Fcr 1 I V LCZJ) ____ ____ ______ _________
cc/2is I t iier t Perfor ar1c2 Check ( or V LCSV) ____ ____ ______ _________
Inter a1 Standard Area and R Su ary
(?cr VIII LCSV)
. Sample Data
TC. Resultz (Fort I LCSV1, LCSV-2)
Tentatjvely Ider.: .fied ctrnccunds ( r ’ I LCSV—
TIC)
Fcr each sarnole:
Reconst: uc:ed total ion c :c ac (RIC) ______ _________
Raw spectra and backg ur. Su cted mass
s ec::a of target ctmpcunds
Quantita:jcn re c:ts
flass s ect:a of TICs with eS li. rary
matches
c. Standards Data (All Ins:: er.S)
Initial Calibration Data VI LCS l, LCSV—) ______
RICs and Quan Re crzs fc: all Szar da:ds ______
C r.tinuing Calibraticn Data (Fcr VII LCSV1,
LCSV—2)
RICa and Quar itatior. Rerorts for all Standards
d. Raw cc Data
DFTPP _ I9t i ________
Blank Data 1W i
Labc:a:crv Ccnt:tl Sarn le Data i __ 9 _
6. Pesticides
a. cc Surnma v
Surrocate Percent Recovery s ary (F n I l LCP) ____ ____ ______
Laboratory Cor.r:cl Sample Rec:v!:y (Fc III LCP) ____ ____ ______
) ethcd Blank Sunmary (FCr IV LOP)
Evidence Audit Photocopy
TC?. DC-2-2 OE.
O ‘ 1 !
_ _ 1 -
1c 14-2.
I# VIo
c:1Ec.
LAB
I—
/ /
/ /
V I V I
/ ___
/ _ /
_______ —
vpg
m
I
I
—
————————
4 ’
1-
—__
EX .ANPLE-12/96
-------
o c ics co i. z SDG Y 112 (CS?) I t OR S Z T (Cant.)
[ E SDG NO.
5%s
_ m4C f SOC NCS. TO FOLLOW —I]
o. -
PAGE NC
PPOK TO LAE EPA
6. P it .c dei (C r t.)
b. S D1 Data
T . RO5UItZ — Organic Arlalysi2 Data Sheet
(?ort I LCP)
Cat (Pri arj CO1i tn)
C ratograxna frcrn second GC co1u n c: .at .o _______
cc Integration report or data eyetem p:it Ut _______
1{a a]. work a eet
c. Standards Data
In .tia1 Calthratjcn of Sincle Ct cr.ent A a1yte2
(Tor n VI LCP—1 and LCP—2)
Initial Calibration of M ltiC C nt , r.a!vtes
( crnt VI LCP—3)
AnaLite Resolution Summary (FC v: L.C -4)
Pe:fcrtance Eva1.uatjon (Form i: LC —E)
Individual Star.da:d Mix4re A (F::m VI LCPG)
Individual Standard Mixt :e B (FC V LC?7
Calibratjcn Verifica:icn su m mary
(form VII LC?—l)
Calibration Verifjcatj SUr_ ary
(Form VII LC?—2)
Analytical Seçuence (F v:Ir - )
?lcrisil Cartr .dge Cheoic ( orm lx LC?)
Pe jcLde Iden:jfjcatjcr. S..—rary for Sir.gle
cmocr .g P .nalvte ( O X LC )
P tLcide Identjf catjcn 5u .ray f
lticomccne Analytes (per X LC 2)
C rmacra. and data vstem pr ntC t
A printot t of retat: cn d
peak areas or pea < he g :
c. Raw QC Oata
3lank Data ____ ____
Labcrater , Car.:: Sarr.ole Daa ____ ____
e. Raw Flcr s..: Data ____ ____
Evidence Audit Photocopy
FO?_ M . cc-:—:
EX A1’!PLE-12/96
-------
ORCA 1ICS CC1GI2 SDG FILE (CS?) DVzNTOR f SBIE (C t.)
[ CASE no. ç y
.
SOC flOS . TO FOLLOW
s s_na. _
PAGE NO
FROM O
i 11* *øtii *ta
orjga]. pre aratior and anaLy i. fCZ or c pie of
preoaratjort and a 1v j 1ccbc k pages
a& p1e and sampLe ex:ac e:anafer o ’iath—
Cfc tOd? reo ds
Sc eening rac rds
?i2.1 th r .inent cut u , inc1 ding st:ip C A 3 f:CCn
5ceoning act vit.es deacribe or 1 .3t)
AJ) t ui-
I . .
I —
. Sb! Cf Cv :q Dcc e t
Ai.rb 113 (No. of o en _)
CAaLn-of-Cu9t dv Rec rds
£a n 1e Tag3
Sample Loc—In Sheet (Lab & DC:)
fisceLlaneous Shi oinc/ eceivinq Re tr S
(derc ibe or lis
; ___
ar ___
4
9. I ter- al t.ab Sa vle i fer ReC a d
S eet (describe or
10. Ot e c r s (desc:jbe or 1i )
11. C e t3 :
Crrnpleted by:
(C:? Lab)
Ver !ed by:
(C? L.&b)
udi d by:
(S g: .ire)
‘ (S .cna re)
(S
(Date)
(Date)
(Date)
Evidence Audit Photocopy
DC-2-4
Ot .C 2.
c c
LAB
ele;hcne C rrj unicazion Loç
4I
L r ‘ - / S i . CLe . sk
(?‘ ted fl. me/ .tle)
z
/
( Ze
p . L b
UaL e/ .: .e)
r
k 4-c9 /cth V Li’d ’-tvc
EXAMPLE- 12 / 96
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EPA-NE - DQO SUMMARY FORM
Page I of I
A separate Form should be compkted for each sampling event. Refer to Attachment A for insmicetans an campicusig this form. A chment B for a complete li
thc parameter codes and Arnchment C (or art example of a complctcd farm.
1.
EPA Program: TSCA RCRA DW 14pDE5 CAA
Other______________________________________
Proj:cted Daccis) ot Sampling . .o — .q .
EPA Site Managtr v c,*tr ,4 -ri —
EPA Case Team Mcmbcrs 1o , v- v.tcsj .
S ire Namc_ rY1 4.Lls JY1O.4SL
Site Location 1 .) svlfl , vtA
Assigned Site LaorudelLongitude_ ° jg M) ° ?3 •
CERCLA SstciSptll tifitt 01 • JL, l1nc ude Operibte Urtit)
Pha c. EM SA Sl pre R1 hasc I. etc.) FS RD LA post-RA
(cirtic one) Other )
2.
QAPJP Title and Revision Date royst PI pr ivla.rsL ‘/q
Approved by: I•kkqi p +k .j Dare of Approval: /i
Title of Approving Official: rr ,c’s ma’ c - Pr -z± qtza .r- organizaciona:________________________________
11 other than EPA. record dare approval author ity waS delegated:___________________________________________________________
EPA Oversight Projcct (citctc one) Y Type o( EPA Oversight (circle one) PR? or FF Other NA
Confirmatory AnaJysis for Field Screening Y If EPA Oversight or Concirmarery: % splits .JA
Are cornparabdicv criteria documented? Y
3 a. Matrix Ccde Scj -
Ii. Pirameter Code - V D A SV ¶ar . 4 a x.ti :i Q1 l -’i
C. i 5 ! .5 I — I
d. Analytical Services Mechanism 1) P S j_______
C. 4o of Sarnote Locations - s.
Field QC:
f. — Fcld Duolicate Pairs I
g. Eauioinenc Blanks - I
b. VOA Trio Blanks - I I — I —
i. Cooler Tensoerarure 3lanics I I ! —
J. ottic Blanks Lo 3b LkA Je2 L of 1 J 57J
Other__________________ —I-
l. PES sent to Laboratory F i
Laboratory QC:
in. Reaccat Blaiiic 1 1
It. NA + O 4D2.J S )
0. Mama Soike 1 k I
p. Macrtx So,ke Duoljc te tilt I P D.
q. f_____
4. Site Iiiforrn.at,on
Site D ,me iop 5C0 c t. x coo
Ltit all potettoafly contaminated mamces u. , L, dJffl JTt
Range of Depth to Grounthvater II —
So J Types Stzthce Subsuriace Other Af*
Sedunent T spes Stteaan Pond Esaiary Wetland Other — Expccted So Sedim iMoisture Content: ligh Law
Whci multiple macrices wilt be sampled during a sampling event. comptere Sections 5.10 for each mac n c. Matrix Code’ U_)
Data Use (circle all that atcplv) Sire lnvesnnanowAssessmert PR? Deternunauon Removal Actions
Nlanue and Extent of Cann .rrunatson Human andIor coLootcal RicA sess ñ Rernedianon Alternatives
Engineering Design Remedial Action
Post-Remedial Action (quarterly monitoring) Other________________
II
Draft DQO Surnriiarv Form 11/96
EXANPLE-12/96
-------
( 4 c 1CE
1
aoolicable
COCS Action Levels
Analytical Method-Cuantitation Limits
‘J ’-5IL.
JTh 5/l
rI c /tiv pke-’i -/
5 t. /L
O /t
5 )Z ..
(circle cechiuque) c j) Low flow pump (Region! method: Yea No) Peristainc Pump
Positive Displacement Pwnp Faucet or Spigot Other____________________
SpIn Spoon Dredge Trowel O t h ___________________
Procedures (SOP name. No.. Rev. A’. and date) St4. ô dt .t , OI-?5 ( C - M flei . I f
Sample Locations ULp dreaf71 d ft aC i /Y)4.f
or Composite
sampled. Yes C . . 2)
(circle) ORP ( j ) Specific Conduc nce Dissolved O Turbidity
Other__________________________________________________________________
Methods and Parameters I
tide/SOP name
Method/SOP
Identiflcanon number
Revision Date
Target Parameters
(VOA. SY. PestIPCB. Metals. em.l I
OLcO; ./-i: t-P5o , .)
V04 1 Sv I
Cnteria (circle one) 1. Reeton!. EPA-NE Data Validation Functional Guidelines for Evaluating Enviroriniental AriaJvses. flI
2. Other Approved Validation Cmena 2rJd€I •/.b c 4cr 3j .,’
= no :) ormi ig Data Validation / roa1 Tier LU:
£iWifDi,ft)e d l Contract Number ‘ - I)55
(e.g. START. RACS. etc.) Cs Work Assignment No. O3- -1 8
Forrn,Tide cn ., iekiThii.ej Date of DQO Summary Form Completion 2./c. -
Matrix Codes t - Refer to Attachment B, Part I
Parameter Codes- - Refer to Attachment B, Part II
Preservation Codes 3
I. MCI to pM 2 7. K Cr:Oi
2. HNO S. Freeze
3. NaH O , 9. Room Tempersorre (avoid exc:ssive heat)
4. H.SO. 10. Other (Spec:fv)
5. Cool @ 4C (± 2) N. Not preserved
6. NaOH
* - To supplement Matrix Codes and/or Parameter Codes contact the QA Unit
Draft DQO Summary Form 11/96
-------
Example Tier III Data Validation Report for
VOA/SV Soil Samples Analyzed under CL? OLMO3.2
-------
REGION I, EPA-NE ORGANIC REGIONAL DATA ASSESS? ’IENT (ORDA)*
CASE 11: fOil SITE NAME: L O(/S 1A .J1dI LL
LAB NAME: OSO ic 1üI c iD 1aJ.x # OF SAMPLES/MATRIX: 2 P S
SDG 11: __________________ VALIDATION CONTRACTOR: TVS
SOW 11/CONTRACT 11: VALIDATOR’S NAME: cVs
EPA-NE DV TIER LEVEL: DATE DP REC’D BY EPA-NE: &
TPO/PO: **ACTION ____ FYI / DV COMPLETION DATE: __________
ANALYTICAL DATA QUALITY SUMMARY
VOA PestIPCB
1. Preservation and Contractual Holding Times ________ — ____________
2. GC/MS I GC/ECD Instrument Performance Check _______ o __________
3. Initial Calibration ________ ________ ____________
4. Continuing Calibration ________ ________ ____________
5. Blanks ______ 0 _________
6. Surrogate Compounds C) _ 0 ____________
7. Internal Standards ________ - ____________
8. Matrix Spike/Matrix Spike Duplicate ________ ________ _____________
9 Sensitivity Check ________ 0 ____________
10. PE Samples-Accuracy Check fn _______ ___________
11. Target Compound Identification ________ C ____________
12. Compound Quantit:cion and Reported QLs 0 ________ ____________
13. Tentatively Identij 4 Compounds & ________ ____________
14. Sernivolatile CleanuplPesticidefPCB Cleanup — Ca . ____________
b. Data Completeness ________ ________ ____________
16. Overall Evaluation of Data fr _______ ___________
o = Data had no problems or were qualified due to minor contractual problems.
m = Data were qualified due to major contractual problems.
z = Data were rejected as unusable due major contractual problems.
ACTION ITEMS: (z items) ‘- r 1 .*ed 1 ¶ C C Z c J’
%
AREAS
-P 0 .. . . k
9u .G . . ’
OF CONCERN: (m items) (“1
r ex4,-a t 4 [ -
r& yp J - 1 L
IS - c d . 4
J 40 O e . 4 - SC L
C 4
t
a. G .. .
L&ra4t r j.
1i2. f 1 /dJ Y’ 1 .(
?
7’O
•‘
44 L JU
COl v [ MENTS: p t -. A. 1 C... O C Lii C,1
‘This form assesses the analytical data quality in terms of contractual compliance only. It does not assess sampling
errors and/or non-contractual analytical issues that affect data quality.
**Check ACTION” only if contractual defects resulted in reduced payment/data rejection recommendations.
Validator: ( fl. 1o & .t.S Date: )
INSTRUCTIONS ON REVERSE SIDE
11/96
EXAMPLE-12/96 -
-------
GUIDANCE FOR COMPLETING THE ORDA.
The ORDA form provides the laboratory’s CLP-TPO and other contract management personnel with an overview
of the contractual analysis and reporting deficiencies found in an analytical data package and identifies those
contractual deficiencies that resulted in reduced payment/data rejection recommendation.s/actions. The ORDA form
is used w summarize analytical data quality only in terms of contractual compliance. Sampling errors and non-
contractual analytical errors that affect data quality are not summarized on this form, but rather are documented in
the Tier I Validation Cover Letter and Tier lull! Data Validation Reports. For instance, if the sampler did not ship
the samples until after the holding time had etpired, a notation would not be made on the ORDA form since the
laboratory is not responsible for the sampler’s actions.
The ORDA form should be completed as follows:
1. Fill in all of the header information (with the exception of the TPO Action/FYI field): Case Number, Site
Name, Laboratory Name, number and matrix of samples in the data package, SDG Number. Validation
Contractor, SOW#/Contract#, Data Validator’s Name, EPA-NE Data Validation Tier Level (i.e., I, II, III
or partial lI/ill), Date the Data Package was received by EPA-NE, and the Data Validation Completion
Date.
2. Summarize the contractual problems discovered during data validation by fraction and by evaluation criteria
in the “Analytical Data Summary table, and in the “Act ion Items” and “Areas of Concern” sections as
described in items 3 through 6 below. Use the Data Validation Memoranda as a guide when completing
the ORDA form.
3. The following qualifiers must be utilized to document contractual problems on the ORDA forms.
0 = Data had no problems or were qualified due to minor contractual problems
m = Data were qualified due to major contractual problems
z = Data were rejected as unusable due to major contractual problems
4. If the data were acceptable, or were qualiiied due to minor contractual problems, enter the qualifier “o”
into the appropriate column (fraction) and row (evaluation criteria). No further documentation is necessary
on the ORDA. form. An example of a minor problem would be a semivolatile compound that slightly
exceeded the SOW-specified %RSD initial calibration criterion.
5. If the data were qualified due to major contractual problems, enter the qualifier in ” into the appropriate
column (fraction) and row (evaluation criteria). Use a different superscript (&, n, etc.) for each major
contractual probEem identified and provide a brief description of each major problem in the “Areas of
Concern” section. An example of a major contractual problem resulting in data qualification would be a
semivolatile internal standard that had extremely low area counts (below the lower limit of the SOW-
specified acceptance criterion) and reanalysis was not performed.
6. If the data were rejected as unusable due to major contractual problems, enter the qualifier “z” in the
appropriate column (fraction) and row (evaluation criteria). Use a different superscript (z’, z , etc.) for
each major contractual problem identified and provide a brief description of each major problem in the
“Action Items” section. An example of a major contractual problem resulting in data rejection would be
contractual holding time criteria that were exceeded for volatiles.
7. Complete the TPO Action/FYI field using the information contained in the “Action Items” and “Areas of
Concern” sections. IpO Action should be indicated with a check mark V) in the space following “Action”
only if the contractual defects resulted in reduced payment or data rejection. If no TPO Actions are
indicated, then a check mark (‘I) should be placed in the space following “FYi”.
8. The validator who completed the ORDA form must sign his/her name in the “Validator” field and enter
the ORDA completion date in the “Date” field.
-------
Christine Clark dune 1, 1997
Regional Sample Control Center B-97-06-FF-02
U.S. EPA Region I
60 Westview Street
Lexington, Massachusetts 02173
RE: WA No. 03-718
SDG SAAO9, Case No. 1011
OSO Fine Analytical Labs
Lou’s Landfill
Organic Data Validation
Volatiles: 6/Soils! SAAO9, SAAb, SAA11, SAA12, SAA13,
SAA1 4
(Soil Field Duplicate Pair/SAA13 and SAA14)
1/Aqueous Trip Blank/SAA15
1/Aqueous PES/SAA25
Semivolatiles: 6/Soils! SAAO9, SAAb, SAA11, SAA12,
SAA13 , SAA14
(Soil Field Duplicate Pair/SAA13 and SAA14)
1/Aqueous Equipment Blank/SAA16
1/Aqueous PES/SAA23
Dear Ms. Clark:
A Tier III data validation was performed on the organic analytical
data for six low/medium level soil samples, two aqueous blanks
(sernivolatile equipment and volatile trip), and 2 aqueous PE
samples collected by U.S. EPA Region I, from the Lou’s Landfill
site. The data validation was performed using the Recion I. EPA-NE
Data Validation Functional Guidelines for Evaluatinc Environmental
Analyses , December 1996 criteria. A CADRE review was not performed
on the data. The volatile and semivolatile soil samples, blanks,
and PESs were analyzed under the CLP RAS program using the OLMO3.2
Statement of Work.
EXANPLE-12/96
-------
Christine Clark
Page 2
The data were evaluated based on the following parameters:
• Overall Evaluation of Data and Potential Usability Issues
* I Data Completeness (CSF Audit - Tier I)
• Preservation and Technical Holding Times
* I GC/MS Instrument Performance Check (Tuning)
• Initial and Continuing Calibrations
• Blanks
• Surrogate Compounds
• Internal Standards
• Matrix Spike/Matrix Spike Duplicate
• Field Duplicates
* I Sensitivity Check
• PE Samples/Accuracy Check
* I Target Compound Identification
• Compound Quantitation and Reported Quantitation Limits
• Tentatively Identified Compounds
• Senhlvolatile Cleanup
• System Performance
* - All criteria were met for this parameter.
Note: Worksheets, except for Worksheet XIII-Sample
Quantitation, are not included for parameters that
have met criteria or for criteria that are not
applicable (NA) to the method.
The fo11owin information was used to generate the Data Validation
Memorandum attachments :
Table I: Recommendation Summary Table - summarizes
validation recommendations
Table II: Overall Evaluation of Data - summarizes Site DQOs
and potential usability issues
Table III: Tentatively Identified Compounds - summarizes
volatile and semivolatile compounds tentatively
identified by GC/MS
Data Summary Tables - summarize accepted, qualified, and rejected
data
EXAMPLE-12/96
-------
Christine Clark
Page 3
Overall Evaluation of Data and Potential Usability Issues
Following is a summary of the site DQOs:
• Data Use - Ecological Risk Assessment & Source
Identification
o Determine ecological risk of soils for the following
compounds: benzene, trichioroethene, tetrachioroethene,
1,2-dichioroethene, 1,1,2,2-tetrachioroethane, 1,2-
dichlorobenzerxe, 1, 2,4-trichlorobenzene, and 1,4-
dichlorobenzene.
• Determine if soils are a source of surface water
contamination for the same compounds listed above.
The field precision for volatile and sernivolatile samples was
outside of acceptance criteria due to suspected heterogeneous
sample matrix, therefore additional samples should be collected and
analyzed to adequately characterize the site. The data user should
assess spatial variability at the site. As a result of the
suspected heterogeneity, sample representativeness is questionable
and thus the achievement of the DQOs is limited. Furthermore, it
appears as if the wrong sampling method and/or analytical method
was used for samples SAA1O and SAA1]. because the percent solids
were below 30%. For high moisture sediment samples, the sampler
should decant, filter and/or centrifuge the sample, and possibly
composite the sample aliquots if necessary prior to shipping to a
laboratory for analysis. Additionally, for problematic soil
matrices such as peat, the field sampling contractor should select
an alternate analytical rnechanistn, i.e., DAS, and an applicable
analytical method.
Volatile
Volatile sample results were qualified as a result of both
analytical error and sampling error, and it is important to
distinguish between the two because the laboratory does not have
control over the sampling error. The following list summarizes the
measurement error associated with sampling: trip blank
contamination, poor field duplicate precision, arid low percent
solids resulting from improper sampling technique.
• In sample SAA11, all results were rejected (R) due to
extremely low percent solids. Dry weight CRQLs cannot be
achieved. This may potentially impact the assessment of
ecological risk and the accurate identification of the source
of contamination.
EXANPLE-12/96
-------
Christine Clark
Page 4
• In sample SAA1O, all non-detects were rejected (R) and all
positive detects were estimated (J) due to low percent solids.
Dry weight CRQLs cannot be achieved. This may potentially
impact the assessment of ecological risk and the accurate
identification of the source of contamination.
• In all field samples, SAAO9-SAA14, benzene, trichloroethene,
and 1,1,1-trichioroethane detects were estimated (J) and non-
detects for those compounds were estimated (UJ) due to poor
field precision attributed to heterogerious sample matrices.
In order to fully characterize this site, data from additional
sample locations may need to be collected. The lack of field
precision for contaminants of concern at this site, benzene
and trichioroethene, impacts the assessment of ecological risk
and the accurate identification of the source contamination.
The following list summarizes the measurement error associated with
analysis: improper sample storage and preservation, unacceptable PE
results, and extremely low internal standard area counts.
• In sample SAAO9, all non-detects were rejected CR) as unusable
because of the possibility of false negatives and all positive
detects were estimated (J) to indicate the potential low bias
due to improper sample preservation and storage by the
laboratory. This may potentially impact the assessment of
ecological risk and the accurate identification of the source
of contamination.
• In all field samoles, SAAO9-SAA14, all tetrachioroethene non-
detects were rejected (R) as unusable because of the
possibility of false negatives and all positive
tetrachioroethene detects were estimated (J) to indicate the
potential low bias due to low recovery (bias) of PE result.
This may potentially impact the assessment of ecological risk
and the accurate identification of the source of
contamination.
• In sample SP Al4, all non-detects quantitated using the
internal standard broniochioromethane were rejected CR) as
unusable because of the possibility of false negatives due to
poor Is recoveries. This may potentially impact the
assessment of ecological risk and the accurate identification
of the source of contamination.
Semivolatile
Sernivolatile sample results were qualified as a result of both
analytical error and sampling error, and it is important to
distinguish between the two because the laboratory does not have
control over the sampling error. The following list summarizes the
measurement error associated with sampling: equipment blank
contamination, poor field duplicate precision, and low percent
solids resulting from improper sampling technique.
EX.ANPLE- 12/96
-------
Christine Clark
Page 5
• In sample SAA11, all results were rejected CR) as unusable due
to extremely low percent solids. Dry weight CRQL5 cannot be
achieved. This may potentially impact the assessment of
ecological risk and the accurate identification of the source
of contamination.
• In sample SAAb, all non-detects were rejected CR) as unusable
and all positive detects were estimated (J) due to low percent
solids. Dry weight CRQLs cannot be achieved. This may
potentially impact the assessment of ecological risk and the
accurate identification of the source of contamination.
• In all field samples, SAAO9-SA.A14, ].,4-dichlorobenzene,
naphthalene, and acenaphthene detects were estimated (J) and
non-detects for those compounds were estimated (UJ) due to
poor field precision attributed to heterogeneous sample
matrices. In order to fully characterize this site, data from
additional sample locations may need to be collected. The
lack of field precision for the semivolatile contaminant of
concern at this site, 1,2-dichlorobenzene, impacts the
assessment of ecological risk and the accurate identification
of the source contamination.
The following list summarizes the measurement error associated with
analysis: instrument calibration variability, low internal standard
area counts, and low surrogate recoveries indicating potential
inability to detect a specific target compound.
• In samples SAA13 and SAA14, 1,2-dichlorobenzene (a contaminant
of concern at the site) and l,3-dichlorobenzene non-detects
were rejected (R) as unusable because of the possibility of
false negatives due to low surrogate recoveries. 1,4-
dichlorobenzene (a contaminant of concern) detects were
estimated (J) due to potential low bias. This may potentially
impact the assessment of ecological risk and the accurate
identification of the source of contamination.
• In samples SAAO9, SAA11, & SAA12, benzo(a]pyrene non-detects
were rejected (R) as unusable because of the possibility of
false negatives and in samples SAAb, SAA13, & SAA14
benzo(a]pyrene positive detects were estimated (J) to indicate
a low bias, due to calibration variability. This may
potentially impact the assessment of ecological risk and the
accurate identification of the source of contamination.
EX.ANPLE- 12/96
-------
Christine Clark
Page 6
Preservation and Technical Holding Times
Volatile
The following table summarizes the volatile samples which failed to
meet the preservation and technical holding time criteria:
Problem
Action_____________
Affected
Samples
Positive Detects
NDs
Sample not properly refrigerated
or light protected by the
laboratory; therefore, did not
meet preservation and storage
criteria.
J
R
SAAO9
Senivolatj].e
All sernivolatile soil/sediment preservation! holding time criteria
were met.
Initial and Continuing Calibrations
Volatile
All criteria were met for volatile calibrations.
Se iivolati1e
The following table summarizes the semivolatile initial calibration
(IC) and continuing calibration (CC) compounds which failed to meet
the calibration criteria of RRF > 0.05 and ‘ D < 25 :
L Instru ment
X
X
Action
Affected
Samples
Conpoumid
IC
CC
Positive
NDa
3/29/97
4/13/97
Detects
Benzo(a)pyrene
Ave. RRF=
J
R
SAA09 14
0.039
Fluorene
D=32%
J
UJ
SAA O9-14
EXANPLE-12/96
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Christine Clark
Page 7
Blanks
The following table summarizes the level of volatile and
sernivolatile blank contamination detected in the laboratory,
equipment, and trip blanks:
Compound
Type of
Blank
Max
Conc.
Action
Level
us/kg
Sample
CRQL
Chloroform
Trip
68 Ug/L
TB
10 ug/L
2-Butanorie
Trip
15 ug/L
TB
10 ug/L
1,2-Dichioroethane
Trip
35 ug/L
TB
10 ug/L
Di-ri-buty lphthalate
Method
44 ug/kg
440
330 ug/kg
Dibenzofuran
Equip.
50 ug/L
EB
330 ug/L
Volatile
Chloroform was detected in the trip blank at a concentration of 68
ug/L. The source of chloroform, which was not detected in any of
the field samples, is unknown. Either another source for the trip
blank water should be used, or additional testing of the trip blank
water prior to use should be performed. The sampler was notified.
(See Phone Log). Chloroform was not detected in any of the field
samples, therefore, no qualifications were required.
The aqueous trip blank collected with the soil samples also
contained 2-butanone and 1,2-dichioroethane at concentrations of 15
ug/L and 35 ug/L, respectively. Of the two compounds, only 1,2-
dichioroethane was detected in the samples. Therefore, no further
action was required for 2-butanone. 1,2-dichioroethane was
detected in three soil samples, SAAO9, SAAb, and SAA11, at
concentrations of 5 ug/kg, 8 ug/kg, and 3 ug/kg, respectively. As
a result of the positively detected 1,2-dichioroethane in the trip
blank, the positive results in samples SAAO9 and SAAJ.O were flagged
TB” to indicate to the user that an undetermined amount of
sampling error has potentially affected the sample results. All
results in SAA11 were rejected due to extremely low percent solids.
Rejected data take precedence over all other qualifications;
therefore, there was no blank qualification in SAA11.
All volatile laboratory blanks were free of contamination.
EX.AMPLE-12/96
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Christine Clark
Page 8
Sernivolatile
Di-n-butylphthalate was detected in a solid laboratory method blank
at a concentration of 44 ug/kg. Since di-n-butylphthalate is a
common laboratory contaminant, the lOx rule applies. Sample
results less than 10 times the blank contaminant concentration but
greater than the CRQL are qualified Ti. Di-n-butylphthalate was not
detected in any of the samples, therefore, no action was taken.
Dibenzofuran was detected in the aqueous equipment blank collected
for the soil samples at 50 ugIL. The positive detects for
dibenzofuran in samples SAAO9 (600 ug/kg) and SAA12 (450 ug/kg)
were qualified “EB” to indicate to the user that an undetermined
amount of sampling error has potentially affected sample results.
Surrogate Compounds
Volatile
All volatile soil samples recovered surrogates within the QC
limits.
S emnivol a tile
The following samples had surrogate spike recoveries outside of the
recovery limits:
Sa p1o
Nu ber
Surrogate
% Rec
QC
Limits
Action
Positive
Detects
NDs
SAA13
1,2-Dichloroberizene-d4
1].
20-130
A
R
SAA14
1,2-Dicbloroberizene-d4
13
20-130
A
R*
*The advisory surrogate, 1,2-dichlorobenzene-d 4 recovered very low
for soil samples SAA13 and SAA14. In accordance with the Region I
VOA/SV Functional Guidelines, sample results are only qualified for
low advisory surrogate recoveries if the recovery is less than 10k.
However, since l,2-dichlorobeflzefle is a contaminant of concern at
the site and was not detected in samples SAA13 and SAA14,
professional judgment was used to reject CR) the 1,2-
dichlorobenzene non-detects as unusable due to the possibility of
false negatives, professional judgment was also used to reject CR)
the 1,3-dichlorobenzene non-detects and estimate (J) the 1,4-
dichlorobenzene detects in samples SAA13 and SAA14 based on the
chemical similarity of these compounds to the advisory surrogate.
Consideration should be given to resampling the affected locaticns.
EKANPLE-12/96
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Christine Clark
Page 9
Internal Standards
Volatile
The following table summarizes the volatile internal standards that
failed to meet the acceptance criteria:
Internal Standard
IS
Area
Acceptable
Range
Action
Affected
Samples
Positive NDS*
Detects**
Bromothlorornethane
L_2100*
13553-54210
R
SAA14
*The area count for bromochioromethane in the volatile
soil/sediment sample SA 14 was less than 2O of the associated
calibration standard.
**Fcr those compounds quantitated using bromochioromethane as the
Internal Standard.
In sample SAA14, all target compounds quantitated using
bromochioromethane were reported as non-detects, and were
therefore, rejected (R) as unusable due to the possibility of false
negatives. Note that the laboratory failed to reanalyze sample
SAAJ.4 in accordance with contract specifications.
Semivolatjle
The following table summarizes the semivolatile internal standards
that failed to meet the acceptance criteria:
Internal Standard
IS
Area
Acceptable
Range
Action
Affected
Samples
Positive
Detects**
NDS**
Acenaphthe e-d . 0
15725*
17GG4-70G5G
J
UJ
SAA 14
*In sample SAIU4, the area count for acenaphthene-d 0 was less than
5O’ of the associated calibration standard (but greater than 2O ).
**For those compounds quantitated using acenaphthene-d 10 as the
Internal Standard.
Note that the laboratory failed to reextract and reanalyze sample
SAA14 in accordance with contract specifications.
EXAMPLE-12/96
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Christine Clark
Page 10
Matrix Spike/Matrix Spike Duplicate (MS/MSD )
Volatile
The following table summarizes the volatile matrix spike and matrix
spike duplicate compounds that failed to meet the recovery
criteria:
SAAO 9
Compound
MS
%REC
MSD
%REC
QC
Limits
PD
QC
Limits
Action
Positive
NDs
Detects
Ch lorobenzene
59
60-133
A
A*
* Although the matrix spike compound chlorobenzene recovered
below the QC limits, professional judgment was used to accept
all sample data since the MS recovery was only slightly below
the QC limits and the MSD recovery was within QC limits.
Semivo].ati].e
All criteria were met for the MS/MSD.
Field Duplicates
Volatile
The following table summarizes the volatile compounds that failed
to meet the field duplicate criteria of RPD < 50 for soils:
Compound
Benzene
Trichioroethene
1 ,1,1-Trichioroethane
SAAU
SAA14
RPD
141
167
131
Action
Affected
Samples
S A09-14
SAP.09-14
SAA0914
Positive
Detects
J
J
J
NEs
UJ
UJ
TJJ
Sample
Conc.
(ug/kg)
29
12
29
Duplicate
Conc.
(ug/kg)
167
133
140
Because the laboratory precision was acceptable, the validator
concLided that imprecision was either a result of poor sampling
technique or a heterogeneous sample matrix at the site. The
sampler was contacted to ascertain if sampling problems were
encountered during collection. The sampler noted that the
EX.ANPLE- 12/96
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Christine Clark
Page 11
duplicate samples looked very different, one was dark and the other
was sandy. The validator suspects that the matrix was
heterogeneous and therefore, professional judgment was used to
estimate (J) all positive detects and estimate (UJ) all
quantitation limits for benzene, trichioroethene, and 1,1,1-
trichioroethane in all other volatile soil samples in the SDG:
SAAO9, SAAb, SAA11, and SAA12. The validator recommends that the
end user assess spatial variability and notes that additional
sampling might be necessary to fully characterize a site with
heterogeneous matrices and a high degree of variability.
Semivolatile
The following table summarizes the sernivolatile compounds that
failed to meet the field duplicate criteria of RPD < 5O for soils:
Compound
SA.A13
SAA14
RPD
Action_____
Affected
Samples
Po3itive
Detects
NDs
Sample
Conc.
(ug/kg)
Duplicate
Conc.
(ug/kg)
1,4-Dichioroberizene
750
4700
145
J
JJ
SAAO9-14
Naphthalerie
480
2100
126
J
UJ
SAA O9-14
Acenaphthene
560
1300
80
J
U .Y
SAAO9-14
As discussed above in the volatile section, the validator suspected
the matrix was heterogeneous and therefore, professional judgment
was used to estimate (J) all positive detects and estimate (UJ) all
quantitation limits for l,4-dichlorobenzene, naphthalene, and
acenaphthene in all other sernivolatile soil samples in the SDG:
SAAO9, SAA1O, SAA11, and SAA12. The validator recommends that the
end user assess spatial variability and notes that additional
sampling might be necessary to fully characterize a site with
heterogeneous matrices and a high degree of variability.
Performance Evaluation Samples - Accuracy Check
Volatile
The field sampling contractor was unable to procure a soil volatile
PES as required in the Region I Performance Evaluation Guidance,
7/96 due to lack of availability. An aqueous volatile PES was
obtained from Region I OEME-QA. Therefore, the aqueous PES SAA25
will be used to evaluate the laboratory’s instrumental ability to
correctly identify and quantitate volatiles. The results of the
performance evaluation sample, EPA number SAA2S, did not meet the
required criteria for the following compounds.
EX 1PLE-l2/96
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Christine Clark
Page 12
The following table notes the score and corresponding action.
Compound
Score
Action
Affected
Samples
Positive
De tee te
NDa
Carbon Tetrachioride
Action High
J
A
SAAO9-15
Tetrachioroethene
Action Low
J
ft
SAAO9-l5
The laboratory has demonstrated an inability to accurately recover
carbon tetrachioride and tetrachloroethene through poor PES
results. Since the results for carbon tetrachioride were above the
acceptance limits, the sample results are potentially biased high.
Since the results for tetrachioroethene were below the acceptance
limits, the sample results are potentially biased low and the
potential for false negatives exists.
Semivolatile
The field sampling contractor was unable to procure a soil
semivolatile PES as required in the Region I Performance Evaluation
Guidance, 7/96 due to time limitations. An aqueous semivolatile
EPA-PES was obtained from Region I OEME-QA. The results of the
performance evaluation sample, EPA sample number SAA23 met all
criteria for the detected compounds, 2-methyiphenol, fluorene,
benzo [ b] fluoranthene, and benzo [ k] fluoranthene.
Compound Quantitation and Reported puantitation Limits
Two soil samples were reported with percent solids below 30%. The
validator suspected that these were sediment samples. Sample SAA1O
had 20% solids and SAA1]. had 8% solids. The positive detects of
SAA1O were estimated (J) and the non-detects were rejected (R) as
unusable since the % solids was below 30% but greater than 10%.
All the results for SAA .11 were rejected (R) as unusable since %
solids was less than 10%. As a result of the low % solids for
these samples, the DQO required quantitation limits were not met.
It was recommended that the sampler obtain samples containing
higher % solids by decanting excess water, filtering or
centrifuging samples in the field and possibly compositing sample
aliquots if necessary. Additionally, other analytical methods
and/or sample prep methods should be used to achieve desired
quantitation limits.
EXANPLE-12/96
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Christine Clark
Page 13
Tentatively Identified Compounds
The laboratory originally reported a xylene isomer as a TIC in the
sernivolatile fraction of soil sample SAA12 and xylene was not
reported in the volatile fraction. The laboratory was contacted
and requested to requantitate the false negative result and report
the result in the volatile fraction. The laboratory complied and
m-xylene was reported correctly on the Data Summary Table.
Seinivolatile Cleanup
GPC Calibration raw data were examined to verify that the proper
collection and dump cycles were utilized to ensure that all
interferences were removed without the loss of target compounds.
All GPC retention time criteria were met and the peak shape
appeared to be symmetrical; however, the resolution between
perylene and sulfur was slightly below the 9O method acceptance
criteria at 88’s. Further evaluation of the sample chromatograrns
determined that there was not a dominant presence of high
molecular-weight interference. Since there was no significant
matrix interference, professional judgment was used to accept all
data.
System Performance
Volatile
One sample recovered an IS area extremely low but the laboratory
failed to reanalyze the sample in accordance with contract
specifications. Therefore, the validator could not ascertain
whether the extremely low is recover . was due to poor laboratory
technique or the result of sample matrix interference. The
laboratory also demonstrated an inability to accurately recover
carbon tetrachlorjde and tetrachioroethene in the PES.
S exnivolatjle
The semivolatj].e soil/sediment sample results do not indicate any
major analytical data quality trends or problems.
EXANPLE-12/96
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Christine Clark
Page 14
Please contact M. Howard at (999) 232-7000 if you have any
questions regarding this information.
Very truly yours,
HOWARD ENVI RONMENTAL
_i l. i-(o jt’ 4
M. Howard
Data Validator
c5
S. Howard
Senior Validator
CC: Victor Herrion, EPA Site Manager
Attachments: Table I: Recommendation Summary Table
Table II: Overall Evaluation of Data
Table III: TIC Summary Table
Data Summary Tables
Data Validation Worksheets
PES Score Reports
Communication/Phone Logs
Field Sampling Notes
CSF Audit (DC-2 Form)
DQO Summary Form
EXANPLE-12/96
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TABLE I
Recommendation Summary Table for Volatiles
Lou’s Landfill
SDG SAAO9
TABLE I: RECOMMENDATION SUMMARY TABLE
Sample Number
Matrix
Qualifier
SAAO9
S/S
J’ 23 ’ 4 R’
SAA1O
S/S
J 235 R 45
SAA11
S/S
R 3
SAA12
S/S
J 3 ’ 4 R 5
SAA13
S/S
J 3 R 5
SAA14
S/S
J 34 R 2
SAA15
AQ
R 5
- Preservation and storage criteria not met: J detects
(Potential low bias)
- Trip blank contamination: Qualify 1,2-dichioroethane detects
“TB (Potential high bias)
- Poor field duplicate precision: J benzene, trichioroethene,
and 1,1,1-trichioroethane detects, UJ benzene,
trichioroethene, and 1,1, 1-trichioroethane non-detects
J 4 - Unacceptable PES results: J carbon tetrachioride detects
(Potential high bias), J tetrachloroethene detects (Potential
low bias)
- Percent solids below the required 30% but above 10%: J detects
R’ - Preservation and storage criteria not met: R non-detects
(Possibility of false negatives)
R 2 - Internal standard recoveries extremely low (< 20%): R non-
detects for compounds quantitated using bromochioromethane IS
(Possibility of false negatives)
- Percent solids less than 10%: R detects and non-detects
R 4 - Percent solids less than 30% but above 10%: R non-detects
- Unacceptable PES result: R tetrachioroethene non-detects
(Possibility of false negatives)
A - Accept all data.
EXAMPLE- 12/96
-------
TABLE I
Recommendation Summary Table for Sexnivolatiles
Lou’s Landfill
SDG SAAO9
TABLE I: RECOMMENDATION StJMMARY TABLE
Sample Number
Matrix
Qualifiers
Acid
B/N
SAAO9
S/S
A
‘ 4 ’ 5 R 1
SAA1 O
s/s
J 6 R 4
J’ 2 ’ 46 R 4
SAA11
S/S
R 3
R 3
SkA l2
S/S
A
3’ 45 R’
SAA13
S/S
A
J’ 2 ’ 47 R 2
SAA].4
S/S
A
J 2347 R 2
SAA1G
AQ
A
A
- %D criteria RD > 25%) J fluorene detects, tJJ fluorene non-
detects
- Average RRF criteria ( P < 0.05): J benzo(a)pyrene detects
(Potential low bias)
- Internal standard recoveries low: J detects and UJ non-detects
of compounds quantitated using acenaphthene-d].0
- Poor field duplicate precision: J l,4-dichlorobenzene,
naphthalene, and acenaphthene detects, tJJ l,4-dichloroberizene,
naphthalene, and acenaphthene non-detects
- Equipment blank contamination: Qualify dibenzofuran detects
- Percent solids below the required 30% but above 10%: J detects
J 7 - Advisory Surrogate l,2-dichlorobenzene-d 4 recovered low which
indicates a problem potentially exists in the accurate
quantitation of target compound l,4-dichlorobenzene: J 1,4-
dichlorobenzene detects (Potential low bias)
R’ - Average RRF criteria (RRF < 0.05) :R benzo [ a]pyrene non-detects
(Possibility of false negatives)
R 2 - Advisory surrogate ].,2-dichlorobenzene-d4 recovered low which
indicates that a problem potentially exists in the detection
of target compound l,2-dichlorobenzene and 1,3-
dichlorobenzene: R 1,2,-dichlorobenzene and 1,3-
dichlorobenzene non-detects (Possibility of false negatives)
R 3 - Percent solids less than 10%: R detects and non-detects
R 4 - Percent solids less than 30% but above 10%: R non-detects
A - Accept all data.
EXM PLE-l2/96
-------
EPA-NE - Data Validation Wotksliect
Overall Evaluation of Data - Data Validation Memuraitduiu - Table 11
VOLATILE ORGANICS
DQO (list all DQOs)
Sampling and/or
Analytical Method
Ai propna(c
Yes or No
Measurement Error
Sampling
Variability**
l’utcntial
Usability
Issues
Analytical Error
—‘
Sampling Error*
•Ecological Risk Assessment
•Source ldcntilication
•Surface waters collected from
this site were found to have the
following contaminants: bcn ene,
trichihoroetliene, tetracliloroetliene,
1 .2-dichloroethietie, and 1.1.2.2-
tetraclihoroeihiane. Are the Site
soils a source of contamination?
Yes, sampling and
analytical uitemliod,
CLP SOW
OLMO3.2,
appropriate for
samples:
SAAO9. SAAt2,
SAAI3, SAA I4
No, sampling and/or
analytical method,
CLI ’ SOW
OLMO3.2,
inappropriate for
samples:
SAA IO. SAAI I
Refer to qualificalioims
iii R/S Key:
i ’ 4
R’ -
Refer to qualiflcations
in RIS Key:
i ”
R 34
•Pøor field (luplicalc piCCiSiOll
iiidicatcs a pm oblcni mu obtannuig
rctncscultatiVC data, luumtung (lie
achievement of DQOs.
‘All tetracliloroethiciie non-detects
arc rejected in all volaijIc
soil/sediment sam Ples due to low
bias ol PI result and possibility of
false negatives. All
tetraChulUIOethIeIle poSitive detects
arc potentially biased low.
‘Alt volatile imn-detccts are
rejected in SAA 10 due to low
percciit 5Ol,(lS and alt positive
detects are estimated.
•All volatile resulis are rejected in
SAAI I due to extretitely low
percent solids.
‘All non-detects quantitated against
broinocliloroinetliafle in volatile
sample SAAL4 are rejected as
iuuiusable due to poor IS recoveries
and the possibility of False
negatives.
•All non-detects in SAAO9 aie
rejected due to imnpioper sample
preservatioll and storage by tile
laboratoiy.
* The evaluation of “sampling error” catinot be completely assessed in data validation.
** Sampling variability is not assessed iii data validation.
1 -v,. Date: -
r i
Validator:
N
12/96
-------
EPA-NE - Data Validation Woikslieet
Overall Evaluation of Data - Data Validation Memorandum - ‘I’able H
SEMIVOLATILE ORGANICS
DQO (list all DQOs)
Saiiipliiig and/or
Analytical Method
Appropriate
Yes or No
Mcasurcnicuit Error
Saniplitig
Variability ’ t
Potential
Usability
Issues
Analytical Error
Sampling Errort
•Ecological Risk Assessment
•Source Identification
•Surface waters collected from
(his Site were found to have the
following contaminants: 1,2-
diclilorobenzene. 1.2,4-
(richlorobenzene, 1,4-
diclilorobcnzene. Arc the site
soils a source of contamination?
Yes.smnplig and
analytical iiictliod,
CLP SOW
OLMO3.2,
appropriate for
smuples:
SAA (J9. SAAI2,
SAAL3, SAAI4
No, sampling and/or
analytical method,
CLP SOW
OLMO3.2,
inappropriate for
samples:
SAA1O, SAAII
Refer to qualifications
in li/S Key:
J 1 ’. 7
Rh
Refer to qualifications
in li/S Key:
J 1 6
l i ’ 4
• Poor field (lul)licalc prccisiou
iiidicatcs a prublciii in obtaining
representative data, lituititig the
achievement ci DQOs.
• I ,2-dichlorobdn7cu lc mul 1,3—
dichloiubenzeiic non-detects arc
rejected due to the possibility of
false negatives and 1,4-
dichlorobcnzeiie positive detects arc
estimated in seniivolatile samples
SAAI3 & SAA I4 due to potential
low bias indicated by low surrogate
recoveries.
• All seuiivolatile iioii-detects are
rejected in SAA IO due to low
percent solids and all positive
results are estimated.
•All seniivolatile results are
rejected in SAA 11 due to extremely
low percent solids.
• l3cn7ol aJpyrene iioii-detects arc
rejected in semivolatile saitiples
SAAO9, SAAII, & SAAI2 due o
lack of instrument stability and the
possibility of false negatives.
Iienzo [ alpyrene positive detects are
estimated an seiiiivolatile samples
SAAb, SAM), & SAAI4 due o
lack of instrument stability and
potential low bias.
,
e
* The evaluation of “sampling error” cannot be completely assessed in data validation.
** Sampling variability is not assessed in data validation.
/ yi, /cz r J
Date: _________
Validator:
12/96
-------
TABLE III: VOLATILE TENTATIVELY IDENTIFIED COMPOUND SUMMARY
There were no reported volatile tentatively identified compounds.
EXA PLE-12/96
-------
TABLE III: SEMIVOLATILE TENTATIVELY IDENTIFIED COMPOUND SUMMARY
I Classification/isomer
SAAO9
SAA1O
SAA1].
SAA12
SAA13
S.AA14
Dodecanoic acid
1
1
17-Pentatriacontane
1
1
1
1
Benzeneacetjc Acid
1
1
1
Heptacosane
1
1
1
Docosanoic Acid
1
1
11H-Benzo(a] fluorene
1 -Hexacosanol
1
1
1
1
The number indicated in the above table represents the number of compounds
of that classification identified in the sample.
EX.ANPLE-12/96
-------
DATA SUMMARY TABLE
Volatile Soil Analysis
ug/Kg
SITE bus Landrill - Anywhere. MA
CASE NO. 1011 SOG NO SAAO9
SAMPLE NUMBER SAAO9 SM1O SN 11 SAA 12 SM13 SAA14
STATION LOCATION. NWI NW2 SEI SE2 Ni Ni
LABORATORY NUMBER LAB O9 LAB 1O LAB 1 1 LA B12 L.AB13 LAB14
COMPOUND CROL.
Chioromelhane 10 R R R 12 U 12 U R
Bromomelhane 10 R R R 12 U 12 U R
Vinyl Chloride 10 R R R 12 U 12 U R
Chloroethane 10 R R R 12 U 12 U R
Methylene Chloride 10 R R R 12 U 12 U R
Acetone 10 R R R 12 U 12 U R
Carbon Disullide 10 R R R 12 U 12 U R
1,1-Dich loroethene 10 I i R R 12 U 12 U R
1.1-Dich loroethane 10 R R R 12 U 12 U R
1 ,2-Dichloroethene(totaI) 10 fl R R 12 U 12 U R
Chloroform 10 R R R 12 U 12 U R
1,2 -O lchloroethane 10 5 J TB 8 J TB R 12 U 12 U R
2-Bulanone 10 R R R 12 U 12 U R
1 ,1 ,1-Trichloroethane 10 fl R R 12 UJ 29 J 140 J
Carbon Tetrachloride 10 R R R 20 J 12 U 13 U
Bromodichloromethane 10 R R R 12 U 12 U 13 U
1,2-Dich loropropane 10 R R R 12 U 12 U 13 U
cis-1.3 -Dich loropropene 10 R R R 12 U 12 U 13 U
Trichloroethene 10 R 75 J R 82 J 12 J 133 .1
Dubromochtoromethane 10 R R R 12 U 12 U 13 U
1,1,2-Trlchloroethane 10 R R R 12 U 12 U 13 U
Benzene 10 16 J 100 J R 12 Ui 29 J 167 J
trans.1 ,3-Dichloropropene 10 R R R 12 U 12 U 13 U
Dromolorm 10 R R R 12 U 12 Li 13 U
4-MethyI -2-Pentanone 10 R R R 12 U 12 U 13 U
2-Hexanone 10 R R R 16 12 U 13 U
Tetrachloroethene 10 22 J R R R R 19 J
Toluene 10 fl R R 12 U 12 U 13 U
1.1,2,2-Tetrach loroethane 10 R R R 12 U 12 U 13 U
1,2-Dubromoethane 10 R R R 12 U 12 U 13 U
Chlorobenzene 10 R R R 12 U 12 U 13 U
E lhy lbenzene 10 R R R 12 U 12 U 13 U
Styrene 10 R R R 12 U 12 U 13 U 17 1
TotalXylenes 10 R R R 13 12 U 13 U
DILUTION FACTOR: 1.0 1 0 1.0 1 0 1 0 1 0
DATE SAMPLED: 03123197 03123/97 03/23/97 03/23/97 03/23/97 03/23/97
DATE ANALYZED: 03/29/97 03129/97 03129/97 03/29/97 03/29/97 03/29/97
% SOLIDS 95 20 8 85 80 75
-------
SITE: Lous Landlill - Anywhere. MA
CASE NO. 1011 SDGNO: S,4A09
SAMPLE NUMBER SAA15
STATION LOCATION TB
LABORATORY NUMBER LAB15
COMPOUND CRQL
Ch loromethane 10 10 U
Bromomelhane 10 10 U
Vinyl Chloride 10 10 U
Chloroethane 10 10 U
Methylene ChlorIde 10 10 U
Acetone 10 10 U
Carbon Disulfide 10 10 U
1 .1-D lchloroe lhene 10 10 U
1.1-Dich toroethane 10 10 U
1.2-Dich loroethene(Iota l) 10 10 U
Chloroform 10 66
I ,2-D chIoroethane 10 35
2-Butanone 10 15
1 .1 .1-Trichloroethane 10 10 U
Carbon Tetrachtoride 10 10 U
Bromodichloromethane 10 10 U
1.2-Dich toropropane 10 10 U
c ls -1.3-Dichloropropene 10 10 U
Tr lchioroethene 10 10 U
Dibromochloromethane 10 10 U
1.1.2-Trichloroethane 10 10 U
Benzene 10 10 U
trans-1.3-Dithtoropropene 10 10 U
Bromoform 10 10 U
4-Methyl-2-Pentanone 10 10 U
2- 1-texanone 10 10 U
Tetrach loroethene 10 R
Toluene 10 10 U
1.1.2.2-Tetrach toroethane 10 10 U
1,2-Dibromoethane 10 10 U
Chlorobenzene 10 10 U
EthyIbenz ne 10 10 U
Slyrene 10 10 U
Total Xytenes 10 10 U
============ ====
DILUTION FACTOR: 1 0
DATE SAMPLED: 03/23197
- ATE ANALYZED: 03(29/97
OA A SUMMARY TABLE
Volatile Aqueous Analysis
ugh
-------
DATA SUMMARY TAI3LE
Semivolatilo Soil An tysls
ug/Kg
SITE I.ous landflht - Anywhere. MA
CASE NO: lOll SDGNO SA.A09
SAMPLE NUMBER SAA O9 SAA IO SMI I SAAI2 SM13 SM I4
SAMPLE LOCATION NWI NW2 SE1 SE2 NI NI
LA OO RATOR’r NUMBER LAB O9 LAB 1O LAB 1 1 1A 012 1A0 13 1A614
COMPOUUD CR0
Phenol 330 350 U Ii I i 390 U 410 U 440 U
bls(2-Chtoroethyl) ether 330 350 U R I i 390 U 410 U 440 U
2-Ch loroplienol 330 350 U R I I 390 U 410 U 440 U
1.3-OIchlorobenzer e 330 350 U R R 390 U R R
1.4-D ichtorobenzene 330 300 J R R 390 Ui 750 J 4700 J
1.2-D lch lorobenzene 330 350 U R Ii 390 U R Ii
2-Methylphenol 330 350 U 560 J Ii 390 U 410 U 440 U
2,2-oxybis(1.Ch loropgopane) 330 350 U R R 390 U 410 U 440 U
4-Methytplienol 330 350 U R R 390 U 410 U 440 U
N-Nitroso-dI-n propylanilne 330 350 U R R 390 U 410 U 440 U
Hexachtoroe lhane 330 350 U R R 390 U 410 U 440 U
Nitrobenzene 330 350 U R R 390 U 410 U 440 U
Isophorone 330 350 U R R 390 U 410 U 440 U
2 -N trophenoI 330 350 11 810 J R 390 U 410 U 440 U
2 ,4-Dimethylphenol 330 350 U R R 390 U 410 U 440 U
b Is(2-Chtoroethoxy)methane 330 350 U R R 390 U 410 U 440 U
2,4 -D lchtoropheno l 330 350 U R R 390 U 410 U 440 U
1,2,4-Tt lch lorobe,izetie 330 350 U 420 J R 390 U 660 670
Naph thatene 330 350 UJ R R 480 J 480 J 2100 J
4-Chloroanlilno 330 350 U R R 390 U 410 U 440 U
Hexathlorobuladiene 330 350 U R fl 390 U 410 U 440 U
4-Ch loro-3-Me lhytpheno l 330 350 U R R 390 U 410 Li 440 U
2 -Me thy lnaphthatene 330 350 U R R 390 U 410 U 440 U
Hexachlorocyclopentadlene 330 350 U R R 390 U 410 U 440 Ui
2.4,6.Irlch lo rophenot 330 350 U R R 390 U 410 U 440 Ui
2.4 ,5•Trlchtoropheno t 800 840 U R R 940 U 1000 U 1100 Ui
2 -Ch loronaphtha lene 330 350 U 660 J R 390 U 410 U 440 Ui
2-Mtroan l ljne 800 840 U 940 U 1000 U 1100 Ui
Dimethytphthatate 330 350 Ii R R 390 U 410 U 440 Ui
Acenaph thylene 330 350 U R R 390 U 410 U 440 Ui
2.6 -D inRrototuene 330 350 U R R 390 U 410 U 440 Ui
3-N utroanflhrm 800 840 U R R 940 U 1000 U 1100 Ui tO
Acenaph lhene 330 620 J R R 580 J 560 i 1300 J
2.4-Dinltrophenol 800 840 U R R 940 U 1000 U 1100 Ui
4-Nltroptienol 800 840 U R R 940 U 1000 U 1100 Ui
Dubenzofuran 330 630 i EB R R 530 i ED 410 U 440 Ui H
2 ,4-Din ltrololuene 330 350 U R R 390 U 410 U 440 Ui
Dle(hytphthatate 330 350 U R R 390 U 410 U 440 UJ
4-Ch lorop lienyl-Phenylelher 330 350 U R R 390 U 410 U 440 Ui
Fluorene 330 350 Ui U R 420 J 410 Ui 440 UJ
4-Nutroanhilne 800 840 U U R 940 U 1000 U 1100 Ui
4.6-D inl lro-2.Me lhytphenol 800 840 U R R 940 U 1000 U 1100 U
N-nhtrosodlphenylamine 330 350 U U U 390 U 410 U 440 U
4-Oromopheny l.Ptienylether 330 350 U U R 390 U 410 U 410 U
Hexac l r horobenze,ie 330 350 U 550 J U 390 U 410 U 440 U
-------
DATA SUMMARY TABLE
Semivolatile Soil Aiialysis
ug/Kg
SITE: Lous Landfill - Anywhere. MA
CASE NO.: 1011 SOG NO.: SPAO9
SAMPLENUMBER: SAA O9 SAA1 O SAA11 SAA12 SAA13 SAA14
SAMPLE LOCATION. NW1 NVV2 SE1 SE2 Ni Ni
LABORATORYNUMBER: LABO9 LAB1O LAB1 I LAB 12 LABI3 LAB14
COMPOUND CR0
Pentachforophenol 800 840 U R R 940 U 1000 U 1100 U
Phenanthrene 330 350 U R R 390 U 410 U 440 U
Anthracene 330 350 U R R 390 U 410 U 440 U
Carbazole 330 350 U R R 390 U 410 U 440 U
Oi-n-butylplithala te 330 350 U R R 390 U 410 U ‘1110 U
Fluoranfliene 330 350 U II R 390 U 410 U 440 U
Pyrene 330 350 U R R 390 U 410 U 440 U
Butylbenzy lphthalate 330 350 U R R 390 U 410 U 440 U
3 ,3-D lchlorobenz ldine 330 350 U R R 390 U 410 U 440 U
Benzo(a)anlhracene 330 350 U R R 390 U 410 U 440 U
Chrysene 330 350 U R R 390 U 410 U 440 U
B ls(2-ethylhexyl)phlhalale 330 350 U R R 390 U 2000 2000
Dl-n-octylphthalate 330 350 U R R 390 U 410 U 440 U
Benzo(b)fluoranthene 330 350 U R R 390 U 410 U 440 U
Benzo(k)tluoranthene 330 350 U R R 390 U 410 U 440 U
Benzo(a)pyrene 330 R 2200 J R R 500 J 530 J
Indeno(1 .2.3 .cd)pyrene 330 350 U R R 390 U 410 U 440 U
Dibenz(a,h)anthracene 330 350 U R R 390 U 410 U 440 U
Benzo(g.hj)pery lene 330 350 U R R 390 U 410 U 440 U
DILUTION FACTOR: 1.0 1.0 1.0 1 0 1.0 1.0
DATE SAMPLED: 03/23/97 03/23/97 03/23/97 03/23/97 03/23I97 03/23/97
DATE EXTRACTED: 03/29/97 03 129/97 03/29/97 03/29/97 03/29/97 03/29/97
DATE ANALYZED: 04/13/97 04/13/97 04/13/97 04113/97 04/13/97 04/13/97
% SOLID: 95 20 8 85 80 75
-------
DATA SUMMARY TAI3LE
Semivolalilo Aqueous Ai aIysIs
ugh
SITE. lous Landlihl - Anywheie. MA
CASE UO. 1011 SOGNO: S A09
SAMPLE NUMBER SI A16
SAMPLE LOCATION EB
LABORATORY NUMBER LAO 16
COMPOUND CR0
Phenol 10 10 u
fs(2.CtitoroeIhyI) ether 10 10 U
2-ChIo ophenoI 10 10 U
1.3-D lcliloroberizene 10 10 U
1.4•Dlc?liorobenzene 10 10 U
1.2•D lchlorobenzene 10 10 U
2-Melhyiphenol 10 10 U
2,2-oxybls(1-ChIoropropar.e; 10 10 U
4-Methylphenol 10 10 U
N.Nilroso-dI-o-propylarn lrte 10 10 U
Hpx c1i!oroe1hsne 10 10 U
Nltrobenzerie 10 10 U
lsophorone 10 10 U
2-N Irophenol 10 10 U
2 .4-Dirnethy lphenol 10 10 U
bIs(2-ChtofoeIlioxy)methano 10 10 U
2.4-D lth lovopheno l 10 10 U
1.2.4-Tulch losobenzene 10 10 U
Naphth tene 10 10 U
4-Ch loroanlilne 10 10 U
HexacIutorobutad lene 10 10 U
4-Chloro-3.Methylpheno l 10 10 Ii
2-Me lhy lnaphthalene 10 10 U
I-IexachIorocyc1open adiene 10 10 U
2,4.6 -Trlchiorophenol 10 10 U
2 ,4.5-Trlchiorophenol 25 25 U
2 -Chloronaphthalene 10 10 U
2-NitroanilIne 25 25 U
DImetliyIpt,tlia late 10 10 U
Acenaph thylene 10 10 U
2.6-Dtni trololuene 10 10 U
3-Nttroaniltne 25 25 U .0
Acenaph lhene 10 10 U C l
2.4-O lnltrophenol 25 25 U
4-Nitrophenol 25 25 U
Dlbenzofuran 10 50
2,4 -Dinllrototuene 10 10 U N
D lethylp lilha ta le 10 10 U
4-ChIoIophenyt.Pheny lethe, 10 10 U
Fluorene 10 10 U
4-Nttroan lflne 25 25 U
4.6-DInItro-2-Melhy lphenol 25 25 U l x i
N-nh lrosodipheny lam lne 10 10 U
4-Bromophenyl-Phenyle lher 10 tO U
Hexac1i orobenzene 10 10 u
-------
SITE: Lous Landlill - Anywhere, MA
CASE NO.: 1011 SOG NO.: SP/ 09
SAMPLE NUMBER. SAA I6
S AMPI.E LOCATION:
LABORATORY NUMBER: LAB 113
COMPOUND CR0
Penlach lorophenol 25 25 U
Phenonihiene 10 10 U
Anthracene 10 10 U
Carbazote 10 10 U
D -n-buIyIphtIia1ate 10 10 U
F Iuor nIIiene 10 10 U
Pyrene 10 10 U
Butylbenzy lpht liala le 10 10 U
3.3 -DichIorobenzIdine 10 10 U
Benzo(a)anttuacene 10 10 U
Chrysene 10 10 U
Bis(2-ethylhexyl)plitl ialate 10 10 U
DI-n-oc lytphthalate 10 10 U
Benzo b)fluoran IIiene 10 10 U
Benzotk)fluoranlhene 10 10 U
Benzo(a)pyrene 10 10 U
ndeno(1.2.3.cd)pyrene 10 10 U
Dibenz(a,h)anthracene 10 10 U
Benzo(g,hj)pery lene 10 10 U
DILUTION FACTOR: 1.0
DATE SAMPLED: 03/23/97
DATE EXTRACTED: 03/29(97
DATE ANALYZED: 04/13/97
DATA SUMMARY TABLE
Semwolahle Aqueous Analysis
ug/L
-------
EPA-NE
Data Validation Worksheet Cover Page - Page 1
Site Name ( . ..ou L€z,,dRcZ
Reference No.
REGION I ORGANIC DATA VALIDATION
The following data package has been validated:
Traffic Report Sample Nos. 5 9 O -
Trip Blank No.
Equipment Blank No. $.9 ’9IA
Bottle Blank No. Vo ’J&- Dme 81 —ni’ Lo1 (( 4/ rD7 . iiy aie’/eed ($ 3. ?o) I J9
Field Duplicate Nos. *Pr13
PES Nos. 5n’
The Reaion I. EPA-NE Data Validation Functional Guidelines for Evaluacin2 Environmental Analyses ,
revision I?-)% was used to evaluate the data and/or approved modifications to the EPA-NE
Functional Guidelines were used to evaluate the data and are attached to this cover page: (attach modified
criteria from EPA approved QAPjP or amendment to QAPJP).
A Tier H or valuation was used to validate the data (circle one). If a Tier II validation with a
partial Tier m was used, then identify samples, parameters, etc. that received partial Tier Ill validation
The data were evaluated based upon the following parameters:
- Overall Evaluation of Data
- Data Completeness (CSF Audit - Tier 1)
- Preservation & Technical Holding Times
- GC/MS & GC/ECD Instrument Performance Check
- Initial & Continuing Calibrations
- Blanks
- Surrogate Compounds
- Internal Standards
- Matrix Spike/Matrix Spike Duplicate
Region I Definitions and Qualifiers:
- Field Duplicates
- Sensitivity Check
- PE Samples/Accuracy Check
- Target Compound Identification
- Compound Quantitation and Reported
Quantitadon Limits
- TICs
- Senüvolatile and Pesticide.’PCB Cleanup
- System Performance
A - Acceptable Data
J Numerical value associated with compound is an estimated quantity.
R - The data are rejected as unusable. The R replaces the numerical value or sample quantitation limit.
U - Compound not detected at that numerical sample quandtation limit.
UJ - The sample quantitation limit is an estimated quantity.
TB, BE, EB - Compound detected in aqueous trip blank, aqueous bottle blank, or aqueous equipment
blank associated with soil/sediment samples.
Va! idator’s Name M . I4 2t d
Date Validation Started /
Company Name 713 Phone Number 7DZDO
Date Validation Completed b / -
Lab Name Q O
,4 ,a
Lj1 ’c J L %b
P St 1 A BL.
SOW/Method No.
Sampling Date(s)
Shipping Date(s)
Date Rec’d by lab
O iO3, -
3.;3 .
Case/Project No. ,oi
SDG No.
. 1.5. ‘
No. of Samples/Matrix
. S 2 4
EXAMPLE-12/96
12/96
-------
EPA-NE
Data Validation Worksheet Cover Page - Page 2
Check if all criteria are met and no hard copy worksheet provided. Indicate NA if worksheet is not applic&’-
to analytical method. ote: there is no standard worksheet for System Performance, however, the valith
must document all system performance issues in the Data Validation Memorandum.
VOA/SV worksheets
VOAISV-PestIPCB COMPLETE SDG FILE (CSF) AUDIT ____
VOAISV-PestJPCB-I PRESERVATION AND HOLDING TIMES _____
VOA/S V-Il GC/MS INSTRUMENT PERFORMANCE CHECK (TUNiNG) ____
VOA/S V-Ill INITIAL CALIBRATION ____
VOAJSV-IV CONTINUING CALIBRATION ____
VOAJSV-Pest/PCB-V-A BLANK ANALYSIS ____
VOA/SV-PestlPCB-V-B BLANK ANALYSIS ____
VOA-VI VOA SURROGATE SPIKE RECOVERIES ____
SV-VI SV SURROGATE SPIKE RECOVERIES ____
VOA/SV-VII INTERNAL STANDARD PERFORMANCE ____
VOAISV -PestIPCB-VIll MATRIX SPIKE/MATRIX SPIKE DUPLICATE ____
VOA1SV-PestJPCB-IX FIELD DUPLICATE PRECISION ____
VOAJSV-Pest/PCB-X SENS 1TIVITY CHECK _____
VOA/SV-PestJPCB-XI ACCURACY CHECK ____
VOAJSV-Pest/PCB-XII TARGET COMPOUND IDENT iFICATION ____
VOA/SV-PestJPCB-XIJI SAMPLE QUANTITATION
VOA/SV-XIV TENTAT 1VELY IDENTIFIED COMPOUNDS ____
VOA/SV-XV SEMIVOLATILE CLEANUP ____
TABLE Il-WORKSHEET OVERALL EVALUATION OF DATA ____
Pesc/PCB worksheet.s
VOA/SV .Pest/PCB COMPLETE SDG FILE (CSF) AUDiT
VOAJSV-Pest/PCB-I PRESERVATION AND HOLDING TIMES
PestJPCB-HA GC/ECD INSTRUMENT PERFORMANCE CHECK-
RESOLUTION
PestJPCB4IB GC/ECD INSTRUMENT PERFORMANCE CHECK-
RETENTION TIMES
PestJPCB-IIC GCJECD INSTRUMENT PERFORMANCE CHECK-
ACCURACY CHECK OF INITIAL CALIBRATION
Pe tIPCB- IID GC/ECD INSTRUMENT PERFORMANCE CHECK
PESTiCIDE DEGRADATION
Pest/PCB-III INITIAL CALIBRATION
Pest/PCB-IV CONTINUING CALIBRATION
VOA/SV-Pe t/PCB-V-A BLANK ANALYSIS
VOAISV-Pe t/PCB-V-B BLANK ANALYSIS
Pest/PCB-VI SURROGATE COMPOUNDS:
SPIKE RECOVERIES AND RETENTION TIME SHIFT
Pes1PCB-VII PESTICIDE CLEANUP
VOA/SV-PestIPCB-VIjI MATRIX SPIKE/MATRIX SPIKE DUPLICATE
VOA/SV-Pest/PCB-IX FIELD DUPLICATE PRECISION
VOA/SV-Pest/PCB-X SENSITIVITY CHECK
VOA/SV-Pest/PCB-XI ACCURACY CHECK
Pesc/PCB-XII COMPOUND IDENTIFICATION
VOA ,’SV-Pest/PCB-XlIl SAMPLE QUANTITATION
TABLE ti-WORKSHEET OVERALL EVALUATION OF DATA
I certify that all criteria were met for the worksheets checked above.
Signature: I A . OviOA Name: (Y1V ‘ -
Date: ________________
12/96
-------
The data validator generates a Data Validation Report, applicable to Data Validation Tiers II and Ill, that consists
of the following components in the order specified below: (Refer to Section 11 for a description of each of the
Data Validation Report components).
1. Organic Regional Data Assessment/Inorganic Regional Data Assessment
(ORDA/IRDA) Form
2. Data Validation Memorandum
a. Narrative
b. Table I-QuaLifier Recommendation Summary Table
c. Table Il-Overall Evaluation of Data
d. Table Ill-Tentatively Identified Compounds
e. Data Summary Tables
3. Standard Data Validation Worksheets
a. Manual
b. Automated Data Review Reports (i.e., CADRE)
4. Support Documentation
a. Copy of non-CLP analytical method, e.g., DAS methods, modified EPA methods
b. Copies of PES Score Reports/Vendor PES QC Acceptance Limits
c. Copies of Telephone Logs/Communication Forms for:
• RSCC communications
• Requests for laboratory data resubmissions/clarifications
• Communications with samplers resolving sampling problems
• Communications with TPO/Lead Chemist to report contractually-deficient data
for rejection/reduced payment
• Communications with EPA Site Manager concerning possible data rejection
• EPA Site Manager authorization for alternate DV tier
d. Copies of data supporting recommendations for reduced payment resulting from CSF
Audit and/or PE sample result evaluation
e. Original data to support recommendations for data rejection/non-payment identified from
Tier II or Tier UI data validation
f. Copies of field sampling notes andlor field report supplied by field sampler
g. Copies of EPA-approved amendments to QAPJP and/or SAP describing modified criteria
to be used for validating site data
5. CSF Completeness Evidence Audit
6. DQO Summary Form
The data validator is responsible for implementing all corrective actions required by the contractor Lead Chemist
in response to EPA-NE data validation oversight findings.
12 /96
EXANPLE- 12/96
-------
1219(t
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(I No)
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i’rc,
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i
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- I
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ioIiacI Sau
I) Ie I of I1 ,
ho Let, I()
DNA
I
A,nlj,ed lion, lr. r.,,,ic,cd
D,Ie I of Ua i I Aclhm Ihie
to (tjial
I
huh ui 1
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to Let, I( )
I.SPIItI%
A I, I
I) tc
IuI uI t r
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to Auti
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WrIl
sfrni ,2
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f Je
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a
Preservation Code:
1. Cool @4°C (± 2°)
2. Preserve viili IlCI to at least p11 2
3. Protect froiii light
4. Freeze
5. Room Temperature (Avoid excessive heat)
(Ex(rrictiuiu Code:)
UL - Liquid/Liquid
SON - Soiiicatioii
SEt’ - Scparaiory Funnel
SOX - Soxhici
SPE - Solid Phase Extraction
Code:
Estiniate (3) 1) iectetl Values
Estimate (W I Nun-Detecird Values
Reject (R) Non-Detected Values
I PA-NE - bat lion
VOA/SV - 1’cstn’i . .is-
Sampler: ZToe. c ,r ;4{-
Company: %iou.’orS & tt’onaiodJ
Contacted:
1’ItESERViVIiON ANt) hOLDING I’1r IES — Circle sample ittinibers with exceeded tcclmical holding limes or omitted preset vatiomi.
List all required preservation codes and circle omitted preservation codes.
Circle all exceeded icclmical holding times.
Identify extraction technique alter “N of Days”/(*Extractiun Code).
Yes
Date:
Action
3-
I .) ) -
C’1
u-h
Valida(or: I
Date:
-------
EPA-NE - Data Validation Wvikshect
VOA/S V-Ill
111. INITIAL CALIBRATION - List all analytes that aie outside calitnation ri itci ia.
Daic .r
ICAL
J,ic , inuicut
Pnrnuuclcr
f%Jnha I x -
I
CwIIinnu,nI % RSI)
1tIU
Siutp les
AIfccIcd
Aciluit
I i
?c
S ’ ’
5tL Q
p rcnc
o.o f
‘ o —Sflr -l4
yz
Comuieiits:
Validator: IY ) . /tO) 1 . 4 7 Date: 6 O . L
‘6
-------
EI’A-NE - Data Validatioti Worksheet
VOA ISV-IV
1V. CONTINUING CALiBRATION - List all analytes that ate outside calibration
c i lid ia.
Date of
ICAI
Date or
CCAI 1
Iiistrtumciit
Pni zuiictcr
1 In(rIx
Coinpotiiid
%D
IUtIr
Saitipics Alfcctctl
Avliuii
l•13•qi
4i3•i
SV
So ’
F/ or ri
—
5i9t9c?-i*’ /1
Comments:
Validatur: (p1.
Datc: 5 . 2O- ’
12196
tO
(N
r 1
-------
EPA-NE - Data Validation Woikshcet
Vth%ISV - I’est/I’CIJ-V-A
V. IILM’11( ANALYSIS
List (lie blank contamination below.
Sampler: Je rviff- Company: f-toL arcI 51yicrn1n /7/ -°
1. Laboratoi-y: Method, Storage mid Instrwiicnl Blanks
Coiiceiiliatioii Level:
Contacted: No Date:_5 I?-. z
1.Jate
Extracted
Dale
Analyzed
I’arnnicter/
MautuI j
I Satiiple No.
(liIa,ik ‘i ypc)
Iuistitiiiient/
Coluiuuui
Compound
Coimc. (iuiil(s)
2fd1
1• A
5V(oiil
i(’,y,d(wd)
?(
mno’i1iiai k
44 g //
2. Field: Equipment (1thmsate , Trip and Bottle lilamiks
Hate
E trncted
Date
Analyzed
l’arnmeter/
lSlatrlx
Sample No.
(Blank Type)
hush urneut!
Coluuini
Cwuupowid
I
Cwic. (units)
N!
3 .l’ .T
vov /p
RAIs&r )
ft
CJ- ((,rOfrn1
I
4’
I
‘
I
‘I’
I
I, icJifo, oc/ aiie
/L
5c . .i — g/L
?• 1
cj j/
5p I4 (fj )
X
O q/L-
Validator: -tM
Dale: 5 ?-O -
-------
E1’A N1 - Data Validation Woikslicct
VOA/SV - I’cst/I’CB-V-Ii
3. lilanik Actions — List (lie niaxiinuin coiicciitiations of blank CoilipoUlidS.
0
rl
r
Coiiipound
Tyke or Blank
l)aie Bl:ink
Sainpled/thiginatcd
f%ln .
Cotic.
(units)
Acliun
Level
(niuils)
Siuiiple
QL
Snuisples
Al(ccted
Action
cJ . iprocvrrr
12- Dcj,/orpi Jfig,i
yi - -
-n -
TJ
I
e
n 4t 0
39 t
3. D i i .9
& - j /L
,ç 17 /i
5r3- /L ..
‘ i
Th
I
ei
3 !Q 1
(O2IjJt
‘°
io I
JQ)A5/t
33okjL
I JonC
Af- O?, St1f /?-
Movie
ND - ,
p/ -J
“18”
“&i 3”
WO -,r a €
5 we ’
Valkiator:
‘-M. k&IAJQAó(
Date: 5 • O .9 ?-
12/96
-------
E1’A-NE - Data Validatioji WoakslieeL
Sy-VI
VI. SV SURROGATE SPIKE RECOVERIES - List all suirogate coIu 1 )oUltd iccoverics that ate outside method QC acceptance ciilciia.
Method
Jinse/NeuIanl Method QC Acceptance C i Itci In
NIJZ-d 5
2-FBI’
TPJ I-d 14
I.2-DCB-d 4 t
Oilier:
OLM O3.2
Water Spji
35.114 23-120
Wa ç Soil
43-11630-115
Watcr Soil
33-141 IU- 137
Water Soil
16-11020-130
OLC O2.l
10-110
30-110
20-140
NA
Ocher:
Satn ,1e NuiiiberlMatiix
% ltccovciy
% Rccvieuy
% Rccuvei-y
% Recovery
% Recincry
Action
S ftI3/5 , (
If
/3
R Lu ti -
- J “ L’c 1 p°S ctd.
c1.4* ?.‘ S1rtc
Method
Avid Method QC Ac
ccptancc Criteria
I’lic Iw1-d
2-PP
2,4,6-T I3P
2 CP .d 1 *
OLlier:
OLM O3.2
Water Soil
lu .11 02cn3
Water Soil
21-11025-121
Water Soil
10-123 19-122
Water Soil
33-11020-130
OLCIJZ.l
15-115
15-110
15-130
NA
Other:
Sample Nuiiuiivi-IMnti i,t
% Recovery
% Recovery
% Recovery
% Recovery
% Rccuvci-y
Action
* Advisory Surrogates - OLMO3.2
Validator: (Vi. Ho c ja_id
Date: 5-?-O-?
12/9(1
-------
EPA-NE - Data Validation Workshcct
YOA/SV-V1 I
VI I. INTERNAL STANDARD [ ‘ERFORMANCE
List the internal standards that ate outside the area count and retention time method QC acceptance criteria.
IS Arca Count method QC acceptance critci in:
IS Retention Time method QC acceptance criteria:________________________________________
Saiiiple
Number
(‘FRY)
Date and Time
Analyzed
Jiistriiineiit
l’araiiietcr
IS Outside Area
Count and/ur
RT Cri( ja
IS Area
RI ’
Shift
Acceplalile
Range
(IS area or IFI sluR)
Ac lkm
S4 -14
3. . /i5:o
A
VQ/\
chIcrcni I4 ne
? /iX
/ S53- 5 ”? -JO
5 E -l1.
t.rYI /n:ti
‘
,v
ic- i t s-
—
I7lh’?- ?oc c( ,___
T,LAJ
0
(%
i-1
I
Validawr: i’A. H.ov c A
Dale: .-O.VI
12/96
-------
EPA-NE - Data Valkiatiori Wo kslieet
VOA/SV - l’est/ I’CIi-VIII
VIII. MA flUX SI’IKE/MATRIX S1’IKE DUI’LICATE - List all MSIMSD aiialytes that ale outside method QC acceptance
criteria.
Use a separate worksheet for each MS/MSD pair.
Sample II S, A 9 Matrix _______ Concentiation Level .0L—
Poranieter
Coiiipowid
MS
%Rec
MSD
%flec
1U’D
Metlioti
QC Liiiiits
Cwiccii(rnfluii
% RSI)
AcUoii
% flcc
1(PD
Unspiked
Sample
T
MS J MSI)
J
Von
J,fcrc&ci 3 ejte-
( 4 c- l33
-
Validator: 1)1 D tc: _________
6
-------
EPA-NE - gaLa Validation Woikslteet
VOA/SV - Pest/ I’CJi-IX
IX. FIELD DUPLICATE PRECISION - List all field duplicate analytes that mc outside ciitciia.
Use a separate worksheet for each field duplicate pair.
Sample Nuiiiber Si’1. / Duplicate Sample Nuiiiber 5 ,q-/4 - Matrix $o&
Parameter J
y 9f ___
L
S’J
Cwupound
1 2J &
l,y—TC.1
W p1- ft- a-k- ie
l 4 -PC .-
&p i* e
Sample
Comic.
1a q(K
‘Licjlk j
lk v
O iqjk4
o j 1
Sample QL
Duplicate
Comic.
t3 (k
1 7-IA JI
i4OAA51J 9
pp I
41po1)kj
13OO 1
Duplicite QL
R1’D
141
I
131
+
go
QC Acceptniice
Criteria IU’D or
NA’
50
I,
o
I
Action
C l
r Lf4 QL
“ -- ‘
,
‘?)cQ
SQL
13
‘V I
)
2 SQI.
f
SQL j 2 SQL
— —
( 2. yI ?4 f i
‘I1oJ(5(IO . 2O.z4qj
* For instances where one duplicate result is ND (or reported less than the sample QL).
Does the MSIMSD data indicate acceptable laboratory precision?
Comments: o 1Q k b I J
Sampler Name: To Contractor Name: flD tJ Eiw cortmc.s .kO Date Contacted: 5 . 1 .q -
Reason for Contact and resolution obtained: 1 ’ de!cmivic ).4 p!ec , ed ai / vistS JIVereac.s in s4 1pJe4 aiS/ 1 -
-there jer c in Iicth ,g Sa r ..-p/er ‘w1c 11 ’- e :fp/e L&. tC d m t& t-mc d k/1/ith. s ’s t. ,
Validator: ( Y . 4-/o xt.ed Date: . .ao •‘7
12/96
-------
E1’A-NE - Dala ValiiJalioii Wozkslicct
VOA/SV - PcstIl’CB-XI
XI. ACCURACY ChECK
SDG No: oe1
(l’crfonnaiice Evaluation Results) — List all analytcs that ale outside C l jieria.
CASE: / 0 / !
Are inoze Luau one—half of the PES analytes within c i itet ia for each patanicter.
I’E
Anuinile
t’arrnnctcr
Type of
Matrix
Ai lalyte
Coiuv.
Region I Ei’A
Noii -I t’A
IES
Saniples Aticcicil
Action
Saitipte
Number
I’ES
PES Scores’
Scores”
Nunibcr
s’ i s
J,
TrUos !
Vc
,
L-
f-
Co b TdracVorjdc
34i 5I
J(1-
/\c e i i( 1 ’ 1 L
ft t4 r Lo
W A
N/
5 e oq 9 iq/
J
* For Region I PESs indicate the Region I PES Score Report Result: Action high; Action Low; TCL MISS;
HIT; TIC MISS; TIC CONTAMINANT
0
For Noui-EI’A PESs iuidicate (lie uioui-El’A PI3S Score: PES COMPOUND MiSS; I’ES COMPOUND CONTAMiNANT; I’ES COMPOUNL
lilT (% Recovery Limits)
Vahidator: f \ . Date:
TCL CONTAMINANT; TIC
12/96
-------
RAS ORGANIC
PE SAMPLE NUMBER: TT0085].
TCL HITS
Analytical Labs
DAS No.: NA
9 503005-25
Contract: 68-D555
SDG No.: SAAO9
Date Received:
Date Analyzed:
TCL MISSES
TCL CONTAMINANTS
TIC HITS
TIC MISSES
TIC CONTAMINANTS
NOT SCORED
Lab
Lab
Lab
Lab
Name: Fine
Code: FAL
Sample ID:
File ID: NA
Carbon Tetrachioride
Tetrachioroethene
03/25/97
/-
73 ug/L
22 ug/L
Action High
Action Low
EX A MPLE-12/96
-------
RAS ORGANIC
PE SAMPLE NUMBER: TT00855
Analytical Labs
DAS No.: NA
9503005-23
2-Me thyiphenol
Fluorene
Benzo (b] fluroanthene
Benzo [ k] fluroanthene
Contract: 68-D555
SDG No.: SAAO9
Date Received:
Date Analyzed:
Lab
Lab
Lab
Lab
Name: Fine
Code: FAL
Sample ID:
File ID: NA
TCL HITS
03/25/97
If
In
Window
32
ug/L
In
Window
22
ug/L
In
Window
19
ug/L
In
Window
39
ug/L
TCL MISSES
TCL CONTAMINANTS
TIC HITS
TIC MISSES
TIC CONTAMINANTS
NOT SCORED
EXAMPLE-12/96
-------
- Data Valiilatioii Worksheet
VOAISV - Pest/I’CB-XIIL
Xlii. SAI\ I l’LE Q UANTI’I’AIiON
Recalculate, hour the raw data, the coriccuitratioris for One positive detect arid one reporlcd samji lc qn:iiitiIatiolI limit for a non-detect iii a diluted saiuupic or soil saruipic
per fraction. (Note: Although Secliuji XIII. C. I .a, rcquircs that one calculation for each fraction in cacti sarirpic tic pcrforuuicd, tire validator is only icquiicd to
reproduce an exairiple, for each fraction, of one pOSitive detect and one sample quauitital ion hunt calculation on this wurkslicct.)
L)o all soil/scdimcut sairipics Inavc % solids grcatcr than 30%?
If no, list sairiple uunrbcrs 4A to . SAA1
Frac llo,i
Colcu!. ’iilouu I
‘OA
(cac000) C 9 )C I)
4 )(Q. 4 )( )CO c) “ —
CR 1_ /0 x = t
( .)(o s’c)
San ple No.:
54M
Rc,i’ cd C.’iii 1 uuiiid:
rn c4itorii 4f enC
Reported Value:
Nut Detected Cunijitwud:
& fl1 1 PCl b• ’
m 4 1 44,e
Reported Quauiritatiun Liriiii
DNA
(I oo)C4o) ’’3X (’)
= —? io - I1C
O’)(30) (t. i)Ci) (0. 5l _)
Qft.QL- 3 > = 34 • 4 3 V - ) -
(ac j) (o. ..c)
Sample No.:
Reported Coiiipuund:
Ikenaeb1lief7
Reported Value:
?OM5!k .
Not Dci cIed Corupourid:
Reported Quirrtitatioii hunt:
D lii t ,Mfv/i
3 O.1e 1IIc4J.
Pestlcfd Il’CD
Sample No.:
Reported_Coruittouwi:
Reported Value:
Not Detected Coui,puuud:
Repu ucd Qua III itutlot, Llsui ii:
Vahidator: P7. c.t
w
( ‘1
r
Date:
12196
-------
EPA-NE - Data Validation Woiksheet
VOA/SY-XIV
XIV. TENTATI VELY iDENTIFIED COMI’O UNJJS (TICs)
List the 5 TICs having (lie highest concentialion for each sample L)alatfle(e1.
Sample Number
l’arametcr
Coiiipumitl
j
IUU’
Esi. Cviic.
Acliun
5Aptoq
,
s441a-
s’ Pc(4
I
I
I
L’
Pe ia Cord c
de a wlc /k S
Pxti’- 1 cjiectceJic 4c
t- I exoç ,ic-f
13.e7o
1 t t 1 ,
14.05
. -5
5’?
55o - ’ l
43oi jL
4cQ4
4IoJ ,4gI _
4J.a.j(f c -
cr
____
4’-1 JO L!O kTIC .
V9IiIt 1Ior: 1 ’l. ( (cu)cL4-c 9 . .
Datc: c a.o
12196
-------
EPA-NE - Data Validation Woiksliee [
VOA/SV-XV
XV. SEMIVOLATILE CLEANUP - List all analytes that are outside method cleanup QC ciieria.
Cleanup
Instrutne,it N
DntclTiuic GPC
Compound
% 11cc
QC
Samples Affected
Action
Procedure
or
Lot N
Calibrated or
Check Solution
Analyzed
Limits
*
Did (lie GPC column meet; resolution requirements? or
peak shape requirements? r N
retention tuite shift requirements? 0 N
Was (lie GPC calibration, Silica Gel cleanup checked at (lie method requited frequency with correct conipouiids and concentrations? Y or N
Were all compounds less than QL for the GPC/Silica Gel/Acid-Partition blank? or N
Did (lie blank surrogate recoveries and IS area counts and RTs (if added) iiieet method QC acceptance criteria? or N
Conunents: L,Ji \z&icjjt. r o enc ( O ,. u ;t-) cmc( D
w ecL az -ctp c{ Ji1.
Validator: 4&- RD .JO4cL . Date: 2c 7. . N
12/96
-------
Rq,uaai C -
C U Br — Libcriw
Iii rc . ‘o dzxa th. foLIa 4 u i. (i):
5M-is (723) _____
In Refe cn o Cisc No(s):
/on S 6 7 5’5 1 9O ?
5u .ry oi Quc /I cs D ’i
Ci &4 (is, - q/I-) M ded-w d
t )p j, fa-
cd- r4 c ,-k’j M- )1 .e
( J -I
I - 4J J, i- e4iia
S ’— .— —..yo( a ca
.
Oir i p Lei .
ccA.z
fp- t&Jp
ja-o ad v, ed * c
i/,14# - -€. iC1 ox.
bIa bs.
(1) L à Ceo, (2) R w C. oy, (3) SMO C y
1io &o.,
Lab C t
C utric L bor3zaI7 Progr
REGZC 4ALILABOP’ATCRY COMMUNICAflON SYSTEM
Te1ep oflc Reconi Lng
•I • 9 r
ll ) ttd &vfrôvm nkO
jb $im 4
r
Youi’ c”-
EX.AMPLE-12/96
-------
In Retc c o Cisc No(z):
/ t911 5D’ttiô. -i4tD ?
lJ.ww.iy O Qw . Ijcg D—’— :
D i’ d so- P -t k C Vl ezO :
sa -pl 4 t/ 0 r €ce
s aL i\ cc c S *- -’-Q .
U
S ,øfP—’—-. -i
.
-kL- 0 S - c — A
4L 4 4L - c
(I) Lab C. u 7 , (2) Rqiuu C cy, (3) SMO C. oy
Daas
-. 1 . ..c 1 -: 1
Conu ct ot Lory PrngT3m
REGIONALJLABORATORY COMMUNICATION SYSTEM
Tdephono Record Log
I 5 .:
Ui : / -4 & i vfr i
___ Zfo _..Sri ,‘- :1-
CaUT.. 43y —
10 dLa f th. (oflowic II
- eJ4. eJ- c - si A-/3
1.
!Y1 9e 1 LJa—(
Labo y - Rzg,co
EXANPLE-12/96
-------
Data of CaU:
L&bofp.&ory t4aa
Lib --
Re d C a
Oil In n r —
lo rtf 4 w data forth. foUow zinhi,(s):
In Rcfe c to Case No(s):
iou bo/th .5rn9 9
Su xy rn Q c ocii1i cs
‘is’)
efl . -kL
s$ L z- --j ?cPrI
S W LJ
The zb “c r<’ L(A 4-; -k-t- d •(‘
o y e R ‘ €- -‘ r pôc
- V-- jOlQ-i’ ( C \.
(1) Lab Copy, (2) Regioo Cooy, (3) SMO Copy
Dia.
Coutroct L.IbOr3LOIY Progi
REGIONAULABORATORY COMMUNiCATION SYSTEM
Telephone R ord Log
5./&
/ y z1q-h’c J Loh c
L F fiie
M.
EXAN LE-12/96
-------
1 3e.: 3. 3.1?- 3?39 - (C o c&. Fre’apc J )
3i# - Lot .’s L u d Lt, ‘ t o s
5 piex: ° - “ -
kfde/La hh de oç ’,1%J O” 3’j iI
00 I 011 - Vo “ SE — - cxo -i s
d&e -t ‘ . 5a-sid , — pictL - ta -j / O -’ h
r f. 0 1 P. 9
I Y. I - 3 - boo N
V ?kQ T p• /o’C-.
- / i’ /s/Jbroci”i.
T2 A Use. Eco (a 1?A5K I
fU4 5p n .$4 41-tpt4’hj &
; Ls ‘ /3 Q I - 5 1 4 /
• • • o w- o-eOA (,U j C &tA j o -, ) T ’ 1 -P. 1/
C& U0Fk T 0 &cD SUOI”z . f tAJ o;
-. 3ot i . Ia- ’-j Lo-f IL 35i ,
o:o o N S W 5 13 5A I*
i p.
sa ô/C — j 6± I2/ OLA)J1 -J-L e te-’ --- i i- do n&’ - .& -‘C
13c c t 2 I cuui S j aj 7 7 ,3ai ie O Ll S c-1 LO.
0:45 NUJQ — Sft/H1) —I.e? ii ’Iz A IVL)
pu 1e t p• 1/0 £ AJ 0 € L i (w c or ôbVaoz 4
tAJ ) , 5If kij, SoiL - ,i d. britu-)r? ) (1 5bi I
I I I
I3Q sei- S AI /00 SE 5 1
V s fr 4 1 sI1 soiL - S flI -
t LL i c fl -
-------
Evidence Audit photocopy
ORG2 NIC3 C. LZ Z S O 7112 (CZ?) fl v CRX
LA ORATOR t C f* L.-* j’( c . .-O
c: y/s A
c.;sz NO. IOU - SOC NO. s sos. o __________
____________ — SA NO. ________
C NTRACNO.
SOW NO. piA 3. -
A1 . doc m.nii d.liiered th tha C pL.te S C• P1. .a ua a o iqinaJ. dcc znan a
wk er osathj.e.
PACE NOs c cx
.tO
1. t v nt r7 Sheet (For DC—2) (Do riot nuxnber) ____ ____ __________
2. S G C.i II ÷
. SOG C. vez Sh tJ ffLc Re ort — __________
4. Vo1at J Data
a. QC 5ui usry
Syeta M c tr..ig c:= tind Sn y ( or 1 VOA) ____ ____ __________
Hat .x SpikafMat ix Spika Dupl.icata Suc e y
( ‘cr I:: 1OA) ____ ) - __________
Method BIa.riJC 5u a— 1 ’ ( cr ri VOA) I r __________
CCfMS p f anca C uc c ( ‘cr V VCA) J , I V
r al. Starida ? x a arid R Sua 7
( c n VI II VOA)
b. Sampla Data ______ 1/ ’
rc. Rezti1t - (?cr I VOA} ______ __________
ancativeLy eriti ied c ccunde ( c I VCA- C) ______ V
Rec .xotod tte.al. icri c .rcatzgra (RIC) f:r
each ea ne1e 1 ’
cr eac i ea n Le:
Raw ec :a ar d ackgr nd- u.ot.racad case
ectra of target cc aund3 ideritifiad / /
Quantjtatjcr2 racer s ______ _________
Ma33 5 ec a of all retorad C3 with three
bezt libra.ry atthas ______ __________
. Standards Data (All tt’ . ent2)
Initial Ca L ratiori Data ( c V1 VOA) ______ V —
arid Q an Retc fot all. Standa.rdz ______ / —
C.nti iri; Calthrati ri Data (?cr V VCA) . / __________
RICa arid Qt antjeatjcn Repcra for all Statda.rds ______ —
d. Raw C Data
3lanic Data ___ ___ _____ ________
‘at: ..x S ke/ at .rix S i e D licaZa Data ____ ______ __________
EXANPLE-12/96 ‘c DC- :-:. c yO2.
-------
Evidence Audit k’ iOtCCO
ORGANICS COMPLETE SDG FILE (CSF) INVENTORY SEEZ (Cant.)
CASZ O.
5G NO. q4o9 s:C NOL. TO FO .OW —
SAL NO.
.
PAGE NO CEEC(
FROM TO EPA
5. Se iat .1e! D t3
a. QC Sur ary
Sur:oga:e Pe::ent Re:overy SW flary (FCr I I! LV) lCD __________
M5/1 SD Suc ta:y (F I1 LV) 101 10 / __________
Method Blank Su ary CFC IV LV) ____
CC/MS r ament per er ance Check (FCr V LV) IO ____
Internal Standard Area and R Su Iay
(F0r v::: sv
b. Sarnple Data I 9
TCI. Res lt (F n SV—l, SV—2}
Tenta:ively Ide :ified ( c:n sv—T:c) ______ 1 /
st: c 2c t: a: inn ca::a. s ( C) fC
each. arn le /
Fc GaC 7 1G
Raw Bpec::a ar.d bank nd —s n aced rnass
s ec::a of tn::e: c:npn n:E
Quar :L:a:i: re;c:s —
Ma22 nec:ra c’ cc t —ee te!: lib:a:
c a’ : ee
G?C c :a:: :a (_f GPC per rr2:) v ’ ______
c. 5:a d a:r (A:: :ns:: : ; tI _ a 1 S
: . : .al Cia: .nn Da:a cr v: sv—:. sv-: ______
R:C a Qa p:::s f:: a . E:ar
C: :....; ca:_tra: :- a:a v:: sv—:, !V—2)
R C ar.d Q a : .:: .:n n::s ai. L:a. :n ______ —
A
-. 1 (4 L / 1 —
a -: a % L 19 ______ 1’ —
a:r.x S: s/M:::.x S: a9 :a:a ____ ______ —
e. Raw C C a: a c’0S ______
6. P szicides
a. Q S . ra::
nça:a Per:n : Re:: ery Su—..—a:y c-= :: i ) i ‘ pJj .. — —
Ms/ s: D n.i:a:eS ary (F 1 1 _ —
: : — .-. :y (F:= : :E: — — — —
F: Y :c-2-: c..MC.
EXANPLE-12/96
-------
Evidence Audit L-’ otocopy
ORGA}flCS CO L2TE SO C FILE (CSF) Ii :O SZEET (C t.)
o. ____________ soc No. s ô1 s c NOS. TO F OZLOW ___________
__________ __________ SAS NO.
PACE NOs C ZCY
F CM TO LAB
Ptj d (Cant.)
b. Sazple Data
TC Resu1t — Or anLc Ana1yE S Data
(Form I PEST)
C 1rcznat gams (Prir ary Colu in)
C ro nagra.m from second CC coL m C tiO
CC I : g:a:icrt r ;o:t or data system printout
Manual work a eets
For çes:icides/Arcolcrs comfLrmed by CC/NB,
copies o ra ectra and cies of backgr r.d-
subc:ac:ed mass c ec:ra cf ta:çe C OUfldS
(sa ples & s anda: s)
C. Standards Data ____ ____
Initial Cali.braticn of Sir.cle CO POr.Ont Analytes
(To t V PZ3—1 arid PEST-2)
In ..tial Caij :a:jo of 1:ic Crert Analytes
(Fcz VI PES—2)
Analyts Resni :i : S r ary (Fc: v: pEs:-4)
Pe: ar:e Eval t : M .x: :e v: PZ!- )
Indivith a1 S aa: xt :e A ( v: E :— )
: id a1 S:a-: -: “_xt_:e (F::
CaL . ::a:j : Ver .::a:nS.- :y
(Tc: v:: Pz!—l)
Calib:a:j : Ve: .ca:j : a:y
(Fc v:: P s:—2
5e-. en :e (F::— v::: PEST.
F2c:is...2. Ca:::j::e (Fo: X ES )
C -: Ca - (F :
: i;a:. . S - a:y f:: £ :.. :
A :e: (F:— X PEST-
Pes:.:ide —— ! .. -a:: f::
- : (To:r X P: )
C:::: :L— a a:a s’:s:e
A :: : of re:e j t. as a : ::::p .n
ea areas C: ?ea e . ::E
d. Ra C a:a
E. .ani Data ‘ ____
N .x S .ke/”a::.>: E:i. .a ;_:a:: a:a ____ ____
:c- —2
EXANPLE 12/ 9 G
-------
s:c . 5 s G NOS. TO FCLLOW
PACE NOs
FROM TO
G. Pe t jdes (Ccnt.)
e. Raw GPC Da
f. Raw Florisil Data
___ ‘ -‘ft
— —
7. Hi3c l1a ec,u Oats
Original preparation and a.ia .ysis fO S C cC ies c
p:e arazion and analysis lcg cck pages
Interia l aazn 1 and sa le e ctra t t ans er c iair1-
c —c. t dy rec r s
Sc: 9nL g rec rds
All ins: en: o :: :, s:r c arE fr :-
!c:eer.ing ac:i i : .es (cescr e C L.s .}
8. E A Sbi a/Receiv.. a cc ents
A .l! (Nc. Cf S erE
C ain-cf-C.s: : y Rec::d
San c .e Ta s
Sa.-.ice Lcg-:n $ -e & c:
e r E
(desc: e
9. tern L Lab Sa i ra sfe Re an TC :C
5 et ! (: e C: ....EZ!
___ IJ
1C. O 4 . e? Re ds (c s:i e ::
_•e —_ —_3 C
e -k
y. 4 k.i 4 7V’M
r
4e - 5p eir Z
2’.2 ‘ (h1
2& ’
——-V •“ -
: ..:...
c C2..
c z NC.
lot!
ORGANICS COMPLETE SG FILE (CS F) INVENORY vjde Audit Fhotocopy
5 ZET (Coat.)
SAS NO. __________
cI zCX
EPA
g30
( J 4
4.
as3
/ J
4.
.4-
EXAMPLE- 12/96
-------
Evidence Audit Photocoprf
DG ? .Z (C3P) (W1TORY S i (Cent.)
CASE O. / fl SDG NO. 5 fr3 9 SCG NOS. TO FOL.CW __________
___________ s s NO. _________
I.:. c eflt
C Ler d by: c ?. . tt” Q 1 s-• -9
cc:p .ab) (sigua .tr ) (P tad NaQ/ i ie) (Data)
Ve L d by: i L 1 yie. / f S 4 — Li ç . c .
(signa t r.) (? ifltad Naa/T t e) (Data)
A dit d by: ______________ D f UxLda3 r -2O•
(EPA) (Sig at3 e) ( P:i ted e/TLt!a ) (Data)
fl’i.H
EXAMPLE-12/96
ZCRY !C-2— CL C .
-------
Site Nagoc L-ø’
Site Location mp
Assigned Site LaflnidelLongtnide ‘ g U..) 4.0 23tJ
CERCLA SiterSpill Identifier Mci. 01 P .14 t ( a (Include Operable (hut)
Phase: ERA SA/S( pro-RI phasc 1. ctz,l FS RD RA post-RA
(circle one) Other
Draft DQO Summary urrn L 1 ,96
EPA-NE - DQO SUMMARY FORM Page I of____
A separate Fotm should be cornpteied far each cvczu. Refer to Atuchnienc A for insmlctions on completing this form. Attachment B for a complete list
- c parameter codes and Attachment C for an example of a completed form.
EPA Program: TSCA RCRA OW NP ES CAA
Other
Projcctcd Daceis) of Sampling 3- !
EPA Sicc Manager j (eJr C( ’
EPA Case Team Members Q & -¼ i v Cje .Ll _
vr eir & i - eS
2. QAPJPT ,deand Revulon Date Su-’ cta c)r tcs r Lac ,U ..
Approved by. )4 J r, ) fp L, g Date of Approval: d -1- 1 -
Title of Approving Official: LDu M M’f Organtzaaon:
1f other than EPA. record daic approval authority was delegated:
EPA Oversight Project (circle one) Y ‘4 Type of EPA Oversight (circle one) PRP or FF 0ther JP
Conilmiatocy Analysts for Field Screening Y If EPA Oversight or Concirniacory: % splits______________________
Arc comoarabiiirv criteria documcntcd? Y &?c
3. a. Matrix Cod& I O 1
b. Paraceerer Cod& CLMO .2 .)’i OLI’.LO!.2Sl
C. Preservation Code’ I 5
d. Analvucal Services Mechanism kLP (2Mk 1_P— 4J
C. No. of Sarriole Locations .5 —
Field QC:
f.
g.
Ii.
I
j.
¼.
I.
Field Duolicate Pairs
‘
/ -
Eoutnmetn Blanks
VOA Trio Blanks
)
•
Cooler Temoerarure Blanks
Boa eBlar,Jce Lo - 3
/
& dJ
‘
: tieI
t o
Other_______________
PES sent to Laboratory
‘
‘
Laborotory QC:
m. Reagent Blank 1 1
C l . Duouicace
0. Maoux5oike / /
p. Mama Soike Dunuicare I’
q. Other____________________ J
4. Site tnaruiaoon
S eDimeris ions 5 co f6. X S ’O 4 .
List all potentially cononuruced matrices Soif.. i._’Q -f
Range of DeDth to Groundwater I I —, / 4”d
Sod Types: Suriace Subsurface Other 4 1 U
Sediment Types: Scream Pond Estuary Wetland O ther.__________________ E.cpec ed StillScdiment Moisture Content High
When multiple matrices will be sampled during a sampting event. comolete Sccnons 5.10 for each mamx. Matrix Cod& SC
‘Data (Ise (circle all that aoply Site lnveaugaciowAsscssmeot PRP Determination Removal Actions
Nature and Etrenc of C.,ncanunaoon Human andJor irical RISK Remedianon Altemanves
Engineering Design Remedial Action
Past-Remedni Action (quarterly nortttocing) Other S utu . .t . I
L’
EXANPLE-12/96
-------
DQOs: V Su-) T & I / ,r e#ei,e ! 1 2- d cfr
g,J$ 5c4 .) . 4 d’ 14 ’i,k. I 2 _ 1 (4-bC .4, l 7t
itc ‘L ôi - e 4 Li) t 1 # ‘i ln c?& ’w .. .. r,w; Co *.( r,
Comokie_Table_if_acouicabk
cocs Action Levels
Analytical Method.Quanniac ion Limits I
io y//e.-
I I
I I
I I
J
I
I)I, -r&d1Ior 21
yIkf
I ’
3oO. ’i/ .
I_____________________
(circle ccchruque) Bailer Low flow pump (Region I method; Yes No) Peru loc Pump
Positive Disolac rnent Pump Faucet or Spigot Other ________________________
Dredge Trowel Other ______________
Proc durcs (SOP name. No. Rev. I. and dateLSpLit ( pp. 3: . ) Qe , . 31’1
Sample Locations m ;c; o’eJ P v ’ Up ra.4eA (5) t4r ’4 6 u Lios’fr i ra . i
Composite ‘ ‘ r
iamoled (Yes) No
(circle) OR) pH Specific Conductance Dissolved O Tutbidity I
Otheti______________________________________________________________
Methods and Pammeters I
title/SOP r a e
Method/SOP
Identification number
Revision Date
Taiget Parameters
(VOA. SV. PestJPCB Metals. etc
Criteria (circle one) 1. Rczionl. EP .-NE Data Validation Functional Ouidelines for Evaluamie nvironmenral Analvses. Ifl
orIV
2. Other Approved V ation Criteria:___________________________________________
(circle one) I ( ) Partial Tier Ifi;
Performing Data Validation 7T3
J.fokJct d G . vrôs,nie..d’ - 0 Conoact Number______________________________
(e.g. START. RACS. etc.) AQ.C.$ Work Assignment No. O -
Date of DQO Summary Form Completion , )./ . 7 —
Matrix Codes:. Refer to Attachment B, Part I
Parameter Cones- - Refer to Attachment B, Part II
Preservation Codes 3
I HCI to pH 2 7. lC Cr O.
2. HNO , 8. Freeze
3. NaHSO 4 9 Room Temperature (avoid eccessive heat)
4 H 5O 10 Other (Specify)
S. Cool 4C (± 2 ) N. Not preserved
6 NaOH
* . To supplement Matrix Codes and/or Parameter Codes contact the QA Unit
Draft DQO Surnmar’ Form 11/96
-------
ATFACIiMENT A
Guidance for Completion of DQO Summary Form
DISTRIBUTION:
1) Copies of completed DQO Summary Forms should be included in the QAPJP/SAP.
2) A. Copies of completed DQO Summary Forms for all CL? RAS work requested by EPA Site
Managers. EPA contractors, including RACS, ROC, and START, and other Federal Agencies
under Interagency Agreements. i.e., ACQE, and States under Cooperative Agreements should be
sent with the quarterly sample projections to the Region I RSCC. Completed DQO Summary
Forms for CLP RAS work be received by the RSCC prior to the sampling event.
B. Copies of completed DQO Summary Forms for non-CL? DAS work performed for EPA Site
Managers and EPA contractors be received by the Region I RSCC prior to the sampling
event.
C. DQO Summary Forms for non-CL? work performed under Interagency Agreements, Cooperative
Agreements, and Grants be completed prior to the sampling event, submitted to the
Authorizing Organization’, as delegated by EPA, and included in the size documents.
3) Copies of completed DQO Sumrriarj Forms also must be included in the Data Validation Report or Tier
I Validation Cover Letter (refer to Part I of the Daca Validation Manual’ in the Region I. EPA-NE Data
Yalidation Functional Guidelines for Evaluatirie Environmental Analyses) , December 1996, or most recent
revision.
INSTRUCTIONS:
Note: A separate Form should be completed for each samoling event. For sampling events involving multiple
environmental matrices, complete Sections 5-10 for each matrix and ensure that the two-letter matrix code
is identified in Section 5. Enter the page number and total number of pages in the top right hand corner
ott the Form.
Section 1:
• Circle the aporopriate EPA Program(s) involved in multi-media, mulri-pro rammacic sampling
events including, TSCA, CERCLA (i.e. Superfund), RCRA, DW (Drinking Water), NPDES,
CAA (Clean Air), or fill in the blank for ‘Other: -.
• List projected date(s) of sampling. The sampling dates should be inclusive of all macrices that will
be sampled during this sampling event.
• Record the EPA Site Manager’s name.
• List the names of the other EPA Case Team Members.
• Enter the site name. Use the NPL site name. If an NPL site name does not exist, then use the
site name assi2ned under CERCLIS.
• Record the name of the city/town and State where the site is located in the ‘Site Location’ field.
• Record the Assirned Site Laticude!Longitude ’. Those numbers should be identical to those
contained in CERCLIS database. Contact the EPA Size Manager to obtain correct
Latin.de!Longicude.
• Record the CERCLA sice!spill identifier number, including the operable unit number. Contact
the EPA Site Manager to obtain the correct identifier numbers.
• Circle the appropriate phase of Supert\ind site work (ERA: Environmental Risk Assessment,
SA/SI: Site AssessmemlSite Investi2ation. RI: Remedial investigation, FS. Feasibility Study, RD:
Remedial Desien, RA: Remedial Assessment. post-RA: post-Remedial Assessment, i.e., quarterly
monitoring). For non-Superfund site work, identify sampling event phase in the ‘Other’ field.
Att. A. Draft DQO Summary Form 11/96
EX NPLE-12/96
-------
Section 2:
• Record the complete title of the final QAPjP and revision date.
• Enter name of the Approving Official.
• Record date that the QAPJP was approved.
• Enter title of the Approving Official.
• Enter name of organization that has approval authority. This will be EPA, unless approval
authority has been delegated by EPA to a State or other Federal Agency.
• If another organization has been delegated approval authority, then enter the date that EPA
delegated approval authority (date of Quality Assurance Management Plan approval).
• Identify whether the project sampling event is an EPA oversight project, circle Yes or No.
• Indicate type of oversight by circling either Potentially Responsible Party (PRP) or Federal
Facility (FF), or complete the blank for Other:____________
• Identify whether confirmatory sampling and analysis is being performed to verify field screening
results, circle Yes or No.
• If EPA oversight or confirmatory analysis will be performed, record the percentage of split
samples to be collected and analyzed.
• If EPA oversight or confirmatory analysis will be performed, identify whether comparability
criteria are documented in the approved QAPjP or SAP, circle Yes or No.
Section 3:
a) List the two letter code for each matrix for samples that will be collected. Refer to Appendix B
for a correct list of matrix codes. If a matrix does not have a corresponding code, then attach a
description of the matrix to the DQO Sumrmiry Form.
Note: The matrix codes correspond to the matrix identifiers contained in the New
England Sample Tracking System (NESTS) database. The current list of matrix
codes are not intended to include all types of environmental matrices. However,
they do represent groupings of similar-type matrices that potentially contain similar
analytic interferences. For example, the matrix code GW (ground water) includes
water from monitoring wells, supply wells, and public wells.
b) For each matrix, identify the analytical parameters for samples that will be collected by recording
the appropriate parame :er code. Refer to Appendix B for a current list of parameter codes. If
an analytical parameter does not have a corresponding code, then the method tide and/or SOP
name, method and/or SOP identification number, and method and/or SOP revision date should be
included and recorded in Section 9 of this Form.
Note: The parameter codes correspond to the analytical method parameters utilized
in NESTS database. Appendix B includes a comprehensive list of analytical methods
that have been used historically for Region I site work.
c) For each matrix and parameter, identify the preservation technique that will be used by recording
the anpropriate preservation code. Refer to the reverse side of this Form for a list of preservation
codes.
d) Record the analytical service(s) mechanism that will be used for each matrix and parameter:
CLP-RAS (CLP-Routine Analytical Service) This service may be utilized by EPA site
managers, EPA contractors including. RACS, ROC, and START contracts. It may also
be utilized under Interagency anreements, i.e., by the ACOE, and under Cooperative
Agreements with the States.
RACS.DAS (Remedial Alternative Contracting Strategy-Delivery of Analytical Services)
- ROC-DAS (Regional Oversight Coctract-DAS)
- START-DAS (Superfuxid Technical Assessment and Remediation Contract-DAS)
- EPA-NERL (EPA-New England Regional Laboratory)
2 Ati. A - Draft DQO Summary Form 11/96
EXA ’fPLE- 12/96
-------
- Regional EPA-NE analytical contract
- State-Non-CLP
• Other Federal Agency Non-CLP
- If another analytical mechanism will be used, describe in detail on a separate page and
attach to the Form.
e) Record the number of discrete locations that will be sampled for each parameter. The “No. of
Sample Locations” count should include the site and background locations sampled.
• Record the number of each type of field QC sample that will be collected and sent to the
laboratory for analysis for each matrix and parameter.
0 Record the number of Field duplicate sample pairs (which will equal ‘1” for each pair of field
duplicates) that will be collected.
g) Enter the number of equipment/rinsate blanks.
h) Enter the number of VOA Trip blanks.
I) Enter the number of Cooler Temperature blanks that will be used.
j) Enter the number of Bottle Blanks that will be analyzed.
k) Describe any other field QC samples and the total number that were collected and that will be sent
to the laboratory.
1) Eater the number of PESs that will be sent to the laboratory in accordance with EPA Rezion
Performance Evaluation Proeram Guidance , July 1996.
Note: The total of “e-l” equals the total number of samples sent to a laboratory for each
matrix and parameter.
• Record the number of each type of laboratory QC sample that will be analyzed with the samples
received.
in) Enter the minimum numbcr of reagent blanks that will be analyzed.
a) Enter the number of laboratory Duplicates that will be analyzed.
0) Enter the number of matrix spikes that will be analyzed.
p) Enter the number of matrix spike duplicates that will be analyzed.
c i) Describe any other laboratory QC samples and the total number that will be analyzed.
Section 4:
• Enter the aoproximate site dimensions with units.
• List all potentially contaminated matrices, rezardless of whether or not they will be sampled
during this sampling event.
• For well sampling, complete “Range of Depth to Groundwater’ to ensure proper pump is utilized.
• For soil sampling, circle Surface or Subsurface or complete Other:_____________
• For sediment sampling. circle Stream. Pond, Estuary, Wetland, or complete Other:____________
• For soil/sediment sampling, circle etpected moisture content: High or Low. Note: Analytical
methods used for high moisture content samples should ensure that DQO.specifled dry
weight quantitation limits are achieved.
Act. A - Draft DQO Summary Form 11/96
EXANPLE-12/96
-------
Section 5:
When multiple matrices will be sampled during a sampling event, complete Sections 5-10 (or each matrix
and enter the Matrix Code.
• Identify the two-letter matrix code for which the information is provided in sections 5-10.
• Circle the potential uses for sample data such as, site investigation/assessmenc, PRP determination,
removal actions, nature and extent of contamination, human arid/or ecological risk assessment,
rernediation alternatives, engineering design. remedial action, post-remedial action, i.e., quarterly
monitoring. A space is available for other potential uses of data.
Section 6;
• Briefly summarize the project DQOs. This section should describe the specific objectives of the
sampling evenc,i.e., to identify health risks to children, ages 1-6, residing on the the who might
be exposed to surface soils located in the area, or to characterize the extent of groundwater
contamination. Identify the purpose of sampling, the decisions that will be made using the data,
action level informaticn, and any related information needed to identify that appropriate analytical
and field sampling methods were chosen. Complete the table with the following information:
contaminants of concern (COC), COC action levels and analytical method quantitation limits for
each COC. Note: Since this information will be used by data validators to identify potential
data usability issues for the user, it is imperative that it is clear arid concise.
Section 7:
• Circle applicable sampling technique(s) used and/or complete “Other to describe an innovative
sampling technique or one that is not listed.
• Identify the SOPs that will be utilized for sample collection. Include SOP name, identification
number and revision number andlor date.
• Record the discrete Background sample station location number(s) that will be sampled.
• Circle if samples will be grab or composite.
• To indicate potential I-Iot spots on site, circle Yes or No.
Secm:on 8:
• Identify the field data that will be collected including, ORP, pH, specific conductance, dissolved
O , tem erature, and turbidity. A space is available to indicate other field testing that will be
performed.
Section 9:
• If an analytical method does not have a Parameter code (required information in Section 3), then
the method title and/or SOP name, method and/or SOP identification number, and method and/or
SOP revision date should be included. Attach a separate page if additional space is needed.
• Record the specific parameters required for analysis.
4 Au. A - Draft DQO Summary Form 11/96
EXAMPLE - 12/96
-------
Section 10: In accordance with Region I QA policy, all data must be validated in accordance with the
most recent revision or Part I the ‘Data Validation Manual: The Data Quality System” of
the Retion I, EPA-NE Data Validation Functional Guidelines of Evaluacinz Environmental
Analyses .
• Circle the data validation criteria required by the QAPJP and/or SAP. In most cases, the QAPJP
andior SAP should cite the itiost recent revision of the Re2iOn I, EPA-NE Data Validation
Functional Guidelines of Evaluntin Environmental Analyses and identify the applicable Functional
Guideline criteria procedures that will be used to validate the data: Parr 1I-Volati le/Semivolatile
Data Validation Functional Guidelines, Part lII-Pesticide!PCB Data Validation Functional
Guidelines, and Part LV-lnorganic Data Validation Functional Guidelines.
If modified criteria or alternate data validation criteria wilt be utilized, the modifled or alternate
criteria must be documented in an approved QAPJP and/or SAP as stipulated in Parr 1, the Dara
Validation Manual: The Data Quality Sysiem, December 1996 revision of the Reeiort I. EPA-N E
Data Validation Functional Guidelines of Eva1uatin Environmental Analyses , December 1996
re’/isioa.
• Circle the Region I Validation Tier that will be used.
• If a partial Tier Ill data validation is required, then the subset receiving a partial Tier Ill should
be specified (e.g., benzene, VGA, etc).
• Identify the company performing the data validation. Circle either Pnnie or Subcontractor.
Section 11:
• Record the field sampling contractor company/organization name
• Contract number
• Name of contract
• Work assignment number
• Name and title of person completing Form
• Completion date of the DQO Summary Form
ALL A - Draft DQO Suniznarv Form 11/96
EXA LE-12/96
-------
ATTACHMENT B - PART I
Matrix Codes’
Aqueous:
DW - Drinking Water
GW - Ground Water
LE - Leachate (includes porewater)
SW - Surface Water
WW - Waste Water (includes scrubber blowdown)
Solid:
SE - Sediment (includes tidal sediments)
SO - Soil
Biota:
BD - Bird Tissue
CF - Crawfish Tissue
Fl - Fish (includes whole fish)
MU - Mussel (includes clam, quahog, and oyster tissue)
OF - Offal
PL - Plant
FF - Fish Fillet
Wastes:
AS - Ash (includes incinerator ash and boiler aggregate)
DU - Dust (includes concrete dust and fines)
01 - Oil (includes waste oil)
SL- Sludge
WD - Wood (includes chips, cuttings, and drillings)
WT - Waste (includes both solids and liquids)
ST - Still Bottoms
Miscellaneous:
AR - Air Samples
DN - DNAPLS
LN - LNAPLs
WI - Wipe Samples
PC- Paint Chips
CT - Concrete
EXANPLE-12/96 Att. B, Part I - Draft DQO Surnxnaiy Form 11/96
-------
AiI’AC1m1 . - .. - PART ii
PARAMETER CODES
PARAMETER CODJ3/M 1 1101)
IDENTIFICATIOt4 NUMOER
MEl HOD lii LE
IUWERENCE
PARAMIfl ER NAME
OLM O3.IP
USEPA CLI’ Statement of Work rot Orgaiiics Analysis - OLMUJ.I
I
Full organics (VOA. SV. P/I’) CLI’ SOW Oigauiic Aiiaiycic
OLMO). I P
USEPA CLP Statement or Work for Organics Analysis - OLMO). I
1
PcsocidciArock’rs Analysis CLI’ SOW Organic Analysis
01 )11)3. IS
USEPA CLI’ Stair,itcnt or Work for Orgaiiics Analysis - OLMO3. I
I
Seiiiivolaiik Orga.ocs Analysis CLI’ SOW Olganic Analysis
OLMO3 IV
USEPA (‘I P Stiiternent of Vork fur Orgaiuics Aiialyck - OLM O3.I
I
Volatile Ouganics Aiialycic CLI ’ SOW Oiganic Analysk
1003
ilalogeitated ilydrucariwius
NIOSII 1003 Volatile on Charcoal ‘IuI ’cs
12190 -1)1
USEPA CLI’ Siate,iient of Work for Attalysis of Pulyclilorcoated Dtheuizo-p.Dioxitis
(PCI)D) nuitl Pulycluluurnnitcd Dulrciu,uulurauis (I’CJ)F). J)FLM I .(). Rev. 12/90
3
12/90 SO V UiuxiiilFuiaui Analysis
130 I
Ilardoess. Total (mgIL) as CaCO,. Coloui,netric. Automated EIYfA
4
llanluucss-Colu ,ui,.uctuic. Auucoinalcd l!iYlA
130.2
llarulncsc. Total (mg/i) as CaCO,. Tilrimeuric. CL) l’A
4
llarduiccSlulriiIiClriC. CDI A
13112007
Toxicity Characteristic Leaching Procedure acid Deterininaliun oF Metals suid Trace
Elements in Water arid Wastes by Inductively Coupled Plasutia-Atomic Euiuission
Spectroniciry
5 & 7
1CLP Iiauuactuuui-Melals Auu%l 515
131 13. IF
Tucucity Charac ccisiic Leaching Piocedure and USEPA CLI’ Slatemeustuf Voik fur
Organica Analysis - OLMOJ. 1
5 & I
ICI. .1’ Eaisactioii-I utl Ouganics VuL tite. Sciouvulattle.
Pestucide/PCB Analysis
13 1 13.lP
Toxicity Characteristic Leaching Procedure and USEPA CLI’ Statement or Work for
Orgaruics Analysis OLMIJJ 1
5 & I
1CLP I3xtractiouu-Pcslicudell ’C 13 Aui ly i
13 1l3.IS
loxicity Characteristic Leaching Procedure and USEPA CLI’ Statement of Vouk for
Otgauiics Analysis- ui.Muii
5 & I
ICLP Extractiuut-SeliiivoIMilC Analysis
131 13.IV
Toxicity Characteristic Leactuiuug Procedurc and USEI’A CLI’ Statement or Work fur
Organics Analysis - OLMU3.1
5 & I
TCLI’ Cxtiaciiouu-Vuhalile Analysis
13118000
Toxicity Cliaraceristic Leaching Procedure and Deicriniuialion oF Organic Arualyles by Gas
Chromatography
5
1CLP Extractinum-Full Organics
.
13118080
Toxicity Characteristic Leaching Procedure and Deternuiiiuation of Organoctiforirue I’esticijes
amid PCOs by Gas Chronialography
5
1CLI’ Extracuioii4’csticide /PCD Analysis
13118240
Toxicity Cliaracterisik Leachiimrg Procedure nmmd Dcternmsuuauiuiu of Volammle Orgaimucs by Gas
Chmmanngra ihiy1Mass Specironicity (GCIMS)
5
1CLI’ Esiracrion-Vulatmte Amiatyxis
13118270
Toxicity Characteristic Leaclmiuig Procedure and Deterrniuiattu,i of Senuivolatmle Organics by
Gas C lmrunuatograpliy/Maas Specrroinetry (GC/MS)- Capillary Cofunuic iccluruique
5
TCLP Extraction-Scmmvulatilc Analysis
I Att. I), Part II - Dralt DQO Suiuutimiy Form 11196
-------
AF1ACIi1 iENT B — I’AIt’I ’ 11
I’ARAMEI’ER CODES
AlkaIjirily 1 irripuctric (l’s I 4.5)
4
1 Uriiiielric Alkalintly
PARAMl TER CODEIMflIIIOD
IDENTIrICATI0F4 NUMOIR
MIfl IIOD1IILE 1
I
RLTL!RCNCE
VARAMr ICI ( I ’IAME I
l60.I
Recidue. Filterable. Gravinreiric. Dried at 180 C
4
lulal Dicculverl Sulidc (I E)S)
I (‘(1.2
((ecidue, r4. ,n lilCcraIiIc_ (raviiiic(ric, DI ted at 1(13.1(15 C
4
‘1 tilal Sticiicuitlcd Stilitic (I SS)
160.3
Residue, Tutal, Giavitnetric, Dried at 103-105 C
4
lural Solids
1613
‘I etra- through Ocla- Cliluriutated Dioauic and rurauic by lsuIu ic I)utulnu,c I IRGCII II(F 1S
( p
t)iuaiuilFuraii I ugh Rccp,kului,n A II.,lycus
200 7
l)eteriuinatii,n al Mctals and Trace Elements in Water and Wastes by Inductively Cuuiulcd
l’Iaciiia — Acuinic Ettii.cscuit S ectitnttetiy (Rev 4 ‘1, 1994)
7
ICP Melals Aitalysis-Fuhl List
200.7XX
Determination oF Metals atid Trace Ele,iicuitc in Water and Wastes by Inductively Coupled
l’Ias,,t a — Atomic Cniission SVccirounctxy (ltcv.4 4. 1994)
7
ICP Metals Annlycuc.XX Specuhic Metals
20 0.9 1C [ )
Deteruu,i,uation iji Trace Eleuiieiitt by Stahithized Teiiiperatu e Caaphiire rurriace Atomic
AIsoi 1ion Spectrunietty (Rev. 2 2, 1994)
7
Graphite Furiiace-Cathuuiiugui
20 0.9/513
l)ctennitiaiittn of Tiace Eletiieittc by Stabilized 1 elliperaluse Graphite Furnace Atomic
Abciimpiioii Spectroulietry
7
Graphite Furiiace-Antiiumtv
20 0.9AS
1)ctcrii iinatiuit of 1 race Elcnicii ls by Stabilized Tcuiipcraturc Graphuilc Fumiiacc Atominc
Alicuilil lull S iectrwiicrsy
7
Crapliitc I urnacc-Arscnuc
204 .2 /SB
Antimony Aft, Furnace
4
Gia 1 ituitc Fumuiacc—Aniuuiiiiuiy
206,2
Arsenic Aft. Furnace
4
GrapPuite FriruIaCe-Ar eirjc
2 13.2/CD
Cadniiutn Aft. Furiiact
4
(iraplnle Furutace-Cadirmini
2320.13
Alkalinity. 1 utration Method
8
Titration Memluud.Alkahuuitty
234013
hardness by Calculation
8
I lardness-Ca lculatiuu
2340C
hlardiic . E1)TA Titri,itctric Method
8
flar ,jnccs ruzriiitctric, EL)IA
254DB
Tutal Solids Dried at 103- lOS C
8
Total Solids
2540C
Total Dissolved Solkis Dried m i o •c
8
C %
Total l)i sulvcd Solids (11)S)
2540D
l ’ .tal Suspended Solids Dried at 103-105 •C
8
c
Total Suspended Solids (TSS)
30 0. OC I
Ion Chromatography
Deier,ii ’niatiuui Iiwrganic Anions in AQ by IC i- I
301) OF
Ion Chirontatugraphty
Ion Clirotii. .Fluoritle
300 0N03
Jon Chromatography
Ititi Clironm.-Nitrnre 121
2
Au. B, Part II — Draft DQO SumInaly 1:01111 u nyu
-------
,VITAC IIMI — I’Atti, II
PARAMETER CODES
PARAMETER CODE/MElt IOU
IDENTIFICA1 ION NUMBER
[ MEHIOI) f1 I LE
I ItWE I 1ENCE
MRAMII I It NAF IL
310 2
Alka Iiiiity. CoIc,,i,iieiric. Autoiiiaied t 4elIiyJ Ora
4
Color iiiiciric—A tkaliui ny
311 39/AS
?nlclals by Electrothermal Atomic Absorption Speciromnictry
8
Ch:Il)llltc ruritace-Arseinic
3113 13/CD
t leialc by Elecirouliermimal Anommic Al urjnumuii SlPecifomncIry
8
Ut n 5 mhite Fiti mace—Cadmium
31 139/SB
l 1elaIs by Electnntl,erntal /ttonimc Absorplinmu Speclrunieury
8
Graphite ruruiacc-Aniiui mny
325.2
Chloride. Culorimetric. Autoniated Ferricyanide AA II
4
Co lorime tric.Cl mlorude
325.3
Chloride. Tiirimmmeiric. Mercuric Nitrate
4
Tuirunuiciric-Cliloride
335 2
Cyanide. iwaI. Titriimictric; Spectrophumntumnuicuric
4
I itt iuneuric—Tumtal Cyanide
340.2
Fluoride. Potentimnetric. Ion Selective Electrode
4
Electrode-Fluoride
350. I
Nitrogen. Aniiiionia Coloriutietric. Autoniaicd Phmemiate
4
Cuhipiim i etr ic—Anitnonia
350.2
Nitrogen. Aiminiuimiua Coloriutiet, ic Tilt ililetric; Poreumtinnietric—Disrul latiomi I’ruicdii re
4
Colormniclm ic. iltriuncti ic. l lciti mile Did —A mmmii mumia
3513.3
Nitrogen. Amiii numia l’otemitiinnctric. limit Selective Electrode
4
Elcctrode—A u uiii m u mnia
351.2
Nitrogen. Kjeldalil. Tutal Culoriinetric, Senim-Automated Block l)mgesier. AA II
4
Coloriuuiclric Semi-Auto-Total Kjclilalml N (FKN)
351.3
Nitrogen. Kjeldalul. Total. Coloriinetric; Titrimnerrie: Potcmiiiotimetrmc
4
Colwinmctric. Titrimnetric, Electrode-i otal Kjeldalil N (1 KN)
352.1
Nitrogen. Nitrate. Colorimnetric, Bruciime
4
Cok;rimnctric-Nitra te
353.1
Nitrogen. Nitrate-Nitrite, Coloririmeiric. Aumonmated. llydrazimme Reduction
4
Culorimmietric. Auto.. llydr-Red .Nitrate
353 2
Nitrogen. Nitrate.Nmtrite Coloritmmetric, Auiomated Cadniiuni Reduction
4
Cotutiummelric, Auto.. Cd-Red.-Nitrate
353.3
Nitrogen. Nitrate-Nitrite. Spectroplmototmmeiric, Cadimmiumim Reduction
4
Spectro.. Cd-Red-Nitrate
3541
Nitrogen. Nitrite. Spectroplmutuinetric
4
Spectroplwtonmctm ic-Nitrite
365.1
l’lwsphorus, All rormmms. Coloritmietric. Automated, Ascorbic Acid
4
Colorittictric. Auto, Ascorbic Acid-l’hmmmsl.lmuius
3G5.2
Pimosplmonis. All rortims. Colorimeiric, Ascorbic Acid. Single Reagettt
4
Coluritmielric. Accoilmic Acid, I Rcag-Plwsplwnis C
365.3
Plwsp!morus. All Fonmis. Colorimmietric, Ascorbic Acid. Two Reagemit
4
Culoriumielric. Accorbmc Acid. 2 Reag-l’ltucplmurus
365.4
Pliodphiorus. Total. Cohoritmietric. Autoniated. Block Digestor AA II
4
Colurumnetric. Auto..Phosplioius r
370.1
Silica. Dissolved, Colorimmmetric
4
Colurimmucumic-Silica
375 I
Sulrate. Colorinietric. Autommiated. Clilura,iilatc
4
Colurimmictric. Autoinatcd.Sullate I
3 Att. 13, Part 11 - DtaIt DQO Swirittary Form 11/96
-------
A’II’ACIIMENT II — P/tRI’ Ii
PARAMETER CODES
PARAMETER CODFJMETI 1OL)
IDENTIFICA 1 JON NUMIJER
MEIIIOI) 1fILE
REFERENCE
PARAME I C R NAME
375.3
Suliate, G,avlti leidc
4
Crav tuetric-Sul latc
375.4
Sulrate, Totl,udii,ieiric
4
1 irti,iJiiuetric—Sultate
376 I
Sullide. lisimettk , Irnlme
4
1 iiriniciiic-Sulflde
376 1
Sulfide, Cotoriinctric, Mctliylciic DIuc
4
Coloritnelnc-Sull ide
41)3
Dicarbotiale
Dicarliotiate
405.1
IJioclietnical Oxygen Demand 1300 (5 day. 20C)
4
5 D y 20C .000
410 I
Clirniical Oxygen Den.aiid, irirnetric, Mid-Level
4
litriniclric-COD Mid. Level
410.2
Chemical Oxygen Deniand, Tirrititeiric, Low Level
4
1 iiriinelric-COI) Low Level
410.3
Chemical Oxygen Dcinaiid, Titriunciric, Iligh Lcvcl fur Saline \Vatcr
4
Tiiriuiiclric-C0t) 11 1gb Level
4104
Clietimical Oxygen Dcinatmd, Cuhurintetric, Automated; Manual
4
SpcclroIdtnklmutcIrIc.COl) v1aiiual/Aiulup
41 tU
Delerntiuuation oF Auiioit by limit Cliruiiuauograpluy
8
Auiioni
413.1
Oil and Grease, Total Recoverable, Gravinietric, Separaloty Fwinel Extraction
4
Gravinmeiric-OtI & Grease
413.2
Di i and Grease, Total Recoverable, Specirophiotornetric, Infrared
4
Oil auid Grease (0 & 0) - IR Slice.
415.1
Organic Carbon. Total, Cosimbustimmn or Oxidation
4
Cnint,umtiuii or Oxidaituun-1OC
415.2
Orga,uic Camixin, Tuimal, L IV Proimiored, Pcrsullaie Oxidation
1OC-Low Level, UV Prunumutcd
418.1
Petroleum Ilydrocaibans. Total Recoverable, Speclruplmotnrnettic. Infrated
4
lR Spcc-TPI1. l’eltuleuna Ilydrocautiumic
4 18. ITPI 1
Petroleuuti l1 drocarbons. Total Recoverable, Speclrvpltotometric, Infrared
4
Total Petroleum Ilydrocarhiotic
4500-PIE
Phosplrnrus. Accorlimc Acid Method
8
Ascombic Actd-P1tncji1ton s
4500-P IF
Pliocp lionis. Atitotmiated Ascorbic Acid Reduction Method
8
Auto. Ascorbic Acid-Plnuspliorus
4500F1C
Fluoride, Ion-Selective Electrode Method
8
Electrode-fluoride
450 0N020
Nitrogen (Nitrite) Cohuriutieleic Method
8
Culoritimetric-Nicrite
450UN03E
Nitrogen (Nitrate) Cadmnimuuti Reduction Method
8
Caditmiumin Red. Mammual .Nitsiie
450(JNO3F
Nitrogen (Nitrate) Auti,iuiated Reduction Method
8
Camhiuuiuiis Red. Atitu.Nitratc
4500N03 1 1
Nitrogen (Nitrate) Autummuuatcd llydraziiie Rediuclini,
8
Autuumimated Ilydia7ine-Nilmate p
tt(I. B, PaiL II - Di aR DQO Suiitiuiary Fouiii ii u
-------
A ’1I’ACIJM r-,,- J - VAR’I ’ 11
PARAMETER CODES
PARAMETER CODE/METhOD
IDENTIFICATION NUMBER
ME1IIOD ‘IITLE
REIERENCE
PARAMEI’ER NAMfi
45005/0
Sulfide, Melliyleire Blue Method
8
Melliyleue Blue Sullide
45005/F
Sulfide, lodoiiieir,c Meihi,id
8
ludusiue tnc-Su lflu le
4500S04C
SuBate, Graviineiric Method with Ignition ut Residue
8
(Jiav.+Ig niiio i .SiiIIate
45005041)
Sulfate, Gravimctric Method with Dryiuq of Residue
8
Grav.+Diyiuig-SuIIa lc
450 0S 1/D
Silica. Mulybdosilicate Method
8
MOlytXJusilIC i lte-StliCa
504.1
1,2-Dibroineihane (E0 13). l.2-Dibroiiro-3-cliloropropane (DIJCP), and 1,2.3.
Tricliloroprupane (123 TCP) in Water by Microextraction and Gas Chromatography (flev.
1.1. 1995)
9
EDO. DBCP & 123 1CP. Mucroexlraclioli & UC
52 10/B
Biochemical Oxygen Demand (DOD), 5 Day 1101) Test
8
5 Day-DOD
5220/C
Chç nical Oxygen Detumand (COD). Closed Rellux, Tutrinietric Method
8
Titriiuetric-COD Mid Level
5220/D
Chemical O ygeui Demand (COD). Closed Reflux, Cnlorhneiric Method
8
Specimjhiutouuieiric-COl) Mauiuah/Aumo
524.2
Measurement of Purgeabic Orgautic Compounds iii Water by Capillary Coluiiiui Gas
Clirounalogiaphy/Macs Spcctruinetry (Rev. 4.0, 1992)
9
Meacurcuncitl of I’uugcablc Oiganic Couuipuundc in Watcr - Capillary
Culuittit by GC/MS
524.2+
Measurement of Purgeable Organic Compounds iii Waler by Capillary Columnii Gas
Chromatography/Mass Spectrotnetty (Rev. 4 0, 1992)
9
524 2 Plus Addiiiouial Coutipounds
525.2
Determination of Organic Conlpound5 in Drinkiiig Water by Liquid-Solid Extraction and
Capillary Column Gas Chromatography/Mass Speclromemry (Rev. 2.0. 1995)
9
1)eterntiiiatioui Of Organic Couiipmuuidc in DW by Liquid Solid
Extraction Capillary Column by GC/MS
5310/B
Total Organic Carbon (TOC) Cunibusliuii-t,ilrared Method
8
Coim mhiustiotu-huufr arcd-1OC
5310/C
Total Organic Carbon (IOC) Persullate-Ultraviolet Oxidation Method
8
Persuhlate-UV Oxidntioii-TOC
5310/0
Total Organic Carbon (TOC) Vet-Oxidatmon Method
8
\VetOxidaiio uiTOC
551.1
Detection oh Chlorination l)kiutfectiomm Byproducts and Cittorinated Solvents, and
hlalogenated PesticRles/hlerbicldes iii Drinking Water by Liquid/Liquid Extraction and Gas
Chromatography with ElectronCapture Detection
9
Bet. Cliloro. Disium Dyprods, Cliluw Sulv. by LL&GC
.
5520/B
Oil and Grease Parlition-Gravimnetric Method
8
H
(Jravimnetric-Oil & Grease
5520/C&F
Oil and Greace Partitton-1,mirared Method and hydrocarbons
8
IR Spec-TM I, Petroleum, hydrocarbon
GUI
Purgeable hlalocarbons frrap-GC/llall Delector.Ehecirolyuic Conductivity Detector)
10
Purgeable Ilalocarbons ‘l ’rap-GC/ELCD
602
Purgeable Arunmatics (Trap-CC/PlO)
ID
Purgeable Arounauics Trap-CC/PhD N
5 All. B, Part II - DraFt DQO Sunitimaty 1 orumi I 1/96
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A ’JTAC1JI’ 1IW41’ II - PARF II
PARAMETER CODES
PARAME1 ER CODE./Mfl 1100
IDENTIFICATION NUMIJER
ME1IIOD TIFLE
1ff I - EflI NCE
I’ARAML 1J R NAME
6 (18
Oiganociituricic Pesticides stid PC [ Is by (GC/ECDJ
10
Org i:uchIuriiie reci I’ciJ -CCfECI)
624
I’iirgea1ile (I raj’-CC /MS)
10
I’iirgcalilc I ciii-IJCIMS
625
D se/Ncuirak a d Acids ((JC/MS)
10 -
Jasc/Nt:iuiralc&A itIc l! ir, Cc/MS
80 15A
Nonliatogensied Volatile Organics by Gas Chromatography
5
Nuiilialoge.uned Volatile Org CC
SU8OA
Orgaiivclilorine Pcsiicldcs and PoIycli orinaied 3.jihciiyls by Gas Ciiroiiiatngra iliy (Rev. I.
l994
5
Orgaiiu !iIorinc I’est&I CIJ by GC/EC1)
8240D
Volatile Olganics by Gas CliroinatograpliylMass Specirumci,y (GC/MS) (Rev 2. 1994)
5
Vijtniile Orgsuic Conipuund5 by CC/MS
8270D
Seinivolatile Organic Compounds by Gas Chromatography/Mass Specironietry (GC/MSJ.
Capillary_Colunrn_Technique_(Rev._2._1994)
5
SeinivoI iiIe Organic CwiiJlou,kJs by CC/MS
290
rulyclulorinaurd Dibenzudiosiris (PCDD5) and rolyclilorinamed Dibeuizofurauis (PCDFs) by
Itigh-Resniution Gas Clironia lograluluy/IIigIi — Resoluitwi Mass S)Jectromnelry
(IIRCJCIIIRMS) (Rev .O. 1994)
5
PCDL)S & PCDI:S by IIRCCIMS
A5TM2974
Siauudard Test Method for Moisture, Ash siuti Organic Maiter of Peat a d Other Orgauiic
Matter
II
TCOC — 1 or Cuuiuliusli lule Oig Ctuusteuit
.
ASTMD42Z
Standard Test Method fur rarticle-Size Aimalysis oF Soils
Ii
Grain Size Analysis
ILMO4IJCN
USEPA CLP SOW rot tumorganics Analysis- ILMO4.0
12
Cyatukie Inorgaumic CL I ’ SOW
ILMU4OMT
USEPA CLI’ SOW rot loniganics Analysis - I1M04 0
12
Metals (no CN) Inorganic CLI’ SOW
ILM O4UTL
USEPA CLI ’ SOW For inurganics Analysis - ILMO4.0
12
Metals & Cyanide Inorganic CLI’ SOW
TO-I
Uelermiuiaiion of Volatile Organic Coutupounds in Ambient Air using Teuaa Adsorption and
GCIMS
13
VOC-AIR. Tenas Tubes
10- 14
Dctenniuratiois of Volatile Orgauuic Compounds ii, Anibiciut Air Using Sunuiura I’assivatcd
Canister_Sampling_and CC An Iysis
13
VOC-AIR, Sui.iuuua Canisters
10-2
Dc,errninatkm of Volatile Organic compounds iii Anibicuuc Au using Carbumu Molecular
Sieve Adsorption and CC/MS
13
VOC-AlIt. Ca. bun Molecular Sievc
NOTE: The otetliud number is Incorporated luilo the I’ama.ucter Code
REFERENCES:
1. USEPA CLI’ Statement ul Work for Organies Analysis, Multi-Media. Mulii-Coircentraiion , OLMO3.1. August 1994
2. NIOSI I Manual of Analytical Methods (Second. Part I). NIOSII MoiiiEor.uig Methods I
6 Ati. ii, Pait II — Draft DQO Sunuiiaty Ponii 11/96
-------
ATJ’ACIlMlisci u - PART It
PARAMETER CODES
3. IJSEPA CLP Statement of Work for Analysis of Polyclulorinated Dmbetmzo.p-bioxlns (I’CDD) artd Polyclilorinated Dubenzofuiatis (PCDP), UPLMUI.UFDFLMUI.I - Rev 12/9 1 ) and Rev. 9191.
4. Methods For C lmeuttical Analysis of \Vater anti Wastes. Erwlmommnreumtal Protection Agency. E1’A-600/4-79-020
5. Test Methods rot Evaluating Solid Wacte. Physmcal/Clmemnical Methods, SW-846. Third Editiuui, July 1992 amid Updalec
6. Method 1613’ Tetra- Through Octa ’ ChlorInated Dloxiuis and Furans (my Isotope Dilutions IIROC /IIRMS. EPA 821-11-94-005. October 1994. Rev 1%.
7. Metlumids for time Deterumminatioru ci Metals hi invrrnmmmnemmtal Saniplec. EPA IOOO!4-91!01U. June 1991, amt I Srrpplenmeimt I, hiI’A4 UmJIfl -94Il 11, May 1994
8. Standard Methods For the Examimination of Water and Wastewater, 19th Edition. 1995
9. Methods for the Determiumatiomu of Organic Compounds in Drinkitig Water. December 1988. EPA! 000/4-88(039 amtd Updates
It). Cudc or rederal Rcgulatiummui. 40 CUlt. Part 136, App A
II. American Society for Testing amid Materials
12. USEPA CLP Statement of Work For litorganics Analysis. Multi-niedma, Multm-concemmtntmnmm. ILMU4.0
13. EPA Compendium or Methods ror t lte Detersimitrattoim of Toxic Organmc Compounds itt Attibmemit Amr, EPA-600/4-84-041. May. 1987.
to
0 m
C l
r;1
7 AU. 13, [ ‘an II - Draft DQO Sutttmtmaty For m 11/96
-------
Attachment 0
“March 7, 1995 Memorandum to Heidi Horahan, ARCS DPO re: CLP-SOW
OLMO3. 1-New Contract Requirements.”
-------
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION I
60 WESTVIEW STREET, LEXINGTON, MA 02173
MEMORANDUM
DATE: March 7, 1995
SUBJ: CLP SOW Or o3.l - New Contract Requirements
PROM: Moira M. Latail1e
Deborah A. Szaro
CLP Technical Project Officers
TO: Heidi Horahan
ARCS Deputy Project Officer
The new CLP Statement of Work for Organic Analyses,
OLMO3.1, is currently being awarded to laboratories.
There are two issues associated with the new CLP SOW that
all field contractors should be made aware of.
First, there is new contract language (Exhibit A,
4.2.1.2.3) that requires the laboratory to monitor and
record the temperature of the sample shipping cooler using
a temperature blank. The SOW requires that tithe
temperature blank be clearly labeled: USEPA COOLER
TEMPERATtJRE INDICATOR”.
Therefore, all field contractors should immediately begin
to include a temperature blank with each sample shipment
cooler sent to a CLP laboratory. And each temperature
blank must be identified and clearly labelled as indicated
above. The validators should assess the impact of non—
compliant shipment temperatures on data quality and
document this in the Data Validation Memorandum.
Secondly, under the new contracts missed holding times are
no longer considered to be a charge assessed under
liquidated administrative damages. Therefore, missed
holding times will no longer be assessed as a defect under
CCS which previously resulted in an automatic reduced
payment to the laboratory. AOB has directed the regions
to assess the actual cost of this non-compliance to the
region on a case-by-case basis.
Therefore, all field contractors should immediately begin
to review all CLP CSFs to assess the impact of missed
holding times on data quality taking into account site—
specific data quality objectives. If the data quality is
adversely impacted by missed holding times, the validators
should submit a request for data rejection or reduced
payment in accordance with the CLP—TPO regional guidance.
-------
Please forward this.information to the field contractors
at your earliest convenience. If you have any questions,
we can be reached at (617) 860—4312.
-------
Attachment P
“The Regional Sample Control Center Guidance for the Contract Laboratory
Program (CLP) and Delivery of Analytical Services (DAS) Program for EPA-
New England”, July 1996
-------
The Regional Sample Control Center (RSCC) Guidance
for the Contract Laboratory Program (CLP) and
Delivery of Analytical Services (DAS) program for
EPA-New England
November 1996
RSCCGuid-O1
-------
Table of Contents
Introduction
A. Contract Laboratory Program (CLP) Background
B. Delivery of Analytical Services (DAS) Background
C. Overview of Contract Laboratory Program (CLP) Operations
D. Overview of Delivery of Analytical Services (DAS) Activities
11. Analytical Services Available
A. Organ.ic Routine Analytical Services (RAS)
B. Inorganic Routine Analytical Services (RAS)
C. Delivery of Analytical Services (DAS)
111. Regional Sample Control Center (RSCC)
A. Overview
B. Activities
1. Quarterly CLP Sampling Projections
2. Weekly Scheduling of RAS Analyses
3. Notification of DAS Events
4. Making Changes to the CLP Analytical Requests
5. Sample Documentation Paperwork
6. Receipt of CLP RAS Data & DAS Data Receipt Notification
7. Contract Compliance Screening (CCS) & Laboratory Response to CCS
8. Data Validation Memoranda
9. Notification of CLASS
10. Distribution of CLP Sampling Paperwork
11. Problem Resolution and Information Services
12. Reports Provided by the RSCC to the Lead Chemists
IV. Definitions/Acronyms
V. Attachments
Attachment I CLP SOW Exhibit C
Attachment II Quarterly Projections
Attachment III RAS Weekly Request Form and DAS Summary Form
Attachment IV Sampling Paperwork
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RSCCGuid-01
Page 1 of 17
Introduction
A. Contract Laboratory Program (CLP) Background
The Superfund Contract Laboratory Program (CL?) was established in 1980 in
response to the increased analytical needs created by the passage of the
Comprehensive Environmental Response, Compensation, and Liability Act
(CERCLA). It is a national program that consists of laboratories throughout the
country which support the Environmental Protection Agency’s (EPA) Superfund
analytical needs. It provides cost effective data of known quality to be used in
environmental decision making and in supporting Agency enforcement actions.
Prior to June 30, 1994 the CL? provided both Routine Analytical Services (RAS)
through inorganic and organic Statements of Work (SOWs) and Special Analytical
Services (SAS) through analytical subcontracts procured by the Sample Management
Office Contract. Presently, the CLP provides organic and inorganic analytical
services within the Routine Analytical Services program.
B. Delivery of Analytical Services (DAS) Background
As per the Superfund 90-Day Study, the Office of Emergency and Remedial Response
(OERR) established a Delivery of Analytical Services (DAS) Task Force in April of
1991 to develop a Superfund long-term strategy for the delivery of analytical services.
The final strategy decision for the delivery of special analytical services, which was
made by the Deputy Assistant Administrator for the Office of Solid Waste and
Emergency Response, was that special analytical services should be regionalized.
This decision was transmitted to the Regions in a memorandum dated 01/27/93 from
Henry Longest II, Director of the OERR. Thus, the ability to ship samples under the
CLP Special Analytical Services (SAS) program, which bad previously handled all the
samples which could not be processed with the RAS program, ended June 30, 1994.
A Region I EPA DAS Workgroup formed in March 1993 to determine the best
mechanism for obtaining special analytical services. The workgroup evaluated
vehicles for obtaining these analytical services.
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RSCCGuid-O1
Page 2 of 17
Given the high sample volumes, cost and the complexity of the analytical needs,
EPA-New England decided on a two-phased implementation plan to obtain future
Superfund special analytical services. EPA-New England’s short-term approach was
to direct the EPA field contractors to procure/obtain special analytical services for
those sites that they worked on, either by subcontracting the analytical services or
utilizing in-house corporate laboratory facilities. The long-term solution would be the
procurement of a Regional Environmental Analyses Procurement (REAP) for special
analytical services. EPA New-England will continue to use the national CLP RAS
services whenever the analytical SOWs meet the project data quality objectives
(DQOs).
C. Overview of the Contract Laboratory Program (CLP) Operations
The Contract Laboratory Program (CLP) is administered by a headquarters
Administrative Project Officer (APO) with Technical Project Officer PO) support in
the regions. The Technical Project Officer oversees the contract compliance of the
laboratories in their region which have contracts under the CLP and is the first line of
contact for the laboratory for resolution of all technical problems.
All CLP samples collected by EPA personnel, EPA contractors, States under
Cooperative Agreements and other Federal Agencies under Interagency Agreements
are tracked by the RSCC.
The Regional Sample Coordinator (RSC) places all Regional requests for CLP
analyses. The requests are submitted to DynCorp Information & Engineering
Technology, under the Contract Laboratory Analytical Services Support (CLASS)
contract.
Analytical requests are processed one week prior to the anticipated sampling date.
The specifics for obtaining CLP analyses are located in detail in the following
sections of this document. The status of the field samples from the date of collection,
submission to a laboratory, receipt of data and completion of data validation are
tracked by the New England Sample Tracking System (NESTS) database maintained
by the RSCC. Routinely, reports containing the tracking information are provided to
the Lead Chemists. These reports are provided at various intervals from weekly to
quarterly. See Section B, Activities, part 12 for a description of the reports.
Standardized sample identification paperwork, including sample labels, tags and
Traffic Reports, are required for all CLP sampling. Accurate completion of
standardized forms ensures that sample authenticity and sample custody are
maintained.
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RSCCGuid-O1
Page 3 of 17
D. Overview of Delivery of Analytical Services (DAS) Activities
Delivery of Analytical Services (DAS) activities refer to all EPA sampling activities
or EPA contracted sampling activities for Superfund not analyzed through the CLP.
DAS samples collected by EPA personnel and EPA contractors and submitted to
either the U.S. EPA NERL, contracted laboratories or corporate laboratories are
tracked by the RSCC. DAS samples collected under Interagency Agreements or
Cooperative Agreements by States are not tracked by the RSCC.
The DAS analytical specification must ensure that the project data quality objectives
(DQOs) for the sampling event are achieved. The organization procuring analytical
services for the EPA is responsible for ensuring that usable data are delivered. To
that end, the field contractor, State or other Federal Agency should review laboratory
quality assurance plans, SOPs and other documentation outlining laboratory policies
and procedures. In addition, technical systems audits, including on-site laboratory
audits should be performed to monitor compliance with contract specifications.
Performance Evaluation Samples (PESs) should also be analyzed by contracted
laboratories to monitor performance prior to and/or during field sample analysis. The
status of the field samples which includes the date of collection, submission to a
laboratory, receipt of data and completion of data validation are tracked with the
RSCC database. The field sampling contractor provides this information to the EPA
RSC with the chain-of-custody form, the DAS Summary Form and DAS Data Receipt
Notification form. Routinely, reports containing the tracking information are
provided to the field sampling contractors. These reports are provided at various
intervals from weekly to quarterly. See Section B, Activities, part 12 for a
description of the reports.
II. Analytical Services Available
The Contract Laboratory Program (CLP) Routine Analytical Services (RAS) include
Organic and Inorganic analyses for single-phase aqueous and soil/sediment samples.
A. Organic Routine Analytical Services (RAS)
The CLP Organic contracts are operating under the OLMO3. 1, or more recent
version, of the USEPA Contract Laboratory Program Statement of Work for Organic
Analysis. A copy of the SOW, Exhibit C, which has the analyte list and contract
required quantitation limits is provided in Attachment I.
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RSCCGuid-0 1
Page 4 of 17
The SOW includes the analysis of soil and aqueous samples for volatile, seniivolatile
and pesticidelPCBs compounds. Analysis techniques include gas
chromatography/mass spectrometer (GC/MS) and gas chromatography/electron
capture detector (GC/ECD) procedures.
B. Inorganic Routine Analytical Services (RAS)
The CLP Inorganic contracts are working under the ILMO4.0, or more recent version,
of the USEPA Contract Laboratory Program Statement of Work for Inorganic
Analysis. A copy of the SOW, Exhibit C, which has the analyte list and contract
required detection limits is provided in Attachment I. The SOW includes the analysis
of soil and aqueous samples for metals, including cyanide and mercury. Analysis
techniques include atomic absorption and inductively coupled plasma procedures.
C. Delivery of Analytical Services (DAS)
The Delivery of Analytical Services (DAS) program consists of primarily one method
of laboratory procurement. The field sampling contractors procure analytical services
in accordance with the “Region I ARCS Delivery of Analytical Services Pilot
Program, Final Report Volume II. Appendices”, 15 March 1994, or as otherwise
directed by the EPA contract Project Officer.
III. Regional Sample Control Center (RSCC)
A. Overview
The Region I Sample Control Coordinator is:
Christine Clark
U.S. EPA, OEME
60 Westview St.
Lexington, MA 02173
(617)860-4615
Fax No. (617)860-4397
Each Region has established a RSCC to centralize scheduling of CLP sample
analyses. The RSC routinely places all Regional requests for CLP analyses,
coordinates with the Contract Laboratory Analytical Services Support (CLASS)
contractor during sampling and sample shipment, and assists with resolving any
problems/issues concerning the samples. The RSC is the point of contact for
questions from sampling contractors and CLASS concerning Regional sampling
efforts.
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RSCCGuid-Ol
Page 5 of 17
B. Activities
1. Quarterly CLP and DAS Sampling Projections
Prior to the beginning of each calendar quarter, CLASS requires quarterly projections
from the Region. The RSC sends a letter requesting Quarterly Projections to all the
potential regional samplers. The projections include Routine Analytical Services
(RAS) samples and Delivery of Analytical Services (DAS) samples. These are broken
down by analysis/matrix/month and summarized for the quarter.
The First Quarter of the fiscal year is October, November and December, Second
Quarter is January, February and March, Third Quarter is April, May and June and
Fourth Quarter is July, August and September.
The EPA RSCC sends a letter with the blank request form in accordance with the
following schedule, see Attachment II:
First Quarter Request is mailed to sampler during the first week of July.
Second Quarter Request is mailed to sampler during the first week of October.
Third Quarter Request is mailed to sampler during the first week of January.
Fourth Quarter Request is mailed to sampler during the first week of April.
2. Weekly Scheduling of RAS Analysis
A sampling event is defined as “scheduled sampling at one site for a designated
period of time”.
To obtain RAS sample slots, the field sampling contractors must contact the RSCC as
soon as it has been determined that samples will be analyzed through the CL?.
Requests must be submitted no later than close of business, the Tuesday prior to the
sampling date.
Requests submitted to the RSCC after the deadline of Tuesday, close of business,
prior to the week of sampling are transmitted to CLASS as late requests. Whenever
possible, CLASS will accommodate late analysis requests; however, these assignments
are not guaranteed.
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RSCCGuid-01
Page 6 of 17
The RAS analysis requests must be submitted by facsimile on the “Region I Weekly
RAS Request Form” provided as Attachment HI. The project “EPA-NE-DQO
Summary Form” located in Attachment J of “Fart I”, Region I, EPA-NE Data
Validation Functional Guidelines for Evaluatin Enviromnental Analyses must be
provided with the request. Receipt of the transmittal by the RSCC must be
confirmed with telephone communication initiated by the requestor.
The Region I Weekly RAS Request Form must contain the following information:
1. Site Name (from the National Priority List)
2. Location (Town, State)
3. The Contract the work is requested under
4. Analysis Turnaround Time Required
5. CERCUS #
6. Purpose Code (Located on the Traffic Report form.)
7. Site Spill ID# with Operable Unit (A six digit code which begins with
01, for Region 1.)
8. Action Code (A two digit code from the project Work Assignment.)
9. Matrix
10. Number of Samples
11. Analysis/Parameter Code
12. Initials of the Contractor making request.
Note: The terms AnalysisfParameter Code and Analytical Method are used
interchangeably in this document.
RAS laboratory requests are for one week, if more than one week requests are
needed, the Region I CL? TPO must be contacted. Authorization must be obtained
by Wednesday at 3:00 pin, two weeks prior to sampling. The TPO may be
contacted at (617) 860-4379. The CLP TPO notifies the RSC of authorization
approval. The RSC will not submit a request for two week assignments without TPO
authorization. A two week request indicates sampling during both weeks, not just the
second week.
Routine data package turnaround time is 35 days from the last sample/per SDG
submitted for analysis. Fast turnaround time 14 day contracts may be requested for
both Inorganic and Organic samples. However, 14 day turnaround must be requested
at the time of RSCC notification of sampling event and written on the “Regional
Weekly RAS Request Form”. The RSC contacts the requesters by COB the Friday
following the initiation of a request with the laboratory assignment and case number.
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RSCCGuid-01
Page 7 of 17
3. Notification of DAS Events
The Region I field sampling contractors’ responsibilities for DAS events include
informing the RSC of the sampling information by using the “Region I Weekly DAS
Summary Form” provided as Attachment Ill. The DAS notification must be
submitted within seven working days of DAS sample shipment. The project “EPA-
NE-DQO Summary Form” located in Attachment J of “Part I”, Rcl!ion I. EPA-
NE Data Validation Functional Guidelines for Evaluating Environmental
Analyses , must be provided with the request. DAS notification includes the same
information as for RAS analyses.
Notification includes:
1. Site Name (from the National Priority List)
2. Location gown and State)
3. The Contract the work is requested under
4. Data Package Turn Around Time (Date samples shipped and date data package
due.)
5. CERCUS U
6. Purpose Code (Located on the Traffic Report Form.)
7. Site Spill IDU with Operable Unit (A six digit code which begins with 01, for
Region 1.)
8. Action Code (A two digit code from the project Work Assignment.)
9. Matrix
10. Number of Samples
11. Analysis/Parameter Code
12. Initials of the Contractor making request.
13. DAS Case Number
14. Laboratory Code (Standardized by the Field Sampling Contractor with the full
reference provided.)
Note: The terms AnalysisfParanieter Code and Analytical Method are used
interchangeably in this document.
4. Making Changes to CLP Analytical Requests
The RSC must be notified of all changes to sample shipments. Changes include the
number of samples shipped, a change in the date of sample shipment, a change in the
analysis requested, cancelling and the reason for cancelling or postponing a sampling
event, etc. An extension for sample shipment may be requested but, it is not
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RSCCGuid-O1
Page 8 of 17
guaranteed that the same laboratory will be available. If the laboratory is not
available the case will be closed. The sampler must send a new RAS Request Form
to the RSCC again by close of business, the Tuesday before the week of sampling,
and a new case number and laboratory will be assigned.
S. Sample Documentation
Within 7 working days of sample shipment, the CLP clients must provide copies of
RAS sampling documentation to the RSC. See Attachment IV.
The RAS sampling documentation includes a copy of sample Traffic Reports/Chain-
of-Custody forms identifying sample numbers, and the QAIQC samples.
The DAS sampling documents include “Region I Weekly DAS Summary Form” and
chain of custody documentation must be submitted to the RSC within 7 working days
of DAS sample shipment. The documents must provide field and laboratory sample
numbers, identify the QAJQC samples, provide the analytical method, the number of
samples and matrix.
The original Traffic Reports/Chain-of-Custody forms must not be sent to the RSCC.
If original Traffic Reports/Chain-of-Custody forms are received by the RSCC, a copy
of the paperwork is generated and filed with the case file. The original documents
are returned to the CLP or DAS client to be included with the final data package.
6. Receipt of’ CLP RAS Data & DAS Data Receipt Notification
Upon receipt of a CLP laboratory data package the RSC date stamps the first page of
the data package and initiates a “Complete SDG File Receipt/Transfer Form”,
Attachment V.
The CLP data package is then identified in the NESTS database. The EPA site
name, NESTS data package number, the CL? client name with the contract are
recorded on the first page of the data packages.
The data package is sent within 24 hours of its receipt to the CL? client who
performed the sampling for validation purposes.
The RSC is notified of DAS data receipt with the “DAS Data Receipt Notification
Form” from the field sampling contractor, see Attachment V I. The form must be
completed and sent to the RSC via facsimile within one day of data package receipt.
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RSCCGuid-0 1
Page 9 of 17
Note: If data packages for Dioxin/Furan analysis are received by the field sampling
contractor, forward the data within 24 hours to the RSC. The RSC will submit the
data for validation. OEME performs data validation on all Region I Dioxin/Furan
data.
7. CLP Contract Compliance Screening (CCS) & Laboratory Response to CCS
CLASS checks laboratory data packages for compliance with CLP contract
requirements. CLASS completes the Contract Compliance Screening (CCS) Reports.
A copy of the CCS Report is sent to the laboratory and another copy is sent to the
Region. The Regional CCS copy is sent to the CLP client. The CCS Reports must
be included with the laboratory data package in the CLP client’s project files.
The RSC receives copies of the laboratory’s response to CCS reports. The responses
are forwarded to the CLP clients to be included with the laboratory data package in
the CLP client’s project files.
8. Data Validation Reports and Tier I Validation Cover Letters
Refer to Sections 10.0 through 14.0 of the Data Validation Manual, Part I of Region
I . EPA-NE Data Validation Functional Guidelines for Evaluation of Environmental
Analyses , for format and distribution of Data Validation Reports and Tier I Validation
Cover Letters.
9. Notification to CLASS for Sample Shipment
All RAS shipment information must be reported to the Region I CLASS Coordinator,
Neil Rogers. The sampler must telephone Neil Rogers at (703)519-1019 or by
facsimile at (703)519-8626 by 5:00 p.m. on the day of shipment.
CLASS must be notified for shipments placed on Friday for Saturday delivery no later
than 3:00 p.m. on Friday. If CLASS is not notified by 3:00 p.m. on Friday it is
considered a late notification and receipt by the laboratory is not be guaranteed.
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RSCCGuid-01
Page 10 of 17
The required shipment infonnation includes:
1. Case Number
2. Date of telephone message or facsimile
3. Shipper - Region I
4. Lab receiving samples
5. Number of samples and analysis
6. Matrix and concentration of samples shipped
7. Date of shipment
8. Expected date of delivery
9. Courier/Airbill numbers
10. Identify whether or not shipping is complete
11. Special comments
10. Distribution of CL? Sampling Documentation
The RSCC manages the distribution of CLP and regional sampling documentation to
Region 1 CLP clients.
On an as-needed basis, CLP clients telephone the RSCC to request CLP sample
Sample Tags, Custody Seals, Inorganic and Organic Traffic Reports/Chain-of-Custody
forms and Inorganic, Organic Labels, see Attachment IV. The CLP clients must call
one week in advance of requiring supplies.
11. Problem Resolution and Infom ation Services
The RSC assists both CLASS and CL? clients when questions and/or problems arise
regarding laboratory or field activities.
When sampling problems occur and/or samples are not shipped as scheduled, CL?
clients must notify the RSC with the reason for the change by telephone as soon as a
change or problem has been identified. The RSC documents this information in a
telephone logbook and communicates the changes to CLASS.
If laboratories encounter problems during sample receipt or analysis, the laboratory
contacts CLASS, who then contacts the RSC to discuss the problem resolution. If
appropriate, the RSC will contact the affected CLP client to resolve the situation.
The field samplers cannot contact the laboratory until data have been received .
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RSCCGuid-O1
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CLP client questions concerning sample shipment, sample analysis, laboratory
contacts, the status of data deliverables, and final data packages are relayed to the
RSC. The RSC is the regional information center for incoming telephone calls,
correspondence, and other inquiries regarding CLP operations for EPA New England.
CLP clients should contact the National Technical Information Service (NTIS) in
Springfield, Virginia 22161, Telephone (703)487-4650 or 1-800-553-NTIS, Facimile:
(703)321-8547 or (703)321-9038, directly for CLP Statements of Work.
12. Reports Provided by the RSCC to the Lead Chemists
The RSC provides reports to the Lead Chemist for each EPA field sampling
contractor. The Lead Chemist is responsible for confirming that the information is
accurate and/or updating the information for the RSCC within seven days of receipt.
These reports must contain complete and accurate data records.
Routine Analytical Services (RAS) Reports:
1. RAS Outstanding Analysis Status Report - Monthly
The RAS Outstanding Analysis Status Report identifies Region I CLP samples
which were shipped to CLP laboratories for analysis. This report is generated
monthly.
The Lead Chemist verifies that this report identifies all the samples they have
shipped and that the ship date, laboratory, Case number, number of samples,
contractor/contract and due date correlate with his/her records.
If there are discrepancies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC within
seven days of report receipt.
If samples have been identified as outstanding, at the laboratory for longer
than the turnaround time, then the Lead Chemist must telephone the RSC
within three days of report receipt to identify the late data by Case Number,
SDG and laboratory. The RSC will ascertain a delivery date.
2. RAS Outstanding Data Validation Memoranda Status Report - Monthly
The RAS Outstanding Data Validation Memoranda Status Report is a summary
of Region I CLP cases which have been in data review for more than 21 days.
This report is generated monthly.
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RSCCGuid-O1
Page 12 of 17
The lead chemist verifies that this report identifies all the cases which are
presently in data validation and that the Case number, contractorlcontract,
laboratory, number of samples and the data package received date correlate
with his/her records.
If there are discrepancies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC, within
seven days of report receipt.
If CLP cases have been identified which have been in data review for more
than 21 days, then the Lead Chemist must provide to the RSC, within seven
working days of report receipt, a letter which identifies by Case Number,
SDG, and laboratory the Outstanding Data Validation Memoranda with the
scheduled date by which validation will be complete.
DAS Activities Status Reports:
1. DAS Outstanding Analysis Status Report - Weekly
The DAS Outstanding Analysis Report identifies DAS samples which were
shipped to DAS laboratories for analysis. This report is generated weekly.
The Lead Chemist verifies that this report identifies all the samples that they
have shipped and that the ship date, laboratory, Case number, number of
samples, contractor/contract and due date correlate with his/her records.
If there are discrepancies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC within
seven days of report receipt.
If samples have been identified as outstanding, at the laboratory for longer
than the turnaround time, then the Lead Chemist must pursue obtaining the
data. The Lead Chemist must provide to the RSC a letter which identifies the
late data by Case Number, SDG and laboratory. The Lead Chemist must
provide within seven working days the date that the data are anticipated or
received.
2. DAS Outstanding Data Validation Memoranda Status Report - Monthly
The DAS Outstanding Data Validation Memoranda Status Report is a summary
of DAS cases which have been in data review for more than 21 days. This
report is generated monthly.
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RSCCGuid-O 1
Page 13 of 17
The Lead Chemist verifies that this report identifies all the casaes which are
presently in data validation and that the Case Number, contractor/contract,
laboratory, number of samples and the data package received date correlate
with his/her records.
If there are discrepacies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC, within
seven working days of report receipt.
If Cases have been identified which have been in data review for more than 21
days the Lead Chemist must provide to the RSC, within seven working days
of report receipt, a letter which identifies by Case Number, SDG, and
laboratory the Outstanding Data Validation Memoranda with the scheduled
date by which validation will be complete.
3. Summary of All Data Packages Report - Quarterly
The Summary of All Data Packages Report identifies the overall status of each
DAS Case Number and SDG number. This report is generated quarterly.
The Lead Chemist verifies that this report identifies all of DAS activities for
the quarter, showing late data/late validation trends, as well as data packages
and/or validation reports which have not been received by the RSC.
If there are discrepancies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC, within
seven days of report receipt.
If samples have been identified as outstanding, at the laboratory for longer
than the turnaround time, then the Lead Chemist must pursue obtaining the
data. The Lead Chemist must provide to the RSC a letter which identifies the
late data by Case Number, SDG and laboratory. The Lead Chemist must
provide within seven working days the date that the data are anticipated or
received.
If Cases have been identified which have been in data review for more than 21
days the Lead Chemist must provide to the RSC, within seven working days
of report receipt, a letter which identifies by Case Number, SDG, and
laboratory the Outstanding Data Validation Memoranda with the scheduled
date by which validation will be complete.
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RSCCGuId-O1
Page 14 of 17
4. QAJQC Tracking Report - Bimonthly
The QAIQC Tracking Report lists all the field QC samples assigned to each
DAS sampling event. This report is generated bimonthly.
The Lead Chemist verifies that field QC samples are taken at the proper
frequency and that the field QC sample numbers are accurate.
If there are discrepancies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC, within
seven days of report receipt.
If it is identified that field QC samples were not provided at the proper
frequency, the Lead Chemist must submit a letter identifying the data by Case
Number, SDG and Laboratory. The letter must defme the discrepancy and
provide an explanation as to why the frequency requirements were not met.
5. Lab Performance With WMD Comments Report - Bimonthly
The Lab Performance with WMD Comments Report is a summaiy of
comments extracted from the DV memo cover letter andIor the “Data
Completeness Worksheet” regarding either the DAS analysis method or
problems/deficiencies with the data package. This report is generated
bimonthly.
The Lead Chemist verifies that this report identifies cases which require the
initiation of corrective action measures with laboratories.
If there are discrepancies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC, within
seven days of report receipt.
If there are problems which require follow-up, either in progress or new
initiatives, by the Lead Chemist regarding issues in the report, then the Lead
Chemist must submit a letter which identifies the data by Case Number, SDG
and laboratory to the RSC within seven working days of report receipt
describing the actions and the status of these activities.
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RSCCGuId-O1
Page 15 of 17
6. DAS Activity Report - Monthly
The DAS Activity Report lists the matrices and analysis/parameter code
requested for each site during a specified time frame. It is generated monthly.
The Lead Chemist verifies that the level and type of DAS activities for each
site are reported accurately.
If there are discrepancies between the Lead Chemist’s records and the report,
then the Lead Chemist must provide updated information to the RSC, within
seven days of report receipt.
If Cases have been identified which the data are erroneous or data have not
been provided to the RSC then the Lead Chemist must provide all information
identified with Case Number, SDG and laboratory to the RSC to make the
records complete and/or accurate.
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RSCCGu id-C I
Page 16 of 17
IV. Definitions/Acronyms
CADRE Computer Aided Data Review and Evaluation
CCS Contract Compliance Screening
CERCLIS Comprehensive Environmental Recovery Compensation and
Liability Information System
CLASS Contract Laboratory Analytical Services Support
CLP Contract Laboratory Program
CLP Client User of CLP Services
CSF Complete SDG File
DAS Delivery of Analytical Services
DAS Client User of DAS services
DPN Data Package Number
EPA U.S. Environmental Protection Agency
ESAT EPA Region I Environmental Services Assistance Team:
Lockheed Engineering and Sciences Corporation
ESD EPA Region I Environmental Services Division
NESTS New England Sample Tracking System
OEME Office of Environmental Measures and Evaluation,
formerly Environmental Services Division
QAJQC Quality Assurance/Quality Control
QAPP Quality Assurance Project Plan (or QAPjP)
RAS Routine Analytical Services
RPO Regional Project Officer
-------
RSC Regional Sample Coordinator
RSCC Regional Sample Control Center
SCC ESAT Sample Control Coordinator
SDG CLP Case Sample Delivery Group
SMO Sample Management Office
SOP Standard Operating Procedure
SOW Statement of Work
TPO Technical Project Officer
RSCCGuid-O 1
Page 17 of 17
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Attachment I
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EXHIBIT C
TARGET COMPOUND LIST AND
CONTRACT REQUIRED QUANTITATION LIMITS
NOTE: Specific quantitation limits are highly matrix—dependent. The
quantitation limits listed herein are provided for guidance and may not
always be achievable.
ll CRQLs are rounded to two significant figures.
The CRQL values listed on the following pages are based on the analysis
of samples according to the specifications given in Exhibit D.
Ycr soil samples, the moisture content of the samples must be used to
adjust the CRQL values appropriately.
c—i OLMO3.O
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ExhibLt C —- Section 1
Volatiles (VOA)
1.0 VOLATILES TARGET COMPOUND LIST ?iND CONTRACT REQUIRED QtTh.NTITATION LIMITS
Quantitation Limits
Low Med. On
Water
Volatiles CAS Nuznber ug/L
Soil
Soil
Co1 n
ug/Kg
ug/Xg
(v.g)
1.. Chioromethane
2. Brornomethane
3. VinyiChioride
4. Chioroethane
5. Methylene Chloride
74—87—3
74—83—9
75—01—4
75—00—3
7 5—09—2
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
(50)
(50)
(50)
(50)
(50)
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
Acetone
Carbon Disulfide
1,1—Dichioroethene
1 ,1—Dichloroethane
1, 2—Dichioroethene
trans—1 , 3-
D ich].oropropene
24. Eromoforu
25. 4 —Hethy l—2—pentanone
67—64—1
75—15-0
7 5—35—4
7 5—34—3
540—59—0
67—66—3
107—06—2
7 8—93—3
71—55—6
56—23—S
75—27—4
78—87—S
10061—01—5
79—01—6
124—48—1.
79—00—S
71—43—2
10061—02—6
7 5—25—2
108—10—1
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 1200
10 10 . 1200
10 10 1200
(50)
(SO)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
(50)
26. 2—Hexanorie
27. Tetrachioroethene
28. 1,1 ,2 .2—
Tetrachiorcethane
29. Toluerte
30. Chlorobenzerte
591—78—6
127—1.8—4
79—34—5
108—88—3
108—90—7
10 10 1200
10 10 1200
10 10 1200
(50)
(50)
(50)
31.
32.
33.
Ethy lbenzene
Styrene
Xylenes (total)
100—41—4
100—42—5
1330—20—7
10 10 1200
10 10 1200
10 10 1200
(SO)
(SO)
(50)
6.
7.
8.
9.
10.
(total)
Chloroform
1, 2—Dichioroethane
2—Butanone
1, 1, 1—Trichioroethane
Carbon Tetrachloride
Bromodichioronethane
1 ,2—Dich3.oropreparte
C is—i, 3-Dichioropropene
Trich1or ethe e
D ibrcu bch3.oromethane
1, 1,2—Trichioroethane
Benzene
21.
22.
23.
10 10 1200 (50)
10 10 200 (50)
10 10 1200 (50)
10 10 1200 (SO)
C-3
012403 .0
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Exhibit C -— Section 2
Semivolatiles (SVOA)
2.0 SEMIVOLATILES TARGET COMPOUND LIST AND COMTP.ACT REQUIR.ED QUANTITATION
LIMITS
Quantitation Limits
Law Med. On —
Water
Semivolatiles ChS Number ug/L
Soil
Soil
Co1um
ug/Kg
ug/ g
(ng) I
34. Phenol 308—95—2 10 330 1000G (20)
35. bis-(2—Chloroethyl) 11F”444 10 330 10000 (20)
ether
36. 2—Chiorophenol 95—57—8 10 330 10000 (20)
37. 1,3-Dichlorobenzene 541—73—1 10 330 10000 (20)
38. 1,4-Dichlorobenzene 106—46—7 10 330 10000 (20)
39. 1,2-Dichlorobenzene 95—50—1 10 330 10000 (20)
40. 2-Methyiphenol 95—4 8-7 10 330 10000 (20)
41. 2,2’—oxybis (1— 108—60—1 10 330 10000 (20)
Ch loropropane) 1
42. 4-Methyiphenol 106—44—5 10 330 10000 (20)
43. N-Nitroso—di—n— 621—64—7 10 330 10000 (20)
propylarnine
44. Hexachioroethane 67—72—1 10 330 10000 (20)
45. Nitrobenzene 98—95—3 10 330 10000 (20)
46. Isophorone 78—59]. 10 330 10000 (20)
47. 2-Nitropheno]. 88—75—5 10 330 10000 (20)
48. 2,4-Dimethyiphenol 305—67-9 10 330 10000 (20)
49. bis(2-Chloroethoxy) 111—91—1 10 330 10000 (20)
methane
50. 2,4-Dichiorophenol 120—83—2 10 330 10000 (20)
51. 1,2,4—Trichioro- 120—82—1 10 330 30000 - (20)
benzene.
52. Naphthalerte 91—20—3 10 330 10000 (20)
53. 4—Chioroaniline 106—47—8 10 330 10000 (20)
54. Hexachiorobutadjene 87—68—3 10 330 10000 (20)
55. 4—Chloro—3— 59—50—7 10 330 10000 (20)
methylpheno l
56. 2—Nethylrtaphthalene 91—57—6 10 330 10000 (20)
57. 1 exachlorocyc1o- 77—47—4 10 330 10000 (20)
pentadiene
58. 2,4,6—Trichlorophenol 88—06—2 10 330 10000 (20)
59. 2,4,5—Trich] .oropheno3. 95—95—4 25 830 25000 (50)
60. 2—Chloronaohthalene 91—58—7 10 330 10000 (20)
61. 2—Nitroaniljne 88—74—4 25 830 25000 (SO)
1 ?reviously known by the nane bis(2-Chloroisopropyl) ether.
C-4 OLM0
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Exhibit C Section 2
Semivolatiles (SVOM
Quantitation Limits
Low Med. On
Water
Semivo lati les CAS Number ug/L
Soil
Soil
Column
ug/Kg
ug/Kg
(ng)
62. Dimethylphthalate 131—11—3 10 330 10000 (20)
63. Acenaphthylene 208—96—8 10 330 10000 (20)
64. 2,6—Dinitrotoluene 606—20—2 10 330 10000 (20)
65. 3—Nitroaniline 99—09-2 25 830 25000 (50)
66. Acenaphthene 83—32—9 10 330 10000 (20)
67. 2,4—Dinitroohenol. 51—28—5 25 830 25000 (50)
68. 4—Nitrophenol 100—02—7 25 830 25000 (50)
69. Dibenzofuran 132—64—9 10 330 10000 (20)
70. 2,4—Dinitroto3 .uene 121—14—2 10 330 10000 (20)
71. Diethylphthalate 84—66—2 10 330 10000 (20)
72. 4—Chiorophenyl— 00S—72—3 10 330 10000 (20)
phenyl ether
73. Fluorene 85—73—7 10 330 10000 (20)
74. 4—Nitroanj1jx 100-01—6 25 830 25000 (50)
75. 4,6—Dinjtro—2— 534—52—1 25 830 25000 (50)
methyipheno 1.
76. N—Nitroso— 86—30—6 10 330 10000 (20)
diphenylamirie
77. 4—Bromophenyl-- 101—55—3 10 330 10000 (20)
phenylether
78. Hexach1orobenzer e 118—74—1 10 330 10000 (20)
79. Penta h1oropheno1 87—86—5 25 830 25000 (50)
80. Phenanthrene 85—01-8 10 330 10000 (20)
81. Anthracene 120—12—7 10 330 10000 (20)
82. Carbazole 86—74—8 10 330 10000 (20)
83. Di—n—butylphthalate 84—74-2 10 330 10000 (20)
84. Fluoranthene 206—44-0 10 330 10000 (20)
85. Pyrene 129—00-0 10 330 10000 (20)
.86. Butylbenzylphthalate 85—68—7 10 330 10000 (20)
87. 3,3’— 91—94—1 10 330 10000 (20)
Djch lorobenzjdjne
88. Benzo(a)anthracene 56-55—3 10 330 10000 (20)
89. Chrysene 218—01—9 10 230 10000 (20)
90. bis(2—Ethylhexyl) 117—81—7 10 330 10000 (20)
phthal ate
9].. Di—n—octylohthalate 117—84—0 10 - 330 10000 (20)
92. Benzo(b)fluoranthene 205—99—2 10 330 10000 (20)
93. Be zo(k)f1uoranthene 207—08—9 10 330 10000 (20)
c—s OLMO3.0
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Exhibit C —— Section 2
Semivolatiles (SVOA)
Quantitation Limits
Low
1(ed.
On
Semivolatiles
CAS Number
Water
Soil
Soil
Co1umn
ug/.L
ug/Kg
ug/Kg
(rig)
94.
Benzo(a)pyrene
50—32-B
10
330
10000
(20)
95.
Indeno(1,2,3—cd)—
193—39—5
10
330
10000
(20)
pyre ne
96.
Dibenzo(a,h)—
53—70—3
10
330
10000
(20)
anthracene
97.
Benzo(g,h,i)pe:ylene
191—24—2
10
330
10000
(20)
C—6 OLHO3.O
-------
Exhibit C —- Section 3
Pest .cidesfAroc1o s (PEST/ARO)
3.0 PESTICIDES/A.ROCLORS TARGET COMPOUND LIST AND CONTR) CT REQUtRED
QUANTITATION LIMITS 2 ’ 3
Quantitatien
Water Soil
Pesticides/Aroclors CA.S Number tig [ L ug/Kg
Limits
On
Column
(pg)
98. alpha—BHC 319—84—6 0.050 1.7 5
99. beta—BHC 319—85—7 0.050 1.7 5
100. de1ta—B C 319—86—8 0.050 1.7 5
101. gamma—BRC (Lindane) 58—89—9 0.050 1.1
102. Heptachior 76—44—8 0.050 1.7 5
103. Aidrin 309—00—2 0.050 1.1 5
104. Heptachler epoxide 111024—57—3 0.050 1.7 5
105. Endesulfan I 959 .98$ 0.050 1.7 5
106. Dieldrjn 60—57—1 010 3.3 10
107. 4,4’—DDE 72—55—9 0.10 3.3 10
108. Eridrin 72—20—B 0.10 3.3 10
109. Endosulfan II 33213—65—9 0.10 3.3 10
210. 4,4—DDD 72—54—8 0.10 3.3 10
111. Endosu1fa sulfate 1031-07—8 0.10 3.3 10
132. 4,4’—Dtyr 50—29—3 0.10 3.3 10
113. Methoxych].or 72—43—S 0.50 17 50
114. Endrin ketone 53494—70—5 0.10 3.3 10
115. Endrin aldehyde 7421—93—4 0.10 3.3 10
116. alpha-Ch3.ordane 5103—71—9 0.050 . 1.7 5
117. galnma—chlordane 5103—74—2 0.050 1.7 5
118. Toxaphene 8001—35—2 5.0 170 500
119. Aroclor—1016 12674—11—2 1.0 33 100
120. Aroc1o —1221 11304—28—2 2.0 200
121. Aroc].or—3 .232 11141—16—5 1.0 33 100
122. Aroelor—1242 5346921—9 1.0 33 100
123. Aroclor—]248 12672—29—6 1.0 33 100
124. ArocI.or—1254 1109769-1 1.0 33 100
125. Aroclor—1260 11096—82—5 1.0 33 100
2 There is no differentiation between the preparation of low and medium soil
Samples in this method for the analysis of pesticides/Aroclers.
lower reportin; limit for pesticide instrument blanks shall be one-half
t CRQL values for water samn 1es.
On] .v the exo-epoxv isomer (isomer B) of heptachior epoxide is reported on
e data reporting forms (Exhibit B).
c-i OLMO3.0
-------
Exl-ltBrTc
INO GX}ZIC. TARGET ANALYTE LIST
C— ]. ILMO4.O
-------
IN0 tG NIC T CET A NALYTE LIST (TAL) — TABLE 2.
- Cor raCt Required
Detection Limit 1 ’ 2
Xnalyte
tuglL)
Alilnun
200
Antimony
60
Arsenic
10
Barium
200
Beryllium
5
Cadmium
S
Calcium
5000
Chromium
10
Cobalt
50
Copcer
25
Iron
100
Lead
3
}tagnesiurn
5000
Ranganese
Mercury
15
0.2
Nickel
40
Potassium
5000
Selenium
S
Silver
10
Sodium
5000
Thallium
10
Vanadium
50
Zinc
20
Cyanide
-—
b
(1) ec to the-restrictions specified in Exhibits D andE, any
analytical method spe ified in ILMO4.0, I hibit D may be utilized as
1on as the docunec ted instrument or method detection limits meet ttie
Contract Reauired Detecti n Limit (CRDL) requirements. Bigher detection
limits nay only be usad in the foUawthg éircumstance:
If the sample conce itraticn exceeds five times the detection Unit of
the instrument armethod in use, the value may be reported even though
the instrument e h d det c joi limit may not equal the Contract
RequiredDe:ection Li. This 1s illustrated -in the exant 1.e beiou:
For lead: ?tethod in use ICP
r.strument Detection Limit (IDL) 40
Sale concentration 220.
Contract Re - ired Detection LimLt CRDt.) 3
The value o 220 may be re?crted even though the instrument detection
limit is greater than CBD . The instrument or method detection limit
must be d cunented as described in Exhibits 3 and B.
(.2) The C .DLs are m njmun levels of detectLen ac ep:able urtder the
contract State-er t o5 Wor3. .
C-? IL 04.0
-------
Attachment II
-------
THIRD QUARTER RAS FY95 PROJECTIONS
April
May
June
INORGANIC_ANALYSES
35 Day TA Full Metals With Cyanide
35 Day TA Cyanide Only
35 Day TA Metals Only
14 Day TA Full Metals With Cyanide
14 Day TA Cyanide Only
14 Day TA Metals Only
ORGANIC ANALYSES
35 Day TA Full TCL
35 Day TA VOA Only
35 Day TA SNA Only
35 Day TA Pesticide/PCB Only
14 Day TA Full TCL
14 Day TA VOA Only
14 Day TA BNA Only
14 Day TA Pesticide/PCB Only
DIOXIN ANALYSES
Fast TA 2,3,7,8-TCDD
-------
THIRD QUARTER DAS FY95 PROJECTIONS
Contractor/Contract:
Site Nante Paran eter/Method Matrix April May June
-------
Attachment III
-------
I WI I J IU ¼I Ut I I’UKLVL
REQUESTS
IE WEEK OF:
CASE VI
LAB
ASSIGNED
SITE NAME!
TOWN & STATE!
TURN AROUND TIME
CERCLIS #1
PURPOSE CODE!
SITE ID-ACTION CODE
-OPERABLE UNIT
MATRIX
4’ OF
SAMPLES
PARAMETER
CONTRACTOR)
CONTRACT
CLASS
0:
I;
AQ
AQ
AQ
AQ
AQ
AQ
SOIL
SOIL
SOIL
SOIL
SOIL
SOIL
VOA
SEMI-VOA
PEST/PCB
METALS
CYANIDE
METALS w/CYANIDE
VOA
SEMI-VOA
PESTIPCB
METALS
CYANIDE
METALS wICYANIDE
0
I:
AQ
AQ.
AQ
AQ
AQ
AQ
SOIL
SOIL
SOIL.
SOIL
SOIL.
SOIL
VOA
SEMI-VOA
PEST!PCB
METALS
CYANIDE
METALS w/CYANIDE
VOA
SEMI-VOA
PESTIPCB
METALS
CYANiDE
METALS w!CYANIDE
0:
I:
AQ
AQ
AQ
AQ
AQ
AQ
SOIL
SOIL
SOIL
SOIL
SOiL
SOIL.
VOA
SEMI-VOA
PESTIPCB
METALS
CYANIDE
METALS wICYANIDE
VOA
SEMI-VOA
PEST/PCB
METALS
CYANIDE
METALS wICYANIDE
-------
WEEK OF:
REGION I WEEKLY DAS SUMMARY FORM
DAS NISDG #/LABCODE/TAT
Site ID#-Action Code-
Operable Unit/Site Name/Location
No. of
Samples
Matrix
Parameter
QC
Sample
Nos.
Contractor/Contract
DASh:
SDGII:
LAB:
SITE ID:
ACTION CODE:
OPERABLE UNIT:
NAME:
CITY:
Ti\T:
D4S#:
SDO#:
LAB:
TAT:
STATE:
SITE ID:
ACTION CODE:
OPERABLE UNIT:
NAME:
CITY:
STATE:
.
.
DASh:
SDGh’:
LAB:
TAT:
SITE ID:
ACTION CODE:
OPERABLE UNIT:
NAME:
CITY:
STATE:
.
DASh!:
SDGN:
LAB:
TAT:
SITE ID:
ACTION CODE:
OPERABLE UNIT:
NAME:
CITY;
STATE:
,
•‘
COMMENTS:
-------
Attachment IV
-------
Guidance for Completion of DQO Summ2ry Form
For sampling events involving multiple cnvironm rn t matrices, complete Sections 4-10 for each matrix and ensure
that the matrix code is identified in section 4.
Copies of the completed DQC SuTrimny Forms should be included in thç QAPjPISAP and also included in the Data
Validation Report Copies of cot lewd i)QO Smnmiry Forms for CLP RAS and non-CLP DAS work should be
sent with the quarterly sample projections so the RSCC. Completed DQO SmT11 ry Forms for CL? RAS and non-
CLP DAS work be received by the RSCC prior to the sampling event
Section One: List all EPA pro ams involved in multi-media, muki .progrimrn ric sampling events.
List the site name, ptoj ed dare(s) of sampling, the EPA Site Manager, Case Team
Members, site location, the CERCLA site/spill identifier number including, and the
operable unit (contact EPA Site Manager for Identifier numbers). Circle the appropriate
phase of Superfund cleanup A Enviior m nt21 Risk Assessment, SA/SI-Site
Assessment/Site Investigation, pre-RI-pre-Remed ial Investigation, RI-Remedial
Investigation, FS-Fcasibllicy Study, RD-Remedial Design, RA-Reniedial Assessment,
post-RA-post-Remedial Assessment). Identify any other sampling event phase.
Section Two: List the matrix code (matrix code corresponds to the regional sample tracking database
matrix identifiers) for each set of samples that sin to be collected. For a list of matrix
codes rcfd to reverse aide of the DQO Strim y Form. Identify the analytinai
parameters requested for each matrix I.e., VOA, SV, etc., as well as the number of
locations that will be sampled. List the total number o lid QC samples that arc to be
collected for each matrix and parameter. The ‘No. of Sample Locations’ ‘count’ should
include the site and background locations sampled. The ‘No. of Field QC Samples and
PESa’ couvt should include the field duplicate sample, field blanks including field
equipment blanks, trip blanks, bottle blanks and FE samples for each matrix and
parameter.
Section Three: Give a brief physical description of the site. List the area of site, the centroid
load tic coordirnth s, potentially cont m red media, analyses andconccntrations
of concein, “hot spots’ and their por irbi1 locations, soil types, and depth to
gxotmdwarer. Attach another page if necessary.
Section Four: Identify the matrix code pertaining to information provided in sections 440. List the
potential uses for the sample data including, site assessment for human health and safety
issues, ecological and bum n risk assessment, evaluation of remediation alternatives,
engineering design, PRP dete on and monitoring removalfremedinl action. A
space is available for any other potential uses of the resulting data that are not listed
above.
Section Five: Describe the specific project DQOs. This section should describe in. detail the specific
objectives of the sampling event, I.e., to identify health risks to children, ages 1-6,
residing on the site who might be expowd to surface soils located in the area, or to
characterize the extent of groundwater conr min fiou. Be sure to idcn1if the purpose of
sampling, use of the data, and any related information needed to Identify appropriate
analytical and field methods. 1dentif whether the project sampling event Is pair of
PRP(Federal Facility ovcrsigiut, and/or confirmation of field screening results; and if It
is, identify the % splits being sent to another laboratory for confirmation. If oversight
and/or field screening confimiatoxy splits were taken, iii ic tc if documented spilt
comparability criteria are available.
-------
DAS DATA RECEIPT NOTIFICATION
Site Name:_______________
Contractor/Contract:______________________________
DAS*:______________________
Lab Code:_______________
SDG No.:________________
No. of Samples:____________
DAS Sample Nos.:___________________________
Blanks:_________________
Duplicates:
Ship to Lab Date:____________________________
Data Package Receipt Date:____________________
CSF Redeipt Date:___________________________
PE Sample Matrix Parameter Sample Count
Numbers
-------
Received for Laboratory by: Date /Time Remarks
(Signatu -si
ENVlflcJ1 MENTAL PROTECTION AGENCY
REGION I
CHAIN OF CUSTODY RECORD
::::J:::c T M E
STATION LOCATION
T S
REMARKS
-
—
—
—
-
-
-
-
-
-
-
-
-
-
by: (Sign.iurv/ —
by: (Sign. I’” ,)
— Date/Time
Date /Time
Received by: (Sign rvrv/
Received by: (Signicural
.1
Relinquished by: (SF,ns:u,si
Relinquished by: (SIgnswrs)
Date
Date
ITIme
(Time
Received by: tSignawriI
Received by: fSignawrcl
slinquished by: (Sign. wi-si Date
Time
-------
Relinquished by: (Signature)
Relinquish ‘Signature)
Inorganic Traffic Report
Con lractlaboratoryPiogram & Chain of Custody Record
r ’f E )J United States EnvI;onmental Protection Agency
(For_inorganic_CLP Analysis)
Case No.
6. Matrix
1. Project Code Account Code 2. Region No. 1 Sampllng Co. 4. Date ShIpped Carrler .
Regional Information . Sampler (Name) - . AIrbill Number . n Column A) .
1. Surface Water
2. Ground Water
Non-Superfund Program . Sampler SIgnature 5. ShIp To . . . 3. Leachale
4. Field OC
5. Soil/Sediment
3. Purposo EaityAth,n long-Term 6 Oil (High only)
Site Name CLEM Mib
• teed — PA I1FS 7. Waste ( 1-ugh
DSF : REM rEIRD - . only)
I I — .IPRP — EI R A • . . . 8. Other (specify
City. State Site Spill ID l IST — SI I O&M . .. . 1n Column A)
LJFED — ESI 1- NPLD AUN: .
, 1 CLP A -B C 0 E— RAS Anal sis F G H I
npIe Matrix Conc. Samph ?reser — — iii i Regional Specific Station Mo/Day/ Corresponding
Nu nbers (from Low Type: vative . on!L P’ L Tracking Number Location Yearlflme . CLP rgn’
(from Box 6) Med Comg (from or Tag Numbers Identilier Sample Sample No.
labels) High Gra OX 7) Collection
.! . 0
— 0 ‘ Z —
7. PreservatIve
(Enter
in Column 0)
1.HCI
2. HNO3
3. NaOH
4. H SO.j
5. K 2 CR 2 0 7
6. Ice ony
7. Other 1 speciçv
in Column D
N. Not preserved
. . .
.
J • K
ainple ‘Field 00
Initials Qualitier
- s • spe..
. 0- Ouplca.
fl • Rb s.Ie
I PE-P on , , E ’sI
•.HotsOC5.n
. —
.
• 1
•
.
I
—
— — — — — — —
1
..
..
.
.
1
.
Shipment for Case Page Sarnple s)To be Used for Laboratory 00 Additional Sampler Signatures of Custody Seal Number(s)
Complete? (YIN)
of . -I. ’
‘I
CHAIN OF CUSTODY RECORD S
Relinquished by: (Signature)- Date / lime Received by: (Signature) Relinquished by: (Sgnawre) . ..Date I 1 Tin e Received by: (Signature)
• • 1. • .
,
. 5
I .
.1
lime
Date
Received by: (Signature)
lime
Date
Rellnquished by: (Signature)
Kecelve br a oraiory oy:
(Signature)
•.Dale/llmo Remarks
—l — _________________
• Date ITime Received by: Stgna(ui ’e,P
• : •
.lscustody seal intact? YIN/none
-------
>
U i
d l
a.’
9
SEE REVERSE FOR AODm0NAL STANDARD INSTRUCTIONS
SEE REVERSE FOR PURPOSE COPE DEFINITIONS
E! A L United Slates Environmental Protection Agency
Contract Lcborolo y Program
C.. 11 ic Traffic Report
& Chain of Custody Record
(For Organic CLP Analysis)
Case No.
6. MatrIx
1. ProJect Code f Account Code 2. RegIon No.]Sampllng Co. 4. Date ShIpped Carrler (Enter
in Column A)
Regional Information Sampler (Name) AirbUl Number
1. Surface Waler
2. Ground Water
Non-Superfund Program Sampler Signature 5. Ship To 3. Leachale
4. FIeld CC
5. SoIl/Sediment
3. Purpose Early Adlon
LongT.:m 6. Oil (High only)
Site Name 1CLEM ActIon 7. Waste
Lead :IPA E1FS (High only)
1SF ...JREM EJAD 8. thor (Specify
ii ID LIST .. .js, k lO&M
City, State JSlteSp l ....JRl LJRA In Column A)
LJFED -JESI L...JNPLD ATrN:
A B C 0 E F G H I
C,bP Matrix Conc.: Sampl Preser RAS Analysis Regional Specific Station Mo/Day! Corresponding
Samp’e (from Low Type: vative — —
Numbers Box 6) Med Como. (from . Trackinci Number Location YearfTlrne CLI’ Inorganic
orTagFlumbers Identifier Sample Sample No.
(from — High Grab dox 7) 0 . Collection
labels) °“ . > W ARC!
— — — _
7. Preservative
(Entei in
Column 0)
1. HC1
2. HNO3
3. NaHSO4
4. H2S04
5. ice only
6. Other
(Specify in
Column 0)
N. Not
preserved
J K
Sample Field ac
Initials QualiFier
o.c& S.Sr 1d
0 .D , 4cata
i .n a.
PE .Pc ri tnCvat
— . N iCC Si.Øe
Shipment for Case Page I Sample(s) to be used for Laboraloty CC I Additional Sampler Signatures Chain of Custody Seal Number(s)
Complete? (YIN) I I
—0 :_I I
CHAIN OF CUSTODY RECORD
Relinquished by: (Signature)
Da to I Time
I
Received by (Signature)
Relinquished by: (Signature)
Dale / Time
I
Received by: (Signature)
Relinquished by: (Signature)
Date / lime
I
Received by: (Signature)
Relinquished by: (Signature)
Date / Time
I
Received by: (Signature)
Relinquished by: (Signature)
Dale I Time
i
Received for Laboratory by:
(Signature)
Date / Time I Remarks Is custody seal Intact? YIN/none
I
I I
Eiu . Region Copy
With. • l.ah Copy for Return to Raritan
Pink • CLASS Copy
Yellow. Lab Copy for fl.turn to CLASS
DISThIBUTION;
EPA Form 9110-2
-------
* U.S. GPOI 95- O2G5d
Case #
Sta on I.oca cn
CLP
#
Con a or Sampls #
Mon y ear
Malnx Designate:
- Camp. Grab
PreservaUves used HCI HNO, !other Speaty
Yes No
(Cirde One)
i CHECK BOX THAT APPUE4
ANALYSES Ii TO ThIS SAMPLE BOT l.E
N/Med SOW VOA Organica
w/Med SOW SernI. .VOAOrgan cs
w,Med SOW Pest(PCBs
Low Conc SOW VOA Organica
Low Cogic SOW Sami•VOA Organics
Low Cone SOW Pest/PCSs ‘
—
LOW/Med SOW Metais
LowlMed SOW Cyanide
Other.
TagNo. 12090111.
Sampler(s) Signatures
REGION I
Low Cone SOW Metals
Low Cone SOW Cyanide
.11
r —-
—
-I .
2
-I
rn
C
U)
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m
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rn
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n - :. -‘t ’ , . ..
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- -, —
- . — , .. .. .- 2.
- -- ‘ -. . .- -.. S — • . :. •.. ‘ .-k..- \
- - . .. . -- ‘—-... • .--. .. -.————- .—-• • - 7.— — .1 %
.
- -
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- j .. . — I--- ---- —.-—- - . . — - - :._
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.——-—-— - --‘- - — - — —
-S - - — . - - ----- - - -- 5-. • —.- -- - - — - - --
1 W
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-------
AMB94 - EXTRACTABLE AMB95 - EXTRACTABLE ANB96 - EXTRACTABLE
) B94 - EXTRACTABLE AMB95 - EXTRACTABLE AMB96 - EXTRACTABLE
A 1B94 - EXTRACTABLE AM395 - EXTRACTABLE N 1B96 -. EXTRACTABLE
AMB94 - EXTRACTABLE AMB95 - EXTRACTABLE A14B96 - EXTRACTABLE
A14B94 - VOA AMB95 — VOA ANB96 - VOX
I - VOA AM595 VOA ANB96 - VOA
AM894 A à95 ANB96
AXB94 ANB9S ANB9G
AN295 MIB9G
AMB95 ANB96
-------
M 7Y16 - TOTAL METALS MMY17 - TOTAL METALS MAJY18 - TOTAL METALS
MAJY16 - TOTAL METALS MAJ’117 - TOTAL METALS MAJY18 - TOTAL METALS
MAJY16 — CYANIDE MAJY17 - CYANIDE MAJY18 - CYANIDE
XAJY16 — CYANIDE M JY17 - CYANIDE MMY18 - CYANIDE
MAJY16 MAJY17 !4A3Y18
MAJY16 MAJY17- MAJY1S
MAJY16 M JY17 MAJY18
-------
IJ.S.E.P.A. CONTRACT LABORATORY I’ROGRAK HIS
CONTRACT LADORA1ORY ANALYFICAL SERVICES SUPI’ORI-OPERATEO BY DYHCORP
ORGANIC CONTRACT CO1IPLIANCE SCREENING SYSTEM
REGION 1 COPY
NMNPINNMNMNNMMNNMNNWMMNNNNNMNNMINNMINNI NNNNNNNNMMNNMNNNN M /
NN.MNNINNMNMMW$NMNNNNPINNNNNNMNNNNNNNNN NNNNNNNNNUNNNNUNNNN K j i// I
NINNNUNNNMMNNNINIINNNNNINNUMNNNINN NNMNNMNNNNNNNNUUNN UNN l
NUN NNNN r( i I’I]( .._ ()1.f aC’i ‘
SCREENING PACKAGE NNNN
SUIIItARY INFORMATION UNN
NNNN NNNN
OLMO1.B VEIl. 7
NNNN NUN
NUN SDGs AEBZO UNN
NUN RESUBMITTED NNNN
NUN NNNN
NUN CASh 23067 NUN
Null INNN
NNNN LAB; SWOK,
M INI NUN I
NUN CONTRACT; 68-D2-0013 1 1 1 1 J
NUN M MI I —
INN I I l(GION* 1 MINI - -
MINI NUN I I I (- ,. •
NUN ORDi 01/20/95 MI I I I. , , •
MM II NUll A2 .,
MMII SOC RECEIPT DATE; 12/15/9 MMII U.S. E j .flii
—. . • t ;1flfi.j
1 1MM SCREEN DATE; 02/01/95 MNMN
M MMI 1 1MM
MINI MAIL DATE 1; 01/20/95 MMMI
MINI MNNN
M MNM MAIL DATE 2* 02/03/95 MNNN
NNNI MMNN
NNNN SCREEHER& Nil/SC NNNN
Null MINI
INNI lOs 12733 NUN
•NNN 1 1MM
MI$NIIMNIMIMNNNNINMN INNNINNMNIIMMNMIMNNNMMMNMMMNMMMNIMNMNINM
MNNNNNNNIMNNNNNNINNNNMNNNNNMMNNNNIMNNNMNMINNNNNNUUUNNIINNIU
N IN INNNU INNNN I UNNMINNNNNNNNNNNNN NUNNNNNNNNNNNMNNMNNN U UN
-------
Attachment Q
“Region I ARCS Delivery of Analytical Services Pilot Program, Final Report
Volume LI. Appendices tt , 15 March 1994
-------
REGION I ARCS DELWERY OF ANALYTICAL SERVICES
PILOT PROGRAM
FINAL REPORT
VOLUME II. APPENDICES
15 MARCH 1994
DEBORAH A. SZARO
MOIRA M. LATAILLE
-------
TABLE OF CONTENTS
VOLUME IL APPENDICES
A. DEFINITIONS AND ACRONYMS A-i
B. ARCS DAS PILOT PROGRAM SCOPE OF WORK AND QUAUTY
ASSURANCE PROGRAM PLAN B-i
C. ARCS DAS PILOT PROGRAM RFP, INCLUDING ANALYTICAL
SPECIFICATIONS C-i
D. REGION I LABORATORY PRE-QUALIFICATION STANDARD
OPERATING PROCEDURE D-1
E. REGION I LABORATORY AUDIT STANDARD OPERATING
PROCEDURE E-i
F. REGION I DAS TRACKING STANDARD OPERATING PROCEDURE .... F-i
TOC-1
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APPENDIX B
ARCS DAS PILOT PROGRAM SCOPE OP WORK
AND
QUALITY ASSURANCE PROGRAM PLAN
B-i
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DEFINITIONS AND ACRONYMS
The following acronyms and abbreviations are used throughout this report:
ARCS Alternative Remediation Contracting Services
BHC Benzene Hexachloride (pesticide isomers)
BNA Base/Neutral-Acid Extractables
BOA Basic Ordering Agreement
BOD Biological Oxygen Demand
CAS Chemical Abstract System
CCS Continuing Calibration Standards
CCV Continuing Calibration Validation
CLP Contract Laboratory Program
COC Chain Of Custody
COD Chemical Oxygen Demand
CRDL Contract Required Detection Limits
CRQL Contract Required Quantitation Limits
CSF Complete SDG File
DAS Delivery of Analytical Services
DI Deionized
DO Dissolved Oxygen
DL Detection Limit
DQO Data Quality Objective
ECD Electron Capture Detector
EPA Environmental Protection Agency
EPTOX Extraction Procedure Toxicity Characteristics
ESD Environmental Services Division
FID Flame Ioni7! aiion Detector
FLAA Flame Atomic Absorption
GC Gas Chromatography
GCIFII) Gas ChromatographyfFlame Ionization Detector
GCIPID Gas ChromawgraphyfPhotoIcniz tion Detector
GCIMS Gas ChrornatographylMass Spectroscopy
GPC Gel Permeation Chromatography
HAZ WRAP Ha rdous Waste Remedial Action Program (DoD/DOE)
HCI Hydrochloric Acid
BPLC High Performance Liquid Chromatography
ICPIAES Inductivity Coupled Plasma
Atomic Emission Spectroscopy
IC Ion Chromatography
IDL Instrument Detection Limit
IR Infra Red (spectroscopy)
LAI Laboratory Audit Jnspection
LC Liquid Chromatography
LCS Laboratory Control Spikes
LFB Laboratory Fortified Blanks
LQAP Laboratory Quality Assurance Plan
C-2
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L MS Laboratory Information Management System
MDL Method Detection Limit
mg Milligram
mg/kg Milligrams per Kilogram
mg/L Milligrams per Liter
MGE Morrison Geotechnical Engineering
MS/MSD Matrix Spike/Matrix Spike Duplicate
NBS National Bureau of Standards
National Environmental Testing
NIST National Institute of Standards and Technology
PAR Polynuclear Aromatic Hydrocarbons
PARCC Precision, Accuracy, Representativeness,
Completeness, Comparability
PCBs Polychiorinated Biphenyls
PE Performance Evaluation
PRP Potentially Responsible Party
QA/QC Quality Assurance/Quality Control
QAN Quality Assurance Manager
QAO Quality Assurance Officer
QAPP Quality Assurance Program Plan
QAPjP Quality Assurance Project Plan
RAS Routine Analytical Services
RFP Request For Proposal
RRF Relative Retention Factor
RSCC Regional Sample Control Center
RSD Relative Standard Deviation
SAS Special Analytical Services
SDG Sample Delivery Group
SIM Selected Ion Monitoring
SMO Sample Management Office
SOP Standard Operating Procedure
SOQ Statement of Qualificafion
SOW Statement of Work
TAL Target Analyte List
TCO Total Combustible Organics
TDS Total Dissolved Solids
TkfF Tetrahydrofuran
TIC Tentatively Identified Compounds
TOC Total Organic Carbon
TPH Total Petroleum Hydrocarbons
TSS Total Suspended Solids
ug/L Micrograms per Liter
gig/kg Micrograms per Kilogram
UV/VIS UltravioletfVisible Spectroscopy
VOC Volatile Organic Compounds
VOA Volatile Organic Analysis
WP/WS Water PollutionIWater Supply
C-3
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iS: i6 LS E R CQITR CT S
v c r i
Scope of Work for Analytical $exvic..
7uly 12, 1993
This scope of work is for t a analysis and data validation of
aqueous, cci i , and air environmental samples in support of the
Suparf’und prograi i.
Task I Project Plannin
Cubtask 1.1 luia.tinga
Th. contractor vi ] ]. attend at least two meetings with EPA to
discuss personnel, analytical method specifications, schedule,
preparation of SOPs, and process of delivering analytical services.
The contractor will attend approximately five (5) cite scoping
meetings to discuss analytical/chemistry requirement..
Bubtask1.2 Document Preparation
The contractor will at a minimum prepare th. following documents:
a. QAPjP/SAP
b. SOPs for:
1. Prequa].ificatjon of laboratoxis.
2. On—site Laboratory Audits
3e Sample Scheduling/Tracking
C. Corrective Action Plan for Laboratory Performance and Method
Problems
d. Final Report on analytical Services which includes a suxnnary of:
3.. overall data quality
2. total cost broken down by activity
3. implementation problems encountered and resolutions
4. future implementation issues and recommendations on avoidance
e. Other documents necessary for the analysis of sample.
Bubtask 13 Document R.visv
The contractor’s QA officer or designee shall perform an internal
review of:
a. QAPjPSfsAPS prepared in support of the project
b. Work plans to •n ure that the following is includ d:
1. a reference to approved pre—qualification and on-sits lab
audit procedures
At+r.
JUL 13 ‘93 15:19
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L5 EP PE 1.ND C T gCT S e12
L./r ,irI
2. a description of the mechanism to be u ad for the delivery of
analytical ear-vices
3. a discussion of DQOs, TALs, DL3, PE aar pl.s, analytical
methods, daita validation and assessment.
Bubtaak 1.4 Cost. flonitoring
The contractor will track and monitor all costs associated with the
preparation for and analysis of samples.
Task 9ami,le Analysia
aubtask 3 1 Laborstory Pre-Qualificatiom
The contractor will perform laboratory (Lee) prequalification and
submit a report to EPA which includes a review of Laboratory QAPS,
SOPs, resumes or personnel, facility and equipment, 1WLa, PES
results, past performance, sample capacity, and the deliverables
package.
Subtask 3.2 On-sit. Audit
Th. contractor will perzorm an on—cit. laboratory audit arid aub uit
a report to EPA.
8u bt&ak 3.3 Sample scheduling/Tracking
Th. contractor shall implement scheduling/tracking procedures for
evid.ntiary purposes to be audited by EPA. The procedures shall
include but not necessarily be limited to the tracking of sampling
paperwork, chains or custody, traffic reports, records of
communication, packing lists, and sampling trip reports.
Task 4 Data validation
The contractor will perform data validation and assessment of all
samples analyzed.
JUL 13 ‘93 15:18 817 5659464 PAGE.012
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?‘13/93 tS: ,4 t S EPfl SL.P U LD c T CTD S
1 ZLD CONTRACTOR DAB QUALITY A88VRANC PROqR2Ix PLAli
Field Contractor Region I Oversight Level of ov.rsigtit
Establishes DAS Establishes minimum Minimum
Quality technical qualifications of
Assurance officer qualifications and Lsad Chemists have
position •xperisncs of QA bean established
independent of Lead personnel. tor all ARCS.
chemist position These criteria vi i ].
and corporate o. suffice for pilot.
Officer. For the For final
duration of the implementation of
pilot, the Lead A1 CS option, formal
chemist function DAS QA Officer
will be filled by qualifications will
the alternate Lead be established.
Ch.mist and the
primary Lead Reviews For pilot, QA
Chemist will serve qualifications of personnel
as the DAS QA QA personnel and qualifications and
officer. organ . ational organizational
chart. chart will be
______________________ ______________________ reviewed .
Develops approach Reviews and
f or accomplishi .nt approves approach
of work, to work.
Develops GOP for Reviews and SOPS will be
prequalifying approves developed in
laboratories. Prequalitication conjunction with
SOP. let ARCS
contractor, then
Develops SOP for Reviews and • used for final
performing on-site approves on—site implementation wiU
laboratory audits. Laboratory Audit remaining ARCS.
sop. sops will include a
certification
statement verifying
that all personnel
involved in the
pilot have read and
understood the
____________________ ____________________ SOPs .
JUL 13 ‘93 15:16 61? 5659464 PRGE.235
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?7’13/93 15:14 J’ pFu ID C 1P T
!Aad Chemist
attends project
Scoping Meetings to
discuss:
DQOS
PALs
DLs
Ana .ytical Methods
Data Validation
and Asessent
Audits Contractor’s
participation in
scoping Meetings.
Audits one vcoping
meeting during
pilot (workplarl for
same project will
be reviewed).
DAS QA o ticar
reviews workplans
to ensure that the
following are
Included:
Approved
Prspaalification
and On-sits
Laboratory Audit
procedures
referenced.
Description
provided for the
DAS rt.Ct an Lam to
be used.
Discussion of;
DQOs
TALS
DLa
PE Samples
Analytical Methods
Data Validation
and Assessment
Audits Contractor’s
development of
Workplanl.
Audits one workplan
during pilot (for
scoping meeting
Attended).
JUL 13 ‘93 15:16 617 5659464 PRG5.206
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ø7’13’93 1 : 14 _ 9-PE FU’1D C T CT S
Based on RGviews and During pilot,
contractor’s approves new co!n only requested
proposal. to msthods othervis. SAS methods will, be
subcontract, the standardized SAS standardized.
DAB QA officer methods are used.
reviews
technical
specifications for
analytical methods,
including
laboratory data
qilal ificat ion
criteria and
diskette
deliverable
requirement..
Bas.d on Reviews laboratory Audits all pr.—
contractor’ a prequalirication qualification
proposal to reports. reports generat.d
subcontract, th. for pilot.
DAB QA officer
p.rf arms
prequalificatien of
subcontracted labs
and prepares
reports,
which include
review of the
following:
Laboratory QAP
Confirm presence
and adequacy of
SOPS
Personnel Resumes
Facility and
Equipment
MDLs
PES results
Pest Performance
+/or reference.
Sample Capacity
Deliverables
Package
DAB QA Officer and Reviews laboratory Audits all on-site
Lead Chemist on-site audit audit reports
perform On—sit. reports and generated for
Laboratory Audit checklist, pilot.
according to cont-
ractor SOP and
prepare. reports . ____________________ ___________________
JUL 13 ‘93 I5 1€ 61? S559464 PRGE.e27
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e?’13 93 L5:15 LS EPR 9.F ij i. cr c s
Includes ESD Maintains and For pilot and final
Psrtorr ano. operates PE i ple entation,
Evaluation (PE) proqra . uses .xisting PE
samples for all Scores PE &mplea Program and DV
available and provides Oversight Proqra
parameters. results to to verify adequacy
Contractor. of:
Contractor
Contractor DAS Audit; D11 program. validation
office performs Method performance
data validation and Laboratory
data assessment. p.rformancs
Establishes Verifies that For final
guidelinse for feedback loop i pl.mentation,
dealing iith poor oxist within A1 cS establishas ESD
erfor ing for dealing with ranking program
laboratories, poor performing through CLPSTS for
laboratories, monitoring
laboratory
performance and
notifying all ARCS
of poor performers.
JUL 13 93 15:17 617 5659464 P GE.228
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e7’t3’93 15:15 LS R SL.FE tND C 4T CT S
Establishes a DAS
RSCC position whose
function includes:
Tracking:
sampling
paperwork, COO,
TRe, records of
communication,
packing lists,
sampling trip
r.ports, etc.
Scheduling:
sampling evants
analytical
services
Develops SOP for Reviews and Audits compliancs
Sample Tracking and approves Sample with SOP (Heidi).
Scheduling. Tracking and
Scheduling SOP
(Heidi).
Track. costs of the
following
components:
Writing Tech
Specs
Solicitation
Proposal Review
Laboratory
Solaction
Sample Scheduling
and Tracking
Data Validatien/
Assessment
JUL 13 ‘93 15:17 G17 4 4
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7’13I9 15:15 t.E EPR SLF U’lD CO’1T CT S
Prepare. final Reviewe final
report on uae of r.port nd revigas
ARCS to provide procsss/QA Program
analytical rvices for full ucale
which ui u arizes: i npleinentation in
Overall data R.gion.
quality
Costa (total arid
broken down by
activity)
In plementation
proble
encounterad and
rszolution
Potential futur.
implementation
iaaues and
ions
to avoid thsi
JUL 13 93 15:17 817 5852464 P GE.eIB
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EXHIBIT A
ATTACHMENT A
ANALYTICAL SPECIFICATION
FOR
METHOD 524.2
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1. SCOPE
The analysis of low level volatile organic compounds measured in groundwater and
surface water using EPA Region I Method 524.2, is required to be perfonned by this
specification. The additional compounds added to the list Qf 524.2 compounds are
acetone, 2-butanone. 2 - hexanone. 4-methyI-2-pentanofle CarbOfl disulfide. and
letrahydrofurari .
The method described herein also includes the required validation of the volatile
analyses by the laboratory, documentation of that validation, and a Lotus spreadsheet
deliverable.
Method 524.2 requires the lab to perform a method detection limit (MDL) study prior
to analysis to determine the theoretical lowest statistically valid detection liniit. This
study must follow the requirements described in 40 CFR 136 Paxt B using at least
seven replicate analyses of the lowest calibration concentration. The study must meet
the detection limits described in Section 6.
This specification also requires that the laboratory validate the data according to the
requirements provided in Section 9 and produce a properly flagged Lotus table (hard
copy and diskette).
2. PURPOSE
The data derived from this anaiysis will be used to further delineate groundwater
contamination, and to deterzniiie if treatment has met human health and ecological risk
objectives.
This method is intended for trace analyses of volaWes in waters that are only slightly
impacted by pollution and is not intended, for use in analysis of industrial effluent,
landfill leachate, or any moderate to highly contaminated surface waters, groundwater
or treatability study influents.
3. DEF1 ITION OF WORK
Surface water samples are to be analyzed by Method 524.2 with the requested
modifications. The modifications to the method are described in Section 7, Analytical
Procedures.
A performance evaluation sample (PE) will be provided with each sample delivery
group to be analyzed along with the field samples. Field samples will include blind
trip, bottle and equipment blanks, as well as blind duplicates.
1
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4. SCflFJMJLE
Samples will be shipped daily. Saturday delivery will be required. Overnight
delivery service will be used. Contacts for shipping and data delivery inquiries ale
specified in Exhibit A, Attachment F.
Holding Time:
Analyses are required to be performed within fourteen (14) days of sample
collection for preserved samples, and seven (7) days for unpreserved samples.
Unpreserved samples will be noted on the chain of custodies.
Delivery of Data:
Data is required to be delivered to M&E within thixty-five (35) days of
laboratory receipt of the last sample per sample delivery group of ten (10)
samples or less.
5. ANALYTICAL REFERENCES
EPA Method 524.2, Methods for the Determination of Organic Compounds in
Drinking Water EPA-600/4-881039 Dec. 1988 with Region I EPA modifications.
2
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6. SAMPLE PRESERVATION AND DETECTION LIMITS
Parameter Detection Limit teseiVatiOri
All analytes listed .1 1 ug/L <2 pH with HC1 at 4°C
Section LI of EPA
Method 524.2
Acetone . 5 ug/L <2 pH with HCI at 4°C
2-Butanone . 5 ug/L <2 pH with HC1 at 4°C
2-Hexanone . 5 ug/L <2 pH with HC1 at 4°C
4-Methy l-2-penta.none 5 ugIL <2 pH with HCI at 4°C
Carbon disulfide . 1 ugfL <2 pH with HCI at 4°C
Tetrahydrofuran . . 50 ugfL <2 pH with HCI at 4°C
7. ANALYTICAL PROCEDURE
EPA Method 524.2 Measurement of Purgeable Organic Compounds in Water by
Capillaiy Column Gas CbromatographylMass Spectromeuy from Methods for the
Determination of Organic Compounds in Drinking Water . EPA-60014-881039
December 1988, modified as instructed in the following paragraphs:
A. The volume of sample analyzed, either five (5) milliliters or twenty-five (25)
milliliters, will be determined by the volume used in the MDL study for the
specific instrument;
B. The following compounds must be included for analysis in all applicable
aspects of the method:
Compound CAS Number Primary Ton Secondary Ion
Acetone 67-64-1 43 58
2-Butanone 78-93-3 72 57
2-Hexanone 591-78-6 43 57
4-Methyl-2-pentanone 108-10-i 43 58
Carbon disulfide 75-15-0 76 78
Tetiahydrofuran 109-99-9 42
3
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C. A Matrix Spike and Matrix Spike Duplicate must be analyzed per sample
delivery group or tewnty (20) field samples, whichever is more frequent. The
spike solution must contain the following compounds: Vinyl chloride, 1,2-
Dichioroethane, Carbon tetrachloride, 1 ,2-Dichloropropane, Trichioroethene,
1,1 ,2-Trichloroethane, Benzene, cis-1,3-Dichloropropene, Brornoforin,
Tetrachloroethene, 1 ,2-Dibromomethane, and 1 ,4-Dichlorobenzene with
50 ng/5 ml (250 ng/25 ml) of each on column. The solution must also contain
2-Hexanone with 250 ng on column, and tetrahydroforam with 1000 ng on
column.
D. M, 0 and P xylenes must be reported as a total. The dichlorobenzene isomers
and cis/trans 1,2-dichioroethene isomers must be resolved and reported as
separate isomers.
E. For 1,2-dichloroethane-d4, m/z 67 can be used as the quantitation ion instead
of m/z 65. However, the same quantitation ion must be used throughout the
analytical sequence, beginning with the MDL.
F. One laboratory fortified blank 2(LFB) containing all analytes at a concentration
of I gIl, 5 &g/1 for ketones and 50 g/l for tetrahydrofuran must be analyzed
daily prior to sample analysis. The parent solution must be from a source
other than the initial calibration standard and continuing calibration standard.
All surrogates and internal standards in LFB must meet recovery criteria in
Section 8.
8. QUALITY CONTROL REQUIREMENTS
The following are the audits required, frequency of audits, QC limits, and required
corrective actions:
Audits
Frequency
Limits
Corrective Action
GCIMS Tuning Every (8) hours Table 3 Method Retune the GCIMS.
524.2 (See Sb) Tune must be
verified prior to
analysis of stds
blanh or samples
Internal Standards All samples, stds RT < 30 sec. EICP Inspect formal
blanks QC samples area -50% to function. Correct -
+100% from latest rerun all affected
8 hr. std samples, b12nk QC
samples
4
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Audits
Frequency
Limits
Corrective Action
Surrogate Recovery
Initial Calibration
5-Point Calibration
Cont. Calibration
Lab Fortified Blank
Method Blank
Matrix spike
Matrix spike dup.
All samples, cal
stds, biks, QC
samples
Initially and when
continuing criteria
not met
Every 8 hours
Daily prior to
sample analysis
Prior to each 8 hour
shaft
Every 20 samples or
every SDG________
1,2 dichoroethane-
d4-83-143 %,
1,2 dichloro
benzene-d4-80
120%. Both
surrogates in criteria
in all samples, cal
stds, blics, QC
samples
% RSD.30%
BR?> 0.05 THF,
1,2 dibromo
3-chioro propane
RF>0.02 (See Se)
RRF - Same as
initialcal %D
within criteria
(See 8e)
% recovery must be
60-140% for all
compounds.
5 compounds can
exceed 140% if not
detected in field
samples. None less
than 60% recovery
Target analytes
< 1 gJ1, 5 gil for
acetone, 2 butanone,
4 methyl 2
pentanone, 2
hexanone _____ for
and Tkik’
80-120% recovery
13% RPD (See 8i)
Renrn all samples
stds, blksorQC
samples with any
one surrogate
outside criteria.
Holding times must
be met. If not
submit both
analyses.
Determine problem
must meet criteria
prior to analysis of
blthiks and samples
Std. re in 1yzed, if
still out initial
calibranon is
performed, cont.
criterium cal must
be met prior to
blank and sample
analysis
Reanalyze and meet
60-140%. Renin all
samples affected.
LFB criteria must be
met prior to sample
analysis
Must be met prior to
sample analysis
Samples reanalyzed
until criteria are met
5
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Addkionaily, this specification requires that laboratory evaluate each quality control
requirement and report the data qualified using specific flags used in the EPA CLP
data validation guidelines in a Lotus table format (Attachment A.2). The following
are the ten (10) QC requirements, definition of the requirement, review procedure 1
criteria, laboratory action, and data reporting action:
a. Holding Time:
Definition: The holding time is the time from sample collection to sample
analysis.
Review Procedure: The holding times are reviewed by evaluating the date of
sample collection on the Chain-of-Custody with the date of sample analysis
reported on Form I.
Criteria: The samples are required to be preserved, therefore, the samples
must be analyzed within fourteen (14) days of sample collection. If the
samples were not preserved due to contpining carbonate or other interfering
substances that evolve gas, and the pH was not 2, then they must be
analyzed within seven (7) days of sample collection.
Laboratory Action: All samples must be analyzed within holding times.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. If the
criterion is not met, flag all positive results as estimated (1) and sample
quantitation limits as estimated (U]). If the preserved samples are not
analyzed within 21 days of sample collection the data must be rejected. If the
unpreserved samples are not analyzed within 10 days of sample collection the
data must be rejected.
b. GCIIvIS Tuning:
Definition: 25 mg of BFB must be analyzed once every eight (8) hours. The
BFB may be analyzed by either direct injection or purging modes of
introduction. The eight (8) hour time period for GCIMS system tuning and
standards calibration (initial or continuing calibration criteria) begins at the
moment of injection of the BFB analysis that the laboratory submits as
documentation of a compliant tune. The time period ends after exactly eight
(8) hours has elapsed acconiing to the system clock.
6
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Review Procedur : Review the Form Vs to check that all associated samples
have been analyzed within (8) hours of BFB injection and that the correct ions
and their abundances meet the criteria specified in Table 3 of 524.2. Check
that the data reported on the form agrees with the raw data.
Criteria: The instrument tune must be verified every (8) hours of analysis
with 25 ng of BFB. This must be verified prior to the analysis of standards,
blanks, or samples. The ion abundances must be within criteria specified in
Table 3 of Method 524.2 and the mass calibration must be correct.
Laboratory Action: If the BFB technical acceptance criteria are not met,
retune the GCIMS system. Whenever corrective action has been taken which
may change or affect the tuning criteria for BFB (e.g., ion source cleaning or
repair, etc.) the tune must be verified prior to analysis of standards, blanks,
or samples and regardless of the eight (8) hour tuning requirements.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. If the
mass calibration is in error, classify all associated sample data as unusable CR).
If the ion abundances are not within the Table 3 criteria but are within an
expanded window of 25 % report the sample data with no qualifiers. If the ion
abundances are not within the 25% expanded criteria, flag all sample data
associated with the tune as unusable CR).
c. Internal Standard Compounds
Definition; The internal standard compounds are Fluorobenzene and
Chlorobenzene-d5. Both must be spiked into all samples, calibration
standards, blanks and quality control samples. Calculate the RF and quantitate
results of each analyte with respect to the internal standard designated in
Attachment A.1.
Review Procedure: Review the Form Vffls to verify that all the retention
times and IS areas are acceptable. Verify that the results reported on the form
agree with the raw data.
Criteria: The internal standard must be delivered with 25 ng/5 ml (125 ng/25
nil) on column. The retention time for any internal standard must not change
by more than thirty (30) seconds. The extracted ion current profile (EICP)
area for any internal standard must not vary by more than a factor of two (-
50% to +100%) from the latest daily (8 hour time period) calibration
standard.
7
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Laboratory Action: The chromatographic system must be inspected for
malfunctions, corrections made as required, and the affected samples, blanks,
or QC samples must be reanalyzed. Check calculations, internal standard
solution stability and instniment performance. It may be necessary to bake-out
the system to remove water from the purge and trap transfer lines of the trap,
to recalibrate the instrument etc.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. If an IS
a.rea is outside -50%, or +100% of the associated standard: a) positive results
for compounds quantitated using that IS are flagged as estimated (3); b) non-
detects for compounds quantitated using that IS are flagged with the sample
quantitation limits classified as estimated (U3); c) if extremely low area counts
are reported, or if performance exhibits a major drop-off, then a severe loss of
sensitivity is indicated. Non-detects should then be flagged as unusable (R).
if an IS retention time varies by more than thirty (30) seconds, the
chromatographic profile for that sample must be examined to determine if any
false positives or negatives exist. For shifts of a large magnitude, the
reviewer may consider partial or total rejection of the data for that sample.
d. Surrogate Compounds:
Definition: The surrogate compounds, 1 ,2-dichloroethane-d4 and 1,2-
dichlorobenzene-d4 must be spiked into all samples, calibration standards,
blanks, and quality control samples. See Attachment A.l for internal standard
assignment. The surrogates must result in 25 ng/5 ml (125 ng/25m1) on
column (except for the initial calibration curve).
Review Procedure: Review the Form II to check that all samples, blanks,
calibration standards and QC samples etc. surrogate recoveries axe within
criteria.
Criteria: The surrogate 1 ,2-dichloroethane-d4 must be recovered between
83%-l43% and 1,2-dichlorobenzene-d4 must be recovered between 80% and
120% or the sample, calibration standard, blanks and QC samples must be
reanalyzed. Both surrogates must be within criteria for all samples, calibration
standards, blanks, and QC samples.
Laboratory Action: If samples must be reanalyzed due to one or more
percent surrogate recoveries being outside of QC limits, submit only the
analysis that had good recoveries and met holding times. If reanalysis did not
solve the problem or holding times were not met, then submit both analyses.
8
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Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. If one
surrogate is out of specification in a sample, but is recovered at greater than
10%, all positive results for that sample are as estimated (3) and all nondetects
are flagged with the sample quantitation limit as estimated (UI). If any
surrogate recovery is less than 10%, all positive results for that sample are
flagged as estimated (J) and all nondetects are flagged as rejected (R).
e. Initial Calibration
Definition: An initial five (5) point calibration curve containing all analytes,
surrogates and internal standards must be analyzed after tuning and prior to the
analysis of the blank and samples. All surrogates and internal standards in the
initial calibration must meet recovery criteria. A 2nd or 3rd order regression
curve may not be utilized. The concentrations of all analyte.s and surrogates
must be 2, 5, 10, 20, and 30 ugh except the ketones which are at 5, 10, 25,
50, and 125 ugh and tetrahydrofuran which are at 50, 100, 150, 200, and 300
ugh. A method blank must be analyzed in the 30 ugh spaxger to demonstrate
that the chamber contains no contamination prior to analysis of any samples in
that chamber. If samples are analyzed and quantified within eight (8) hours of
a compliant initial calibration analysis, it is not necessary to analyze a
continuing calibration standard.
Review Procedure: Review the Form VI which have the RRFs and %RSDs
reported. Check that all the compounds specified in the specification were
analyzed. Check that all the reported response factors and all reported relative
standard deviations are within criteria.
Criteria: The response. factor for each analyte, (other than the exceptions
specified below) and surrogate compound must be greater than 0.05. The
ketones, THF and 1 ,2-dibromo-3-chloropropane must have a minimum
response factor (RF) of 0.02. The relative standard deviation of the response
factors for each analyre and surrogate in the initial calibration must be below
30.0%. The response factors from the 10 ugh initial calibration standard (25
ugIL for ketones) must then be used for quantitation of samples if no
continuing cahlration needs to be performed. For field samples, all target
compound concentrations must not exceed the upper limit of the initial
calibration range, and no compound’s primary quantitation ion may saturate
the detector.
Laboratory Action: If the calibration criteria are not met, the source of the
problem must be determined and corrective action must be taken. It may be
necessary to clean the ion source, change the column, service the purge and
9
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trap or take other corrective actions to achieve the technical acceptance
criteria. The calibration criteria must be met prior to blank and sample
analysis.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. If a
compound has an average RPF of less than 0.05 or 0.02, whichever is
applicable: 1) Flag all positive results for that compound as estimated (3) for
all samples associated with that initial calibration and subsequent continuing
calibrations. 2) Flag non-detects for that compound as unusable (R) for all
samples associated with that initial calibration and subsequent continuing
calibrations.
If any compound has a %RSD of greater than 30%: 1) Flag all positive resuLts
for that compound as estimated (3) for all samples associated with that initial
calibration and subsequent continuing calibrations. 2) When the %RSD is
greater than 50%, flag all non-detects for that compound as estimated (Ui) for
all samples associated with that initial calibration and subsequent continuing
calibrations.
f. Continuing Calibration
Definition: The initial calibration must be verified at the beginning of each
eight (8) hour shift with the analysis of a continuing calibration standard if an
initial calibration curve was not generated daily. The continuing c i1fbration
standard (daily) must be used for sample quantitation. The continuing
calibration standard must contain all analytes and surrogates at 10 ugh 25 ug/L
for ketones and 150 ig/L for tezmhydrofuran. The internal standards must be
spiked into the continuing calibration standard at the correct concentration.
All surrogates and internal standards in the continuing calibration must meet
recovery criteria.
Review Procedure: Review the Form Vhs which have the RRFs and %Ds
reported. Check that all the compounds specified in the specification were
included in the continuing calibration. Check that all the reported response
factors and the percent differences are within criteria.
Criteria: The response factor for each analytc (other than those specified
below) and surrogate compounds must be greater than 0.05 and must be within
30.0% of the mean response factor value measured in the initial calibration.
The ketones, nii and l,2-dibromo-3-chloropropanc must have a minimum
response factor (RF) of 0.02 and be within 30.0% of the m n RF value
measured in the initial calibration.
10
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Laboratory Action: If the calibration criteria are not met, corrective action
must be taken and the standard must be reanalyzed. See Section 9.3.6 of
Method 524.2 for possible remedial actions. If the continuing calibration still
does not meet criteria, an initial calibration must be analyzed. The continuing
calibration criteria must be met prior to blank and sample analysis.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. If any
compound has a relative response factor of less than 0.05 or 0.02, whichever
is applicable: 1) Flag all positive results for that compound as estimated (J)
for all samples associated with the continuing calibration. 2) Flag all non-
detects for that compound as unusable CR) for all samples associated with that
continuing calibration.
If any compound has a percent difference between the initial and conthuing
calibration of greater than 30%: 1) Flag all positive results for that compound
as estimated (3) for all samples associated with that continuing calibration. 2)
When the %D is greater than 50%, flag all non-detects for that compound as
estimated (U]) for all samples associated with that continuing calibration.
g. Laboratory Fortified Blank:
Definition: One laboratory fortified blank (LFB) containing all analytes at a
concentration of 1 ugIL, ketones at 5 ugfL, and 50 rg1l for tetrahydrofiiran
must be analyzed daily prior to sample analysis. The parent solution must be
from a source other than the initial calibration standard and continuing
calibration standard. All surrogates and internal standards in the LFB must
meet recovery criteria.
Review Procedure: Review the Form V, analysis scheme section, to ensure
that an LFB was analyzed daily prior to sample analysis. Review the logbook
pages which verify that it is from a separate source other than the initial
calibration standard and continuing calibration standard. Check the LFB
reporting form to ensure that the LPB contained all the compounds and that
they axe at the specified concentration. Review the LFB reporting form to
verily that the recovery criteria were met. If the recovery criterion wasn’t met
for any one compound, verify that the compound was not detected in any of
the associated field samples.
Criteria: The percent recovery for each analyte must be between 60-140%,
It is acceptable for up to five (5) compounds to exceed the 140% recovery
criteria on any given day of analysis as long as those compounds are not
detected in any of the field samples.
II
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Laboratory Action: If an LFB compound has a recovery of greater than
140% that compound was detected in a field samp’e analyzed that day,
then both the LFB and the affected field samples must be reanalyzed and the
compound must meet the 60-140% recovery criteria. It is not acceptable for
any compound to have a recovery of less than 60%. The LFB criteria must be
met prior to sample analysis.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. Samples
should not be qualified with regard to the LFB results because all criteria must
be met for field sainplesto be analyzed. If any compound has a recovery
greater than 140% and was not detected in the samples, then the nondetects
must be estimated (tJJ) for that analyte in all samples analyzed that day.
h. Method Blank
Definition: A method blank must be analyzed prior to the analysis of any
samples during each eight (8) hour shift. All surrogates and internal standards
in the method blank must meet recovery criteria.
Review Procedure: Review the Form V, analysis scheme portion, to ensure
that a method blank was analyzed daily prior to sample analysis. Review the
Form IV to verify that no contamination was present in the method blank. If
cont mination was present in the method blank, verify that it was within the
allowable criteria.
Criteria: If any target compound analytes axe present as contamination, the
concentration must be less than 1 ug/L for the EPA Method 524.2 list and
carbon disulfide, less than S uglL for Acetone, 2-Butanone, 4-Methyl-
2-pentanone, 2-Hexanone, and less than 50 jig/L of tetrahydrofuran.
The laboratory must demonstrate there is no carryover from a high
concentration sample before data from subsequent analyses can be used.
ConL min2tion can originate from the trap and lines or sparger.
Laboratory Action: If the criteria are exceeded, the laboratory must consider
the analytical system to be out of control. The source of the contamination
must be investigated and appropriate corrective measures must be taken and
documented before sample analysis begins.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. The
12
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results must be corrected by subtracting any blank value. No positive
sample results should be reported unless the concentration of the compound
exceeds 10 times the amount in any blank for the common contaminants listed
below, or five times the amount for other compounds. Specific actions are as
follows:
1) If a compound is found in the blank but in the samples, no action is
necessary.
2) Any compound (other than the four (4) listed below) detected in the
sample, which was also detected in any associated blank, must be
qualified (by raising the sample quantitation limit to the level detected
and flag the value with a U) when the sample concentration is less
than five times the blank concentration. For the following four
compounds, the results are qualified by elevating the limit of detection
to the level detected in the sample and Flag the value with a when
the sample concentration is less than ten (10) times the blank
concentration.
Common laboratory contaminants:
a. methylene chloride
b. acetone
C. toluene
d. 2-butanone
3) There should be no compounds present in the blank greater than the
reporting limit. See Criteria.
Matrix Spike and Matrix Spike Duplicate
Definition: One matrix spike and matrix spike duplicate must be analyzed for
every twenty (20) field samples or per sample delivery group, whichever is
more frequent.
Review Procedure: Review the Form III to ensure that all the required
compounds were spiked and that all recovery and %RPD criteria were met.
Criteria: The spike solution must contain the following compounds at 10
ugfL: Vinyl chloride, trichloroethene, 1 ,2-dichloroethane, carbon
tetrachioride, benzene, 1 ,2-dichloropropane, bromoform, 1,1,2-
trichloroethane, cis-I ,3-dichloropropene, tetrachloroethene, 1 ,2-dibroznoethane,
and I ,4-dichlorobenzene. The solution must contain 2-hexanone at 25 ugh.
Samples requiring dilutions and chosen as the matrix spike/matrix spike
13
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duplicate must be analyzed at the same dilution as the original unspiked
sample. The percent recovery results must be 80-120% with RPD values less
than or equal to 13.
Laboratory Action: The samples must be reanalyzed until the criteria are
met. Samples shipped for analysis by this method should no experience
matrix effects, since they are drinking water, surface water or ground water
samples.
Data Reporting Action: Provide a one-page narrative which discusses in
detail all criteria which were not met and the specific data qualifiers (which
samples affected, which qualifiers, which compounds etc.) applied. If any
recovery results are greater than the criteria, then estimate (3) positive results
for this compound in the entire SDG.
If any recovery results aregreaterthanoreqUaltO 10%, but less than the
criteria, then estimate positive results for this compound in the entire SDG.
If any recovery results are less than 10%:
a) Flag positive results for that compound as estimated (3) for all the
samples in the SDG.
b) Flag non-detects for that compound as rejected CR) for all the samples
in the SDG.
If any results have an RPD greater than the contract QC limits stated on
Form ifi:
a) Flag positive results for that compound estimated (1) in all the samples
in the SDG.
The reviewer must use professional judgement to determine if the %RSD of
the results of the unspiked compounds in the sampling MS and MSD warrant
qualifications of the results for that compound.
j. Overall Assessment of Data
I.f multiple problems affect an individual sample or compound within a sample,
then the reviewer must use professional judgement to qualify the data. The
logic decision process, and the resultant qualification must be documented in
the case narrative.
14
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9. ANALYTICAL DELIVERABLES
A. The data package deliverables must resemble as closely as possible the Routh e
Analytical Services (RAS) Organic SOW OLMOI.8 or the latest revision data
package. The forms provided in the RAS Organic SOW OLMO1.8 or the
latest revision must be utilized where appropriate. The data qualifiers utilized
in the RAS Organic SOW OLMO1.8 or the latest revision must be applied to
the data provided.
I A narrative must be provided describing the procedure performed by
the laboratory, the volume of sample purged and any deviations from
the method. Problems encountered during analysis, problem resolution
and any factors which may affect the validity of the data must be
addressed. This specification, signed and dated chain of custody
documentation; sample tags, shipping airbills, and telephone logs must
be included. The data package must be paginated and in good copy
quality.
• A data reporting (validation) one page narrative must be supplied which
discusses in detail all criteria which were not met and the specific data
qualifiers (which samples affected, which qualifiers, which compounds
etc.) applied. The narrative must be broken down by QC parameter
(Section 8), and it must specify the criteria which were not met, which
qualifiers were applied to specific analytes, fractions, and samples etc.
• The raw data must be provided for all blanks, spikes, standards, PE
samples and field samples and must include:
• reconstructed total ion chromatogram
• instrument quantitation report containing the following
information: laboratory sample identification number, M&E
sample number, date and time of analysis, RT or scan number of
identified Method 524.2 or additional compound ion used for
quantitalion with measured area, analyte concentration, copy of
area table from data system, GC/MS instrument ID, lab file ID,
column, trap composition and operating conditions
• raw and enhanced spectra for all positive results
• daily continuing calibration standard reference spectra for all
positive results
15
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• The surrogate results must be provided in a tabulated format on a
modified RAS Form IL All standards, blanks, samples, and QC
samples which were analyzed must be reported on the form. The
results must be flagged according to the RAS SOW procedures.
• The matrix spike and matrix spike duplicate sample results for all non-
spike compounds must be tabulated on RAS Form I, modified to
include all compounds analyzed for in the Region I Modified Method
524.2. The concentration added, percent recoveries and relative
percent differences must be reported on a modified RAS Form lii for
the spiked compounds. The results must be flagged according to the
procedures contained in Section 8 of this specification. Raw data must
be included. Mass spectra for the spike compounds is not required.
• The method bl nk and associated samples must be summarized on
RAS Form IV.
• The tuning results must be tabulated and reported on RAS Form V.
The instrument nonnalized mass listing and the mass spectrum must be
provided.
• The initial calibration results must also be reported in a tabulated
format on a modified RAS Form VI. The relative response factors and
the percent relative standard deviation must be calculated for all
analytes and surrogates. The concentration and source of the standards
analyzed must be provided. Raw data must be included for all
standards analyzed. The spectrum for each compound in the initial
calibration standard does not have to be included.
• The 10 iigfL continuing calibration standard must be reported in a
tabulated format on modified RAS Form VII. The raw data must be
included. The percent differences and daily response factors must be
reported for all analytes and surrogates. A RAS Form VU must be
provided if the initial calibration standard curve 10 ppb standard was
utilized for quantitation of samples. The spectrum for each compound
in the continuing calibration standard does not have to be included.
• The Laboratory Fortified Blank (LFB) must be reported in tabulated
format on a RAS Form I modified to include all compounds analyzed
for in the Region I Modified Method 524.2. Raw data must be
included, excluding the spectra of all spike analytes. The percent
recoveries must be calculated and spike concentrations summa.rized on
the modified RAS Form I. The source of the spike and the acceptable
recovery limits must also be reported.
16
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• Provide the internal standards results on a modified RAS Form V I I I.
The retention time and area counts of the quantification ion for the
internal standards in all blanks, samples, and QC samples must be
reported on this form.
• An example calculation must be provided for positive results and
detection limit values reported.
• The laboratory must supply all results (hard copy and diskette) using
the Lotus spreadsheet template which is provided. A diskette will be
furnished with work order authorization. All field samples and QC
samples must be reported in this format. All Form I results must be
reported with the data reporting action qualifiers which are defined in
Section 8 of this specification.
B. Complete Sample Delievry Group File (CSF) Audit
Due to the litigative nature of each Superfund site, Region I EPA requires that
all analytical data, quality control data, and tabulated raw or supporting data
be delivered with each sample delivery group (SDG). With each sample
delivery group an EPA Region I Complete SDG File Completeness Evidence
Audit must be carried out. The CSF Completeness Evidence Audit Forms axe
included in Attachment A.3 and must accompany each sample delivery group
(data package). The laboratory through these audit forms must demonstrate
that each piece of sample data, raw data, calibration data and any other data
requirements of this specification is included by the laboratory in the data
package.
The forms included in Attachment A.3 are for all types of data packages. For
this specification the laboratory will use the forms supplied to the best of their
ability where deliverable items are applicable.
10. EXCEPTIONS
If QC requirements or action limits are exceeded; or if analytical samples axe
destroyed or lost; or if matrit interference is suspected, contact:
Andrew F. Bdiveau
Metcalf & Eddy, Inc.
(617) 246-5200 ext. 4433
17
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AI’I’ACHMENT A.1
Fluorobenzene - Internal Standard
DichJorodifluoromethane
Chioromethane
Vinyl Chloride
Bromomethane
Chloroethane
Trichiorofluoromethane
1,1 -Dichloroethene
Acetone
Carbon Disulfide
Methylene Chloride
Trans-I ,2-Dichloroethene
1, 1-Dichioroethane
2 ,2-Dich lampropane
2-Butanone
Cis-1 ,2-Dichloroethene
Chloroform
Bromochloromethane
1,1 ,l-Trichloroethane
1, 1-Dichloropropene
Carbon Tetrachloride
Benzene
1 ,2-Dichloroethane
Trichicroethene
I ,2-Dichloropropane
Bromodichioromethane
Dibromomethane
4-Methyl-2-Pentanone
Trans-I ,3-Dichlcropropene
Toluene
cis-1 ,3-Dichloropropene
1 ,I,2-Trichloroetha.ne
2-Hexanone
Tetrachloroethene
I ,3-Dichloropropane
I ,2-Dichloroethane-d4 (surrogate - Primary ion 65, secondary ion = 102)
18
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Chlorobenzene-dS - Internal Standard
Dibromochiorornethane
Bromofotm
Isop r opylbenzene
1 ,2-Dibromoechane
Chlorobenzene
Ethylbenzene
1,1,1 ,2-Tetrachloroethane
1,1 ,2,2-Tetrachloroethane
Xylenes
Styrene
Bromobenzene
N-Propylbenzene
1 ,2,3-Trichloropropane
2-Chiorotoluene
1 ,3,5-Trimettiylbenzene
4-Chiorotoluene
Tert-Butylbenzene
1,2 ,4-Trimethylbenzene
Sec-Butylbenzene
4-Isopropyltoluene
1 ,3-Dichlorobenzene
1 ,4-Dichlorobenzene
N-Butylbenzene
1 ,2-Dich1or benzene
1 ,2-Dibromo-3-Chloropropane
I ,2,4-Trichlorobenzene
Hexachiorobutadiene
Naphthalene
1 ,2,3-Trichlorobenzene
1 ,2-Dichiorobenzene-d4 (surrogate)
19
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ATIACHMENT A.2
LOTUS REPORTING FORMAT
20
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Voisnis A Iya$s
Pi.tcatf £ E Speculation for
P4.thod 524. &iydrolur.n with
Icetion.
JL
NZ€ SAIW&I M) EI: YVX 1 X OOrX I000cX XiOO X X OOO( X OOcX X aOCC
STATIOlI LOCATIOl: )OOO X X)OOCX X OO(X xmox moocx xxxxx xx ocx
LAIOATO*T J4aII: oo ) oo xx x oox )000X IQoocX oao x
CONPUJUD CR01
Toluen. 1 “U “U “U --U --U --U --U --U --U --U
Chtorobenzen. I “U “U “U “U “U --U --U --U --U --U
Ettiytb enmn. 1 --U --U --U “U --U --U --U -•U --U --U
Styler.. 1 --U --U “U “U “U “U “U --U --U --U
,tsIXytene. 1 U U “U U “U U --U --U --U “U
1 1 3- Olchtorobenzen. 1 --U --U --U --U --U --U --U --U --U --U
i4-Olctdorobqniens 1 U -- U U -- U -- U -- U U U -- U -- U
Trlchloref(uoro.*th.n. 1 -- U -- U U -- U -- U -- U -- U -- U -. U -- U
Dlbro.o.ethsns 1 “U “U “U --U --U --U --U --U --ii --u
1 1 1 1 2-T.trsthIoro.thone 1 Ii -. U -- L I •• U -- Ii U U U U -. U
1,2 1 3-TrlcMoropicçi.n. I -- U -- U -- U •- U -- U -- U -- U -- U -. U -• U
I .2-0ibrc.o-3-d Ioroprop.n. I •- U •- U -- U •- U -- U -- U -- U -- U -- U -- U
4-Chtorototusns 1 --U --U --U -- U -. U -. U --U -- U -- U -- U
Dlchiorod lftuorcssthans 1 -. U •• U -- U •- U -- U •- U U -- U •- U -- U
Bro.obenzen. I “U “U ••iJ “U “U “U “U “U --U “U
n•Prcpylb.nzen. I --U --U --U --U --U --u --ii •-u --u
2-chiorotoluene I -- U •- U - - U -- U -- U -- U -- U -- U -- U -- U
%,3 .S-Trimsthylbenz.ns I -- U •- U -- U •- U •- U •• U -. ii -- u -- u •- u
tert-Iuty tb.nzen. I -U --U -U --U --U --U --U --U --U --U
I.24-TrI..thylb.nzone I -- U -- U -. U •- U -- U -. U -- u -- u -- u •- u
sec-Sutytbenun. I -- U -- U -. U -- U -- U -- U •- U -- U -- U -- U
4-Iscpiop ItoIusns I --U --U --U --U --U --U --u --u --u
n-eutylbsni.n. I --U --U “U --U --U -U --U •-U --U
.2DtchIorcb.nz.n. I --U “U --U --U --U --U --U --U --U
1 .Z .4-jr lchtoqob.nz.ne I -- U -- U •- U -. U -- U -- U -- U -- u -- u -- u
Hophth.t.n. 1 --U --U --U --U --U --U --U --u --u --u
HcMschtojobutadisns I --U --U -•U --U --U •-U --U --U --U --U
12,3-TjIchlorob.nz.n. I U -- U -. U -- U -- U -- U -- U •- U -- U -- U
Ieopropylb.nz.n. (Oa.n.) I -- U -- U -- I I -- U -- U -- U -. U •- U -. U U
Chlorom.th.n. I “U “U “U -U “U “U --U --U --U --U
Bro.u.sthon I --U “U --U --U --U --U --U --u --u
Vinyichiorids I --U --U --U --U --U --U --U --U --U --U
Chtoro.than. I --U “U “U -U --U --U --U --U --U --U
M.thyl..wOiIortds I U “U U “U “U “U “U “U
Acetone S “U “U “U “U “U “U “U “U “U “U
CsrbonDisuIfId . I U “U “U “U --Il --U --U --U --U --U
1 1-DIch(oro..tji.n. I --U --U --U --U --u --u --u --u --u --u
1.1-D idiloro.th ene I --U --U --U --U --U --u --u --u --u --u
Z2-Dlchtoropeop.n. I -. U •- U -- U -- U -. U -- U -- U -. u -- u -- u
cIs-1 2-Dtchtoroethsne I -- U -- U -- U -- U -- U U U -- U -- U “ U
tr.ns-I 1 2-Dichloro.th.n, I •- U -. U -- U -- U -- U -- U -- U U -- U -- U
Chiorofora I --U -U “U --U --U --U --U --U “U --U
12-Dichtoro.thsn. 1 -- U -. U -- U -- U -- U •- U -- ii -- U -- u -- u
Z-Uutsnon. S --U --U “U “U “U “U “U “U “U •-U
1 1 1 1-TrIchIoro.th.n. I --U --U -- U --U --U --U --U -- u -. u --ii
-------
VoI.tit. Aqi.ous An*Iys s
4.tcsif 6 dd ’ DAS $p.cific.tion for
I sthod SV..2 I. T.tr.hycfrofur n with
146L $odificationi
SIT $ ug/L
P*OJCCT WO.
IU SPJ1PL€ W J(BU: EO(XX 3000 1K X)O IXX XXXXX X)0(XX XXXXX XX]OCX xxmcx
STATION LOCATION: X)O(XX XXXXK 30001K xmx xxxxx xxxxx xxxxx 300001
LASOATOU ktJi8LI: 300001 30001K 300001 30001* xaox xxxxx xxxxx X)O00 X)OtJO(
ClOt.
1 .1-D ichLorcproperim I --U -U “U “U --U “U “ U --U •-u
Cerbon T.tr. h(erId. I -. U -- U -- U -- U -- ii -- u •- u -. u •- u --
Br dIch(oro..thin. I -. U - U -- U -. U -- U •- U -- u - - u -- u - - u
1,2-DicMorcprop.n. I •- U -- U -. U -. U -. U - - u -- u -- u -- u - -
cI.-I.5-Otchlorcpropuns I -- U -- U -- U •- U -- U -. u -. u -- u •- u -- u
Trichtorosthin. I -. U -. U U -• U -- U -- U -- u -. u •. --
Dibromochtorcmsthsns 1 -. U --U -- U -. U -- U -- U •- U --U -- u •. u
1 1 1 Z-TrIchLoroethwis 1 U -- U U -. U -. U “ U -- U U -- U -. U
I 2-O ibrc.o .thsn. 1 --U “0 “U “U •-U --U --U --I i --U --u
Benztn. I “U “0 “U “U “U •-U -U --U --u --u
tr .ns-1 3-DIchIoroprop.n. I “U -. Ii -- L I -- U LI -. U U U - - U - - U
Bro .ofor 1 --U --Ii --U --U --U --U --U --U --u --u
-N.thyt-Z-P.ntanon . S •- U •- U •- U •• U -. U -- U - - U - - U - u -. u
2-N.*snons 5 --U “U “U “U “U “U “U --U --U
T.tr.chloro.th.ns 1 --U --U --U --U --U •-U --U --u --u .-
1,3-Dichloropropsns I --U “U U “ U “U --U --U --U --u
Bro c1i(orv..th . I --U “ II “U --U --U --U -U •-U --U --L i
1 .I2 2-7.tr.chtoro.than. I -- U -- U U U -. U -- Ii -- U -- U -. U -- U
T.tr.*iydiofuran SO --U --U “U --U --U --U --U --U • -u
DILUT*ON A TO ; 301 XX XX XX XX XX XX xx xx xx
DATE SAMPLID XX/XK/XX XXF)OC/W1 XX/XX/XX XX/U/XX XXIXX/X* XX/u/u xx/xx/xx xx,xx,xx ri/xx,xx xx/xxjxx
DATE *XALUED XX/)OCJYI XXIXXFXX IOC/U/XX XXIXXIU XX/XX/jlX KX/XX/XX XX/XX/XX XX/KX/XX Xxixxixx xx,n
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ATFACHMENT A.3
CSF AUDIT FORMS
22
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LOW CONCENTR.ATION VATIP. FOR ORCANICS COMPLETE SDG FILE (CS?) INVENTORY SHUT
LA10*ATOIY L1J ______________________________________ C TT/3TATE
CA iO. _______ soG O. _______ CwO$.TOFOLL J _______
rucT O. — T1I MO.
All documents delivered in the complete SDG file rLIt be original documents
vhe e possible. (R.EFER CE (ThIT B, SECTION II, PARAGRAPH 5, and SECTION III,
PARAGRAPH 16.)
PAGE NO. CHECX
FROM TO LAB EPA
Inventor, Sheet (Form DC-2) (Do not number) ____ ____ _______
SDQ Case Narrative ____ ____
Tiraff Ic Retort ____ ____ _______
Volatile, Data
a. QC Suary
Surrogate Perq ent Recovery S” ry (Tori II LCV) ____ ____ ________
Lab Control Sample Recovery (Froi III LCV) ____ ____ ________
Method Blank Stt ry (Form IV LCV) ___ ___ ______
Tuning and Mass Calibration (Tori V LCV) ____ ____
b. Sample Data
TCL Results • (Tori I LCV)
Tentatively Identified Compounds (Tori I LCV-TIC)
Recoc,atxucted total ion chromatogram.s (RIC)
and Quantitation Reporta for each sample
For each sample:
Ray spectra and background-subtracted
mass spectra of target compounds identified
Mass spectra of all reported TICs with three
best library matches
c. Standards Data (All Instruments)
Initial Calibration S i ..ary (Form VI LCV) _______
RICa and Quan Reports for all Standards _______
Continuing Calibration (Tori VII LCV) _______
RICa and Quint Reports for all Standards ________
Internal Standard Area and RY S” ry
(Tori VIII LCV)
d. QC Data
BTh ____ ____ ________
Blank Data ____ ____ ________
LCS Data ____ ____ _______
PES Data
Seni7olatiles Data
a. QC Surn i*ry
Surrogate Percent Recovery S” ’ry (Form II LCSV) ________
Lab Control Sample Recovery (Tori III LCSV) ________
Method Blank Suary (Form IV I.CSV) _______
Tuning and Mass Calibration (Form V LCSV) ________
FORM DC-2-l
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ONCENTRATION VATER. FOR ORCANICS COMPLETE SDG FILE (CSP) INVENTORY SHEET (Cont.)
G 0$.TOFOLL _
PAGE Os CHECX
FROM TO LA3 EPA
mi’VQl$tile3 Deri (cOnt.)
b. Sample Data
TCL Results (Form I LCSV)
Tentatively Identified Compounds (Form I LCSV-TIC)
Reconstructed total ion chromatogramS (RIC)
and Quantitation Reports for each sample
For each sample:
Raw apeccra and background subtraCted
sass spectra of TCL compounds
Mass spectra of TICs with three best library matches
GPC chroentograas (if CPC performed)
c. Standards Data ‘(All Instruments)
Initial Calibration Suw”ry (Form VI LCSV) ________
RICa and Quan Reporc .s for all Standards _______
Continuing Calibration (Form VII LCSV)
RICa and Quan Reports for all Standards ________
Internal Standard Area and RT S’” ry
(Form VIII LCSV)
. C Data
DF!PP
hank Data
I.CS Data
PES Data
a QC S”-zy
Surrogate Percent Recovery S ’ 7 (Form II LCP) ________
Lab Control Sample Recovery (Form III LCP) ________
Method Zlank Srnv.ry (Form I V LCP)
b. Sample Data
TCL Results . Organic Analysis Data Sl eet
(Form I LCP)
Chromacogrw (Primary Column)
C roaatograaa from second GC column confirmation ________
CC Integration report or data system printout and
calibration plots
Manual work sheets
For pesticides/A.roclors confirmed by GC/MS, copies
of raw spectra and copies of background-subtracted mass
spectra of target ccmpound (samples & standards)
FORM DC-2-2
10/9 2
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LOW CONCZNTL%TION WATER POR ORGANICS COMPLETE SDG FILE (CS7) INVVFrOLT SHEET (Cont.)
CAStPO. — GuO. G OI.TOFOLL J — 5 *3 10.
PAGE NO. CBEC C
FROM TO lAB EPA
Pesticides (conc.)
c. Standarda Data
Initial. Calibration Data (Form VI LCP)
Calibration Verification (Form VU LCP)
Pesticides Analytical Sequence (Form VIII ,
LCP-l and •2)
PesticideFlorisil Cartridge Check (Form IX. LCP)
Pesticide Identification (Form X LCP)
Standard chromacograms and data system printout
for ill Standards
For pesticides/Aroclors confirmed by CC/MS. copies
of spectra for standards used
d. Qd Data
Blank Data ____ ____ _____
LCS Data ____ ____ _____
PES Data ____ ____ _____
Miscellaneous Die ;
Original preparation and analysis forms or copies of
preparation and analysia logbook pages
Internal sample and sampl. extract transfer
chain-of-custody records
Screening records
All instrument output, including strip charts
from screening activities (de.àribe or list) ____ ____ _____ ________
EPA inf/Recetviug bocu ent3
Airbills (No. øf shipments _)
ain-of-Custody Records ________
Sample Tags
Sample Log.In Sheet (Lab & DC1)
SDC Cover Sheet
Miscellaneous Shipping/Receiving Records
(describe or list)
Internel. Lab Samvle Transfer Records end Trackina Sheets
(describe or list)
FORM DC-2-3
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NCENTRATION WATER FOR ORGAflICS COMPLETE SOC 1 112 (CS?) INVENTORY SHUT (Ccet.)
_______ G O. ________ WG . TO FOU ______ _______ _______ SA$ O.
PAGE ZIOs CHECX
FROM TO LU EPA
Other Records (de3cribe or list)
T.lephone Counication Log
leced by: _________________________
LP Lab) (Signature) (Printed Name/Title) (Date)
(Signature) (Printed Name/Title) (Date)
FOR ’( DC. -4
10/92
-------
Co t d SMO &Qd aflac rcw o( tesolutioi
R icwc4 3 r.
SAMPLE LOG-IN SILEET 1
Rciceivcd By (Print t hme): Log-in ta: _______________
Receiv Sy(Si natu:c): —
CORRESPOND G
Ca.s. Nwt bci
5&açlo DcUvu 7
C m p No.:
SAS Numh r
EPA
SAMPLE
I
SAMPLE
TAG
0
A IGNED
L 3
0
REMARKS:
CONDITION
OF SAMPLE
SI MENT, ETC.
REMARXS:
I. C ody SciJ(i)
2. Ci&siodySufl’tos .:
3. Oi ai -o( -Outody
4 Ta c Repocu
P LL
5.
6. Airb UNo.
7. Saaçl. Tqa
Sa 1oTq
I . Ss p1o Euoo
Prcic c/Abu*
fau /3iokcs
cc fAb.c
Pr .sc tFAbsc
A cktr
Prc c s/A
thwd
0I
0
t ,.wB uk i1
9. Doci 1ài az oo os
— c
rtpocli. & d — tip
YwNo
10. Dite Rtcciv d it L.i&
12. T Rcccnrcé ________
Sa pI.Tr*us(.r
o:
Area 1
3r
O :
—
-
.—
.
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to bookHa. —
L book Pigi No:
DC. 1
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APPENDIX C
ARCS DAS PILOT PROGRAM REP, INCLUDING
ANALYTICAL SPECIFICATIONS
C-’
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METCALF & EDDY, INC.
REQUEST FOR PROPOSAL NO.
93-004609-092
LAB ORATORY ANALYTICAL
SERVICES
in support of
ARCS REGION I PROGRAM -
DAS PILOT PROGRAM
(EPA CONTRACT NO. 68-W9-0036)
July 28, 1993
Prepared by:
M Metcalf & Eddy
M .Ajt & W t& Te ios Ca, paiiy
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INSTRUCTIONS TO BIDDERS
RFP NO. 93-004609-092
1.0 RFP
This RFP consists of the following documents:
• Instructions to Bidders.
• The Proposal/Bid Form and attachments thereto which shall be
completed by the Bidder and submitted as part of the Bidder’s
Proposal.
• Prequalification Questionnaire which shall be completed by the bidder
and submitted as part of the Bidder’s proposal.
• Model Subcontract and exhibits and attachments thereto.
2.0 METHOD OF SUBM1T AL
Bidder shall submit a technical proposal and a separate commercial proposal (two (2)
copies of each) in separate sealed envelopes appropriately marked ‘Technical
Proposal” or ‘Commercial Proposal” and further identified:
‘RFP No. 93-004609-092”
“Proposal for Laboratory Analytical Services’
“Name of your Firm _______
3.0 TiME AND PLACE OF SVBM1T AL
Proposals, signed by an authorized officer of your firm, must be received no later
than 5 PM on Monday, August 16, 1993, at the following address:
F DELIVERED BY COURTER: iF BY MATL :
Metcalf & Eddy, Inc. Metcalf & Eddy, Inc.
30 Harvard Mill Square P.O. Box 4043
Wakefield, MA 01880 Woburn, MA 01888-4043
ATrN: Denise I. Hatabian KITN: Denise I. Hatabian
3.1 A Bidder’s conference will not be held.
1
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3.2 Bidder is advised that any proposals received after the bid due date and time
may result in disqualifying the proposal from consideration. Facsimile
proposals may be received by the bid due date and time and will be considered
provided the original proposal is received not later than three (3) business days
following the bid due date at the address indicated above.
4.0 COMMERCIAL SECTION
4.1 Bidder is requested to submit its firm-fixed unit price to perform the Work
described herein by completing and returning the enclosed Proposal/Bid form
and other documents described therein.
4.2 Bidder is to include provisions for all applicable permits, licenses and taxes in
its proposed price.
4.3 The price bid for each Proposal/Bid form item is to include all costs to
complete the work outlined in Exhibit A arid it’s attachments.
4.4 Bidder is not require to bid on each and every Proposal/Bid form line item in
order for proposal to be considered responsive.
5.0 TECHNICAL SECTION
The work described herein will be conducted in support of the EPA - Region I ARCS
Program. This is a six (6) month pilot program for procurement of analytical
services for Superfund sites.
The scope of work is presented in Exhibit A and attachments thereto of the attached
subcontract. Specifically the laboratory will be required to perform one or more of
the following analyses on aqueous, soil, and/or air environmental samples:
• Volatile Organic Compounds (VOCs) in drinking water, EPA Method
524.2
• Volatile Organic Compounds (VOCs) in ambient air using ST.TMIIA
passivated canister sampling, Method TO-14
• Low Level Pesticide and PCB’s in surface water
• Total Organic Carbon (TOC), Total Combustible Organics (TCO), and
Grain Size Distribution
2
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• Water Quality Parameters: Alkalinity, Chloride, Chemical Oxygen
Demand (COD), Nitrate/Nitrite-N, Phosphorous, Sulfate, Total
Dissolved Solids (TDS), Total Suspended Solids (TSS), and Total
Organic Carbon (TOC)
Data derived from all analyses must be produced in order to satisfy EPA Data Quality
Objective Level IV (CLP), and be suitable for use in a court of law. Additionally, all
data must be suitable for use in ecological and human health risk assessments. All
analyses must be performed using the prescribed methodologies and must include the
quality control protocols and quality control samples requiied herein.
Bidder’s proposal shall include technical responses to this RFP, as follows:
5.1 A detailed Laboratory Quality Assurance Plan (LQAP) which at a minimum
includes:
5.1.1 Organiz2tion and Personnel
a. QA policy and objectives
b. QA management plan
c. Organization chart
d. Key and other personnel relevant to the bid
1) resumes
2) relevant education and experience
5.1.2 Facilities and Equipment
5.1.3 Document Control Procedures
a. Laboratory notebook policy
b. Sample tracking/custody procedures
c. Logbook maintenance/archiving procedures
e. Case File organization, preparation, review
f. Standard Operating Procedure (SOP) preparation, approval,
review, and revision
g. Technical and documentation revision procedures
5.1.4 Analytical Methodology
a. Calibration procedures and frequency
b. Sample preservation/extraction procedures
c. Sample analysis procedures
d. Standard preparation procedures
e. Decision process, procedure, and initiation of corrective
action
3
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5.1.5 Data Generation
a. Data collection procedures
b. Data reduction procedures
c. Data validation procedures
d. Data reporting and authorization procedures
5.1.6 Quality Control
a. Solvent, reagent, adsorbent check analysis
b. Reference material analysis
c. Internal quality control checks
d. Corrective action/determination of QC limits
e. Responsibility designation
5.1.7 Quality Assurance
a. Systems/internal audits
b. Performance/external audits
c. Corrective action procedures
d. QA reporting procedures
e. Responsibility designation
5.1.8 Safety Programs
5.1.9 Compliance with Environmental Regulations
a. Air pollution
b. Aqueous effluent
c. Hazardous and non-hazardous waste management
5.1.10 Standard Operating Procedures (SOPs) - relative to analytical
methods included in this bid
a. Scope and application
b. Definition
c. Responsibilities
d. References
e. Procedures
f. QC limits
g. Corrective action procedures
h. Documentation description and example forms
1. Miscellaneous notes and precautions
5.2 A Statement of Qualifications pertinent to the laboratory specifications in this
bid which at a minimum include:
4
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5.2.1 Equipment Inventory
a. instrument type, make, model, and age
b. computerization descriptions
C. maintenance programs! repair records
5.2.2 Facility Description
a. Disposal options
b. Waste handling methods
c. Hazardous waste management options
5.2.3 Analytical Capacity (tabular or chart format)
a. Number of instruments
b. Number of personnel
c. Sample analysis on a per day, per week, per month and per
year basis
5.2.4 Experience (Form 254) and References
a. Nawre of the work
b. Client name and telephone
c. Contract type and value
d. Work performed for EPA, DOD, DOE, CLP, COE, state
and/or local agencies
5.2.5 Performance Evaluation Program Participation and Certifications
a. Recent (under six months) program results
b. Federal, state, local and/or industrial organizations
5.2.6 Deliverables
a. Submit entire deliverable package proposed to be submitted
relevant to the Laboratory specifications being bid
b. Raw and supporting data need not be included in bid
submittal
c. Package to include:
1) sample number
2) laboratory number
3) dilution factors
4) analytical parameters
5) detection limits
6) instrumentation used
7) method blanks
8) surrogate analysis
9) calibrations
5
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10) internal standards
II) laboratory control samples
5.2.7 Method Detection Limit (MDL) Studies
Required for those relevant analytical methods requiring a current
MDL study.
5.3 If Bidder proposes to subcontract any of the work, it will present a detailed
subcontracting plan indicating:
5.3.1 The scope of the work to be subcontracted.
5.3.2 The reasons for subcontracting the work.
5.3.3 The name of the firm that will carry out the subcontracted work.
5.3.4 Information pertaining to the firm to be subcontracted (a
presentation folder including all of the information required from
Bidder).
6.0 EXCEPTIONS AND INTERPRETATIONS
Requests for clarification of the RPP documents will be received, and clarifications
and interpretations will be issued by written addenda. No interpretation or
clarification given orally or separately will be effective to alter or affect the RFP
documents unless confirmed by written addendum. Exceptions or qualifications to the
RFP documents are discouraged and may result in disqualifying the proposal from
consideration.
Requests for clarifications and interpretations must be addressed, in writing, to the
addressee shown in item 3.0 by not later than 48 iours prior to the bid due date and
time.
7.0 ADDITIONAL I 4FORMATION
This RFP shall not create any relationship, contractual or otherwise between
Metcalf & Eddy and Bidder, and Metcalf & Eddy shall not be liable for any expenses
incurred by Bidder in the preparation and submittal of any quotation. Metcalf &
Eddy reserves the right to accept or reject any proposal received, to accept other than
the lowest proposal and to reject any proposal in whole or in part, or to accept any
proposal which contains deviations from the requirements hereof, or to reject all
proposals with or without notice or reason, and if no proposal is accepted, to abandon
6
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the work or to have the work performed in such a manner as Metcalf & Eddy may
elect.
Metcalf & Eddy reserves the right to negotiate any proposal received by Metcalf &
Eddy.
7
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PROPOSAL/BID FORM
RFP NO. 93-004609-092
BIDDER: __________________________
TO: METCALF & EDDY
The undersigned has carefully examined the Instructions to Bidders, Subcontract Agreement,
and all other bid documents, and submits this proposal for a Subcontract for performance of
the Work described therein in strict accordance with said documents.
1.0 BID PRICE SCkLEDIJLE
1.1 Bidders need not bid on each item . All entries in the entire bid must be
made clearly and in ink; prices bid must be written in both words and figures.
Bidders must insert extended item prices obtained from quantities and unit
prices.
2.0 BIDDER REPRESENTS THAT
2.1 ()The Bidder has no pre-hiring collective bargaining agreements.
-OR-
() The Bidder has pre-hiring collective bargaining agreements, and has
ascertained that the undertaking of Work from Metcalf & Eddy on this Project
shall not violate any provisions of such pre-hiring collective bargaining
agreements. Further, there is attached hereto either an excerpt from. or a
project agreement amending , each such pre-hiring collective bargaining
agreement, providing that there shall be no strikes, slowdowns, picketing,
secondary boycotts or work stoppages during the performance of the Work.
1
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2.2 () The Bidder can and shall provide Metcalf & Eddy with an insurance
certificate, within five (5) business days immediately following any
award of a Subcontract and before commencing the Sublet Work, which
shall fully satisfy the requirements of the Subcontract.
-OR-
() The Bidder cannot. Bidder shall state here why it cannot comply with
Metcalf & Eddy’s insurance requirements.
3.0 REQUIRED INFORMATION
3.1 List of the proposed lower tier subcontractors by name, type of work and
percentage of total work which Bidder intends to sublet. Bidder shall not
subcontract more than 50% of the sublet work.
If none, Bidder shall so state: ____________
Percentage of
Name Type of Work Total Work
1.
2.
3.
4.
2
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3.2 List separately any commercial or technical exceptions taken to the RFP
Documents.
If none, Bidder shall so state: ___________________________________
If Bidder, takes any exceptions to the REP documents, Bidder shall include
the proposed monetary value for each exception. Bidder agrees to withdraw
any exception at the proposed value stated herein.
4.9 TECHNICAL INFORMATION
(as required by the Instructions to Bidders. Use as many additional pages as
required).
5.0 ADDENDA
Addenda to bid documents received prior to submittal of this bid and made part of this
proposal are:
Addendum No.: ___________ Date: ___________
Addendum No.: ___________ Date: ___________
Addendum No.: ___________ Date: ___________
6.0 CONTRACTOR’S LICENSE
State of______________________
Engineering License No. ______________
and/or Contractor’s License No. _________________
Bidder is a _______________________________(Proprietorship, Partnership,
Corporation) existing under the laws of _______________________________
If a partnership, the partners are:
3
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The undersigned certifies that the bid prices contained herein are firm, and have been
carefully checked, are submitted as correct and final, and are firm for acceptance for a
period of 90 days, extended from the bid due date.
Bidder: ___________________________________
(Type or Print)
By: ____________________________
Signature
Title: ______________________
Type or Print
Name: ____________________________
Address: _______________________
Dated: _________________
Phone Number: ____________________
Telex and Fax Number: _____________
Note: In order for your proposal to receive full consideration, it must
include answers to all questions. all attachments , and must be received on
Attachments:
1. Representations and Certifications
2. Prequalificatiori Questionnaire
4
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Subcontract No. 93-004609-092
SUBCONTRACT AGREEMENT
BETWEEN
METCALF & EDDY, INC.
AND
FOR
LABORATORY ANALYTICAL SERVICES
THIS AGREEMENT, made this _______ day of ________ 1993, by and between
Metcalf & Eddy, Inc., with offices at 30 Harvard Mill Square, Wakefield, Massachusetts
01880 (mailing address, P.O. Box 4043, Woburn, Massachusetts 01888-4043), hereinafter
called “M&E” and ___________________, with offices at ______________, (mailing
address, j, hereinafter called “Subcontractor.”
WITNESSETH:
WHEREAS, M&E has entered into a Contract with the U.S. Environmental Protection
Agency, hereinafter called the “Client, to provide services for remedial planning activities at
selected uncontrolled hazardous waste disposal sites in Region I, hereinafter called the
“Project;”
WHEREAS, Subcontractor represents that it has the expertise, knowledge, ability and is
qualified to render certain laboratory, analytical, and data management services which
include, without limitation, testing for chemical composition of material supplied by M&E,
the encoding, archiving and reporting of tests and other data as directed by M&E;
WHEREAS, M&E desires to employ Subcontractor to render certain laboratory, analytical
and data services in connection with or related to the Project; and
WHEREAS, Subcontractor is willing to provide such services under the terms and conditions
contained herein;
NOW, THEREFORE, in consideration of these premises and of the mutual promises,
covenants and agreements contained herein, the paities agree as follows:
ARTICLE 1- ENGAGEMENT OF SUBCONTRACTOR
1 of 4
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1.1 M&E hereby engages and the Subcontractor hereby accepts the engagement to
perform and provide the services set forth in Exhibit A and it’s attachments hereof,
hereinafter referred to as the “Work,” in connection with the Project in accordance
with the terms and conditions of this Subcontract.
1.2 Subcontractor shall perform the Work as an independent contractor with exclusive
control of the maimer and means of performing the Work in accordance with the
requirements of this Subcontract. Subcontractor has no authority to act or make any
agreements or representations on behalf of M&E or the Client, and no contractual
relationship exists between Subcontractor and the Client. This Subcontract is not
intended to create, and shall not be construed as creating, between M&E and
Subcontractor, the relationship of principal and agent, joint venturers, co-partners or
any other such relationship, the existence of which is hereby expressly denied. No
employee or agent engaged by Subcontractor shall be, or shall be deemed to be, an
employee or agent of M&E.
ARTICLE 2- SUBCONTRACT DOCUMENTS
2.1 This Subcontract shall consist of the following subcontract documents:
2.1.1 Subcontract Agreement.
2.1.2 Exhibit A, Scope and Schedule of Laboratory Services, including Attachments
thereto.
2.1.3 Exhibit B, Payment Schedule, including Attachments thereto.
2.1.4 Exhibit C, Supplementary Conditions for Laboratory Services.
2.1.5 Exhibit D, General Conditions for Laboratory Services.
2.1.6 Exhibit E, General Safety Rules.
2.2 The above documents constitute the entire Subcontract between M&E and
Subcontractor and supersede all prior and contemporaneous negotiations, statements,
representations, agreements, letters of intent, awards, or proposals, either written or
oral. This Subcontract may be modified only by a written instniment signed by both
parties.
2.3 In the event of any inconsistency between the provisions of the subcontract
documents, the inconsistency shall be resolved by giving precedence in the order
listed below.
2 of 4
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2.3.1 Subcontract Agreement
2.3.2 Exhibit C, Supplementary Conditions
2.3.3 Exhibit D, General Conditions
2.3.4 Exhibit A, Scope of Work and Schedule for Services, including Attachments
thereto
2.3.5 Other Exhibits and Documents
2.4 Headings of sections and other parts of this Subcontract are for purposes of reference
only and are not to be construed as a part of this Subcontract.
ARTICLE 3- COMPENSATION
3.1 As full consideration for the complete, satisfactory and timely performance by
Subcontractor of work contemplated by this Subcontract in strict accordance with the
requirements hereof, M&E shall pay to Subcontractor the firm, fixed unit prices set
forth in Exhibit B.
3.2 In the event that the actual quantity of samples varies from the estimated quantity
more than twenty-five percent (25%), the unit price of such items shall be equitably
adjusted, upon demand of either party. The equitable adjusimern shall be based upon
any increase or decrease iii costs due solely to the variation above one hundred
twenty-five percent (125%) or below seventy-five percent (75%) of the estimated
quantity.
3.3 The total funding hereof is limited to $ . In no event shall Subcontractor
perform services which would result in billings in excess of the total funding
limitation.
ARTICLE 4- PROSECUTION AND COMPLETION OF WORK
Subcontractor shall prose:ute and complete all Work under the Subcontract in accordance
with the schedule set forth in Exhibit A.
ARTICLE 5-INSURANCE
Prior to commencement of the Work, Subcontractor shall provide, and maintain in full force
and effect during the term of this Subcontract, the insurance coverages upon Subcontractor’s
operations hereunder as specified in the Supplementary Conditions, plus such other insurance
coverage as M&E may require.
3 of 4
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ARTICLE 6 - LAWS
This Subcontract shall be construed and governed by the laws of the Commonwealth of
Massachusetts. Subcontractor shall comply with all laws, statutes, ordinances, rules and
regulations of any governmental entity having jurisdiction and Subcontractor shall indemnify
and hold harmless M&E from any fines, penalties, costs or liability arising from
Subcontractor’s failure to comply therewith. Subcontractor represents that it is duly
authorized to do business in all of the locations where the Work is to be performed, it has
the knowledge, capability and expertise to act as the Subcontractor and shall evidence said
authorization and capability to M&E upon request.
ARTICLE 7- PARTIAL INVALTDITY
If any provision of this Subcontract is determined to be invalid under any applicable law,
such decision shall not affect the remaining portion, which remaining portion of the
Subcontract shall continue in full force and effect as if it had been executed with the invalid
portion eliminated.
ARTICLE 8- EFFECTIVE DATE
The Effective Date set forth on page 1 of this Subcontract shall be the date as which all
Contract Documents and provisions thereof have reference for purposes of coordination of
their meaning and effect. The price relates to the Work as described in the Contract
Document in their condition on that date. Changes after the effective date shall be dealt with
in accordance with the provisions for changes. Any work commenced and any payments
made pursuant to an Award or Letter of Intent shall be deemed to have been done and paid
after the Effective Date and under the terms of this Subcontract.
IN WITNESS WHEREOF, the parties hereto have executed this Subcontract, effective the
day and year first above written.
______________ METCALF & EDDY, INC.
By: By:_____________________
(Signature) (Signature)
(Printed or Typed Name) (Printed or Typed Name)
Title:______________________________________ Title:.
Date: ____________________________________ Date:
4 of 4
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PROPOSAL/BID FORM
iboratory Analytical Services
P No. 93-004609—092
Company Name:
Date:
Volatile Organic Compound (VOCs)
in ambient air — TO—14
Low Level PesticidefPCB’s
Total Organic Carbon (FCC)
Grain Size Distribution
sample
sample
sample
sample
sample
sample
sample
sample
sample
sample
sample
sample
sample
60
TOTAL BID PRICE ‘ S S S
20
72
72
72
72
72
72
72
72
72
6
15
D i Combustible Organics (TCO)
sample
5
Item
‘
‘
Unit
•Es ffl ated
Quantity
Unit
S
Cost
‘ Extended
Compound
m
(VOCs)
ethod 524.2
sample
20
Water Quality Parameters:
A1k2 tin ity
Chloride
Chemical Oxygen Demand (COD)
Nitrate/Nitrite-N
Phosphorous
Sulfate
Total Dissolved Solids (TDS)
Total Organic Carbon (FCC)
Total Suspended Solids (FSS)
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EXHIBIT A
-SCOPE AND SCHEDULE OF
LABORATORY SERVICES
1.0 SCOPE OF WORK
1.1 Except as otherwise expressly provided herein, Subcontractor shall provide
each and every item of expense necessary for providing analytical services in
support of EPA Region 1 DAS Program, hereinafter referred to as the Work.
1.2 Scope of Work
The Scope of Work shall include, but shall not necessarily be limited to,
providing analytical services for aqueous, soil, and environmental air samples
originating from Superfund (CERCLA NPL) sites. Data derived from all
analyses must be produced in order to satisfy EPA Data Quality Objective
Level IV, and be suitable for use in a court of law. Additionally, all data must
be suitable for use in ecological and human health risk assessments. All
analyses must be performed using the prescribed methodologies and must
include the quality control protocols and quality control samples required
herein. Laboratories must be capable of meeting the required detection limits,
and prove such limits with a recent method detection limit (MDL) study as
indicated.
1.3 The Work shall be performed in strict accordance with the following
specifications, and other attachments hereto, which are specifically
incorporated herein and made a part hereof:
1.3.1 Attachment A - Volatile Organic Compounds (VOCs) in drinking
water, EPA method 524.2
1.3.2 Attachment B - Volatile Organic Compounds (VOCs) in ambient air
using SUMMA passivated canister sampling, TO-14
1.3.3 Attachment C - Low Level Pesticide and PCB’s in surface water
1.3.4 Attachment D - Total Organic Carbon (TOC), Total Combustible
Organics (TCO), and Grain Size Distribution
1.3.5 Attachment E - Water Quality Parameters: Alkalinity, Chloride, COD,
Nitrate/Nitrite-N, Phosphorous, Sulfate, Total Dissolved Solids, Total
Suspended Solids, and Total Organic Carbon (TOC)
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1.4 No performance of service is authorized hereby.
1.5 The performance of specific services is authorized by the issuance to the
subcontractor of a written work order (“Work Order”) in the format of
Attachment 1.
Subcontractor shall perform services only pursuant to the receipt of a written
work order, specifying the task(s) to be performed, the schedule for
performance of each task, and the maximum funding authorized. The
subcontractor will sign each Work Order signifying its acceptance thereof and
agreement therewith.
1.6 Subcontractor shall not perform services which would result in the total
maximum funding authorized by each Work Order being exceeded.
2.0 PERIOD OF PERFORMANCE
2.1 The period of performance hereof is six (6) months commencing September
01, 1993 and ending February 28, 1994.
Sample specific schedule and data delivery requirements are addressed in
Attachment F.
2.2 M&E shall have the option of extending the period of performance hereof by
twelve (12) months at the unit prices set forth in Exhibit B. This option may
be exercised by M&E providing the Subcontractor written notice within ninety
(90) days prior to the end of the original term of this Subcontract.
2.3 Time is of the essence in the performance of this Work. Subcontractor shall
make whatever adjustments in working hours, manpower, equipment, etc.
deemed necessary to complete the work in accordance with the Subcontract
period of performance and the specific schedule requirements thereof.
3.0 REPORT AND DATA REQUIPEMENTS
3.1 All reporting and data requirements are detailed in Attachments A, B, C, D,
andE.
3.2 All data must conform to EPA Data Quality Objective Level IV (CLP).
3.3 All data must be suitable for use in ecological and human health risk
assessments, as well as for use in a court of law.
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4.0 M&E FURNISHED ITEMS
4.1 M&E will furnish Subcontractor with all samples to be analyzed. Saturday
delivery of samples will be required if necessitated by the sampling schedule.
4.2 Performance Evaluation (PE) samples will be provided to the Subcontractor
for those analytical methods specifying this requirement in the prescribed
methodology.
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EXHIBiT B
PAYMENT SCHIDULE
çv
1.0 SUBCONTRACT PRICE
1.1 M&E shall pay Subcontractor, on a unit price basis, foi complete, satisfactory
and timely performance of the Work in strict accordance with the requirements
hereof, the foUowing firm-fixed unit prices, which include all applicable taxes
and which are not subject to escalation:
Item
Unit
Estimated
Quantity
Unit Cost
Extended
Cost
Volatile Organics (VOC) Sample 20 $ $
EPA Method 524.2
Volatile Organics (VOC) Sample 6 $ $
Method TO-14
Pesticides/PCBs Sample 60 S $
Total Organic Carbon Sample 15 $ $
(TOC)
Total Combustible Sample 5 $ $
Organics (TCO)
Grain Size Sample 20 $ $
Water Quality:
Ailcalinity Sample 72 $ $
Chloride Sample 72 S $
Chemical 02 Demand Sample 72 $ $
Nitrate/Nitrite-N Sample 72 $ $
Phosphorous Sample 72 $ $
Sulfate Sample 72 $ $
Total Dissolved Solids Sample 72 $ $
( DS)
Total Suspended Solids Sample 72 $ $
(TSS)
Total Organic Carbon Sample 72 $ $
(TOC)
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1.2 In the event that the actuai quantity of any unit-priced item varies from the
estimated quantity more than twenty-five percent (25%), the unit price of such
items shall equitably adjusted, upon demand of other party. The equitable
adjustment shall be based upon any increase or decrease in costs due solely to
the variation above one hundred twenty-five percent (125 %) or below
seventy-five percent (75%) of the estimated quantity.
1.3 The total funding hereof is limited to $
When the total expended amount reaches seventy-five percent (75%) of the
total funding limitation, Subcontractor shall immediately notify M&E who,
may, at M&E’s option, provide additional funding.
In no event shall Subcontractor perform services which would result in billings
in excess of the total funding limitation.
The Subcontractor may exceed any individual funding limitation set forth in
Section 1.1, however, Subcontractor shall not perform services which would
result in billings in excess of the total funding limitation set forth in this
Section 1.3.
1.4 The funding limitation set forth herein shall not be considered to be an
obligated commitment by M&.E who shall be liable only to the extent of the
work actually performed.
1.5 The unit prices set forth in Section 1.1 include all of Subcontractor’s costs not
specifically identified.
2.0 METROj) OF MEAStjR 1 ’j’
2.1 The following subsections describe the measurement of and payment for the
work to be done under the items listed in Section 1.1.
Each unit or lump sum price stated in the Section 1.1 shall constitute full
compensation as herein specified for each item of work completed in
accordance with the work described in Exhibit A, Scope of Work, including
all services, labor, equipment use, materials and supplies. No other payments
for any specified or indicated work nor any work implied therefrom shall be
made.
The quantities stated in the Section 1.1 are approximate only and are for the
specific purpose of comparing bids. The Engineer does not gualantee that
these items or quantities will be performed. Metcalf & Eddy reserves the right
to vaiy the quantities or delete items in their entirety, and the Contractor will
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EXHIBIT A
ATFACHMENT E
ANALYTICAL SPECIFICATION
FOR
ALKALiNITY, CHLORIDE, CHLM1CAL OXYGEN DEMAND,
NITRATE/NITRITE-N, PHOSPHOROUS, SULFATE, TOTAL DISSOL VEX)
SOLIDS, TOTAL SUSPENDED SOLIDS, AND TOTAL ORGANIC CARBON
IN AQUEOUS SAMPLES
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SCOPE
Anaiysis of aqueous samples for Alkalinity, Chloride, Chemical Oxygen Demand
(COD), Nitrate/Nitrite-N, Phosphorus, Sulfate, Total Dissolved Solids (TDS), Total
Suspended Solids (TSS), and Total Organic Carbon (TOC) by EPA Methods for
Chemical Analysis of Water and Wastes.
The laboratory must meet the required detection limits and prove those detection
limits with a recent MDL study.
2. PURPOSE
The data obtained from samples will be used to further delineate contamination and to
determine the treatability of the contaminated water.
3. DEFINITION OF WORK
Surface water samples are to 1)e analyzed for the above referenced water quality
parameters. Additionally, i.nfiuent and effluent samples from treatability/piot studies
will also require the above analyses.
4. SCHEIT)ULE
Samples will be shipped daily as collected. Saturday delivery will be required.
Overnight delivery service will be used. Contacts for shipping and data delivery
inquiries are specified in Exhibit A, Attachment F.
Holding Time:
Sample analysis must be within holding times stated in Section 6 of this
specification.
Delivery of Data:
Sample data must be delivered to M&E within thirty-five (35) days of
laboratory receipt of the last sample in each sample delivery group of twenty
(20) samples or less.
5. ANALYTICAL REFERENCES
The laboratory is required to use EPA methods for Chemical Analysis of Water and
Wastes; EPA-6(J014-79-020 with updates to Rev. 3-83. Alkalinity - Method 310.1;
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Chloride - Method 325.3; Chemical Oxygen Demand (COD) - Method 410.1;
Nitrate/Nitrate-N - Method 353.1; Phosphorus - Method 365.4; Sulfate - Method
375.4; Total Dissolved Solids (TDS) - Method 160.1; Total Suspended Solids (TSS) -
Method 160.2; and Total Organic Carbon (TOC) - Method 415.2.
6. SAMPLE PRESERVATION AND DETECTION LIMITS
Parameter
Method’
Reporting Limit
(mgIl
Holdinfi
Time 4
Preservation
Alkalinity
310.1 - Tit.rimetric
2.0
14 days
Cool 4°C
Chloride
325.3 - Titrimetric
2.0
28 days
Cool 4°C
COD
410.1 - Titrinietric
50
28 days
Cool 4°C,
H 2 S0 4 ph<2
Nitrate!
Nitrite-N
353.1 - Colormetric,
Automated, Hydrazine
Reduction
0.1
28 days
Cool 4°C,
H SO 4 ph <2
Phosphorus
365.4 - Colorimetric
0.1
28 days
Cool 4°C,
H 2 SO ph<2
Sulfate
375.4 - Turbidimetric
2.0
28 days
Cool 4°C
TDS
160.1 - Gravimetric
10.0
7 days
Cool 4°C
TSS
160.2 - Gravimetsic
4.0
7 days
Cool 4°C
TOC -
low level
415.2 - UV Promoted,
Persulfate Oxidation
0.1
28 days
Cool 4°C,
H 2 S0 4 ph <2
From EPA Method for Chemical Analysis of Water and Wastes; EPA-600/4-79-020
with updates to Rev. 3-83.
2. Holding time is defined as the time between sample collection and sample
preparation/analysis.
7. ANALYTiCAL PROCEDURES
a. Alkalinity - Method 310.1 (Titrimetric)
1. Analysis for ailcalinity must begin as soon as possible since atmospheric
caibon dioxide can affect the results. If portions from the same sample
container are to be analyzed for other parameters, complete the pH and
alkalinity analyses first.
2. Appropriate aliquots should be used to avoid a titration volume greater
than 50 mIs.
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3. Follow Section 4.1 for pH specifications. At least two different pH
solutions must be utilized for standardizatiOn. The solutions must
bracket the expected pH of the samples. Repeat adjustments of
successive portions of the two buffer solutions until readings are within
0.05 pH units of the buffer solution value. A separate source pH check
standard must then be analyzed to verify the calibration. In the event
that the pH meter is not equipped with temperature compensation, all
calibration solutions and standards must be read at the same
temperature. All standardized procedures must be documented in a
laboratory notebook and provided with the final data package.
4. A normality check of the titrant must be performed prior to sample
analysis. If the concentration is within 10% of that initially
determined, the newLy determined value must be used in the
calculations. If it is not within 10%, a fresh titrant must be prepared.
The normality of the fresh titrant must be within 20% of that specified
by the method.
5. Follow Section 6.1 for the preliminary titration of the sample to
determine the normality of the titrant to be used. Then follow
Section 6.2 for high alkalinity samples or Section 6.3 for low alkalinity
samples. The normality of the titrant used for each sample must be
documented in a laboratory notebook and included with the final
deliverables.
6. A method blank using laboratory pure water (deionized distilled) must
be performed using all reagents. The method blank should be run in
conjunction with the standardization and before every twenty
(20) analytical samples. The method blank must not have more than
half the reporting limit of the method or the source of water must. be
changed to a cleaner source and all samples relating to that blank must
be reanalyzed.
7. One sample in twenty (20) field samples must be performed in duplicate
and the percent difference between results must be less than 20% D. If
the result is greater than 20% D, then the analysis of both samples must
be repeated. If the results are still >20% D, flag the results with
8. Initially, an EPA check standard must be analyzed 3 consecutive times
with each analytical batch (twenty (20) samples or less), prior to blank
and sample analysis. All three (3) analyses must be reported in the
deliverable package. The final or third analysis must meet recovery
criteria. The EPA check standard must also be analyzed one (1) per
ten (10) field samples and at the end of the analytical sequence. If a
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check sample is not available, a 2.0 mg/L CaCO 3 standard, which is
from a source independent of that used to check the normality of the
titrant, may be used. Results must agree within 15% of the true value.
If the recovery criteria are not met, a normality check must be
performed 1 and another EPA check standard, method blank and all
associated fIeld samples analyzed. Criteria must be met prior to sample
analysis.
b. Chloride - Method 32.5.3 (Titrizn€triC)
A sample aliquot must not contain more than 20 mg CI per 50 ml in
order to avoid using a large titration volume.
2. FoUow the procedure exactly as described in Section 6 of the method
with the following exceptions: If the sample contains less than
0.1 mg/I, then there is no need to concentrate. If the sample aliquot
contains less than 2.5 mg of chloride, then another aL4uot must be
analyzed using 0.0141N mercuric nitrate titrant in step 6.6. Record the
normality of he titrant used in a laboratory notebook and include with
the final deliverables. If the end point of the titration is difficult to
detect, Section 6.7 of the method must be completed and reported with
the sample results.
3. Four practice runs must be made before field sample analysis begins.
They must be clearly documented in the laboratory notebook and
provided with the final deliverables.
4. Initially, an EPA check standard must be analyzed three (3) consecutive
times with each analytical batch (twenty (20) samples or less), prior to
blank and sample analysis. All three (3) analyses must be reported in
the deliverable package. The final or third analysis must meet recovery
criteria. The EPA check standard must also be analyzed one (1) per
ten (10) field samples and at the end of the analytical sequence. If a
check sample is not available, a 2.0 mgfL standard, which is from a
source independent of that used to check the normality of the titrant,
may be used. Results must agree within 15% of the true value. If the
recovery criteria are not wet, a normality check must be perfonned,
and another EPA check standard, method blank and all associated field
samples analyzed. .Ciiteria must be met prior to sample analysis.
5. A normality check of the titrant must be performed prior to sample
analysis. If the concentratiOn is within 10% of that initially
determined, the newly determined value must be used in the
calculations. If it is not within 10%, a fresh titrant must be prepared.
4
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The normality of the fresh titrant must be within 20% of that specified
by the method.
6. A method blank using laboratory pure water (deionized distilled) must
be performed using all reagents. The method blank should be nm in
conjunction with the standardization and before every twenty
(20) analytical samples. The method blank must not have more than
half the reporting limit of the method or the source of water must be
changed to a cleaner source and all samples relating to that blank must
be reanalyzed.
7. One (1) sample in twenty (20) field samples must be performed in
duplicate and the percent difference between results must be less than
20% D. If the result is greater than 20% D then the analysis of both
samples must be repeated. lithe results are still >20% D, flag the
results with N$U•
8. A matrix spike must be performed at a frequency of one (1) in twenty
(20) samples. The sample must be fortified at a concentration of
10 mg/L and the recovery must be within 80-120%. lIthe spike is
outside the limits, repeat the analysis. If the results are still outside the
limits, flag the results with a
c. Chemical Oxygen Demand (COD) - Method 410.1 (Titrinietic)
1. Follow the procedure for sample analysis outlined in Section 7.0 of the
method. Since the samples may contain volatile organic compounds,
use an AllThn Condenser and add the sulfuric acid-silver sulfate solution
(as described in Section 7.1.1 of the method) to avoid volatilization.
2. A normality check of the titrant must be performed prior to sample
analysis. If the concentration is within 10% of that initially
determined, the newly determined value must be used in the
calculations. If it is not within 10%, a fresh titrant must be prepared.
The normality of the fresh titrant must be within 20% of that specified
by the method.
3. For every batch of twenty (20) samples or less, a distilled water method
blank must be refluxed. The method blank must be analyzed at the
beginning of the analytical sequence, following the analysis of the
calibration curve and the check standard, but prior to the analysis of
any samples. If contamination is present at concentrations exceeding ½
reporting limit (RL), redigest a new blank, A check standard and all
associated field samples. Criteria must be met prior to sample analysis.
5
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4. An EPA check sample must be analyzed (carried though the entire
analytical procedure) with each group of samples refluxed. If
unavailable, a mid-range potassium acid phthalate standard may be
used. Results must agree ±15 % of the true value. If the results do not
agree within 15%, a new normality check must be performed and the
source of the problem must be identified and corrected prior to sample
J)’ is. All associated samples must be reanalyzed (including the
reflux step) and a new EPA check standard must be analyzed. Steps
taken to identify and remedy the problem must be recorded in a
laboratory notebook and included in the final data package.
5. An EPA check sample which is not refluxed must be analyzed three (3)
consecutive times prior to sample analysis. All three analyses must be
reported in the deliverable package. The final or third analysis must
meet recovery criteria. If unavailable, a mid-range potassium acid
phthalate standard may be used. The EPA check standard or standard
must also be analyzed one (1) per ten (10) samples and at the end of the
analytical sequence. Results must agree within ±15% of the true
value. If the results do not agree within 15%, a new normality check
must be performed and the source of the problem must be identified
and corrected prior to sample analysis. Steps taken to identify and
remedy the problem must be recorded in a laboratory notebook and
included in the final data package.
6. A method blank using laboratory pure water (deionized distilled) must
be performed using all reagents. The method blank should be run in
conjunction with the standardization and before every twenty
(20) analytical samples. The method blank must not have more than
half the reporting limit of the method or the source of water must be
changed to a cleaner source and all samples relating to that blank must
be reanalyzed.
7. One (1) sample in twenty (20) field samples must be performed in
duplicate and the percent difference between results must be less than
20% 1). If the result is greater than 20% 1), then the analysis of both
samples must be repeated. If the results are still >20% D, flag the
results with .
d. Nitrate/Nitrite-Nitrogen - Method 353.1 (Colormetric, Automated,
Hydrazine Reduction)
Check the pH of the sample upon receipt. If the pH is greater than 1,
document the pH in the narrative.
6
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2. During the comparison of NO 3 vs. NO 2 standards, (Method 353.1,
Section 7.3), if the reduction efficiency is not 100%, adjust the
concentration of the hydrazine sulfate solution appropriately and repeat
the check for reduction efficiency. Reduction efficiency must be 100%
prior to sample analysis. Document the results in a laboratory
notebook for inclusion with the final deliverables.
3. An EPA check standard must be analyzed after the calibration standards
and blank but before samples are processed as well as after every ten
(10) samples and at the end of the analytical sequence. If an EPA
check standard is not available, a 0.1 mg/L standard from a source
independent of the calibration standards may be used. Results must
agree within 15% of the true value. If the criteria are not met, a fresh
standard curve must be prepared and all samples analyzed since the
previous acceptable check standard must be reanalyzed.
4. A calibration curve must be generated each day that samples are
analyzed. The curve must consist of a blank and five (5) standards.
The concentration of the lowest standard must be equal to the reporting
limit and the range of the standards must bracket the concentration of
the samples. The correlation coefficient must be greater than 0.995.
Calibration criteria must be met prior many samples being analyzed.
5. A matrix spike must be performed at a frequency of one (1) per twenty
(20) samples. The sample must be fortified at a concentration of
0.5 mg!L and the recovery must be within 80-120%. If the spike is
outside the limits, repeat the analysis. If the results are still outside the
limits, flag the results with a ‘# .
6. A method blank using laboratory pure water (deionized distilled) must
be performed using all reagents. The method blank should be run in
conjunction with the standardization and before every twenty
(20) analytical samples. The method blank must not have more than
half the reporting limit of the method or the source of water must be
changed to a cleaner source and all samples relating to that blank must
be reanalyzed.
7. One sample in twenty (20) field samples must be performed in duplicate
and the percent difference between results must be less than 20% D. If
the result is greater than 20% D then the analysis of both samples must
be repeated. If the results are still >20% D, flag the results with .
e. Phosphorus - Method 365.4 (Colorimetric)
7
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Any &psswaj’e used must be acid washed in hct 1:1 HCI and rinsed
with distilled water (Method 365.3, Section 6.2). This should be
foliowed for any glass ware used in the analysis, including that used for
the preparation of associated reagents.
2. A 5-point calibration curve must be generated daily, prior to sample
analysis. The lowest standard must be at the reporting limit and the
range of the calibration must bracket the concentration of the samples.
The calibration coefficient must be greater than 0.995. If the criteria
are not met, fresh standards must be prepared and a new standard curve
generated. Samples may not be analyzed until the criteria are met. If a
sample result falls outside the calibration range, either dilute the sample
or recalibrate using standards to span the desired range.
3. An EPA check standard, which is digested with the samples, must be
analyzed prior to the samples, every ten (10) samples and at the end of
the analytical sequence. If one is unavailable, a 0.1 mg PIL standard
from a source independent from that of the calibration standa.rds may be
used. The results must be within 15% of the true value. If the results
do not agree, a new standard curve must be generated and all associated
QC samples and field samples must be redigested and reanalyzed.
Limits must be met prior to sample analysis. Report the source of the
check standard in the final deliverables.
4. An EPA check sample which is not digested must be analyzed three (3)
consecutive times prior to sample analysis. All three (3) analyses must
be reported in the deliverable package. The final or third analysis must
meet recovery criteria. If unavailable, a mid-range standard from a
different source must be used. The EPA check standard or standard
must also be analyzed one (1) per ten (10) samples and ax the end of the
analytical sequence. Results must agree within ±15% of the true
value. If the result do not agree within 15%, a new normality check
must be performed and the source of the problem must be identified
and corrected prior to sample analysis. Steps taken to remedy the
problem must be reported in a laboratory notebook and included in the
data package.
5. For every batch of twenty (20) samples or less, a distilled water method
blank must be digested. The method blank must be analyzed at the
beginning of the anaiytical sequence, following the analysis of the
calibration curve and the check standard, but prior to the analysis of
any samples. If contamination is present at concentrations exceeding ½
RL, redigest a new blank, EPA check standard and all associated field
samples. Criteria must be met prior to sample analysis.
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6. A matrix spike must be performed at a frequency of one (1) per twenty
(20) field samples. Spike a sample prior to digestion at a concentration
equal to the mid point of the calibration curve. Recovery must be
within 80-120%. If limits are not met, redigest and reanalyze the
spiked sample. If the results are still out, flag the results with a “#“.
7. One (I) sample per twenty (20) field samples must be performed in
duplicate and the percent difference between results must be less than
20% D. If the result if greater than 20% D, then the analysis of both
samples must be repeated. If the results were >20%, flag the results
with
f. Sulfate - Method 375.4 (TurbidimetriC)
1. The sample aliquot must not contain more than 40 mg SO 4 IL.
2. Suspended matter and color will interfere. Correct by analyzing blanks
from which the barium chloride has been omitted as per Sections 2.2
and 6.4 of the method.
3. A normality check of the standard acid must be performed prior to
sample analysis. If the concentration is within 10% of that initially
determined, the newly determined value must be used in the
calculations. If it is not within 10%, a fresh solution must be prepared.
The normality of the fresh solution must be within 20% of that
specified by the method.
4. Record all readings, at thirty (30) second intervals during the four (4)
minute period, in a laboratory notebook and provide with a final
deliverables.
5. A five-point calibration cure must be generated on any day during
which samples arc to be analyzed. The lowest standard must be equal
to the reporting limit and the range of the standards must bracket the
concenirations of the samples. A blank must also be included in the
curve. The correlation coefficient must be >0.995.
6. A method blank using laboratory pure water must be performed using
all reagents. The method blank should be nm in conjunction with the
standardization and before every twenty (20) analytical samples. The
method blank must not have more than the reporting limit of the
method or the source of laboratory pure water must be changed.
9
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7. A mid-range continuing calibration check standard from a different
source must be analyzed prior to sample analysis, after every four (4)
samples and at (he end of the analytical sequence. The results must be
± 10% of the true value. If the limits are not met, reanalyze the
calibration curve, the continuing calibration check and any samples
analyzed since the last acceptable continuing calibration standard before
proceeding.
8. A duplicate sample must be analyzed of one (1) per twenty (20) field
samples. The percent difference must be less than 20%. Unacceptable
duplicate samples are to be reanalyzed. If the reanalysis is still
unacceptable, report both sample results and flag with an asterisk .
9. A matrix spike must be performed at a frequency of one (1) per twenty
(20) field samples. Spike a sample at a concentration equal to the
midpoint of the calibration curve. The recovery must be within ±20%.
Unacceptable spike samples will be reanalyzed. If the reanalysis is still
unacceptable, flag the results with a
g. Total Dissolved Solids - Methods 160.1 (GraviinetriC)
I. The samples must be run as soon as possible so the analysis can be
completed with the required seven (7) day holding time (in the event
that the check standard is outside acceptable limits and all associated
samples must be reanalyzed).
2. The analytical balance utilized for measurements must be checked
before each batch (twenty (20) samples or less) of weight values
obtained, using class “S weights. The results must be recorded in a
log book an supplied in the final deliverable package. The check
weight must be within the manufacturer’s tolerance range or the balance
must be recalibrated.
3. Glass fiber filters must be prepared according to Section 7.1 of the
Method. The procedure must be documented in a laboratory notebook
and must be provided with the final deliverables. The manufacturer
and model of the filters must also be recorded and supplied with the
deliverables.
4. The evaporating dishes must be prepared according to Section 7.2 of
the Method. The procedure must be documented on a laboratory
notebook and provided with the final deliverables.
10
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5. Record the temperature of the drying ovens twice daily and provide the
documentation with the final deliverables.
6. A method blank using deionized water must be prepared and analyzed
for each type of filter used and for each group of twenty (20) samples
or less prepared at the same time. Any concentrations of interference
detected must be less than ½ reporting. If the criteria are not met then
the samples, EPA check standard and another blank must be reprepared
and weighed. The results must be document in the final data
package.
7. An EPA check standard at 10 mgfL must be prepared and analyzed
with each batch of samples and per filter type. The results of the
analysis must be within ± 15% TV. If the results are not within ±
15%, then the procedure must be repeated for .ethod blank, EPA
check standard and all field samples.
h. Total Suspended Solids - Method 160.2 (Gravimetric)
1. The samples must be run as soon as possible so the analysis can be
completed with the required seven (7) thy holding time (in the event
that the check standard is outside acceptable limits and all associated
samples must be reanalyzed).
2. The analytical balance utilized for measurements must be checked
before each batch (twenty (20) samples or less) of weight values
obtained, using class ‘S” weights. The results must be recorded in a
log book and supplied in the final deliverable package. The check
weight must be within the manufacturer’s tolerance range or the balance
must be recalibrated.
3. Glass fiber filters must be prepared according to Section 7.1 of the
Method. The procedure must be documented in a laboratory notebook
and must be provided with the final deliverables. The manufacturer
and model of the filters must also be recorded and supplied with the
deliverables.
4. Section 7.2 of the Method must be adhered to for sample volume
determination.
5. Record the temperatures of the drying oven twice daily and provide the
documentation with the final deliverables.
11
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6. A method blank using deionized water must be prepared and analyzed
for each type of filter used and for each group of twenty (20) samples
or less prepared at the same time. Any concentration of interference
detected must be less than 1 /i reporting. If the criteria are not met, then
the samples, EPA check standard and another blank must be reprepared
and weighed. The results must be documented in the final data
package.
7. An EPA check standard at 4 mgIL must be prepared and analyzed with
each batch of samples and per filier type. The results of the analysis
must be within ±15% TV. If the results are not within ± 15%, then
the procedure must be repeated for the method blank, EPA check
standard, and all associated field samples. Criteria must be met prior
to sample analysis.
Total Organic Carbon - Method 415.2
All samples must be analyzed in duplicate and both analyses must be
reported. The %D must be no greater than 20%.
2. Follow the manufacturer’s instruct ions to set up the instrument.
Perform the system clean-up and calibration procedure each day before
analyzing any samples, Section 8.2 of the Method.
3. The analysis procedure is provided in Section 8.0 of Method 415.2.
Check the effectiveness of the CO 2 scrubber as described in
Section 8.3. The results must be recorded and provided in the final
data package.
4. A system blank as specified in Section 8.2 and defined in Section 3.4 of
the Method must be performed as part of the initial instrument set up
procedure. The system blank must be analyzed until two consecutive
readings within 10% of each other are obtained. If limit is exceeded
identify the problem, make appropriate corrections and reanalyze the
system blank. Criteria must be met prior to sample analysis.
5. A method blank must be analyzed after calibration of the instrument
and before samples are run. The method blank must not contain
concentrations of TQC exceeding ½ RL. The water used for the
method blank must be the same as what was used for the calibration
standards. If concentrations of TOC are present greater than ½ RL a
new source of water which meets criteria must be used.
12
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6. Calibrate the instrument according to Section 8.5 of the Method. A
blank and five standards at 0.1, 0.2, 0.5, 1.0 and 2.0 ppm must be
analyzed. A correlation coefficient equal to 0.995 or better must be
obtained prior to sample analysis. AU sample results must be within
the calibration curve.
7. An EPA check standard or a 100 ugh QC check standard from a source
other than the calibration standards, must be analyzed prior to sample
analysis, after every 10 analyses and at the end of the analytical
sequence. The recovery must be within 85% - 115%, if not, the
instrument must be recalibrated and all associated analyses must be
reanalyzed.
13
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Limits
Corrective Action
EPA Check
Standard
FreouencY
Duly prior to
sample analysis
1/20 samples or less
prepared at one time
and for each type of
filter used.
1/batch prior to
sample analysis and
per filter type used
1120 field samples
Within the
manufacturer ’s
tolerance range
. 1/2 Reporting
Limit (Rl )
± 15% True Value
The balance must be
recalibrated by the
manufacturer
If> 1/2RL the
samples, EPA check std
and another blank must
be repreparod.
If outside the limits, re-
filter another method
blank, EPA check
standard and all
associated field samples.
If outside the limits,
repeat the analysis of
both the sample and the
duplicate. If still outside
the limits, flag the results
with an
f. Total Organic Carbon, (TOC) Method 415.2
Calibration
EPA Check
Standard
Fru uency
Daily prior to
sample analysis
1/20 samples or less
analyzed at one
time. Prior to
sample analysis.
Daily prior to
sample analysis
lThatch prior to
sample analysis,
after every ten
samples and as the
final analysis per
each day of analysis
Limits
Two readings within
10% of each other
and the last
instrument system
blank
. 1/2 Reporting
Limit (RI)
Correlation
Coefficient .. 0.995
± 15% True Value
( IV )
Corrective Action
If criteria are not met
identify the problem and
make appropriate
corrections. Criteria
must be met prior to
sample analysis.
If> 1/2 RI, the
samples, EPA check s4
and another blank must
be reanalyzed. Criteria
must be met prior to
sample analysis.
Criteria must be met
prior to sample analysis
If outside the limits,
recalibrate the insui mcnt
and reanalyze a check
standard before any field
samples are analyzed or
reanalyze *11 associated
field samples if
applicable.
Audits
AnaJytical
Balance Check
Method Blank
Duplicate
%D < 20%
Audits
System Blank
Method Blank
18
-------
Duplicate All samples %D <20% If outside the limits.
reacalyze the sample and
the duplicate. If still
outside the limits, flag the
results with an.
9. ANALYTICAL DELIVERABLES
a. The foliowing requirementS for all analytes must be delivered with each
package of data. Data packages must be delivered to M&E under custody
seal.
• A recent (within six (6) months) MDL study must be delivered with the
package. The results of the MDL study must meet the reporting limits
detailed in Section 8. The MDL study must have been run as described
in 40 CFR Part 136 App. B, Section 10.3.
• A narrative which must include an explanation of all anomalies and
corrective actions performed 1 and a tabulation of the M&E sample
numbers with the corresponding laboratory sample numbers.
• Tabulate all positive results and the reporting limit for non-detected
results. The reporting limits are listed in Section 8.
• Raw data for all field samples, QC samples and calibration standards
must be provided. The raw data must include all bench sheets,
preparation logs, analysis logbooks and all instrument strip charts and
printouts.
• Tabulated duplicate results (%D) and matrix spike analyses
(%Recovery), tabulation of QC check standards (%Recovery), EPA
check sample results (%Recovery), calibration verification results,
normality check results, nitrate reduction results, and blank results.
The true value and the actual concentration of spikes must be provided
19
-------
with the percent recovery tabulation. Raw data, which is specified
above, must be provided.
• The calibration curve raw data with print-outs and concentrations must
be provided. Plot the standard curves and include the linear regression
equation.
• Example calculations which descriptively define how sample results
were generated for each analysis must be provided. All equations,
dilution factors, and information required to reproduce the laboratory
results must be provided.
• Original signed chain-of-custody forms, sample tags, and shipping air
bills. Copies of the laboratory’s telephone logs from any conversation
with M&E samplers or project personnel. A copy of this analytical
specification (complete).
• All log-in sheets and records of the cooler temperature and sample
preservation checks on samples upon arrival at the laboratory.
• Data package must be paginated and of good copy quality.
• The data package must be as much lice EPA CLP package as possible.
b. Complete sample delivery group file (CSF)
Due to the litigative nature of each Supexfund site, Region I EPA requires that
all analytical data, tabulated raw or supporting data be delivered with each
sample delivery group (data package). Accompanying each SDG must be a
Completeness Evidence Audit carried out by the laboratory. The CSF
Completeness Evidence Audit Forms are included in Attachment E. 1 and must
accompany each data package. The laboratory through these audit forms must
demonstrate that each piece of sample data, raw data, calibration data, and QC
data and any other requirement of the analytical specification is included in the
data package.
The forms included in Attachment E. 1 are for all types of data and data
packages. For this specification the laboratory will use the forms supplied to
the best of their ability where deliverable items are applicable.
10. EXCEYFIONS
If QC requirements or action limits are exceeded; or if analytical samples are
destroyed or lost; or if matrix interference is suspected, contact:
20
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A.F. Beliveau
Metcalf & Eddy
(617) 246-5200 ext. 4433
21
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LOW CONCENTRATION VATER FOR ORCANICS COMPLETE SOC FILE (CS7) INVENTORY SHEET (Cent.)
1cff . __
PAGE NOs CHECX
FRO ( TO LAB EPA
mj’vojitLles Deti (cont.)
b. Sample Data
TCL Results (Form I LCSV)
Tentatively Identified CompOUl1dS (Form I LCSV.TIC)
Reconstructed total ion roaatogr .5 (RIC)
and Qu.antitaciOn Reports for each sample
For each sample:
Raw spectra and backgroUfld3 t cted
mass spectra of TCL compounds
Mass spectra of TICs with three best library matches
GPC chroaatograms (if CPC performed)
c. Standards Data ‘(All Instruments) ______
tniti l Calibration Su*ry (Form VI LCSV)
RICa and Quan Reports for all Standards
Continuing Calibration (Form VII LCSV)
RICa and Qua.n Reports for all Standards
Internal Standard Area and ET
(Form VIII LCSV)
d. QC Data
DF PP
Blank Data
LCS Data
PES Data
a. QC SttT E7 ______
Su.rrcate Percent Recovery 5 aL7 (Form II LCP)
Lab Control Sample Recovery (Form III LCP)
Method Blank Siiii ry (Form I V LCP)
b. Sample Data
ICL Results Organic Analysis Data Sheet
(Form I LCP)
Chromatograil (Primary C.oh n)
Chromatograms frog second GC column confirmatiofl
GC Integration report or data syste3 printout and
calibration plots
Manual work sheeti
For pesticides/ArOCl0rZ confirmed by GC/MS. copies
of raw spectra and copies of backgrOu d_subtracted mass
spectra of target compounds (samples & standards)
FORM DC-2-2
10/9
-------
NCEWrRATION v i FOR ORCANICS COKPTITE SDG Fill (CS?) INVE NTOLT SHZE (Cont. )
CASE NO. _________ wc wo. _________ SOC $01. TO F .L J ________ _________ ________ US NO.
PACE NOa C}iECX
FROM TO TAB EPA
e,ticides (cont.)
Standards Data
Initial Calibration Data (For2 VI LCP)
Calibration Verification (Form VII LCP)
Pesticides Analytical Sequence (Yor VIII,
LCP-l and -2)
PesticideFlorisil Cartridge Check (Form IX . LCP) ________
Pesticide Identification (Form X LCP)
Star.d .ard chro atogram.i and data system printout
for all Standards
For pesticides/Aroclors confirmed by CC/MS, copies
of spectra for standards used
QC Data
Blank Data
LCS Data
PES Data
llaneois Deta
Original preparation and analysis forms or copies of
preparation and analysis logbook pages
Internal sample and sample extract transfer
chain-of-custody records
Screening records
All ins crt ene output, including strip charts
from screening activities (describe or list)
t A Thi vtn tReceivina Doc nt3
Airb ills (No. of shipments _)
Chain-of-Custody Records
Sample Tags
Sample Log-In Sheet (Lab & DC1)
SDC Cover Sheet
Miscellaneous Shipping/Receiving Records
(describe or list)
- rnal Lob Sa le T*nsfer Records end Trsckth2 Shee 1
nbc or list)
TORN DC-2-3
-------
EXHIBiT A
ATTACHMENT B
ANALYTICAL
SPECIFICATION
FOR
EPA METHOD TO-14
-------
1. SCOPE
This specification is for the Volatile Organic Analysis of gases produced during soil
gas extraction using EPA Method TO-14. The volatile organic compounds listed in
Table 1 of the method, plus Trans 1 ,2-dichloroethene, dibromo chloromethane, and
bromodjchjoromethane are required by this specificanon. Tentatively identified
compounds (TICs) must be reported following the procedures in EPA SOW
OLMO1.8 Exhibit D-VOA Section IV paragraph 9.2 and 10.4.
This specification requires one (1) of the following proofs (detailed in Section 9.A) of
laboratory capability generated during the last six (6) months:
• Method detection limit (MDL) study conducted according to 40 CFR
136 Appendix B with practical quantitation limit (PQL) of O.5 ppbv
for each individual analyte.
• A laboratory fortified blank analysis containing all analytes listed in
Section 6 of a 0.5 ppbv standard with a recovery of 80 to 120 percent
of the true value.
• An initial calibration meeting the criteria presented in Section 7 h.
The compounds must be those in Attachment B. 1 of this specification.
In addition the laboratory must demonstrate their capability to perform the analysis by
analyzing an EPA performance evaluation (PE) sample supplied by M&E along with
the initial shipment of environmental samples.
2. PURPOSE
The TO-14 analysis will be used to measure a soil vapor extraction system’s
efficiency.
3. DEFINITION OF WORK
The laboratory will supply M&E with eight (8) cleaned (accompanied by certification
of cleanliness), evacuatecj canisters and flow controllers for all the environmental
samples. The laboratory is required to analyze two (2) performance evaluation
samples (two (2) of the eight (8) canisters) and generate proof of laboratory capability
in meeting a method detection limit of O.5 ppbv that was reported in accordance
with one of the three methods described in the scope.
1
-------
The performance evaluation (PE) canisters and flow controllers should be sent directly
to:
Andrew F. Beiveau
Metcalf & Eddy, Inc.
30 Harvard Mill Square
Wakefield, MA 01880
The laboratory will be required to supply six (6) air canisters (in two sampling rounds
of 3 canjsters each) cleaned, evacuated, and accompanied by certificates of cleanliness
for the environmental samples. The flow controllers must also be accompanied by
certificates of cleanliness. Four (4) canisters will be returned to the laboratory for
analysis of volatile organics. Two (2) canisters used for field calibration of the flow
meters, will also be returned to the laboratory; however, no analysis will be required
to be performed on these canisters. Sample canisters axe to be shipped as follows:
Meg Himmel
Metcalf & Eddy
30 Harvard Mill Square
Wakefield, MA 01880
Additional equipment needed to be supplied by the laboratory is detailed in Section 7.
Information pertinent to the canister and flow controller cleanliness certification is
detailed in the TO-14 method.
4. SCF1J DT1jLE
Samples will be shipped daily as collected. Saturday delivery will be require.
Overnight delivery service will be used. Contacts for shipping and data delivery
inquiries are specified in Exhibit A, Attachment F.
Holding time:
Samples must be analyzed within fourteen (14) days of sample receipt. PE
samples must be analyzed with seven (7) days of receipt.
Delivery of Data:
Sample data must be delivered to M&E within thirty five (35) days of
laboratory receipt of the last sample of each sample delivery group.
2
-------
Performance Evaluation (PE) Samples:
Results of the PE samples and the laboratory proof of meeting the reporting
limits must be received at M&E within seven (7) days after laboratory receipt
of the PE samples.
5. ANALYTICAL REFERENCE
Method TO-14 Determination of Volatile Organic Compounds (VOCs) in Ambient Air
using SUMMA Passivated Canister Sampling and Gas Chromatographic analysis in
Second Supplement to Compendium of Methods for the Determination of Toxic
Organic Compounds in Ambient Air EPA/600-4-89-018 June 1988.
6. SAMPLE PRESERVATION AND DETECTION LIMITS
Preservation:
None necessary
Detection Limits Required:
Parameter Method Detection Limit
Volatiles as per 0.5 ppbv
TO-14 (Table 1)
trans 1,2-dichloroethene 0.5 ppbv
Dibromochloromethane 0.5 ppbv
Bromodichloromethane 0.5 ppbv
7. ANALYTICAL PROCEDURE
A. Equipment to be supplied by the laboratory must include:
• Two (2) canisters and flow controllers for the PE samples; precleaned
and evacuated with certificates of cleanliness on both
• Six (6) canisters and flow controllers of each of two sampling rounds
for the analysis of samples; precleaned and evacuated with certificates
of cleanliness on all.
- Four (4) canisters for field samples
3
-------
- One (1) canister for calibration of flow controllers
- One (1) canister for trip blank, equipment blank
• Manometer for measuring the vacuum with each canister after sample
collection and at the time of receipt at the site
B. Equipment description:
• The canisters are 6-liter, StIMMA canisters as specified in Section
7.1.1.2 of Method TO-14. Canisters and flow controllers must be
precleaned and evacuated in accordance with Sections 11.2 and 12.5.1
of the method. A certificate of cleanliness and documentation of
performance of a leak check for each canister and flow contreller must
accompany the shipped canisters and must also be submitted with each
data package. Information pertinent to the canister cleanliness
certification is detailed in the method.
• Six (6) stainless-steel flow controllers (critical orifices) with particulate
matter filters as specified in Section 7.1.1.5 of Method .TQ-14 capable
of sustaining a flow rate of 16.7 mI/mm or llJhour for 4 hours. Flow
variability must be <2 % for a period up to 24 hours under conditions
of changing temperature (20-40°C) and humidity as specified in Section
7.1.1.4 of method TO-14. Porting should be 1/4w NFl ’.
C. The detector must be the GC-MS-SC& . as described in Section 10.1.1, for
full scan identification of the target analytes. The target analytes are listed in
Attachment B.1 and Table I of Method TO-14 and also include trans 1,2-
dichioroethene, dibromoch1oromet1 ane and bromodich1oromem e The
required quantitation limit for each of the target analytes is 0.5 ppbv.
Technical information pertinent to the analysis of the additional analytes not
included in Table 1 (sec Attachment B. 1) is as follows:
rnpound CAS Number Priniaiy IQfl Secondary Ion
trans l, 2 -Dichjoroethene 540-59-0 96 61,98,63
DibrornochlOmmethane 124-48-1 129 127,131
BrmodlichJomm ane 75-27-4 83 85,47
D. Nontarget compounds shill be library searched for the purpose of tentative
identifica jon. TIC identification will be analyzed following the procedures
descrjb j in EPA SOW OLMO1.3 Exhibit D-VOA, Section IV, Paragraphs
9.2 and 10.4.
4
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E. Standards - A gas standard containing 10 ppmv of analytes as listed in Section
8.2 of Method TO-14 and including Trans 1,2-Dichioroethane,
dibromochioromethane, bromodichioromethane, must be used for preparation
of the calibration standards. This standard must be of known origin traceable
to a National Institute of Standards (NIST) Standard Reference Material (SR .M)
or to a NIST/EPA approved Certified Reference Material (CRM).
F. Three internal standards must be used: bromochioromethane, chlorobenzene-
d 5 , and 1 ,4-difluorobenzene. These should be introduced in gaseous form into
the cryogenic trap during the analysis of each standard, blank, sample, and QC
sample. The concentration of gas and the volume introduced should be chosen
to result in a mid-range concentration between 0.5 ppbv and the high-point
standard concentration (20.0 ppbv is suggested). The volume of gas and the
concentration introduced must be identical for every analysis and standard.
G. Three surrogate compounds must be fortified into each canister prior to
shipping into the field. These should be compounds generally not found at
hazardous waste sites or in the environment: Toluene4, 4-
brornoflourobenzene, and I ,2-dichloroethane-d 4 are recommended. These
should be introduced in gaseous form into the cryogenic trap for each
standard, blank, sample, and QC sample. The concentration of gas and the
volume introduced should be chosen to result in a mid-range concentration
between 0.5 ppbv and the high-point standard concentration (20.0 ppbv is
suggested). 10.0 ppbv is recommended.
H. Calibration and tuning must be performed as specified in Section 10.2 of
Method TO-14, with the following modifications:
• A five-point initial calibration must be performed.
• The lowest calibration standard must be 0.5 ppbv.
• The upper most calibration standard defines the upper working range of
the analysis. Concentrations of 0.5, 5.0, 20.0, 50.0 and 100.0 ppbv
are suggested. For samples of high concentration, it may be necessary
to expand this calibration range or dilute the samples as described in
Section 10.4.2 of Method TO-14. All sample aliquot analytical results
must be bracketed by the standard curve. The response factors for all
compounds must be greater than 0.1.
• A continuing calibration must be performed every twelve (12) hours
after the initial calibration. The concentration of the continuing
calibration standard should be at the mid-point of the calibration range.
The 20.0 ppbv standard is suggested.
5
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I. After the instziiment is calibrated, a humid zero air test must be run as
described in Section 10.2.3 of Method TO-14 to demonstrate that the GC-MS
system is certified clean.
J. After the humid zero air test is performed, a laboratory-fortified canister
standard (LCS) must be analyzed to ensure calibration accuracy. This
standard must be prepared by spiking a certifiably precleaned and evacuated
canister with a standard gas mixture (as described in 7e). The volume of the
standard gas mixture should be chosen to result in a fortifIed canister standard
of 1.0 ppbv concentration. The LCS must be generated from a different
source than the calibration standards.
K. Replicate analysis must be performed on one canister from each sampling
round or on each canister that requires a dilution, whichever is more frequent.
It is expected that performing a dilution or reducing the sample volume pulled through
the Cryogenic Trap as per Section 10.4.2.3 of TO-14 may be necessary to bring the
concentration of some compounds within calibration range.
8. QUAlITY CONTROL REQUIREMENTS
Analysis of the PE samples and proof of reaching the required reporting limits must
be met prior to analysis of any environmental samples. In addition, the following
requirements must be met:
Audits Required
Frequency of Audits
QC Criteria
Corrective Actions
PE Samples
Once prior to analysis of
samples
Not available for
the laboraxory
None
MDL
Once prior to analysis of
samples. Delivered with
PQL 5.0 ppbv
Repeat until within limits
or
bid.
Once prior to analysis of
100 ± 20%
Repeat until within limits
Fortified Blank
samples. Delivered with
recoveiy of true
bid.
value of 0.5 ppbv
or
athndard
Initial calibration
Once prior to analysis of
±25% RSD
Repeat until within limits
for !fleeting
samples. Delivered with
inininium PQL
bid.
with 5.0 ppbv
low concentration
standad
This specification requires the following be met:
6
-------
Audits Required
Frequency of Audits
J QC Criteria
Corrective Actions
Cleanliness All canisters <0.5 ppbv for Reclean all non-compliant
analysis (prior to all compounds canisters and reanalyze.
canister delivery) (Cleanliness criteria must be
met before shipment.)
Tuning Once per 12 hour analysis As per Table 4 of Repeat until within limits.
run TO-14 Criteria must be met prior to
sample analysis.
Internal Added to every sample, Area must be Reanalyze once if exceed
Standards blank, standard, and spike ±30% of those criteria. If still out, flag
for the calibration associated data with an
standards. RT asterisk (*) and report all
±0.50 minutes analyses
Initial calibration Once prior to analysis of ±25% RSD Repeat initial calibration
samples unless continuing RF >0.1 until criteria are met.
calibration exceeds limits Criteria must be met prior to
sample analysis.
Continuing Once per 12 hour analysis ±30% RPD Perform initial calibration
Calibration run at the end of analytical RF >0.1 and reanalyze all samples
analyzed since last compliant
calibration
Humid Zero Air Following each initial and <0.5 ppbv for Repeat until clean, criteria
Blank continuing calibration all compounds must be met prior to sample
analysis.
Laboratory Following each initial and 100 ±30% Perform initial calibration
Fortified Canister continuing calibration recovery of true and reanalyze until criteria
Standard value prior to arc met
sample analysis
Replicate analysis One sample from each ±25% RPD Reanalyze once if exceed
sample round CrItena . If still out, flag -
associated data with a cross
(+) and report all analyses
Surrogates All samples, blanks, 50%-150% Reanalyze samples, blanks,
standards, QC samples recovery QC samples, and
calibrations. If still outside
Limits report results followed
_______________ by a (#) .
7
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9. ANALYTICAL DELIVERABLES
A. Initial Deliverables related to laboratory proofs, depending on what method is
chosen by the laboratory to satisfy the requirement the following is to be
delivered:
Method detection limit (MDL) study
The MDL study results must be provided in a tabular format. The
formula and associated constant values utilized in the calculation of the
MDL for each analyte must be provided. The standard deviation of
each analyte must be clearly presented in the tabulated format. The
narrative of the report must explain the MDL procedure utilized to
generate the values. The column, instrument, trap description, and
operating conditions must be clearly displayed on the raw data.
Laboratory fortified blank analysis
The fortified blank results must be provided in tabular format. An
example calculation must be included for the determination of MDL, or
quantitation limits, including clear explanation of any assumptions
made.
Initial calibration criteria
The spiked standard concentration, laboratory results, and the %
difference between the actual and theoretical must be tabulated. A
narrative explaining any deviations from the set criteria is required.
The column instrument, trap description and operating conditions must
be clearly displayed on the raw data.
• Associated tune data in CLP format for any of the methods.
• The initial calibration results and continuing calibration results
must be in CLP format reported on modified RAS Form VI. The
response factors and percent RSD must be calculated. A narrative
expliining any deviations from set criteria is required. The
column, instrument, trap description and operating conditions must
be clearly displayed on the raw data.
• Tabulated results and raw data must be provided for the BFB tune,
initial five point calibration, continuing calibration, method blank,
and the seven replicates used for the MDL study.
8
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1. The tuning results must be tabulated and reported on RAS
Form V. The instniment’s normalized mass Listing and the
mass spectrum must be provided.
2. Reconstructed ion chromatograms (RIC) for all calibration
standards and the seven replicates must be provided.
3. Instrument quantitation reports. The report must contain
the laboratory replicate number, laboratory file ID, time
and date of analysis, scan number or retention time,
quantitation ion, measured area and analyte concentration.
It must be easy to determine what internal standard was
used for which compound.
4. Raw and enhanced spectra for one (1) of the seven (7)
replicates.
5. The initial calibration results must be reported on a
modified RAS Form VI. The relative response factors and
the percent relative standard deviation must be calculated
for all analytes and surrogates. The spectrum for each
compound in the initial calibration does not have to be
included. A RAS Form VU must be provided if initial
calibration standard curve 20.0 ppbv standard was utilized
for the quantitation of the seven replicates.
6. The suggested 20.0 ppbv continuing calibration standard
must be reported in a tabulated format on modified RAS
Form VU. The percent differences and daily response
factors must be reported for all analytes and surrogates. A
RAS Form V I I must be provided if the initial calibration
standard curve 20.0 ppbv standard was utilized for the
quantitatian of the seven replicates.
B. For each sample delivery group the following deliverables are required:
• A case narrative should be included describing the analyses and any
unusual circumstances or problems with the canisters, sampling system,
or analysis system. The naimtive must clearly state the M&E
sample number, the laboratory sample number, the number of samples,
the sample receipt date, and the sample analysis date.
• Canister and flow controller cleanliness ceitification data, including
chromatograms, must be provided with canisters prior to sampling.
9
-------
Copies of these data must also be included in the data package. The
data must be reported in a format similar to EPA CLP Form 1. The
Form 1 must be modified to include all analytes listed in Table 1 of
Method TO-14 and include trans 1,2-dichioroethene,
dibrornochioromethane, and bromodichlromethane. A Supplemental
Form 1 must include all TICs identified and quantified.
• Documentation of performance of a leak check must be provided.
• All calibration data, tuning data, and spiking data must be reported on
CLP forms and must adhere to CLP format as much as possible.
Deliverables include all items listed in EPA SOW OLMO1.8. Exhibit
B-VOA Section .
• Form 1 must be modified to include all analytes listed in Table 1 of
Method TO-14 and include trans 1,2-dichioroethene,
dibromochloromethane, and bromodichloromethane. Supplemental
Form 1 must include all TICs identified and quantified.
• All raw data must be included such as chromatograms, integration
tables, ion chromatograms, mass spectra of TIC identifications.
• All bench records or log in sheets must be included describing canister
pressures, canister condition, gas screening, or sample quantities
introduced into the GCIMS.
• All raw data must be clearly labeled with M&E sample number,
laboratory number, and sample analysis date and time. This includes
raw data foc standards, blanks, samples, spikes, etc.
• An example calculation must be included for the determination of MDL
and/or quantitation limits, including a clear explan2tion of any
assumptions made.
• All quality control data such as method blanks, surrogates, internal
standards, tuning, initial and continuing calibrations must be
summarized on appropriate CLP SOW summary forms so the reviewer
may check retention times, response factors, tune criteria, % RSDs,
and QC data.
• The data package must include a copy of this specification, chain of
custody, sample tags, custody seals, shipping receipts, sampler
preparation notes, and laboratory tracking records.
10
-------
• All copies of log in sheets for canisters recording the canister arrival
time to certify verified time of sample receipt.
C. Complete Sample Delivery Group File (CSF) Audits
Due to the litigative nature of each superfund site being studied, Region I EPA
requires and M&E requires that all analytical data and all raw supporting data
be delivered with each sample delivery group (SDG). With each SDG the
CSF Completeness Evidence Audit must be carried out. The CSF
Completeness Evidence Audit Forms are included in Attachment B.2 and must
accompany each data package. The laboratory using these audit forms must
show that each piece of sample data, raw data, calibration data, and any other
requirements of the statement of work or analytical specifications are included
in the data package.
The forms included in Attachment B.2 are for all types of data packages. For
this analytical specification the laboratory must use these forms supplied to the
best of their ability where deliverable items are applicable.
10. EXCEPTIONS
If the QC requirements or action thnit are exceeded; or if analytical samples are
destroyed or lost; or if matrix interference is suspected, contact:
Andrew F. Eeliveau
Metcalf & Eddy, Inc.
(617) 246-5200 ext. 4433
U
-------
ATTACHMENT B.1
ADDITIONAL ANALYTE LIST
Freon 12 (DiChlorodifluoromethane)
Methylene Chloride
Viny! Chloride
Methyl Bromide
Ethyl Chloride
Freon 11 (TdChJorofluommetl1 e)
Vinylidene Chloride
DiChloromethajje
Freon 113 (1,1 ,2-Trjchlorol , 2 , 2 -triiluoroethane)
1,1 -Dich1oroe jie
Cis-1 2 -Dich1oroethy1ene
Chloroform
1 , 2 -Dichloroeth e
Methyl Chloroform
Berizene
Carbon Tetrachjoi-jde
1 , 2 -Dichloropmpane
Trichloroethylene
cis- I, 3 -Dichloropropene
trans-i , 3 -Dichloropropane
1, l, 2 -TrichJoroeth e
Toluene
1 , 2 -Dibrornoethane
Tetrachloroethy lene
Chlorobenzene
Ethy lbenzene
m-Xyleae
p-Xylene
Stryene
1,1 , 2 7 2 -Tetrachjoroethane
o- 3 yLene
1 , 3 ,S-Trmethyl n
l, 2 1 4 -Trimethylbenzene
m-DicWombe ne
Benzyl Chloride
O-Dichlombenzene
p-Dichlorobenzene
l, 2 , 4 -Trichlombe ne
Hexachlombu djene
Trans 1 , 2 -Dichjoroethene
Dibmmocfflommeth e
Bromo chJomm e
12
-------
ATTACHMENT B.2
CSF - EVIDENCE AUDIT
WORXSTWFTS
13
-------
ATFACHMENT B.2
CSF AUDIT FORMS
-------
LOW coNcEx xrIo WATER FOR ORGANICS COMPLETE SOC FILE (CS?) rNVKNTORT su z’
L&$aATOly — CITY/STATE
CA UO. ________ GlO. _________ GNO3. ________ ________
NO. ____
TL*CT NO. ______________________________________________________________ NETH NO.
A]]. docuI aflC3 delivered in the coizplete SDG file iu..it be original docuient -
where po sibl.. (REF .cE I3IT B, SECTION II. PARAGRAPH 5. and SECTION III,
PARAGRAPh 16.)
PAGE NOg CHECX
PROM TO TAB EPA
Thven tory Sho (Fori DC -2) (Do not nube r) ____ ____
SDC Case N11ve — ________
Traffic Re ,o — ____ ________
Volatile, D4fl
a. QC S14ry
Surrogate Percent Recovery Sir’vi -.ry (Por II LCV) ____ ____ _____
Lab Control Saitple Recovery (From III LCV) ____ ____ _____
Method Blank Su sry (For2 IV LCV) ___ ___ ____ ______
Ttming and Mass Calibration (For2 V LCV) ____ ____ _____ _______
b. Sa. ple Data
TCL Result, - (Fora I LCV) ____ _____
Tentatively Identified Co pourtda (Pora I LCY-TIC) _____ ______
Reconstructed total ion chro atogra s (RIC)
and Quantitacjon Reports for each saaple
For each saapl.:
Raw spectra and background-subtracted
assa spectra of target coapounds identffie
Mass spectra of a].]. reported TICs with three
beat library astchea
c. Standard, Data (AU Inatru enca)
Initial Calibration Stt ary (Pora VI LCV) ____ ____ _____
RICa and Quan Reports for all Standards ___ ___ ____
Continuing Calibration (Por2 VII T 4 CV) ____ ______
RiCa and Quant Raports for all Standards
Internal Standaxd Area and RT S” ’.’ry _______
(Fora VIII LCV) ______
d. QC Data
3F3
Blank Data
LCS Data
PES Data
S jvo1atj1es Oati
a. QC Su *ry
Surrogate Percent Recovery Swmn.*ry (Fora II LCSV)
Lab Control Sa3ple Recovery (Fora III LCSV) _______
Mt thod Blank Su ary (Fora IV LCSV)
Tuning and Mus Calibration (Fora V LCSV)
FORM DC.2-l
-------
W CONCENTRATION WATER FOR oRc i4IcS coxpiz’rI SDG FILE (CST) INVENTORY SHEET (Cont.)
PAGE NOs
FROM TO
C ECX
LAB EPA
‘. Semivolatile, Data (cont.)
b. Sample Data
TCL Results (Form I LCSV)
Tentatively Identified Compounds (Form I LCSV-TIC)
Reconstructed total ion chromatogra ( PlC)
and Quantitacion Reports for each sample
For each sample:
Raw spectra and background-subtracted
mass spectra of TCL compounds
Mass spectra of TICs with three best library matches
GPC chromatograsa (if GPC performed)
c. Standards Data ‘(All Ins tniments)
Initial Calibration St w*ry (Form VI LCSV)
RICa and Quan Reports for all Standards
Continuing Calibration (Form VII LCSV)
RICa and Qu.an Reports for all Standarda
Internal Standard Area and RT Su P.azy
(Form VIII LCSV)
d. QC Data
DFIPP
Elank Data
LCS Data
PES Data
i. Pesticides
a QC S” ’—ry
Surrogate Percent Recovery StTI I .17 (Form II LCP)
Lab Control Sampl. Recovery (Form III LCP)
Method Blank S’zmn ry (Form I V LCP)
b. Sample Data
TCL Results - Organic Analysis Data Theet
(Form I LCP)
Chromatograas (Primary Column)
C romatograms from second CC column confirmation
CC Integration report or data system printout and
calibration plots
Manual work sheets
For pesticides/Aroclors confirmed by cc/KS, copies
of raw spectra and copies of background-subtracted mass
spectra of target compounds (samples & standards)
( CA3 . . — w . TO FCLLOII — AS MO. 1
FORM DC-2-2
-------
LOW CONCENTRATION WATER FOR ORCANICS COMPLETE SDG FILE ( CS ?) INVENTOR! SNEET ( Cant. )
CASE NO• — SOG O. _________ SOG 501. TO FOLL ________ _________ ________ lAS 50.
PAGE NOs CHECX
FROM TO LAB EPA
5. Pesticides (cant.)
c. Standards Data
Initial Calibration Data (Form VI LCP)
Calibration Verification (Form VII LCP)
Pesticides Analytical Sequence (Form VIII,
LCP-l and -2) ____ ___ ____ _______
PesticideFlorisil Cartridge Check (Form IX. LCP) ____ ____ _____ ________
Pesticide Identification (Form X LCP) ____ ____ _____ ________
Standard chroaatogram.s and data system printout
for all Standards
For pesticides/Aroclors confirmed by CC/NS, copies
of spectra for standards used
d. QC Data
Blank Data
LCS Data
PES Data
Xiscollanea .s Data
Original preparation and analysis forms or copies of
preparation and analysis logbook pages
Internal sample and sample extract transfer
ehafn -of-custody record.s
Screening records
All inscnent output, Including strip charts
frog screening activities (describe or list) _____ ________
• EPA Sbi oi Recetvin ocn cnes
Airbills (No. of sbipment.s _)
Chain-of-Custody Records
Sample Tags _____ _______
Sample Log-In Sheet (Lab & DC1) ___ ____ ______
SDG Cover Sheet ____ ____ _____
Miscellaneou.s Shipping/Receiving Records
(describe or list)
• Internal Lab $a npje Transfer Records and Tracking Sheets
(describe or list)
FORM DC- -3
-------
OW CONCENTRATION WATER FOR ORCANICS cOX1LET! SDG Fill (CS?) tNVENTORT SUEZI (Cant.)
:0. 9 her R.ecords (describe or list)
Telephone Coomunication Log
11. i ent3I
Co3pleted by:
(CLP Lab)
Au .ted by:
(EPA)
(S igna ture)
(Signature)
(Printed Naae/’ritle)
(printed Naae/Titls)
(Date)
(Date)
FORN DC-2•4
SOG NO. — — SOC M . TO FOLL J SAS NO
PAGE
FROM
NOs
TO
citzcx
TAB EPA
10/9
-------
SAMPLE LOG.!N SHEET
Lab t4aa c:
Pago . . . . . . _o(
Reccived By (Print Name):
Received By(Signaturc): —
Cuø Numbc —
S&o Dcivcry
Group Ho :
LAAS Ntim —
R fARXS:
• Cu.uody Scii(,)
2. C utodyScaWo&: ______
3. iJD.O(-O.LriOdy
4. Tri c R pocu
P c n Ua
S. Au
6. Ai,bW No.: _______
7. S nrLe Tq,
S&rzçlc Tag
I .
9. Doea cru I .Lice Os
a a ody r dj. i c
re ii. ted uc Ic iigs
YwWo
Ia. L6R c edULaIx ______
11. Tio e Reczi,rd ________
Saixiple Tranthr
Fricios
Area t
Br
Ou:
• Co u SMO iod auath re rd o(resoluuos
R ieved r __________________
Due:
Log.in Daia:
PrcsroilAbuat
CONDITION
OF SAMPLE
SIiU’MENT, zrc.
bd c
Pre cot/Abaca t
PreundAbseiit
Li MIN Uj od
04
Q isudy
tnuwBn,kesf
Lc a g
Lo bookNo —
Logbook Page Ho:
FOR2 4 DC .I
-------
EXHIBiT A
A11 ACHMENT C
ANALYTICAL SPECIFICATION
FOR
LOW CONCENTRATION PESTICIDES
AND POLYCHLORINATED BIPHENYLS
IN AQUEOUS SAMPLES
-------
SCOPE
Analysis of pesticides and individual PCBs utilizing EPA CLP SOW Low
Concentration Water for Organics Analyses 10/92 and further modifies the procedure
to reach lower concentrations. The first modification requires a concentration of the
extract to 0.5 ml and a second modification requires that if PCBs are detected in the
initial pesticide analysis, then a three (3) point calibration for the specific PCB(s)
detected must be conducted.
A performance evaluation sample will be sent with the first environmental samples
and is required to be analyzed and reported. Failure to analyze this sample in the
required time and within the required limit (unknown to lab) may mean corrective
actions may be required.
The detection limits required for the analyses are detailed in Attachment C.2.
2. PURPOSE
The data derived from pesticideiPCB analysis on these samples will be used for
ecological risk-assessment purposes requiring low detection limits.
3. DEFINITION OF WORK
Surface water samples will be analyzed for low concentration pesticides and PCBs.
4. SCH1 DULE
Samples will be shipped daily as collected. Saturday delivery will be required.
Overnight delivery service will be used. Contacts for shipping and data delivery
inquiries are specified in Exhibit A, Atachment F.
Holding Time:
The samples must be extracted within five (5) days of verified time of sample
receipt (VTSR). Samples must be analyzed within twenty-one (21) days of
extraction.
Delivery of Data:
Sample data must be delivered to M&E within thirty-five (35) days of
laboratory receipt of the last sample per sample delivery group (ten (10) -
fifteen (15) samples). PE sample results required within seven (7) days of
VTSR.
1
-------
S.. ANALYTICAL REFERENCE
EPA CL? SOW Low Concentration Water for Organic Analysis 10/92 modified to
reach nominal detection limits of 0.003 to 0.005 ppb for pesticides and 0.05 ppb for
PCBs. The PCBs found require a three (3) point calibration for individual Aroclors
as detailed in Section 7, Analytical Procedure. Attachment C.! is the analytical
method.
6. SAMPLE PRESERVATION AND DETECTION LIMITS
Samples are to be cooled to 4°C. Detection limits required are detailed in
Attachment C.2.
7. ANALYTICAL PROCEDURE
The laboratory will follow the general instructions of the low concentration SOW
10/92. The following are the specific modifications that must be followed.
a. The laboratory will receive 1000 mL of aqueous sample, which will be
brought to a final extract volume of 0.5 mL. This will allow for the desired
detection limits of 0.05 1 zgIL for PCB analysis and nominal detection limits of
0.003-0.005 ig/l for pesticides. See Attachment C.2 for detailed detection
limits.
The laboratory will receive a PE sample with the first SDG and must follow
the instruction with the sample for analysis.
b. The instrument(s) is calibrated for pesticide/PCB as per the instructions in the
CLP SOW for Low Concentration Water for Organics Analysis, 10/92. No
florisil or GPC cleanup is required.
c. The surrogate solution is defined in the CL? SOW for Low Concentration
Water for Organics Analysis, 10/92 except only 50 ul. of the surrogate
solution is added to each sample, matrix spike, matrix spike duplicate, and
blank analysis.
d. The samples are quantitated for the pesticides at the detection limits required in
Attachment C.2. If a PCB is identified during the initial sample run then the
PCB(s) will be subsequently quantified using the three (3) point calibration
scheme described in subsections e through i.
e. A sulfuric acid cleanup step is required for the remaining sample extract to be
quantitated for PCBs. The sample extract (0.5 mL minus the pesticide
2
-------
injection loss) should be placed in a vial with an equal volume of concentrated
sulfuric acid. The two (2) phases should be shaken vigorously together for
one (1) minute. Allow the phases to separate and carefully pipet off only the
hexane layer. The hexane extract is now ready for PCB analysis.
f. The calibration sequence for the PCB analysis will be modified from the CLP
SOW for Low Concentration Water for Organic Analysis, 10/92, to require
that if ANY PCBs are detected in the sample, a three (3) point calibration
curve must be performed for each PCB detected. This must be performed
within twelve (12) hours of the submittal sample pesticide analysis time.
Because of the possibility that two (2) or more PCBs can be found in these
samples, the calibration seqt ence must reflect the two or more individual
PCBs. Mixtures of non-coeluting Aroclors (1242/1254, 1242/1260) can be
used as calibration standards as long as they are shown not to coelute and can
be quantitated separately.
The following is a theoretical analytical example run sequence which must be
followed if more than one PCB is identified:
1. Resolution checks
2. Aroclor 1016/1260
3. Aroclor 1221
4. Aroclor 1232
5. Aroclor 1242
6. Aroclor 1248
7. Aroclor 1254
8. Low Aroclor #1 standard
9. Low Aroclor #2 standard
10. Middle Aroclor #1 standard
11. Middle Aroclor #2 standard
12. High Aroclor #1 standard
13. High Aroclor #2 standard
14. Instrument blank
15. Method blank
16. Sample analysis for 12 hours
25. Method blank
26. Continuing calibration (midrange Arocolor #1 and midrange of
Aroclor #2)
27. Instrument blank
etc.
The requirements for the run sequence stated above apply to both GC columns
used for analysis and confirmation.
3
-------
The low point standard concentration must be 50 ng/mL. Concentrations of
250 nglrnL and 1000 ng/mL ale recommended for the medium and high point
standard mixtures respectively. Different mid and high point concentrations
may be chosen by the contractor, provided: the mid-point concentration is at
least four (4) times the low point and the high point is at least sixteen (16)
times the low point. The high point concentration defines the upper end of the
concentration range for which the calibration is valid. The high point
concentration should be selected so that the quantitation peak of each Aroclor
is 50% to 100% of full scale but never over 100%. All criteria for the initial
calibration defined in the CLP SOW for Low Concentration Water for
Organics Analysis, 10/92, apply.
g. Prepare a matrix spike/matrix spike duplicate solution using Aroclor 1232 at a
concentration of 100 ng/mL. For each of the samples designated by the
sampler for matrix spike and matrix spike duplicate analysis, add 1 mL of
matrix spike solution. Additional sample will be provided for MSIMSD
analysis and these samples will be designated on the chain of custody forms.
h. The continuing calibration must beperforrned using the midrange standard of
A.roclor #1 followed by the midrange standard of Aroclor #2. An Instrument
Blank must also be run before the midrange standards. The midrange standard
calibration factor must have a maximum 20% difference from the initial
calibration factor. The instrument blank must be totally free of any Aroclor
(any PCB) or corrective action described in Section 8 must be taken. The
continuing calibrations and method blanks and instrument blanks must be run
after every ten (10) samples.
In the event that an Aroclor other than #1 or #2 is detected, a three (3) point
calibration for that Aroclor must be run. This must be performed within
twelve (12) hours of the initial sample (pesticide) analysis time.
8. QUALiTY CONTROL REQUIREMENTS
The following are the audits required, frequency of audits, QC limits, and required
corrective actions:
4
-------
Resolution Check
Mixture
Initial Calibration
(for both columns)
At the beginning of
the initial calibration
sequence
As per the CL? SOW
for Low Conc. Water
for Organics Analysis.
10/92 and Special
Technical Instructions
I per Sample
Delivery Group
As per the CL? SOW
for Low Conc. Water
for Organics
Analysis. 10/92
RSD . . 20%
-------
9. ANALYTICAL DELiVERABLES
a. The following items are required as documented de [ iverables as well as
meeting the required detection limits stated in Attachment C.2:
• All applicable CLP deliverables required in the CLP SOW for Low
Concentration Water for Organics Anaiysis, 10/92.
• The results of the performance evaluation sample must be reported
separately within seven (7) days of VTSR in CLP format as per S•Ow
10/92.
• The MSIMSD recoveries must be reporte rn a form similar
to CLP SOW OLMO1.U. cs Analysis, inc’uding revisions
through OLMO1.8, Form 3F but modified for Aroclor 1232 as the
spike. Nonspiked Aroclors detected must be quantitated and reported
on Form 1 and on the PCB identification summary for multicomponent
analytes (Form 1OL PCB in the CLP SOW for L incentration
Water for Organics Analysis, 10/92).
• All samples, blank, and MSIMSD data must be reported in zg/L.
• All sample tracking reports, chain of custody forms, sample tags,
custody seals, and any telephone logs referring to the samples must be
delivered with the package.
• A copy of this Analytical Specification
• Copies of sample log in sheets indicating the cooler temperature and the
sample arrival thne and date.
• Submit bench sheets for method of sample extraction, surrogate solution
identification and surrogate amounts added, matrix spike solution
identification, and matrix spikeimatrix spike duplicate amounts added,
quantitation dates and instrument run times, dates and pH determination
bench sheets.
• The run numbers and concentrations of the surrogates used for the
initial calibration, continuing calibration, blanks, samples, QC samples,
and PE samples must be clearly defined on the data. The percent
recovery must be calculated.
• The source of all standardizing materials must be documented. The
concentrations of all standards must be indicated.
6
-------
• A form detailing the retention times and retention time windows of all
peaks used for Aroclor identification.
• A formula showing how the results were calculated with an example of
an actual calculation where a positive PCB result was found (if not
detected then a surrogate should be used in the example).
• A case narrative explaining methodology used, problems
encountered,and problem resolutions. The narrative must also show all
laboratory sample numbers and their corresponding M&E sample
numbers.
• All chromatograms (with peaks used for quantitation noted,
chromatographic conditions, volume injected, and instrument number)
for calibration verifications, surrogate recoveries, samples, QC
samples, PE samples, and spike recoveries must be included in the data
package.
• The data package must be paginated and of good readable copy quality.
b. Complete Sample Delivery Group File (CSF) Audit
Due to the litigative nature of each Superfund site, Region I EPA requires that
all analytical data and all tabulated raw or supporting data be delivered with
each sample delivery group (SDG). With each SDG the CSF Completeness
Evidence Audit must be carried out. The CSF Completeness Evidence Audit
Forms are included in Attachment C.3 and must accompany each data
package. The laboratory using these audit forms must show that each piece of
sample data, raw data, calibration data, QC data and any other requirement of
the statement of work or analytical specifications are included in the data
package.
The forms included in Attachment C.3 are for all types of data packages. For
this analytical specification the laboratory will use the forms supplied to the
best of their ability where deliverable items are applicable.
10. EXCEPTIONS
IS QC requirements or action limits are exceeded; or if analytical samples are destroyed
or lost; or if matrix interference is suspected, contact:
Andrew F. Beiveau
Metcalf & Eddy, Inc.
7
-------
617-246-5200 ext. 4433
8
-------
ATrACEMENT C.1
ANALYTICAL METHOD
-------
SUPER.FUND ANAL TICAL METHODS
FOR
LOW CONC TRATION WAT FOR ORGANICS ANALYSIS
10/92
10/92
-------
STATEMENT OF WORK
bl of ConC fl .1
Q(IBIT B: REPORTING AND DELIVERABLES REQUIRKE
QIIBIT C: TARGET COMPOUND LIST (TCL) AND CONTRACT REQUIRE QUANTITATION
LIMITS (CRQLiI)
iIBIT D: ANALYTICAL METHODS
Vo lati lCs
Se ivo1atile3
Pes tic ides
10/92
-------
IBIT
REPORTING AND DELIVERA8I E5 guIa (EN’rS
10/92
3 - 1
-------
SECTION I
CONTZACT RZPORTS/DELIV!RA. l2S DISTRIBUTION
The following table reiterates the Contract reporting and deliverables
requtre ents specified in the Contract Schedule and specifies the
distribution that is required for each deliverable. NOTE: Specific recipient
names and addresses are subject to change during the tern of the contract.
The Sample Man.age enc Office (S f0) will notify the Contractor in writing of
such changes when they occur.
No.
Item Copies
Delivery
Schedule
Distribution
(1)
(2)
(3)
1. Updated SOPs 3 Sub iC as specified X X
in the BOA.
*2. Sample Traffic 1. 3 days after X
Reports receipt of last
sample in Sample
Delivery Group
(SDG).**
***3• Sample Data 5uzm ary 1 14 days after X
Package receipt of last
sampl. in SDG.
***4• Sample Data Package 2 14 ( 1 3y3 afte X X
receipt of last
sample in SDC.
***5• Complete SDG File 1 14 days after X
receipt of last
sampl. in SDG.
6. CC/MS Tapes Lot Retain for 365 days As Directed
after data subais-
aton, or submit with-
In 7 days after
receipt of written
request.
Distribution:
(1) Sample Management Office (Sf0)
- (2) EMSL-LV
k3 Region-Client (Technical Project Officer)
10/9 2
-------
SECTION II
REPORT DESCRIPTIONS AND ORDER 0? DATA DELIVEBABZ2S
The Conc accor laboratory shall provide reports and other deliverables as
specified in the Basic Ordering Agreeaeflt. The required content and form of
each deliverable is described in this Exhibit.
All reports and documentation SHALL BE:
o Legible
o Clearly labeled and co pleted in accordance with instructions in this
Exhibit
o Arranged in the order specified in this Section
o Paginated consecutively in ascending order starting froa the SDG Narrative
o All data reporting forms shall be typewritten
If submitted documentation does not conform to the above criteria, the
Contractor will be required to resubmit such documentation with the
deficiencies corrected 1 at no additional cost.
Whenever the Contractor is required to submit or resubmit data as a result of
an on-site laboratory evaluation, through a SXO action, or through a Region.al
Data Reviewer’s request, the data shall be clearly marked as ADDITIONAL DATA
and shall be sent to all three contractual data recipients (S?cO. E2(SL/LV, and
Region). A cover letter shall be included which describes what data are
being delivered, to which EPA Case(s)/SDCs it pertains, and who recueseed the
Whenever the Contractor is required to submit or resubmit data as a result of
Contract Compliance Screening (CCS) renew by SMO. the data shall be sent to
all three contractual data recipients (SMO, DISL/LV, and Region), and in at].
three instances shall be accompanied by a color-coded COVF SHEET (Laboratory
Response To Result:. of Contract Compliance Screening) provided by SMO.
Descriptions of the requirements for each deliverable itee cited in the 8asic
Ordering Agreement (BOA) are specified in this Section. Iteaz submitted
concurrently SHALL BE arranged in the order listed. The components of each
item SHALl. BE arranged In the order presented in this Section when the item
is submitted.
Section III contain, the form instructions to assist the Contractor in
providing all the required data. Section IV of this Exhibit contains copies
of the required data reporting forms.
8.6 10/92
-------
O MLIT1 ASS 7RANCE PL&N AND STANDARD OPERATING FROCZDQRZI
See the BOA for requireaents.
2. SAMPLE TRAFFIC REPORTS
2.1 Original Sampi. Traffic Report page marked Lab Copy for Return to 5N0
with Lab receipt information and signed in original Contractor
signature, for each sample in the Sample Delivery Group.
2.2 Traffic Reports (TB...) shall be submitted in Sample Delivery Group (SOG)
56t3 (i.e., TRs for all samples in an ZDC shall be clipped together).
with a.n SDC Cover Sheet attached.
2.3 The SDG Cover Sheet shall contain the following items:
o Lab name
o Contract n ber
o Sample analysis price - full sample price from contract.
o Case ni ber
o Ust of EPA Sample Numbers of all samples in the SDC.
identifying the first and samples received, and their dates
of receipt (LPDa).
(I Jhen more than one sampl. is received in the first or last SDG
shipment, the ¶first sample received would be the lowest sample number
(considering both alpha and numeric designations); the lut’ sample
received would be the highest sample number (considering both alpha and
numeric designations).
2.5 The EPA Sample Number of the first sample received in the SDG is the
SDC number. Each Traffic Report shall be clearly earked with the SDG
Number. This information shall be entered below the tab Isceipt Data
on the TL The TI for the i. a.t sample received in the last SDG
shipment shall be clearly marked ‘SDG - FINAL SANPLE.
2.6 If samples are received at ths laboratory vith multi-sample Traffic
Reports (TB..), ill the samples on one multi-sample TI may not
necessarily be in the same SDG. In this instance, the laboratory’ shall
make the appropriate number of photocopies of the TI. and submit one
copy with each SDG cover sheet.
3. SA)ITPLE DATA S1 ]O(AIT PACXACZ
3.1 As specified in the Delivery Schedule 1 one Sample Data S .zmmary Package
shall be delivered to SMO concurrently with delivery of other required
sample data. The Sample Data SI? v ry Package shall be submitted
separately (i.e., separated by’ rubber bands, clips or other means)
directly oreceding the Sample Data Package.
‘3.2 The Sample Data Sumsary Package consists of specified items from the
Sample Data Package in the following order:
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ssae data package 1 the Contractor shall submit a copy of the SDC cover
sheet vith copies of the TRs.
4.5 Volacjjes Data
4.5.1 Volatiles QC Suary
If more than a single form is necessary, each typ. of form
shall be arranged in chronological order by iaztrument.
o Surrogate Recovery (Form II LCV)
o Laboratory Control Sample Recovery (Form III LCV)
o Method Blank Su n*ry (Form IV LCV)
o CC/MS Tuning and Mass Calibration • BFI (Form V LCV)
o Internal Stand.ard Area and Retention Tim. Su arf (Form
VIII L.CV)
4.5.2 :V01&t 5 Sample Data
Sample data, including PES, shall be arranged in packses vith
both of the Organic Analysis Data Sheets (Form I LCV and Form I
LCV-TIC) • folloved by the ray data for volatile samples. These
sample packets shall then be placed in increasing EPA Sampls
Number order.
4.5.2.1 Organics Analysis Data Sheet for target compound
results (Form I LCV).
4.5.2.2 Organics Analysis Data Sheet for tentatively
identified compounds (Form I LCV-TIC). This form
shall be included even if no TIC’s are found.
4.5.2.3 Reconstructed total ion chrom.atogram.s (RIC)
The P lC for each sample, extract, standard, and
blank shall be normalized to eb. largest norijolvene
component, and shall contain the folloving header
information:
o EPA Sample Number
o Date and time of analysis
o CC/MS instrument ID
o LabfilelD
Internal standard and surrogate spiking compound.s
are to be labeled vith the tames of the compounds,
either directly out from the peak, or on aprine-ouc
of retention times if retention times are printed
over the peak.
1-10 10/92
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4.5.2.4 Quaneitacion Report
If automated data systems are u-sed for qu.aneitation
of the target compounds, the complete data system
qu.antication report shall be included in *1]. sample
data packages, in addition to the reconstructed ion
chromatogram. The complet. data system qu.antieation
report shall include all of th. information listed
belov. For laboratories which do not .ue the
automated data system procedures, a laboratory rav
data sheet quancitation. report containing the
following infor mation shall be included in the
sample data packa e in addition to the chromatogram.
o EPA Sample Number
o Date and time of analysis
o RT or scan number of identified target
compounds
o Ion used for qLLantitation with measured
area
o Copy of the area table from the data system
o GC/M5 instrument ID
o Labfil.ID
In all instances where th. data system report has
bean edited, or where manual integratton or
quantitation has been perfor ed, the GC/flS operator
shall. Ldeneify such edits or aaunal procedures by
initialing and dating the changes iada to the report
and includ, the scan rang, integration.
4.5.2.5 Target Compound teas Spectra
For each sample, by each compound identified, copies
of raw spectra and copies of background-subtracted
mass spectra of target compounds that are identified
in the sampl, and corresponding background.
subtracted target compound standard sue spectra are
required. The raw spectra and the background.
subtracted spectra shall be labeled with the EPA
Sample Number, lab file ID, date and time of
analysis, and CC/MS instrument ID. Compound names
shall be clearly marked on all spectra.
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4.5.2.6 TentatiVely Identified Compound Mass Spectra and
Library Matches
For each sample. by each compound identified, copies
of mass spectra of non-target and non-surrogate
organic compounds (Tentatively Identified Compounds)
with the associated spectra of the three best
library matches an, labeled with EPA Sample Number,
lab file ID, date and time of analysis, and CC/MS
instrument ID.
4.5.3 Volatiles Standards Data
4.5.3.1 Initial Calibration
All initial calibration data shall be included for
all analyses associated with the SDC. When more
than one initial calibration is performed, the
recon.structed tori chromatOgraaS and quixztitation
report.s and each type of form shall be put in
chronological order, by instrument.
Initial Calibration Sitiv .I*ry (Form VI LCV).
Internal Standard Area and Retention Time Summary
(Form VIII LCV)
Volatile standard(s) reconstructed ion chromatog a.ma
and qu.antitation reports for the initial (five
point) calibration are labeled as in Paragraphs
4.5.2.3 and 4.5.2.4. Spectra an, not required.
4.5.3.2 Continuing Calibration
When more rhin ona continuing calibration is
performed. th. reconstructed ion chromatogram and
qu.axttitatiofl reports and each typ. of form shall be
in chronological order, and by instrument if eons
than one instrument is used.
Continuing Calibration SL1 r7 (Form VII LCV)
Internal Standard Area and Retention Time Stv .ry
(Form VIII LCV)
VOA standard(s) reconstructed ion chromatograms and
quantitation reports for all continuing (12 hour)
calibrations are labeled as in Paragraph 4.5.2.3 and
4.5.2.4. Spectra are not required.
B- 12 10/92
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4.5.4 Volacj les QC Data
4.5.4.1 CC/MS Tuning Data
CC/MS Tuning • BFB data for each 12-hour period.
shall be arranged in chronological order by
instrument far each CC/MS syste. utilized.
CC/MS Tuning and Mass Calibration - BFB (Form V LCV)
Bar graph spectr , labeled as in Paragraph 4.3.2.3.
Mass listing, labeled as in Paragraph 4.5.2.3.
4.5.4.2 Blank Data
Blank data (method, storage and instrument) shall be
arranged in chronological order by instrument.
NOTE: This order is different from that used for
samples.
Blank data shall be arranged in packets with both of
the Organic Analysis Data Theeta (Form I LCV and
Form I LCV-TIC), followed by the raw data for
volatile samples (see paragraph.s 4.5.2.1 to
4.5.2.6).
4.5.4.3 Laboratory Control Sample Data
Organics Analysis Data Sheet for target co pound
results (Form I LCV). Form I LCV-TIC is not
required.
Reconstructed ion chromatogram(a) and quantitation
report(s), labeled as in Paragraph 4.5.2.3 and
4.5.2.4. Spectra are required.
4.6 Semivolatile, Data
4.6.1 Se.aivolatilea QC
If mars than a single form is necessary, each type of form
shall be arranged in chronological order 1 by instrument.
o Surrogata Recovery (Form II LCSV)
o Laboratory Control Sample Recovery (Form III
LCSV)
o Method Blank Su arj (Form IV LCSV)
o CC/MS Tuning and Mass Calibration • DFTPP (Form
V LCSV)
o Internal Standard Area and Retention Time
Sui ary (Form VIII LCSV-1, LCSV-2)
3-13 10/92
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o EPA sample Number
o Volume injected (ul)
o Data and time of analyseS
o CC column LdanCifiCItiOfl (by stationary
phase and internal diameter)
o CC instrument identification
o Scaling Factor
o PositiVely identified compounds shall be
labeled with the names of compounds,
either directly out from th. peak, or
on a priflt .OUt of retentIon times if
retention times are printed over the
peak.
4.7.2.5 Copiea of pesticide chromatO&r8 from the second CC
column, labeled S i in Paragraph 4.7.2.4.
4.7.2.6 Data System Printouts
Data system printout5 of retention time and
corresponding peak areas or height ihall accompany
each chromatogram and are lab.led with the following
information:
o EPA Sample Numbet
o Volume injected (ul)
o Date and time of analyses
o CC colt identificatiofl (by stationary
phase and internal diameter)
o CC instrument identification
o Scaling Factor
o positively identified compounds shall be
labeled with the ames of compounds,
either directly out from the peak, or
on a print-out of retention times if
retention times are printed over the
peak.
In all instances where the data system rsport has
been edited, or where anu.*l integration or
quantitltiOfl baa been performed, the CC/!C operator
shall, identify such •dit3 or manual procedures by
B .18 10/92
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initialing and dating the changes made to the report
and include the integration time rang..
4.7.2.7 Manual work sheets.
4.7.3 Pesticide/ArOCl0t SeandardJ Data
4.7.3.1 Initial Calibration
Data sh*ll be included for all calibration analyses
pertaining to the SDG. Vhen more than ens initial
calibration is performed. the data and each type of
form shall be put in chronological order, by
instrument and CC co1uz t.
Initial Calibration for Single Component Analytes
(Tori VI LCP.1, LCP-2).
Initial Calibration for Mu1tico portent Analytes
(Tori VI LCP-3).
ResolUtiOfl Check S ’ ry (Form VI LCP-4).
Analytical Sequence (Form VIII LCP), containing
lnitia1, calibration standards.
4.7.3.2 Calibration Verification
Calibration Verification S” ” ry (Form VII LCP) for
all CC colt ts.
When more than one calibration verification is
performed, f’ .s sha1. ... in chr o1o ica1 order, by
instrument and CC column.
4.7.3.3 Chroastograms and data system printouts are required
for j),] standards and arranged in chronological
order by instrument and each CC co1i :
o Reaolutio Check Mixture.
o Performance Evaluation Mixtures, each initial
calibration and all those that bracket samples
in th SDC.
o Individual Standard Mixture A, at three
concentration ’, each initial calibration,
plus al] those that bracket samples in
the SDG.
o Individual Standard Mixture B, at three
concentrations, each initial calibration,
plus all those that bracket samples in
the SDG.
3-19 10/92
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o Al] ulticoaP0fl C an.alyees (loxaphens
and Axoclorl), each initial
calibration.
o All ulticO p0fle analyte standards
analyzed for confirmation.
4.7.3.4 Data system printouts of retention timu and
corresponding peak areas or peak heights shall
accompany each chromatogram. In addition, all
chromatogrami arid data system printouts are required
to be labeled with th. followinç
o EPA Sample Number for the standard,
i.e., INDA1. INDA2. etc. (See Forms
Instructiofl S for details).
o Label all standard peaks for all
individual compowid.s either directly
out from the peak or on the printout of
retention times if retention times ars
printed over th. peak.
o Total nznogram.$ injected for each
standard.
o Date and tim . of injection.
o GC colt identification (by stationary
phase and internal diameter).
o CC mnitz ent identification.
o Scaling factor
In all instances h.rs the data system report has
been sditsd, or ibers manual integration or
quantit*tLOfl has been performed, the GG/!C operator
shall identify such edits or manual procsdurss by
initialing and dating the changes mad. to the report
and i cl de the integration time range.
4.7.4 Pesticide/AroclOr QC Data ,
4.7.4.1 3lank Data
Blank data Lnstr eflt . grouped by type of blank
(i.e.. method and sulfur) and arranged in
chronological order. NOTE: This order La different
from that used for samples.
Organics Analysis Data Sheet for target compounds
(Form I LCP).
3-20 10/92
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Blank data shall be arranged in packets with the
Organics Analysis Data Sheet (Form I L.C?) followed
by the raw data (paragraPh 4.7.2.2, to 4.7.2.7).
4.7.4.2 Laboratory Control Sample
Organics Analysis Data Sheet for target compounds
(Form I LCP).
Chroa.atOSrS.mS and data system printouts are labeled
as in Paragraph 4.7.2.4 and 4.7.2.6.
4.7.4.3 Florisil Cartridge Check
Florisil Cartridge Check (Form I X LCP), for all lots
of cartridges used to process samples in the SDG.
Each Form IX LCP shall be followed by the
chrow.atograls and data system printouts, labeled as
in 4.7.2.4 and 4.7.2.6.
5. COMPLE?! SD FIll
As specified in the Delivery Schedule, one Complete SDG File (CSF)
including the original sample data package shall be delivered to the
Region concurrently with delivery of copies of the Sample Data Package
to SMO and F2(SL/LV. The contents of the CS? shall be numbered
according to the method described in Section III of Exhibit 3. The
Document Inventory Sheet, Form DC-2,, is contained in Section IV. The
CS? shall contain all original documents where possibls. No copies
shall be placed in the CS? unless the originals are bound in a logbook
which is maintained by the laboratory. The CS? shall contain all
original documents specified in Section III, and Form DC-2 of Exhibit B
of this Superfund method.
The CS? shall consist of the following original documents in the order
listed in paragraph 5.1 through 5.6 belov
5.1 The original sample data package (see Exhibit 3, Section 4).
5.2 A completed and signed Document Inventory Sheet (Form DC-2).
5.3 All original shipping documents, including, but not limited to, the
following documents:
o EPA Chain of Cu.seody Record
o Airbills
o EPA Traffic Reports.
o Sample Tags (if present) sealed in plastic bags.
5.4 All original receiving documents, including, but not limited to, the
following documents:
3-21 10/92
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o Form DC-I
o Other receiving form.s or copies of receiving logbook.s
o SDG Cover Sheet
5.5 All original laboratory records, not already submitted in the sample
Data Package, of sample transfer, preparation and analysis, including,
but not limited to, the following documefltE
o Original preparation and analysis forms or copies of preparation
and analysis logbook pages.
o Internal sample and sample extract transfer ch.ain-of-custody
record.s.
o screening records.
o All instrument output, including strip charts from screening
activities.
5.6 All other original SDG -related documents in the possession of the
laboratory, including, but not limited tO, the following documents:
o Telephone contact• logs
o Copies of personal logbook pages
o All hand written SDG -specific votes
o Any other SDG specific documentS not covered by th. above.
NOTE: All SDG-r.lated documentation ay be used or admitted as
evidence in subsequent legal proceedings. Any other SDG-specific
doc enC3 generated after the CS? is sent to the Region, as weLl as
copies that are altered in any fashion, are also daliverablss to the
Region. (Original to the Region and copies to SMO and (SL/T..V).
If the laboratory does submit SDG -speCifiC documents to the Region
after submission of the CS?, the documents shall be numbered as an
addendum to the CS? and £ revised DC-2 form shall be submitted, or the
documents shall be numbered is a new CS? and a new DC-2 form shall be
submitted. The revised DC-2 form is sent to the Region only.
6. GC/1 S TAPES
See the BOA, Attachment 3, page 3 of 6.
7. EXTRACTS
The Contractor shall store sample extracts at 4C (±2C) in
bottles/vials with Teflon-lined septa. Extract bottles/vials shall be
labeled with EPA Sample Number, Case number and Sample Delivery Group
(SDG) number. A logbook of stored extracts shall be maintained,
listing EPA Sample Numbers and associated Case and SDG numbers.
3-22 10/92
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The Contractor L required o retain extracts for 365 days following
data sub L sio . D .iring that ci e, the Contractor shall submit
extracts and associated logbook pages within seven days following
receipt of a written request.
3-23 10/92
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SECTXOM III
FOR t INSU CTION GUIDE
This section includes specific instructions for the completion of all
required Loris. Each of the fora.s L a specific to a given fraction (vol&cii ,
senivolattle, pesticide/Aroclor). The Contractor slia1 . aubmit only those
Loris pertaining to the fractions analyzed for * given sampl. or san ples.
For instance, if a sample is schedulad for volatile analysis only, subnit
only VOA forns. There are two pages relating to the semivolaeil. fraction
for Forns I. VI, VII. and VIII and four page. relating to the
pesticide/Aroejor fraction for Torn VI. Whenever senivolaei2eg or
pesticides/Aroclors are analyzed and one of th. abov. named Loris is
required, all pages (LCSV-l, LCSV-2, etc.) shall be subnitted. These
iascructIons are arranged in the folloving order:
1. General. Inforaacion and Header Infornation
2. Organic Analysis Data Sheet (Porn I. All Fractions)
3. Surrogate Recovery (Porn II, All Fractions)
4. Laboratory Control Sample Recovery (Torn III, All Fractions)
5. Method Blank Su ry (Tori IV, All Fracrion.s)
6. GC/XS Tuning and Mass Calibration (Form V LCV, LCSV)
7. Initial Calibration Suaury (Form V I, All Fractions)
8. Pesticide Resolution Check Stmary (Porn VI LCP.4)
9. Continuing Calibration St ary (Torn VII LCV, LCSV)
10. Calibration Verification St ary (Tori VII LC’)
11. Internal Standard Area and Retention Tine Stn ry (Torn VIII LCV,
LCSV)
12. Pesticide/A.recler Analytical Sequence (Porn Viii L,CP)
1]. Pesticide/A.roclor Florisil Cartridge Check (Torn LX LCP)
14. Peseicide/Aroclor Identification (Form X LCP)
15. Sample Log-In Sheet (Porn DC-i)
16. Document Inventory Sheet (Torn DC-2)
1 -24 10/92
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I .. GENERAL INFQRI1A ’f ION AND H!.ADER IN10RXAI
1.1 Values shall be reported on the hardcoPY forms according to the
individual form LnstruCtiOn1 in this Section. For example, results for
concentrations of VOA target compounds shall. be reported to two
significant figures if the value is greater than or equal to 10.
1.2 For rounding off numbers to the appropriate level of precision, observe
the following coOfl rules. If the figure following those to be
retained is less than 5, drop it (round down). If the figure is
greater than 5, drop it and increase the last digit to be retained by 1
(round up). If the figure following the last digit tO be retained
equals S exactly, round up if the digit to be retained is odd, and
round down if that digit is even.
1.3 811 characters which appear on the data reporting forms presented in
the contract (Exhibit 8, Section IV) shall be reproduced by the
Contractor when submitting data, and the format of the forms submitted
, hpll be IdentiCal to that shown in this Superfund method. No
informat .ofl may be added, deleted, or moved from its specified position
without p jor written approval of SMO. The names of the various fields
and compoundS (1..., ‘Lab Coda’, ChloromethanS ’) on the uncompleted
forms shall appear as they do in this Superftmd method (Section IV of
this exhibit), except that the us. of uppercase gxi lowercase letters
is optional.
1.4 Alphabetic rie made on the forms by the Contractor shall be in
UPPERCASE letters.
1.5 Fotms II, IV, V, VIII, IX, and X contain a field labeled ‘page — of —u
in the bottom left-hand corner. If the number of entries required on
any of these forms exceeds the available space, continue entries on
another copy of the same fraction SPOCifiC form, duplicating all header
information. If a second page is required, number them consecutively,
as ‘page 1 of 2’ and ‘page 2 of 2.’ If a second page is not required.
number the page ‘page 1 of 1.’ NOTE: These forms sri
fraction-specific. For example, Form II L.CV. Form II LCSV. and Form II
LCP are for different datz. Therefore. number the pages of all
three versions of Form I as ‘1. of 3, 2 of 3, sec.’ Only number pages
within a fraction SpeciftC form.
1.6 Six pieces of information are co on to the header sections of each
data reporting form. They are: Lab Name, Contract, Lab Code, Case No.,
SAS No., and SDG No. This information, if it applies, shall be entered
on every form and shall match on every form.
1.6.1 The ‘Lab Name’ shall be the name chosen by the Contractor to
identify the laboratory. It say not exceed 25 characterS.
1.6.2 The ‘Lab Code’ is an alphabetical abbreviation of up to 6
letters, jsi ned by $ , to identify th. laboratory and aid in
data processing. This lab code shall be assigned by SMO at the
time a contract is awarded, and 1 4l1 be modified by the
Contractor, except at the direction of SMO. If a change of
8-25 10/92
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name or ownership occurs at th. laboratory. th. lab coda will.
remain the same until the ConC:aCtOr La directed by SMO to use
another lab code assigned by Sf0.
1.6.3 The case No. is the assigned Case Number (up to 5 digits)
associated with the sample, and reported on the Traffic Report.
1.6.4 The Contract is the number of the contract under which the
analyses were performed.
1. 6.5 When more than one sample is received in th. first or last SDC
shipment, the first’ sample received votald be the lowest
sample number (considering both alpha and numeric
designations); the ‘last sample received would be the highest
sample number (considering both alpha and numeric
designations).
1.6.6 The SAS No. is the assigned number for analyse . performed
under Special Analytical Services. If samples are to b.
analyzed under SAS only, and reported on these forms, then
enter SAS No., and leave Case No. blank. If samples are
analyzed according to the Routine Analytical Services ( 1F3)
protocols have additional SAS’ requirements, list both
Case No. and SAS No. on all forms. If the analyses have no SAS
requirements, leave ‘SAS No. blank. NOTE: Some samples in an
SIDG may have a SAS No. while others do not.
1.7 EPA Sample Number
1.7.1 EPA Sample Number shall be entered on several of the forms.
This field appears either in th. upper rigJat .h id corner of the
form, or as rh. left col of a tabi. z’i -rizing data from a
number of samples. Jhen EPA Sample No. is entered into the
triple-spaced box in th. upper right-hand corner of the form,
it should be entered on the middle line of the this. lines thac
comprise the box.
1.7.2 U samples, including Laborato 7 Control Samples and
Performance Evaluation Samples, blanks, and standards shall be
identified with an EPA Sample Number.
1.7.3 For samples, the EPA Sample Number is the unique identifying
number given in the Traffic Report that accompanied that
sample. In order to facilitats data assessment, the following
identification scheme shall be used for samples:
— EPA Sample Number assigned by Sf0
X CRZ re-analyzed sample
) CCDL — sample analyzed at a dilution
X CCCCDL2 — sample analyzed at a secondary dilution (for PEST
only)
3-26 10/92
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1.7.4 The EPA Sample Number J all be .rnicu . for each Laboratory
Control Sample within an 50G. The EPA Sample Number for a
Laboratory Control Sample shall be FLCS#*, where:
F — fraction (V for volatiles; S for seaivolatjjes; P for
pesticide.i/Aroclors).
LCS indicates a Laboratory Control Sample.
— suffix consisting of characters or numbers or both that
makes the EPA sampie Number for the LCS unique in the SDC.
1.7.5 The EPA Sample Number shall be uniaue for each blank within an
SDG. Within a fraction, a laboratory shall replace the u a
terminator of the identifier with one or two characters or
numbers, or a combination of both. For example, possible
identifiers for volatile blank.., would be VBLX1 , VBLKi, VELXAI ,
V L (32. VBLX1O, VBLXA3, etc.
Volatile method blanks shall be identified a.s VBL
Volatile storage blank shall be identified in vszLx##.
Volatile instrument blank shall be identified as VIM. *
Semivolatjle method blanks shall be identified as S3L fts.
Peseicide/A.roclor method blanks shall be identified as p uc# .
Pesticide/Aroclor instrument blanks shall be identified as
PI3UC ..
If a. separate sulfur cleanup blink is required (e.g., when not
all Pescicide/Arocior samples assoc ated with a given method
blank are subjected to sulfur cleanup) the Pesticide/Araclot
sulfur cleanup blanks shall be identified i.e PC3LX.*..
1.7.6 The EPA Sample Number shall be wiicue for oath standard vithj
an SOC.
The EPA Sample Numbers for volatile and eamivolatile etantiard.,
shall be ISTD , where:
F fraction (V for volatiles; S for seaivolatjleg).
STD — indicates a standard.
the concentration in ug/L of volatile standards (i.e.,
001, 002, 005, 010) or the amount injected in ng for
semivolatile standards (i.e., 005, 010, 020, 050, and 080).
These designa iona till have to be concatenated with other
information to uniquely identify each scardard in the SDG.
8-27 10/92
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For pescicide/Ar0C 0r standards, the followthg icheac shall be
used to enter EPA Sample Number.
g Sa le Number
Individual Mix A (low point) INDAL#
Individual Mix A (aid point) INDAM *
Individual Mix A (high point) INDAH#
Individu*1 Mix 8 (by point) IND3L#*
Individual Mix I (aid point) INDIM#*
Individual Mix I (higi’ point) IIID3B#
Resolution Check RZSC
Performance Evaluation Mixture
Toxaphens TOXAPH#
Aroclot 1016 AR1O16#*
Aroclor 1221 A&1221*
Azoclor 1232 AR1232#*
Aroclor 1242 AR12 42 #*
Aroclor 1248 ARl248
ArQc] .or 1254 ARi.254#*
Ar clor 1260 AR1260**
Aroclor 1016/1260 AR166O#*
The Contractor shall create a miquS EPA Sample No. • within an
SDC by replacing the two_character u## tsrsinator of the
identifier with one or two characters or numbers, or a
combinatiOn of both.
If the standards are injected onto both GC col a on the same
i str eflt sj*u_lranso’ual7. the sass EPA Sample !i b.r say be
used for rsporting data for the standards for both co1 s. If
simultaneous injections rs fl2. . then the sass n b.r say
be used.
1.8 Several other pieces of infors*tioU are co o to the header
information on some of the data reporting forms. These include: Lab
Saap]e ID, Lab File ID, Purge or Sample Volt e, CC Col - ID,
IU3tn Cnt ID, Time Analy2ed , Data Received, Extracted, and Data
Analyzed.
1.8.1 •Lab Sample 1D is an optio *l laboratorY genarated internal
identifier. Up to 12 alpha nuaertc characters may be reported
her..
1.8.2 1ab File 1D is the 1aboratOrYZeflet ttd name of the CC/MS
data system file containirtg information pertaining to a
particular analysis. Up to 14 l ha nUII5ric characters say be
used here.
1.8.3 Purge Volume or Sampl e Volume is the total volume of water
that was purged or extracted, in milliliters.
g-28 10/92
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1.8.4 There ar. — - - fields to be .nt .tsd under CC Column - ID. ’
Enter the stationary phase of the CC column after ‘cc Column’
and enter the thcernal diameter in millimeters after ‘ID’
1.8.5 ‘Irtstrument ID ’ La the identifier that distinguishes each
instrument used for analysis Ln the SDG.
1.8.6 The TLme Analyzed’ shall be in military ti m ..
1.8.7 ‘Dat. Received’ is the date of sampl. receipt at the
laboratory, a.s noted on the Sample Traffic Report (i.e., the
Validated Time of Sample Receipt). ‘Dat. Received’ is entered
as MM/DD/YY.
1.8.8 Enter the data on which the extraction procedure was started
for ‘Date Extracted.’ ‘Date Extracted’ is entered LI *(/DDP1Y.
1.8.9 For each fraction, the ‘Date Analyzed’ is the date of the
sample analysis. The data of sample receipt viii be compared
with the extraction and analysis dates of each fraction to
en .Iure that contract holding times vera not exceeded. ‘Data
Analyzed’ is entered as MX/DD/YY.
1.9 For pesticide/Arociors, analyses on two CC columns are required. The
information on the two analyses is differentiated on some of the forms
as ‘Date Analyzed (1)’, ‘Date Analyzed (2)’, etc. The order of
reporting is not important, but shalL be consistent with the
information reported on Form X. When simultaneous injection La made on
both CC column,, the dates (and times) will be the seas. If
simultaneous injections are mad ., the (1) shall refer to the first
analysis, and (2) the second. If only one analysis is required, leave
the fields for the second analysis blank.
2. PICANIC A ALTSIS DATA 5 E!T (YQRX I )
2.]. Target Compounds. Form I LCVI LCSV1, LCSV2, and LCP
This form is used for reporting the dot.cted concentrations of the
target compounds in the samples, Laboratory Control Samples,
Performance Evaluation S&iplee, and all blanks analyzed, including
method blanks, instrument blanks, sulfur cleanup blanks, and storage
blank.i.
Complete the header information on each Form I required, according to
the instructions in paragraph 1.
Enter 1 for the ‘Dilution Factor’, if a sample va.s not diluted or
concentrated for analysis. If a simple has been diluted for analysis,
enter the ‘Dilution Factor’ as a single number, such as 100 vhen a
sample is diluted by a factor of 100. Enter 0.1 wher a sample is
concentrated by a factor of 10.
For volatiles, the ‘Purge Volume’ La the total volume (in ml..) purged
for the analysis.
3-29 10/92
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P - This flag is used for a . 5 cicid./Az ’0db0r target analyta when
there is a greater’ than 25.0% differenCe between the
concentration calculated fro. th. two GC colusna (see Form X).
The ç er of the two values is reported on Form I and flagged
with a
X - Other specific flags .ay be required to properly define the
results. If used, they shall be fully described and such
degcriptiOfl attached to the Sample Data SwmFf Package and the
SOC Narr’atiVe. Zegifl by using X. If mars than on. flag is
required, u .s . 1’ and Z’. as nsedsd. If mare than five
qualifiers are required for a sample result, use the X• flag
to combifle several flags, as nesdad. For instance, the X
flag might combine the A’, ‘V. and ‘0’ flags for some sample.
2.2 Non-target Compounds. Form I LCV.TIC and LCSV-TIC
Fca I LCV-TIC and LCSV-TIC are used for reporting the tentative
i enti ication and estimated concentration for up to 10 of the non-
surrogate and non-target organic compounds in the volatile fractIon and
up to 20 of the non-surrogate and non-target organic compounds in the
semivolatile fraction.
Include a Form I LCV-TIC or LCSV-TIC for every volatile and
samivolatile fraction of every sample, Performance Evaluation Sample,
and blank analyzed. Form I LCV-TIC or LCSV-TIC shall be provided for
erv anal sli (except for the Laboratory Control Samples) that
:equires a Fora I for target compound1 . including required dilutions
and reaxialyse s , even if no TICS are found.
Fill in all header inforP Iti0fl as in Section 2.].
Report tentatively identified compounds (TICS) including CAS number,
compound name, retention time, and the estimated concentration
(criteria for re?orting TICs are given in Exhibit 0). Retention time
shall be reported in minutes and decimal minutes, not seconds or
minutes and seconds.
If in the opinion of the mass spctr’ interpretation specialist, no
valid tsntativs identificatiOn can be mada, the compound shall be
reported as g cnoVfl .
Total th. number of TICs found and enter this number in the ‘Number
TICs found.’ If no TICs were found, entar ‘0’ (zero).
If the name of a compound exceeds the 28 spaces in the TIC column,
truncate the name to 28 characterS. If the compound is an un3cnovn,
restrict descriptiOn to no more than 28 characterS (i.e., tmlctovn
hydrocarbon. etc.).
All TIC results, except ‘generics’ (See N flag) are flagged JN’ in the
‘Q ’ colu t to emphasize the quantitatiVS qualitative uncertainties
associated with these data. This includes ‘unknowns.’
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S. SURROGATE PECO ’Y . FOIU1 II LCV. LCSV - AND IC !
Form II is used to report the recovery of the surrogate compounds added
to each sample. blank. aboratOry Control Sa.zspl., and Performance
Evaluation Sample.
Complete the header information on each Form ii required, according to
the instructions in paragraph 1.
In the table, enter EPA Sample NumberS for each analysis as described
in paragraph 1. For each sample, report the percent recovery for each
surrogate to the nearest whols number.
Flag each surrogate recovery outjid the QC limits with an asterisk
(*). The asterisk shall be placed in the last space in each appropriate
column, under the 0 symbol. In the far right-hand column, total the
number of surrogate recoveries outside the QC limits for each sample.
If no surrogates were outside the limits, enter 0.’
If a sample or extract is diluted and the surrogate recovery is below
the recovery limits in any analysis, enter th. calculated recovery or
0 (zero) if the surrogate is not detected. Flag the surrogate
recovery with a ‘D in the column under the 1 symbol. Do n include
results flagged D in the total number of recoveries for each sample
outside the QC limits.
Pesticide/ArOClOr samples are analyzed on two CC columns, and
surrogates recoveries shall b. reported for both analyses. Enter the
inforaation on the stationary phases and internal diameters of the two
CC columns, as described in paragraph 1.8.4, differentiating the CC
columns as (l) and (2). Enter the recoveries of the two surrogates
for each column in a similar fashion.
Number the Form II pages as described in paragraph 1.5.
4. La opXrORT CQFT OL SANPI2 RZCOVEP Y. TOBI( TI! LCV. LCSV. AND C1P
Form III is used to report the recovery of the spiked ..n.alytu in the
Laboratory Control Sample (LCS).
Complete the header information on each Form iii required, according to
the instructions in Sections 1 and 2.
The LCS Lot No. • is an identification number assigned to th. LCS
spiking solution, if the so1utio is provided wider thLS contract.
If the LCS solution is purchased by the Contractor from a third party,
report the identification number used by the laboratory under ULCS Lot
No.
The • .CS Aliguot is the volume in aicroliters of LCS spiking solution
that was added tO reagent water before purging or extraction.
For pesticides. the LCS is reported for both CC columnS. Enter the
Instrument ID and CC Column - ID for analyses on both CC columns. The
3-33 10/92
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order of reporting is not important, but shall be consistent with the
information reported on Form X. If simultaneoua injections are
made, the ‘Date Analyzed’ La the earlier date of the two LCS analyses.
In the upper box in Form III, under • 3 ADDED’, enter th. amount in
nanograms of each analyte added to the sample. Under ‘AMOQNT
p (ytJ p fl. enter tie amount in nenograms of each analyt. in the sample
calculated from analysis. Calculate the percent recovery of each
compound in the sample to the nearest whole percent, according Co
Exhibit D, and enter under % EEC.’ Enter the limits for each s.nslyes
in the column for ‘QC LIMITS. • The limits should b. sneered as two
whole numbers (lover and upper limits) separated by a hyphen. Flag all.
percent recoveries which do not me.t the contract requirements with an
asterisk (*). The asterisk aL ll be placed in the last space of the
percsnc recovery column, under the # symbol.
SLtn Rrize the values outside the QC limits at the bottom of the page.
5. XET 0D 3L NI S XAM. FQRX IV LCV. LCSV. AND LCP
Form IV lists the sample. including LCS and PES associated with each
method blank. A copy of the appropriate Form IV is ruquired for each
method blank.
Complete the header information on each Form IV required, according to
the in.,truction.s in Sections 1..
For semivolatils and peseicide/Aroclor method blanks, enter the dat. of
extraction of the blank.
For pesticida/Aroclots , enter th. ‘flats Analyzed’, ‘Tine Analyzed’,
‘I tr nt ID’. and ‘CC Colu - ID ’ for analyses on both CC columns.
For all three fractions, as appropriate, s”’rize the samples,
including LCS and I’ES associated vith a given method blank in tlie.table
b 1ow the header, entering EPA Sample !h b.r and Lab Sampl. ID. For
volatiles enter the Lab File ID and Time Analyzed for each sample.
For seaivolatilei, enter the Lab File ID and flats Analyzed. For
pesticides/Aroclors. enter the Data Analyzed on each CC colu for each
sample.
I
For pesticides/A.roclors, enter ‘Y’ or N ’ (for yes or no) under ‘Sulfur
Cleanup.’ If a separate sulfur cleanup blank ii prepared, when all
samples associated with a method blank are subjected to sulfur cleanup,
then complete a Form IV for the sulfur cleanup blank, listing
the EPA Sample No. of the blank, ma described in paragraph 1.9.6, in
the box in the upper right hand corner of th. form. These samples
associated with the sulfur cleanup blank will be listed in the lower
portion of the form, as well as on a copy of Form IV for their
associated method blank. Whenever all the samples and their associated
method blank are subjected to sulfur cleanup, no separate sulfur blank
is required, and only one Form IV need.s to be completed.
Number the Form IV pages as described in paragraph 1.5.
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6. CC/M5 ru 4fl C #IND MASS CALThP.ATIOL YOBM V LCY AND LCSV
This form is used to report the results of CC/MS tuning for volatites
and semivolaCiles, and to 3 t . . ., ,i rtze the date and time of analysis of
amples, standard-s. and blanks associated with each CC/MS tune
(including Laboratory Control and erform ce Evaluation Samples).
Complete the header information on .ach Form V required, according to
the instructions in paragraph 1.
Enter the Ub Fil. ID ’ for th. injection containing the CC/MS tuning
compound (BFB for ‘colatiles, DFTPP for semivolattl e s). Enter the date
and time of injection of the tunir. compoui d. Enter injection time as
military time.
In the upper table, for each ion listed on the form, enter the t
Relative Abundance in the right -hand column. Report relative
abundances tO the number of significant figures given for each ion in
the ion abundance criteria colt .
Note that for both 3F8 and DF1 PP. one or more of th high mass ions may
exceed the abundance of the ion Listed on the form is the base peak
(m/Z 95 for BFB, and m/z 198 for DFI’PP). Despite this possibility, all
ion abundances are to be normalized to the nominal base peaks listed on
Form V (see Exhibit D).
All relative abundances shall be reported as a numb.r. If zero, enter
‘0’ not a dash or other non-numeric character. h.re parentheses
appear, compute the percentage of th. ion abundancs of th. sass given
in the appropriate footnote, and enteV that valu in the parentheses.
In the lover half of the form, list all samples. standards, and blanks
axtalyz: f under that tune i? hron0l0 dl order , by time of analysis
(in military time). Refer tO paragraph 1 for specific instructions for
identifying standards and blanks. Enter E1’A Sample No.’, ‘Lab Sample
ID’, ‘Lab File ID • ‘Data Ax%.alyZe1d. and Time Analyzed for all
ndtrds, samples including LCS and PES, and blanks.
Number the Form V pages as described in paragraph 1.5.
7. IIITr1AL CALI3RATION SWO1AR’T. TOV( V I LCV. LCSV1. LCSV-2. LCP-l. LCP1
AND LC?-1
For each fractIon, after a GC/MS or CC system has *md rgone an initial
calibration, and after aU initial calibration technical criteria hays
been met, the Contractor shall complete and subait all Form VIa for
initial calibrations performed relevant to the samples including LCZ
and P1.5 and blanks in the SDG, regardless of when that calibration was
performed.
Complete the header information on each Form VI required, according to
the instructions in paragraph 1.
3-35 10/92
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Enter the Caae No.’ and ‘SDC No. for the current data package,
regardless of the original Case for which the initial calibration was
performed. Enter ‘Inserusent ID’ and Calibration Date(s).’ If the
calendar dat. changes during the calibration procedurs, the inclusive
dates should be given on Fore VI.
For the volatile and seajvolatjle fractions, enter the ‘Lab File ID ’
for each of the five calibration standards injected. Coaplet. the
response factor data for the five calibration points. The relative
respons, factor (BPS) La reported for each t.arg.c coapo md and
surrogate. The Contractor shall r.port th. average REP and the percent
relative standard deviation (%RSD) for th. iRis for each target
coapound and surrogate.
The initial calibration of pesticides and Aroclor . involves the
determination of retention tises, retention time windows, and
calibration factors. For single coaponent pesticide target compounds,
these data are calculated Eros th. analyses of the Individual Standard
Mixtures A and B at three different concentration levels. For the
multicoaponent target compound.s, these data are calculated froa a
single pdtht calibration.
Complete header information on Form V I, LCP-l and LCP•2 according to
the in.etructjong La paragraph 1. For th. thre. analyses of Individual
Standard Mixture A (low point, aid point, and high point), and the
three analyses of Individual Standard Mixture 3 performed on each CC
column during an initial calibration, complete ona copy of Form VI for
epch CC col used. Enter the In.str ent ID, CC Col , and ID as
described previously. Enter the dates of analysis of th. first and
last of the six standards on each form wider ’Dat.(a) Analy.d. ’ Under
‘Level (x low)’, enter the concentration of the low point, mid point,
and high pof vie calibrittion stal 4rds as ltiplier of the low point.
Therefore, for the low point, entar ‘1.0.’ Th. concentration of the
aid point standard ii specified in Thfbit D as four tises the low
point, therefore, enter ‘4.0’ for ‘aid.’ If the concentration is n
exactly 4.0 times the low point, eater the appropriat. aleiplier in a
similar format. The high point standard shall be at least 16 times the
low point, but say be higher if that value lies within the linear range
of the instrument, as specified in E hibit D. Therefors, enter the
appropriate eultiplier to the high point standard concentration to one
decimal place.
For the pesticides/A.roclors fraction, one Form VI (LCP-l and LCP.2) is
required for each initial calibration performed on each CC col . In
the table, on Form VI LCP-l, enter the retention time of each analyt.
in the low, aid, and high point Standard Mixtures £ and 3 in the
columns labeled ‘iT of Sta dzrds.’ Us. the values froa Standard
Mixture A for the surrogates. Calculate and report in the appropriate
column the mean retention tine and the retention tine windows for each
analyte. Report the retention tine window for each analyte as a range
of tvo values, i.e., from 1.44 to 1.54. Enter the lower value of the
rar e in the column under ‘iT WINDOW’ labeled ‘FROM. • Enter the upper
value of the range in the column under ‘TO. • Do flg . separate the two
values with a hyphen, and do enter the retention time window as a
3-36 10/92
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p1us/ inu.s value such aa ±0.05. NOTE: y definition, the center of the
retention tine vjndov shall be cbs sean retention tine listed to the
left of the retention tim. window.
On For3 VI LCP-2, calculata the calibration factor for each analyte in
the low. aid. and high point Standard Mixtures A and R. Use the values
froa Standard Mixture A for the surrogates. Report the valuec under
the column.s libeled CALIBRATION FACTORS. • Calculate the ean of the
three calibration factors and the percent relative standard deviation
(%RSD) for the calibration factor values for each analyr.. Report the
calculated values under the 9CEAN and %RSD colu a, respectively.
On Form VI LCP-3. for the initial calibration of ultice ponent
analytes, enter the amount of standard injected in nanogram.. of each
analyt., under the AMOUNT column. The number of peaks with an
asterisk under the Peak colt indicates the minimum number of peaks
calibrated for each analy-te. Enter the retention time of each peak
used to qu.antitata under the RT colt . Data for two additional
peaks may be reported for each multicomponent a.nalyts. Calculate and
report the calibration factor for each peak used under •CALI3RATION
FACTOR.
8. PESTICIDE 325QLUTIC CaZCX SV ART. 70R VI LCP-k
Pesticide Resolution Check Su’”isry Form VI La uaed CO report the
resolution of each analyce in the Resolution Check Mixtur. analyzed at
the beginning of each initial calibration on each CC coli .
Complete the header information on each Form VI required according to
the instruction.. in paragraph 1.
For each CC column, enter the EPA Sample Numb.r of the Resolution
Check Mixture, as described in paragraph 1.9.7 • for the mixture
injected on the first CC colt . Enter the Lab Sample ID, Dat.
Analyzed (1), and Time Analyzed (I).
In the table, under Az(ALfrV, enter the name of each analyt. as it
appears on Porm I • in elution order, starting vith’ the first target
analyte or surrogat. to slut.. Enter the retention tim . of each of the
analytes listed under RT.
Calculate the percent resolution between each pair of consecutive peaks
according to Exhibit D. Enter the percent resolution of each pair in
the R.ESOL1JTION field of h. analyc. that •lutea earlier (the analyt.
listed first). The resolution shall be calculated for each adjacent
peaks so that the resolution of peak 1 and peak 2 is calculated, as
well as peak 2 v i. peak 3, peak 3 vs. peak 4, etc. The R.ESOWTION
field will be left blank for the last analyte in the table. The
percent resolution shall meet the QC limits listed at the bottom of the
page.
Complete the information for the second CC column in the same fashion.
3.37 10/92
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9. CONTINUING CALI RATI0N SUMMARY. FORM VII LCV LCSV-l AND LCSV 2
The Continuing Calibration Suiaz’y Form VII La us•d to verify the
calibration of the CC/MS system by the analysis of specific calibration
standards. Form VII is required for each 12 hour ti m. period for both
volatile and semivolatile analysis.
Complete the header information on each Pore VII r.quir.d, according to
the instructions in paragraph 1..
Enter dat. and time of continuing calibration stait.rd analysis, the
Lab FL].. ID of the continuing calibration standard, and date(s) of
initial calibration. Civ. inclusive dates if initial calibration is
performed over more than one date. Enter the average relative response
factor (RRF) for each target compound that was calculated from the
initial calibration data (referred to in the initial calibration
date(s) analyzed field). Report th. relative response factor for each
target compound and surrogate from the continuing calibration standard
analysis.
10. PESTICID /AROCLO1 CALIbRATION VERITICATICM
Calibration Verification $wma ’7. Form VII LCP-] and LCP-2
The Calibration Verification SIt1 a 7 Fore VII is used to report the
result., of the Performance Evaluation Mixtures (P f), ins tri ent
blank.s, and Individual Standard Mixtures A and 3 analyzed at the
beginning and end of a twelve hour sequence. The Contractor shall
submit this form for each twelVe hour sequence analyzed.
Complete the header information on each Form VII required according to
the instructions in paragraph 1.
Enter the initial calibration data(s) analyzed. Give inclusive dates
if initial calibration is performed over more - “ on. date.
On Form VII, LCP-1, enter the EPA Sample No., Lab Sample ID, Data
Analyzed, and Time Analyzed for the instr’. enC blank that preceded the
tvel4e hour sequence (P 1311). For the P ( that initiated or tereinat.d
the twelve hour sequence (P Z, enter the EPA Sample No., Lab 5 aapis
ID, Date Analyzed, and Time Analyzed.
When reporting data for the P ( at the berirming of the initial
calibration sequence, leave blank the EPA Sample No.’. ‘Lab Sample
ID ’ • and ‘Date’ and •Tiae Analyzed’ fields for th. inatr snt b1 nk
(PIBLX), as n. instrument blank La analyzed before this PDI. When
reporting all other P ( analyses, the instrument blank fields shall be
completed.
In the table, report the retention time for each an.alyte in the PD( a.s
well as the retention time vindows. For each analyte in the PE (, enter
the amount of the analyte in nanogram.s, to three decimal places,
calculated to be in the P (, under ‘CALC AMOUNT. • Enter the nominal
amount of each analyte in the P 2( under NOM AMOUNT.’ Calculate the
3.38 10/92
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relative percent difference between the calculated amount and nominal
amount for each analyti according to Exhibit D. Report th. values
under %D.
Calculate the percent breakdOlJfl for endrin and 44’-DDT, and the
combined percent breakdown in the PV( according to Exhibit D. Enter
the values for the breakdown of .ndri and 4,4’-DDT in their respective
fields immediately undet the tibia.
Form VII LCP-2 is used to report the dates and times of analysis of the
instrument blanks and the results of th. analyses of the midpoint
concentrations of Individual Standard Mixtures A and S that, along with
the P (, brackst each 12-hour period of sample analyses. On. copy of
Form VII LCP-2 shall be completed each time the I dividua1 Standard
Mixtures are analyzed, for each CC co].t used. The form is completed
in a similar fashion to Form VII LCP-l. entering the EPA Sample No.,
Lab Sample ID, Date Analyzed, and Time Analyzed for the instrument
blank immediately preceding the Individual Standard Mixtures A and 5,
and for the standards themselves. The upper table on the form contains
the retention time and amount data for Individuil Standard Mixture A
compounds. The lower table contains the data for Mixture 5. Enter the
data in these tables In a fashion similar to that for the P (.
Complete copies of Form VII LCP-l and 2 for each standard reported in
Form VIII LCP.
11. INTERNAL STANDARD AREA AND RZT TION TIME SUMMARY FORM VIII LCV. LCSV-l.
AND LCSV 2
Form VIII is used to summarize the peak areas and retention times of
the internal standards added to all volatile and semivolitile samples
and blanks. Form VIII is also used to check the internal standards in
the initial calibration sequences. Th. data are used to determine when
changes in internal standard responses viii adversely affect
qu.antitation of target compounds. This form shall be completed each
time an initial calibration OV a continuing calibration is performed,
or when samples are analyzed under the same CC/MS tw s as an initial
calibration.
Coaplets the header information Ofl each Form VIII required, according
to the instructions in paragraph 1.
Enter the Lab File ID, Date Analyzed, and Time Analyzed for the
continuing calibration standard. If samples are analyzed immediately
following an initial calibraCLOfl, before another CC/MS tm. and a
continuing calibration. Form VIII shall be completed for the initial
calibration standard that is the same concentratIon as the continuing
calibration standard. Enter the Lab File ID, the date and time of
analysis, the areas and retention times of this initial calibration
standard in place of those of a continuing calibration standard.
From the results of the analysis of the continuing calibration
standard, enter the area measured for each internal standard and its
retention time under the appropriate column in the row labeled •12 HOUR
STD. For each volatile internal standard, calculate the area upper
5.39 10/92
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limit as the area of the particular internal standard pI.u.s 40 percent
of its area, and th. area lower limit as the area of the internal
standard minus 40 percent of its area. For each semivolacil. internal
standard, calculate the area upper limit as the area of the particular
standard plus 100% of its area (i.e. • two times the area in the 12 HOUR,
STD box) • and the area lover limit as the area of the internal standard
minus 50% of its area (i.e., one half the area in the 12 HoUR STD box).
Report these values in the boxes labeled 9JPP LIMIT’ arid LOVE
LIMIT’ rssp.ctively.
For each volatile and ieiiivolatils internal standard, calculat. the
retention time (RT) upper limit as the RT of the particular internal
standard plus 0.33 minutes. The lover limit is the 2 ! of the internal
standard ainu.s 0.33 minutes. Report these values in the boxes labeled
‘U?P 1 LIMIT’ and LOWE LIMIT’ respectively.
For each sample including LCS and PES and blank analyzed under a given
continuing calibration, enter the EPA Sample Number and the area
measured for each internal standard and its retention time. If the
internal-standard area or retention time is outside the upper or lover
limits calculated above, flag that value with an asterisk (*). The
asterisk shall be placed in the far right hand spac, of the box for
each internal standard area or retention time, directly under the s
symbol.
If samples are analyzed i adiataly following an initial calibration as
described above, enter the EPA Sample Number, internal standard areas,
and retention times for all fiv, of the initial calibration standards.
Number the Form VIII pages as described in paragraph 1.5.
12. PES?ICIDE/A1OCLOI ARALTZICAL SE0 ENCE. F0R vi ii LC ?
Form VIII LCP is required for each analytical sequence for each CC
system and for each CC column used to analyze pesticide/Aroclors in an
SDC.
C aplet. the header information on each Form VIII required, according
to the instructions in paragraph 1.
Enter the initial calibration date(s). Give inclusive dates if initial
calibration is performed over more than one date.
At the top of the table, report the mean retention time for surrogates
tetrachloro-.-xylene and decachlorobiphenyl calculated frog the initial
calibration sequence *mder TCXb and ‘DcZ ’ • respectively. For every
analysis associated with a particular analytical sequence starting with
the initial calibration, enter the EPA Sample Number, Lab Sample ID,
Date Analyzed, and Time Analyzed. Each sample analyzed as part of the
sequence shall be reported on Form VIII LCP even if it is not
associated with the SDG. The Contractor may use the EPA Sample No. of
‘7777- 1’ to distinguish all samples that are not part of the SDC being
reported. Report the retention time of the surrogates for each
analysis under TCX RT ’ and ‘DC3 RT.’ All sample analyses shall be
3-40 10/92
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bracketed by acceptable analyses of instrument blanks, a PD(. and
Individual 5ta d&td Mixtures A and R. Given the fact that the initial.
calibration may remain valid for soae rime (see Exhibit D), it is
necessary to report the data from 12-hour periods when g samples in an
SDG were run. The Contractor ll deliver the Form VIII for the
initial calibration sequence, and Forms that include the PEXi and
Individual Standard Mixtures that bracket and jfl samples in the
SDG. While the data for time periods between the initial calibration
and samples in the SDC is not a utine deliverable, it shall be made
available on request during on-sits eva].u.atioitl, etc. Hers again, non-
EPA samples may be indicated with 77’- .
Flag all those values which do not meet the contract requirements by
entering an asterisk (#) in the la_st column, under the *. If the
retention time cannot be calculated du. to interfering peaks, leave the
RT column blank for that surrogate . enter an asterisk in the last
(i.e., under DC3 ’) column, and document the problem in the SDG
Narrative.
Number the Form VIII pages as described in paragraph 1.5.
13. PES1ICID!/A OCLOP. FLORISIL cARTRIDGE C ECX. FORX II LC2
Form IX is required for each lot of Florisil cartridges that is used
with samples associated with the SDG.
Complete the header information en each Form IX required, according to
the Instructions in paragraph 1.
Enter the Case No.’ and ‘SDG No.’ for the current data package,
regardless of the original Cu. for which the cartridge check was
performed. Enter the ‘Florisil Cartridge Lot Numbez. Enter under the
‘Date Analyzed’, the date the Florisil cartridge check solution va.s
analyzed.
In the upper table, enter the amount of spike added and spike recovered
in nanograms for each axialyte.
Calculate to the nearest whole percent, and enter the percent recovery
in the ‘% REC’ field. Flag each spike recovery outside the QC limits
with an asterisk (*). The asterisk shall be placed in the last space
in the % Rec’ column, under the ‘# ‘ symbol.
In the lower table, enter th. ’EPA Sample No.. the ‘Lab Sample ID’,
and ‘Date Analyzed’ for each sample and blank that was cleaned up using
this lot of Florisil cartridges.
Number the Form IX pages as described in paragraph 1.5.
14. PESTICIDE/AROCLUR. IDENTIYICATION. TURM I ICY-I.. LC?-
Form X summarizes the data used to identify and quantify all
pesticide/Aroclor target analytes detected in a given sample. Form X
LCP-l is required for each sample (including PES and LCS) or blank in
Z-4l 10/92
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which any single component analytes La detected. Form X LCP-2 is
required for each sample (including PES and LCS) or blank in which any
uLtLcompOflent ar%alyce is detected. If no single component an*1.yts or
multicompofleflt an.alyte is detected in a sample, no copy of the
applicable Form X is required for that sample.
Cowplete the header information on each Form X required. according to
the instructions in paragraph I ..
For each target pesticide or £roc]Or detected, enter the name of th.
analyte on Form X in the col labeled Analyte, spelling the name as
is appears on Form I. For the uu ] .ticompofleflt analytei • there are
spaces (fields) for up to 5 peaks for each analyte. The asterisks
indicate the number of peak3 that are required. and data for additional
peaks may be reported. The retention time, retention time window, and
concentration are calculated separately for each peak used for a
multicomponent an.alyte. For each CC co].t . enter the retention times
of the analytes detected in the sample next to the appropriate column
designation (1 or 2). Enter the retention time windows on each column
of the appropriate standard. The lover value is entered wider the
FROM cQlumn, the upper value under the T0’ col% . Do not use a
hyphen. These data shall correspond with those on Form VI, and are
entered in a similar manner. Calculate the concentration of the analyte
using the calibration factors derived from the initial calibration
sequence. For the multicompoflent analytes. calculate and report the
mean concentration by averaging the concentration values from the peaks
used for quantitation. Calculate a nd report the percent difference to
a tenth of a percent between the concentration values (or mean
concentration values for ulticompofleflt ane]yts) on the two CC colt a
under •% • as described in Exhibit D.
Number the Form X pages as described in paragraph 1.5.
THE POLWVING AU DOCW Z cOfI3OL 7OL
çro be submitted as hardcopy only)
15. SA) PT ! LOG-IN s zZT (TORtI DC-fl
This form is used to document the receipt end inspection of samples and
containers. On. original of Form DC-i is required for each sample
shipping container. If the samples in a single sample shipping
container (e.g.. coolers) she].]. be ssigned to more than on. Sample
Delivery Group, the original Form DC-i ibmil be placed with the
deliverables for the Sample Delivery Group with the lowest sample
number and a copy of Form DC-]. shall be placed with the deliverables
for the other Sample Delivery Group(s). The copies should be
identified as copy(ies). and th. location of the original should be
noted on the copies.
Sign and date the airbi].]. (if present). Examine the shipping container
and record the presence/absence of custody seals and their condition
(i.e.. intact, broken) in item 1 on Form DC-i. Record the custody seal
numbers in item 2.
3-42 10/92
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Open the contatnsr. remove the enclosed sampie documentation, and
record the presence/absence of chain-of-custody record(s), SMO forms
(i..., Traffic Reports, Packing Lists), and airbilis or airbill
stickers in items 3-5 on Form DC-i. Specify if there is an airbill
present or an aLrbiiL sticker in item 5 on Form DC-i. Record the
.airbill or sticker number in item 6.
Remove the samples from the shipping container(s), exaaLn. th. samples
and the sample tags (if present), and record the condition of the
sample bottles (i.e., intact, broken, leaking) and presence of absence
of sampl. tags in items 7 and 8 on Form DC.l.
Review the sample shipping documents and complete the header
information described in Part A. Compare the information recorded on
all the documents and samples and mark the appropriate answer in item 9
on Form DC-i.
If there are no problems observed during receipt, sign and date
(include time) Form DC-i, the chain-of.cu.stody record, and Traffic
Report, and write the sample numbers on Form DC-i. Record the
sppropriace sample tags a.nd assigned laboratory numbers if applicable,
The log-tn date should be recorded at the top of Form DC-i and the date
and time of cooler receipt at the laboracory should be recorded in
items 10 and ii. Cross out unu.sed columns and spaces.
If there are problems observed during receipt or an answer marked with
an asterisk (1..., ‘absent*) was marked, contact SMO and document the
contact as veil as resolution of the problem on a CL? Co unicaeion
Log. Following resolution, sign and date the forms as specified in the
preceding paragraph and note, where appropriate, the resolution of the
problem.
Record the fraction designation (if appropriate) and the specific area
designation (e.g., refrigerator number) Lu the Sample Transfer block
l3cated in the bottom left corner of Form I. Sign and data the Sample
Trans far block.
16. D0CV1 INT i v H’rQRT S EZT (‘FQRX DC
This form is used to record the inventory of the Complete SDG File
documents and coimt of documents in the original Sample Data Package
which La sent to the Region.
Organize all complete SDG file documents as described in Exhibit 3,
Section II, paragraph 5 As emble the documents in the order specified
on Form DC-2, and stamp each page with a consecutive number. (Do not
number the DC-2 form). Inventory the CSF by reviewing the document
numbers and recording page number ranges in the columns provided in the
Form DC-2. If there are no documents for a specific document type,
enter an •NA in the empty space.
-43 10/92
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Certiin 1abor&torY specific documents r.lsted to the CSF y c fit
into a clearly defined category. The laboratory ihould review DC.2 to
determine if it is most appropriate to place them under No. 7, 8, 9, or
10. Category 10 should be used only if there is no appropriate
previous category. These types of documents should be described or
listed in the blanks under each appropriate category.
10/92
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iIBIT 0
METHOD FOR TILE ANALYSIS OP LOW CONC T3ATION VATFI FOR
PESTICIDES AND AROCLOLS
PEST D-]. 10/92
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I Le of Conteflti.
Page
SECTION I: Introduction PEST D-3
SECTION II:
Part A Sample Storage and Holding
Times PEST D-4
Part B Equipment and Standards PEST D-5
SECTION III: Instrument Quality Control Procedures
and ReqUirements
Part A - Instrument Operating Conditions PEST D-15
Part B - Calibration of the GC/ECD System PEST D-16
SECTION IV: Sample Preparation. Extraction and
Cleanup PEST D-28
SECTION V. Sample Analysis and Compound
Identification and Qu.ax titati0fl PEST D-36
SECTION VI: Sample Quality Control Procedures
and Requirements PEST D-45
PEST D-2 10/92
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SECTION I
IITrRODUCTI0N
The analytical method that followe La designed to analyze water in order to
determine the presence and concentration of th. chlorinated pesticides and
Aroclors found in the Target Compound List (Exhibit C). The majority of the
samples are expected to be from drinking water and veil/ground water sources
around Superfund sites. The method can be used for determining analyte
concentrations as low as ten parts per trillion. The method is based on EPA
Method 608. Quality control requirements are incorporated in the method in
order to maximize GC/ECD sensitivity and colun resolution and to minimize
contaninatiofl of the samples from laboratorY sources.
Resolution difficulties have been a..,sociated with the following pairs of
co pound. using this method:
o On a D3-608 or equivalent column, DDE and dieldrin; Methoxychlor and
Endrin ketone; and Endosu].fafl I and gni ma-Chlordane.
On a DB-1.701 or equivalent column, Endosulfan I and ga!m La-ChlOrda.fle and
Methoxychlor and Endosulfan sulfate.
PEST D-3 10/92
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sEc-r 0t( II
PART A SMPLE STORAGE AND }iOLDINC TIflES.
I .. PRQC!DCR!S FOR. SA IPL STORAGE
The samples shall be protected from ligi t and refrigerated &C eC
(.±2C) from the time of receipt w cL]. 60 days after delivery of a
complete reconciled sample dat.a packag. to the Region. After 60 days
the samples may be disposed of in a wu er that compliss with all
applicable regulations.
The samples shall be atored in an atmosphere demonstrated to be free of
all potential contaminant, and in a refrigerator used only for storage
of samples received under this contract.
Sample., sample extracts, and standards shall be stored separately.
2. fROC DURZ T0R SA11 PL I1RACT STORAGE
Sample extracts shall be protected from lig ae and stored at 4’C (±2C)
until 365 days after delivery of a complete data package to the Region.
Sample extracts shall be stored in an atmosphere demonstrated to be
free of all potential contaminants.
Samples, sample extracts, and standards shall be stored separately.
3. C )NTP.Ac7 Z0U ED HOLDING TIMES
The extraction of al]. samples shall be started within 5 days of the
Validated Time of Sample Receipt (VTSR).
Analysis df samples shall be completed within 40 days following the
start of extraction.
PEST D-4 10/92
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‘ART B - EQUIPMENT AND STANDARDS
4. 51T)OIARY OF MZTHOD
4.1 A one liter aliquot of simple is spiked With the surrogate solution and
extracted with methylene chloride by using a continuous liquid-liquid
extractor. The methylene chloride extract is dried and concentrated,
exchanged to hexane, cleaned up to remove interferences, and adjusted
to a final volume of 2.0 iL ..
4.2 The hexan. extract is injected onto two vids-bor. capillary colt %.s in
a gas chromatograph (CC). The gas chromatograph is temperature
progra. ed to separate the pesticides and Aroclora which are then
detected with an electron capture detector (ECD). Calibration and run
sequence specifications of the CC/ECD method apply independently to
both CC columns.
4.3 A single component pesticide is identified if a peak is detected within
its appropriate retention time window on each of two CC columns.
Quantitative analysis of pesticides/Aroclors shall be accomplished by
the external standard method. Single component analytes and the
surrogates shall be analyzed at thre. concentrations during the initial
calibration.
4.4 Toxaphena and Aroclors are identified primarily by pattern recognition,
but retention times of three to five major peaks shall also be taken
into consideration. Single-point calibrations for multicomponent
analytea are sufficient for quantitatton by this method. Standards for
identified Aroclors and Toxaphene shall be run within 72 hours of the
sample analysis In which they were observed. These standards are used
to verify identification only; quantitacion is based on the standards
analyzed during initial calibration.
5. INmKPEPZNCES
5.1 Method interferences may be caused by contaminants in solvents,
reagents, glassware, and sample processing hardware. These
contaminant, lead to discrete artifacts or to elevated baselines in gas
chroa.atogrw. Thea. materials shall be routin.ly demonstrated to be
free from interferences under the sample preparation and analysis
conditions by analyzing instrument blanks and method blanks.
Interferences caused by phc.halae . esters can pose a major problem in
pesticide analysis. Because co on flexible plastics contain varying
amounts of phthalates which ar. easily extracted during laboratory
operations • cross-contamination of glassvar. frequently occurs when
plastics are handled. Interferences from phvhalaces can best be
minimized by avoiding the use of such plastics in the laboratory.
5.2 Matrix interferences may be caused by contaminants that are co-
extracted from the sample. The extent of matrix interferences will.
vary- considerably from source to source 1 depending upon the nature of
the site being sampled. The cleanup procedures in Section 13 shall be
used to remove such interferences in order to achieve the Contract
Required Quantitation Limits (CRQL).
PEST D-5 10/92
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6. APPAP.AT 7S AND MATERIALS
Brand names, suppliers, and part nuab.rs are for illustrativ. purposes
only. Jo endorsement is implied. Equivalent performance may be
achieved using apparatus and materials other than chose specified here,
but demonstration of equivalent performance meeting the requirements of
the method is the responsibility of the Contractor.
6.1 Gas Chromatogr&ph/EleCtr0 Capture Detector (GC/ECD)
,.t.1 Ca.. chromatogriph
6.1.1.1 The gas chromatograPh (CC) system shall regulate
temperature in order to giv, a reproducible
temperature program and have a flow controller that
maintains a constant column flow rate throug1 out the
temperature program. The system shall be suitable
for splitlesi injection and have all required
accessories including syringes, analytical colurLl,
and gases.
6.1.1.2 Cu chromatogr*PhS that are available from some
manufacturers may have difficulty in meeting certain
method qc requirements because of Endrin and DDT
breakdown in the injector. This problem can be
minimized by operating the injector at 200-205’C,
using a bx i (not quarts) methyl silicons
deactivated injector liner, and deactivating any
metal parts in the injector with dichiorodimethyl
silazis. In some cues, using a 0.25-inch packed
column injector converted for use with 0.53
capillary columns works better thin a Grob-type
injector. If a Gr typ4 inlector is used, a 4
liner may be required to meet breakdown criteria.
6.1.2 Gas Chromatograph Columns
6.1.2.1 Two wide-bore (0.53 ID) fused silica CC colu=ts
are required. A separate detector is required for
each col . The specified analytical colt s are a
D5.1701. 30 m z 0.53 — ID, 1.0 * film thickness,
j&w Scientific, Folsos, CA, and a D5-606, 30
0.53 — ID, 0.5 to 1.0 um film thickness from .I&W
Scientific. Equivalent columns may be employed if
they meet the requirements in Section III.
6.1.2.2 Columns are mounted in 0.25-inch injector ports by
using glass adapters available fro. a variety of
co miercial sources (J&V Scientific, Supelco, Inc.,
Hevlett.Packard, Varian, Inc., Perkin Elmer, or
equivalent). The two columns may be mounted into a
single injection port with a tee adapter, (Supelco,
Inc., Bellefonte, PA, Catalog No. 2-3660, or
equivalent). Use of this adapter allows
PEST D-6 10/92
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simultaneous injection Onto both columns.
Laboratories sho*.tld follow the manufacturer’s
reco eridacion on mounting 0.53 capillaries into
injection ports.
6.1.3 The carrier gas for routine applications is helium.
Laboratories ma)? Choose to use hydrogen as a carrier gas, but
they shall clearly identify its use in the SDG Narrative and on
£11 divider pages preceding raw chrowatographic data in
submissions. Laboratories that choos. to us. hydrogen are
advised to exercise caution in its use. Us. of a hydrogen leak
detector is highly recc ended if hydrogen is used as a carrier
gas. All CC carrier gas 1 inca shall be constructed from
stainless steel or copper tubing. Non.polytetraf luoroechy lene
(PT Pt) thread sealants, or flow controllers with rubber
components are not to be used.
6.1.4 Electron Capture Detector - The makeup gas shall be p - S , p.j
(argon/methane) or nitrogen according to the instrument
specification. The GC/ECD system shall be in a room in which
the atmosphere has been demonstrated to be free of all
contaminants which say interfere with the analysis. The
instrument shall be vented to outside the facility or to a
rapping syste, which prevents the release of conta. inants into
the instrument room.
6.1.5 Data Syscas - A data system shall be interfaced to the CC/ECD.
The data system shall allow the continuous acquisition of data
throughout the duration of the chrosatographic progras and
shall permit, at the minimum, the output of time vs.
(peak height or peak area) data. Also, the data system shall
be able to rescaic chros.atographic data in order to report
chrom.atograas meeting th. requirements listed within this
method.
6.2 Glassware - A set of glassware sufficient to meet contract requirements
shall be reserved for exclusive us. in this contract.
6.2.1 Continuous liquid- liquid .xtractors equipped with Teflon or
glass connecting lines for use with aethylene chloride
(Hershberg-Wolf Extractor, Ace Glass Company, Vineland, NJ. P/N
6841-10, or equivalent).
6.2.2 Concentrator tube - Eudern.a-Danish, 10 aL, graduated (1 onte ,
Vinalaxid, NJ X -570050-1025 1 or equivalent).
6.2.3 Evaporative flask • )Cuderna .Danish, 500 mL (Kontes K-57000].
0500, or equivalent). Attach to concentrator tube vith
springs.
6.2.4 Snyder column - Kuderna-Danish, three-ball macro (Xontas
K-50300-0121, or equivalent).
PEST D-7 10/92
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6.2.5 Drying column, chroElatograPhic column epproxi .ately 400 long
x 19 ID, with coarse frit. (Substitution of a small pad of
disposable Pyrex glass wool for the frit will help prevent
cross.cofltamiflation of sample extracts.)
6.2.6 Pipet. Volumetric 1.00 eL or 2.00 mL (optional).
6.2.7 Z1icrosyringe, 1.0 uL and larger, 0.006 inch ID needle.
6.2.8 Syringe, 1.00 L or 2.00 eL (optional).
6.2.9 Flask, Volumetric 10.00 iL.
6.2.10 Flask, Volumetric 1.00 .L or 2.00 aL (optional).
6.2.11 Snyder column. micro two or three ball with a 19 ground
glass joint.
6.2.12 Glass vials minimum of 20 al., with screw cap and Teflon or
Aluminum foil liner.
6.2.13 Vials, 10 ml ., with screw cap and Teflon liner (optional).
6.2.14 Vials and caps, I or 2 aL for GC auto samplet.
6.2.15 Bottle or test tube, 50 al. , with Teflon-lined screw cap for
sulfur removal.
6 .2.16 Centrifuge tubes, calibrated, 12 al., for sulfur removal.
6.2.17 Micropipet, 250 uL, with disposAble tips.
6.3 pH Paper, wide range.
6.4 Boiling chips. -
6.6.1 Silicon carbide boiling chips, approximately 10 to 40 mesh.
Heat the chips to 400’C for 30 minutes or solvent rinse before
use.
6.4.2 Teflon boiling chips (optional). Solvent rinse the chips
before use.
6.5 Water bath, heated, with co ce tric ring cover, capable of temperature
control. NOTE: To prevent the releaSe of solvent fumes into the
laboratory, the water bath shall be used in a hood.
6.6 Balance. Analytical, capable of accurately weighing ±0.0001 g. The
balances shall be calibrated with class S weights once per each 12-hour
vorkshift. The balances shall also be annually checked by a certified
technician.
6.7 Nitrogen evaporation device equipped with a heated bath that can be
maintained at 30 to 35’C (N-Evap by OrganomatiOn Associates. Inc..
PEST D-8 10/92
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South Berlin, MA, or squivalent). To prevent the r.leas. of solvent
fumes into the laboratory, the nitrogen evaporation device shall b.
used in a hood.
6.8 Florisil Cleanup Equip eflt
6.8.1 Florisil bonded silica. 1-g cartridges with stainless steel or
Teflon fritz, Catalog No. 694-313 (Ana].ytichea, 24201 Frampton
Ave., Harbor City. CA, or equivalent).
6.8.2 Vacuum system for eluting multiple cleanup cartridges. Vac
Elute Manifold, AflalytiChem International (J.T. Baker, or
Supelco) or equivalent.
6.8.3 Vacuum trap aade from a 500 mL sidearm flask fitted ‘with a one-
hole stopper and glass tubing.
6.8.4 Vacuum pressure gauge.
6.8.5 .ack for holding 10 iL volumetric flasks in the manifold.
6.9 Mechanical shaker or mixer, for sulfur removal.
7. REAGENTS
7.1 Sodium su.lfats, granular.&nhydloUl reagent grad. • heated at 400C for 4
hours, or at 120’C for 16 hours, cooled in a desiccator, and stored in
a glass bottle. Each lot shall be extracted with hexane and analyzed
by CC/ECD to demonstrate that it is free of interference before use (J.
T. Baker arihydrou.s granular. Catalog No. 3375, or equivalent).
7.2 Methylene chloride, hexane, acetone, toluerte, iso-octane, and methanol
(optional), pesticide quality, or equivalent. It is reco sended that
each lot of solvent be analyzed to demonstrate that it is free of
interference before it is used. Methylefle chloride shall be certified
as acid free or shall be tested to demonstrate that it is free of
hydrochloric acid. Acidic aethylerte chloride shall be passed through
basic alumina and then demonstrated to be free of hydrochloric acid.
7.3 Mercury, triple distilled, for sulfur clean-up.
7.6 Copper powder (optional), fine, granular (MallinckrOdt 4649 or
equivalent). Copper may be used instead of mercury for sulfur clean-
up. Remove oxides by treating with dilute nitric acid, rinse with
distilled water to remove all traces of acid, rinse with acetone, and
dry under a stream of nitrogen.
7.5 Sodium hydroxide solution (10 N). Carefully dissolve 40 g of NaOH in
reagent water and dilute the solution to 100 aL.
7.6 Concentrated sulfuric acid, (Sp. Cr. 1.84).
7.7 Nitric acid, dilute, for sulfur removal with copper.
PEST D-9 10/92
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7.8 Reagent water. Reagent water is defined as a water in which no target
analyte is observed at the CRQL for that compound.
7.8.1 Reagent water may be generated by passing tap water through a
carbon filter bed containing about 453 g (1 lb.) of activated
carbon (Caigon Corp.. FiltrajOrb 300 , or equivalent).
7.8 .2 Reagent water may be generated using a water purification
system (Millipore Sup.r-Q or equivalent).
7.9 Ten percent acetone in bexaxis (v/v). Prepare by adding 10.0 ml. of
acetone to 90.0 L of hexans. NOTE: Prepar. this mixture accurately
or the results from the Fiorisi]. cartridge cleanup viii b. adversely
affected. Water in the acetone viii also adversely affect F].orisil
performance.
8. sTA.NDARDS
8 . 1 The Contractor shall provide all standards to be u.ied with this
contract. The. . standards may be used only after they hav, been
certiftea. The Contractor shall be able to verify that the standards
are certified. Manufacturer’s certificates of analysis shall be
retained by the Contractor and presented upon request.
8.2 Stock standard solutions (1.00 ug/uL) . Stock standard solutions may be
purchased as certified solutions or preparsd fro. pure standard
materials.
8.2.1 Prepare stock standard solutions by accurately weighing about
0.0100 g of pure material. Dissolve the matinal in tolusne,
diluts to volume in a 1.0 m l. volumetric flask with toluens or
acetone. Larger volumes may be used at the convenience of the
analyst.
8.2.2 When compound purity is assayed to be 97 percent or greater.
the weight may be used without correction to calculate rh.
concentration of the stock solution. If ths compound purity is
assayed to be less than 97 percent. th. weight shall be
corrected when calculating the concentration of the stock
solution.
8.2.3 Fresh stock standards shall be prepared once every tvelvs
months, or sooner, if standards have degraded or concentrated.
Stock standards shall be checked for signs of degradation or
concentration just prior to preparing working standards fr
them.
8.3 Working Standards
8.3.1 Surrogate Standard Spiking Solution
The surrogates, tetrachloro.mXYlefle and decachlotobiphenyl,
are added to all standards, samples, and blanks. Prepare a
surrogate spiking solution of 0.20 ug/mL of each of the two
PEST D-lO 10/92
-------
compounds In acetone. The solution should be checked
frequently for stability. The solution shall be replaced after
six onchs or at an earlier tine, if the solution has degraded
or concentrated.
8.3.2 Resolution Check Mixture
The ResolutIon Check Mixture is composed of the pesticides and
surrogates at the concentrations listed below in hexana or iso .
octane. The ixcure shall be prepared every six months or
sooner, if the solution has degraded or concentrated.
Co oound.s Concentretion (ng/eL )
g2 ! t Chlordane 10.0
Endosulfan I 10.0
p,p -DDE 20.0
Dieldrin 20.0
Endosulfan sulfate 20.0
Endrin ketone 20.0
?(ethoxycb lor 100.0
Tecrach loro-m-xylene 20.0
Decachlorobipheny l. 20.0
8.3.3 Performance Evaluation Mixture
The Perfor,itr ce Evaluation Mixture is prepared in hexane or
130-octane as listed below. The PD( shall be prepared weekly
or more often, if the solution has degraded or concentrated.
Com ounda Concentration (nt/eL
10.0
alpha- HC 10.0
4,4 1 .D 100.0
beea . .BHC 10.0
Endrin 50.0
Methoxychior 250.0
Teerachlore .e-xylena 20.0
Decachiorobiphenyl 20.0
8.3.4 Single Component Pesticides
The Individual Standard Mixture solutions shall be prepared in
either he v e or iso-octane. The concentrations of the
pesticides in the low point standard mixtures a e given baby.
The midpoint concentration shall be 4 times the Lov point
concentration for each analyt., including th. surrogates. The
high concentration shall be at least 16 times the low point
concentration for each analyte. including the surrogates, but a
higher concentration may be chosen by the Contractor. The high
point concentration defines the upper end of the concentration
range for which the calibration is valid. The solution shall
PEST D-11 10/92
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be prepared every 6 onChi or sooner, if the solution has
degraded or concentrated.
Lov point Low Point
Individual Concentration Individual Concentration
Standard Mix A ( ngJ L) — Standard Mix B ( n JaL )
alpha-BHC 5.0 b.ta 3liC 5.0
Heptach] .or 5.0 d.lt.43liC 5.0
____ 5.0 Aidrin 5.0
Endosulfan I 5.0 HeptachiOr epoxida 5.0
Dt.1 .drin 1.0.0 a lpht.Chlordifla 5.0
Endrin 10.0 gaitim.CblOrd afl* 3.0
p,p’-DDD 10.0 p,p-DDE 10.0
p,p’-DDT 10.0 Endosulfan sulfate 10.0
Mechoxychior 50.0 Endrin aldehyde 10.0
Tetrachloro. -Xy1efle 5.0 Endrin ketone 10.0
Decachiorobipheflyl 10.0 Endogulfafl II 10.0
TetraCh l orO2 .XYlefle 5.0
Decach lorobLPheDY l 10.0
8.3.5 Multico poneflt Standards
Toxaphena and Aroclor standards ihall be prepared individually
except for Aroclor 1260 and Aroclor 1016 which aay be combined
in on. standard Rixturs. The calibration standards for the
Aroclors shall be preparsd at concentrations of 100 ng/aL,
except for Aroclor 1221 which shall be prepared at 200 ngJ3L.
Toxaphene shall be prepared at 500 ng/3L. All u1tico2ponent
standards shall con’ ” the surrogates at 20.0 ng/sL. The
Aroclor and Toxaphene solutions shall b . prepared in hexane or
iso-octane. Each solution shall be prepared every 6 aonths or
sooner, if the solution has degraded or concentrated.
8.3.6 Florisil Cartridge Check Solution
Prepare a 0.10 ug/aL solution of 2,4,5-trich lorophenol in
acetone. The solution shall be prepared every 6 onth s • or
sooner, if the solution has degraded or concentrated.
8.3.7 Laboratory Control Simple (LCS) Spiking Solution
Prepare a laboratory control sample (LCS) spiking solution that
contains each of th. .valytas at the concentrations listed
below in echano1 or ecetons. The LCS solution shall be
prepared every six poaths or sooner, if the solution has
degraded or concentrated.
Cp vo .mda Concentration (uç/ L1
gaa-BMC 0.10
Heptachior epoxide 0.10
Die ldrin 0.20
PEST D.12 10/92
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4 ,4’-DDE 0.20
Endrin 0.20
EndosulfIfl sulfate 0.20
8 a.ChlOrdafle 0.10
8.4 Storage of Standards
8.4.1 Store the stock and second .a17 standard solutions at -10’C to
-20C in Teflofl4ifled screw-cap aiiber bottles.
8.4.2 Store the working standard solution.I at 4C (±2C) in Teflon-
lined screw-Cap amber bottles. The working standards shall be
checked frequentlY for signs of degradation or evaporation.
8.4.3 protect all standards fro2 lig1 C.
8.4.4 Samples, sample extracts, and standards shall be scored
separately.
PEST D-13 10/92
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SECTION III
ThS•TR 1XXN? QUALITY coN’raoL PROCZDUR S AND LEQUIR 7S
PEST D-14 10/92
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‘ART A - IHSTRUMEIfI 0P ATINC CONDITIOMS
9. CiAS CtRQXAIQGRAfl / EIICTRON CAPTUR1 DETECTOR .
The following are the gas chromatograPhic analytical condition.s. The
conditions are recoended unless otherwise noted.
Carrier Gas: Heli
Column Flow: 5 iL/am
Make-up Gas: Argon/Xethan e (P S or P.10) or N 2
(rc ;uired)
Injector Temperature: 200C (required)
Injection Technique: Onco1t 1
Injection Volume: 1 or 2 ul (sea note below)
Injector Grob-type, s:litlesS
Initial Temperature: 150’C
Initial Hold Time: 1/2 mm
Temperature Ramp: 5C to 6 ’C/min
Final Temperature: 275’C
Final Hold Time: After Decachlorobiphenyl has elutad
(approximately 10 minutes)
Optimize CC condition.i for a.nalyta separation and sensitivity. Once
optimized, the same CC conditions shall be used for the analysis of all
standards, samples, blanks, performance evaluation samples and
laboratory control samples. NOTE: Manual injections shall be 2.0 uI..
Auto injectors may use 1.0 uL volumes. The same injection volume shall
be u.3ed for all stand.arda, blanks, and samples.
The linearity of the ECD may be greatly dependent on the flow rate of
the make-up gas. Care shall ha taken to maintain stable and
appropriate flow of make-up gas to the detector.
Cold (ambient temperature) on-colt injectors that allow injection
directly onto a 0.53 ID colu may be used as long as the acceptance
criteria for resolution, calibration, and arLalyte breakdown are met.
PEST D-15 10/92
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PART B - CALIBRATION OF THE GC/ECD SYSTEM
10. INITIAL CALIBRATION
10.1 Summary
Prior to samole analysis, each CC/ECD system shall be initially
calibrated at a ainia of three concentrations for single component
analytes in order to determine instrument sensitivity and the linearity
of CC response. Each multicomponenc an.alyte is analyzed at one
conceritra tion.
10.2 Frequency
Each CC/ECD system shall be initially calibrated upon award of the
contract, vtienever major instrument maintenance or modification is
performed (e.g., colt n replacement or repair, cleaning or replacement
of ECD, etc.), or if the calibration verification technical acceptance
criteria have no: been met.
1Q.3 Procedure
10.3.1 Set up the CC/ECD system as described in Section 9.
10.3.2 Prepare the initial calibration standard.s using the procedures,
the analytes, and the concentrations according to Section 8.
10.3.3 All standards, samples, and blanks shall be allowed to warm to
ambient temperature before preparation or analysis.
10.3.4 Analyze the initial calibration sequence as given below. NOTE:
;s 16 and 17 are as pax . .,Z the c•libracian
verification as veil (see Section 11).
INITIAL CALIBRATION SE UENCZ
1. Resolution Check
2. Performance Evaluation Mixture
3. Aroclor 1016/1260
4. Aroclor 1221
5. Aroclor 1232
6, Aroclor 1242
7. Aroclor 1248
8. Arocior 1254
9. Toxaphene
10. Low Point Standard A
U. Low Point Standard 3
12. Midpoint Standard A
13. Midpoint Standard B
14. High Point Standard A
15. High Point Standard 3
16. Instrument Blank
17. Performance Evaluation Mixture
PEST D-16 10/92
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.0.6 Calculations
10.4.1 For each single co ponenC pesticide and surrogate, a retention
tiae (RT) is seasured in each of three of the calibration
scandard.i analyses (by paint, aidpoint, hig i point) during the
initial calibration for Individual Standard Mixt e A and
Individual Standard Mixture B. The RT for the aurrogatsa is
euurud froc the Individual Standard Nixture £ analyses. The
aean RT La calculated as the average of th three values.
Calculate a een absolute retention tie. (AT) for each single
coponent pesticide and surrogate using Equation D.22.
— n RTj
EQ. D.22. RI —
I— ].
RT — Mean absolute retention time of analycs.
RTj — Absolute retention tLae of analyte.
a — Nuaber of easure entz (3).
10.4.2 A retention tixe vindov is calculated for each single coeponenc
analyts and surrogate and for the w.ajar peaks (3 to 5) of each
ultico ponent .nalyt. by using Table D l2. Windova are
centered atound the average absolute retention tias for the
axtalyt. established during th. initial calibration.
TABLE D.12
Rr rrIo! :IME WIND.,w FOR SI LE AND MULTICOI ON r
ANALYTES AND SURROGATES.
- Coapowid Identification
Co o u nd Windov ( inuteg )
alpha. B RC ±0.05
beta - BRC ±0.05
±0.05
de lta-BHC ±0.05
Heptachior ±0.05
Aidrin, ±0.05
alph a -Chlordane ±0.07
gazu-Ch lordane ±0.07
Beptachbor epoxide ±0.07
Die ldrin ±0.07
Endrin ±0.07
Endrin aldehyde ±0.07
PEST D-L7 10/92
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TA L.E D.12 (concinued)
RETENTION TIME WINDOVS FOR SINGLE AND MULTICOMPONEW
ANALYTES AND SURROGATES.
Compound Identification
Comt ,ound Vindov (minutes)
Endrin keton. ±0.07
ODD jO.07
DDE ±0.07
DOT ±0.07
Endosulfan I ±0.07
Endosulftn II ±0.07
Endosulfan sulfate ±0.07
Methoxychior ±0.07
Aroclors ±0.07
Toxapheue ±0.07
Tecrach loro-m-xy leue ±0.05
Decachlorobipheny l ±0.10
10.4.3 The linearity of the instr’. enc is determined by calculating a
percent relative standard deviation (%RSD) of ths calibration
factors fro, a three-point calibration curve for etch of the
single component pesticide and surrogates. Either peak area or
peak height may be used to calculat. calibration factors used
in the %RSD equation. For example, it j 4 p.r*ttt.d to
calculate linearity for sndrin based on peak aria and to
calculat. linearity for aidrin bas.d on peak height. It ii
permitted within a %R.SD calculation fo an analyt. to use
calibration factors calculated from both peak area and peak
heig it. For example, it La permitted Co calculat, the
calibration factor for the by point standard for endrin using
peak height and calculate the midpoint and high point standard
calibration factors for eridria using peak area.
10.4.3.1 Calculate the calibration factor for each single
component pesticide and surrogate aver the initial
calibration rang. using Equation D.23.
10.4.3.2 Calculate the mean and the %RSD of th. calibration
factors for each singl, component pesticide and
surrogate over th. initial calibration range u.sing
Equation 0.24 and Equation 0.25.
EQ. 0.23 CF — Peak Ares (or Height) of the Standard
(ass Injected (ng)
n
— £ CF 1
EQ. D.24 CF — i—i
n
PEST 0-18 10/92
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EQ. D.25 % RSD SD
100
CF
lit —
I (CFj — CF) 2
Where SDQ’ — J i —i and n—3
n - i
%RSD — Percent relative standard deviation.
SDQ — Standard deviation for calibration factor,.
CF j Calibration factor.
C l — Mean calibration factor.
10.4.4 A calibration factor is calculated for each peak in £ selected
set of three to five w.ajor peaks for each mu].ticomponenc
ar a1yte using Equation D.2 3.
10.4.5 Ca1c .i1aee the percent breakdown of DDT. the percent breakdown
of Endrin, and the combined breakdown of DDT and Endrin in the
Perforaance Evaluation Mixture using Equations D.26, D.27 ,
D.28, and D.29.
EQ. D.26
Amount found (in ng) — Peak area (or Peak height) of eo ound in P
CPmp
CF — The calibration factor for the compound determined from the
midpoint standard in the moat recent initial calibration.
Noes: If during the initial calibration, linearity vu
determined based on peak area for the compound, then the
aidpothe CF shall be based on peak area. If during the initial
calibraejon, the linearity for the compound yes determined
based on peak height for the compound, then the *idpoine CF
shall be based on peak height.
EQ. D.27
% Breakdown DDT — Amount found in t (DDD+DDE) * l0Q
Amount in zig of DDT injected
EQ. D.28
% Breakdown Endrin —
moune found in nt (Endrin Aldehyde 4 Endrin 1 etone) • 100
Amotmt in zig of Endrin injected
EQ. D.29 Combined i Breakdown — %Breakdovn DDT + %Breekdown Endrin
10.4.6 Calculate the percent difference for each pesticide and
surrogate in the Performance Evaluation Mixture arid Individual
Standard Mixtures A and 5 using Equation D.26 and Equation
D. 30.
PEST D-19 10/92
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EQ. D.30 %D C 1 0 - C 1 j c
— — xL00
Cnom
tD — percent Difference
— nominal concentratiOn of each analyts
C jC Calculated concentration of each an.alyta from the
analyses of the standard
10.4.7 Calculate the resolution between the an.alytes in the Resolution
Check Mixture end the 2 Ldpoiflt conc.ntatiOfl1 of individual
standard mixtures A and 3 using Equation D.31.
EQ. D.31 % Resolution x 100%
V — Depth of the valley between the two peaks. The depth of
the valley is measured along a vertical line from the level
of the apex of the shorter peak to th. floor of the valley
- between the two peaks.
H — Hei 1 t of the shorter of th. adjacent peaks
10.5 TechnicAl Acceptance Criteria For Initial Calibration
All initial calibration technical acceptance criteria apply
independently to both CC col r’ .’
10.5.1 The initial calibration sequence shall be analyzed according to
the procedure and in the order listed in Section 10.3. at the
concentratioT2 . 5 listed in Section 8. and at rh. frequency listed
in Section 1.0.2. The GC/ECD operating conditions optimized in
Section 9 shall be followid.
10.5.2 The resolution between two adjacent peaks in the Resolution
Check Mixture shall be greater than or equal to 60.0%. On the
D8-1701 GC col , resolution difficulties are most likely
between Endo UlfAfl I and gsao* .Cblordana and between
MethoXyChlOt and .ndosulfifl sulfate. On the D3-608 GC coli ,
the poorest resolution will probably be between pp ’ -DDE and
Dieldrifl MechoxychlOr and Endrin katon.; and Endosulfan I and
g*T!!1 la -Ch1OrdaflS.
10.5.3 All single component pesticides and surrogates in both rwts of
the Performance Evaluation Mixture (PE2() shall be 100 percent
resolved.
10.5.4 The absolute retention rises of each of. the single component
pesticides and surrogates in both n ina of the P I shall be
within the retention time vthdoV determined from the three-
points initial calibration in Section 10.4.2.
iO.5.5 The percent difference of the calcUl.2ted amo mt and the tr’.ie
amount for each of the single component and surrogates in both
PEST D-20 10/92
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of the PEM runs shall be greater than or squel. to .25 percent
and less than or equal to 25 percent using Equation 0.30.
10.5.6 The percent breakdown of DOT and andrin in each of the PEM r’..zn.s
shall be less than or equal to 20.0 percent. The combined
breakdown of DOT and endrin shall be less than or equal to 30.0
percent.
10.5.7 m c RSD of the calibration factors for etch singi. component
target compound shall be less than or equal to 20.0 percent,
except as notad. The 1RSD of the caUbration factor, for the
surrogates shall be less than or equal to 30.0 percent. Up
to two single component target compounds (but not surrogates)
may exceed the 20.0 percent limit for %R.SD, but those co pounde
shall have a IRED of less than or equal to 30.0 percent.
10.5.8 The resolution between any two adjacent peek.i in the midpoint
concentrations of Individual Stand.ard Mixtures A and B in the
initial calibration shall be greater than or equal to 90.0
percent.
10.5.9 All inscrunenc blanks shall meet the technical acceptance
criteria in Section 20.3.4.
10.5.10 The identification of single component pesticides by gas
chromacographic methods is based primarily on retention time
data. The retention time of the apex of a peak can only be
verified from an on-scala chromatogram. The identification of
multicomponent analytea by gas chromatographic methods is based
primarily on recognition of patterns of retention times
displayed on a chroaatogram. Therefore, the following
requirements apply to all data presented for single component
and multicomponenc analytes.
10.5.10.1 The c roa.atograaz that result from th. analyses of
the Resolution Check Mixtu.rs, the Performance
Evaluation Mixture, and Individual Standard Mixtures
A and 3 during the initial calibration sequence
shall display the single component asialytes present
in each standard at greater than 10 percent of full
scale but less than 100 percent of full scale.
10.5.10.2 The chromatograxes for at least one of the three
analyses each of Individual Standard Mixtures A and
3 from the initial, calibration sequence shall
display the single component analytes it greater
than 50 percent and less than 100 percent of full
scale.
10.5.10.3 The chromatograms of the standards for the
mulcicomponent an.alytes analyzed during the initial
calibration sequence shall display the peaks chosen
for identification of each a.r*lycs at greater than
25 percent and less than 100 percent of full scale.
PEST D-21 10/92
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10.5.10.4 For all Resolution Check Mixtures, Performance
Evaluation Mixtures, Individual Standard Mixtures,
and blanks, the baseline of the chroutogram shall
return to belov 50 percent of full scale before the
elution tim . of alpha .ZHC , and return to baby 25
percent of full scale after the elution time of
alpha-BHC and before the elution time of
decachiorobiphenyl.
10.5.10.5 If a chromaeograa La replotted electronically to
meet requirements. th. scaling factor used shall be
displayed on the chromatogram.
10.5.10.6 If the chromatogram of any standard needs to be
reploeted electronically to meet these requirement,,
both the initial chroa.atograa and the repbotted
chromatograa shall be submitted in the data package.
10.6 Corrective Action
10.6.1 If the technical acceptance criteria for the initial
calibration are not met, inspect the system for problems. It
may be necessary to change the column, bike out the detector,
clean the injection port, or take other corrective actions to
achieve the acceptance criteria.
10.6.2 Contamination should be suspected as a cause if the detector
cazmot achi.vis acceptable linearity using this method. In the
cue of low level contamination, baking out the detector at
elevated temperature (350C) should be sufficient to achieve
acceptable performance. In the case of heavy concu.thation,
passing hydrogen through the detector for 1.2 hours at elevated
rm u erit .re may corr.” the pro _. . In h. cue of severe
contamination, the detector may require servicing by the ECD
manufacturer. DO NOT 0P THE DETECTOR. THE ECD CONTAINS
RADIOQI 1CAL SOURCES.
10.6.3 If a laboratory decontamin.atU a detector using elevated
temporaturs, the ECD electronics shall be turned off during the
bake out procedur..
10.6.4 Aftar bake out or hydrogen reduction, the detector shall be
recalibrated using th. initial calibration sequence.
10.6.5 Initial calibration technical acceptance criteria SHALL be met
before any samples (including the LCS and PES) or required
blanks are analyzed. Any samples (including the LCS and PES)
or required blanks analyzed after the initial calibration
criteria have not been met will require reanalysis at no
additional cost.
PEST D-22 10/92
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CALIBP.ATIQ! VERIYICkTION
11.1 Su ary
Three types of analyses are used to verify the calibration arid evaluate
instrt ent perforaance. The analyses of irutruaent blanks 1 Perfor arice
Evaluation Mixtures (P () • arid the aid point concentration of
Individual Standard Mixtures A and B constitute the continuing
calibration. Saizple data are riot acceptabi. unless bracketed by
acceptable analyses of instruaenc blanks 2 (S and both Individual
Standard Mixtures A and 3.
11.2 Frequency
11.2.1 An Lnstrunent blank arid the Perfor ance Evaluation Mixture
shall bracket one end of a 12-hour period during which sanpie
data are collected, and a second instruaenc blank and the id
point concentration of Individual Standard Mixtures A and B
shall bracket the other end of the 12-hour period.
11.2.2 or the 12-hour period ixnediacely felloviug the initial
calibration sequence, the instrument blank and the P!2( that are
the last two steps in the initial calibration sequence bracket
the front end of that 12-hour period. Thi injection of the
instruaent blank starts th. beginning of that 12-hour period
(see Section 14.3). Samples may be injected for 12 hours from
the injection of the instrument blank. The first three
injections inediately that 12-hour period shall be an
instrument blank, Individual Standard Mixture A, and Individual
Standard Mixture ft. The instrument blank shall be analyzed
first, before either standard. The Individual Standard
Mixtures may be analyzed in either order (A ,3 or B,A).
11.2.3 The an*ly*es of the instrument blank and Individual Standard
Mixzures A and 3 i sediately following one 12-hour period may
be used to begin the subsequent 12-hour period, provided that
they meet the acceptance criteria in Section 11.5. In that
instance, the subsequent 12-hour period shall be bracketed by
the acceptable analyse. of an instrument blank and a Th(, in
that order. Thos. two analyses may in turn be used to bracket
the front end of yet another 12-hour period. This progression
may continua every 12 hours witil such time as any of the
instrument blanks, P (s, or Individual Standard Mixture, fails
to meet the acceptance criteria in Section 1L5. The 12-hour
time period begins with t h. injection of the instrument blank.
Standards (PD( or Individual Standard Mixtures), samples and
required blanks may be injected for 12:00 hours from the time
of injection of the instrument blank.
11.2.4 If more than 12 hours have elapsed since the injection of the
instrument blank that bracketed a previous 12-hour perIod, &n
acceptable instrument blank and PD( shafl be analyzed in order
to start a nev sequence. This requirement applies even if no
analyses were performed since that standard(s) was injected.
PEST D-23 10/92
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tiae of a lpha-BHC. and return to belov 25 percent of
full, scale after the elution tue of alpha.BHC and
before the elutiofl ci a . of decachlOrobipheflh l.
11.5.7.3 If a chrom&tOgr is replotted el.ctronical]y to
jeec these rsquireaeflt st the scaling factor used
shall be displayed on the chroaatOgr 5 .
11.5.7.4 If the chrowatOgr of any standard or blank need.s
to be replotted electrOniCallY to eet these
requirewenti • both th. initial chroa.atOgraa and the
rep].otted chroaato8rI (5) shall be subaitted in the
data package.
11.6 Corrective Action.
11.6.1 If the technical acceptance criteria for the calibration
verification are not wet, inspect the systea for problew.s and
take corrective action to achieve the acceptance criteria.
11.6.2 Major corrective actions guch as replacing he CC coluwn or
baking out the detector viii require that a nv initial
calibration be perforaed mud aeet.3 the technical acceptance
criteria.
11.6.3 Minor corrective actions aay not require p.rforaing a nay
initial calibration, provided that a nev analysis of the
standard (P ( or IndividUli Mixtures) that originally failed
the criteria gn an associated in.str’aeat blank tiediately
after the corrective action do weet all the acceptance
criteria.
11.6.4 If a Perfornance Evalu tiOfl Mixture or Individual Standard
Mixturs does not meet th. technical acceptance criteria listed
abovs, it hal1 be reinjected iaiediately. If th. second
injection of the P ( or Individual Standard Mixture meeta the
criteria. sa3pll analysis way conti Ua. If the second
inj ection does not west the criteria • al] data collection shall
be stopped. Appropriate corrective action shall be taken, m d
a n .y initial calibration sequence shall be run before more
saaple data are collected.
11.6.5 If an tnstruaent blank does not meet rh. tec!m(cal acceptance
criteria listed in Section 20.3.4, all data collection shall be
stopped. Appropriate correCtivs action shall be taken to clean
out the systems and an acceptable instrument blank shall . be
analyzed before wore sample data are collected.
11.6.6 Analysts are cautioned that running an instrueeflt blank and a
Perfora .ance Evaluation Mixture or Individual Standard Mixtures
once every 12 hours are the sinimum contract require eflt5.
Late eluting peaks aay carry over from one injection to the
next If highly coaplex saiples are analyzed or if the CC
conditions are unstable. Such carryover is unacceptable.
PEST D-26 10/92
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Therefore, it may be necessary to run instrument blanks and
standards more often to avoid discarding data.
11.6.7 If a successful jnstrument blank and P 4 cannot be run after an
interruption in an.alySi 5 (Section 11.2.5), an acceptable
initial calibration huil1 be run before sample data may be
collected. All acceptable sample analyses shall be preceded
and followed by acceptable standards and instrument blanks, as
described in SectiOn 11.2.
11.6.8 Calibration verification technical acceptance criteria shall be
met before any samples (including the LCS and the PES) and
required blanks are reported. Any samples, including LCS and
PES required with a calib ’stion verification which did not meet
the technical acceptance criteria will require reanalysis at no
additional COSt.
PEST D-27 10/92
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SEC7ION IV
SA PLZ PPIPABATIOM, zrrLqCrION. AND CLL(NV?
PEST D-28 10/92
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MXARY
12.1 This method is designed for analysis of samples that contain low
concentrations of the pesticides and Aroclors listed i EXhibit C. The
majority of the samples are expected to come from drinking water
sources and well/ground water around Superfurtd sites. If, upon
inspection of a sample, the Contractor su.,pects that the sample is not
amenable to this method, contact SMO for instructions.
13. PIP.OCEMTB.Z
13.1 Extraction
Continuou.s Liquid-Liquid Extraction 13 required for the extraction of
the samples.
13.1.1 Add aethylene chloride (100 to 250 m l .) to the bottom of the
extractor and fill it to a depth of at least one inch above the
bottom sidearm.
13.1.2 Measure out each 1.0 liter sample aliquot in a separate 1 liter
graduated cylinder. Measure and record the pH of the sample
with wide range pH paper and adjust the pH to between 5 and 9
with 10 N sodium hydroxide or concentrated sulfuric acid, if
required. Samples requiring pH adjustment shall be noted in
the SDC Narrative. Transfer the sample aliquoc into the
continuous extractor. Rinse the cylinder with 30 ml. of
aethylene chloride and also transfer to the continuous
extractor.
13.1.3 Using a micrapipec with disposable tip, add 200 uL of the
surrogate solution to all samples and aethod blanks.
13.1.4 Adjust the level of aethylene chloride in the extractor so that
the bottom sidearm is half filled with solvent.
13.1.5 If the eample was received in a 1 liter container, rinse the
empty’ container with 60 mL of aetbylene chloride after caking
the sample sliquot. Add the rinaat. to the continuous
extractor.
13.1.6 Add sufficient methylene chloride to the distilling fla k to
ensure proper solvent cycling during operation. Extract the
solution for 18 hours. Allow to cool, then detach the
distillation flask and label.
13.2 Extract Drying and Concentration
13.2.1 Assemble a Kuderna .Danish (K-D) concentrator by attaching a 10
aL concentrator tube to a 500 ml. evaporative flask. Other
concentration devices or techniques may be used in place of the
K-D, if equivalency is demonstrated for all the target
pesticides and Aroclors listed in Exhibit C.
PEST D-29 10/92
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through each cartrLdg. is approxizsately
equal. DO NOT ALLOW ThE CARTRIDGES TO
GO DRY AF? ThEY HAVE 8E 4 WASHED.
13.4.2.2.4 After the cartridges in the manifold
are washed, the vacuua is released, and
a rack containing labeled 10 al,
volumetric flasks is placed inside the
manifold. Care shall be taken to
ensure that the solvsnt line frog each
cartridge i. placed mud, of the
appropriate volumetric flask as the
manifold top is replaced.
13.4.2.2.5 Transfer th. 1 p.1, extract to the top
frit of the appropriate Florisil
cartridge. Rinse the concentrator tube
twice with 0.5 m l . of bexane/acetone
(90:10) and transfer each rinse to the
top fric of the cartridge.
13.4.2.2.6 The pesticides/Aroclora in the extract
concentrates are then elured through
the co1* with 8.0 ml. of
hexans/aceton. (90:10) and are
collected into the 10 ml. volumetric
flasks held in the rack inside the
vacuum anjfo1d.
13.4.2.2.7 Transfer the eluate in each volumetric
flask to a clean c.ntrifug. tube or 10
ml. vLc 1 17 g. two additional 1 m l .
hex.ane rinses to ensure quantitative
transfer of th. cartridge eluate.
13.4.2.2.8 Concentrate the extract to 2.0 ml. using
either a micro Snyder column or
nitrogen evaporation (Section 13.5).
Measure the final volume with a syringe
or by transferring th. extract to a
volumetrtc flask.
13.4.2.2.9 If cry ta1s of sulfur are evident or if
the presence of sulfur La suspected,
proceed to Section 13.4.3. Sample
analyses with interference caused by
sulfur are not acceptable and the
extracts shall be cleaned up and
reanalyzed.
13.4.2.2.10 If the extract is not contaminated with
sulfur, transfer the sample to a CC
vial and label the vial. The extract
is ready for GC/ECD analysis. Proceed
PEST D-32 10/92
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to Section 14. Star. the extracts at
4’C in the dark until analyses are
completed.
13.4.3 Sulfur Removal
Sulfur can be removed by one of Cvo method3, according to
laboratory preference. Interference vhich is due to sulfur is
not acceptable. If the sulfur concetttZ 5ti01% is such that
crystalliZaCiOfl occurs in the concentrated extract, centrifuge
the extract to settis the crystalS, and remove the sample
extract with a disposable pipette. leaving the excess sulfur in
the centrifuge tube. Transfer the .xtract to a clean
centrifuge tube or clean concentrator tube before proceeding
with further sulfur cleanup.
13.4.3.1 If only part of a set of samples requires sulfur
cleanup, then tvo blanks are required for that set:
one that is shaken vith mercury or copper, and one
that is not. If only part of a set of samples
requires sulfur cleanup, do subject the
associated method blank to sulfur cleanup, but
prepare a separate sulfur cleanup blank as described
below. If all the samples are subjected to sulfur
cleanup, procesS the method blank along with the
samples. In this case. no additioflil sulfur cleanup
blank is required.
Sulfur cleanup blank. Add 200 uL of surrogate to
1.0 ml. of surrogate spiking solution and 9.0 ml. of
hexane in a clean centrifuge tube or 10 aL vial.
Concentrate the solution to 2.0 ml. by using either
nitrogen b1c :Vfl or a ..Ib.ro Sny r colt t. The
concentrated volume of the blank shall be the same
as the final volume of the samples associated with
the blank. Measure the volum. with a syringe or by
transferring the solution to a volumetric flask.
Proceed with the sulfur removal using h. same
technique (mercury or copper) as the samples
associated with the blank.
]3.4.3.2 Mercury techniqus
Add one to three drops of mercury to each hexane
extract in £ clean vial. Tighten the top 00 the
vial and agitate the sample for 30 seconds. Filter
or centrifuge the extract. Pipet the extract to
another vial and leave all solid precipitate and
liquid mercury. If the mercury appears shiny,
proceed to Section 14 and analyze the extract. If
the mercury turns black, repeat sulfur removal as
necessary. CAUTION: Waste containing mercury
should be segregated and disposed of properly.
PEST D-33 10/92
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NOTE: Mercury is a highly toxic metal and
therefore, shall bi used with great cars. Prior to
using mercury. it is reco ended that the analyst
become acquainted with proper handling and cleanup
techniques a socLated with this metal.
13.4.3.3 Copper technique
Add approxi2.at.ly 2 g of cleaned copper powder to
the extract in th. centrifuge or concentrator cube.
(2 ,g will fill the tub. to about the 0.5 at mark).
Mix the copper and extract for at laa.st 1 minute on
a mechanical shaker. Separate the extract from the
copper powder by drawing off the extract with a
disposable pipet, and trarLsf r the extract to a
clean vial. The •xtract transferred to the vial
still represents the 2.0 at final volume. Th..
separation of th. extract from the copper powder is
necessary to prevent degradation of the pesticides.
If the copper appears bright, procaod to Section 14
and analyze the extract. If the copper changes
color, repeat the sulfur removal procodur. as
necessary.
13.5. Extract Concentration
Two different techniques ar. permitted to concentrate the extract to
1.0 at (volue. before Florisil. cleanup) or 2.0 at (extract volume
before I stru ent.al analysis). They ar. the aicro Snyder column and
nitrogen evaporation techniques.
13.5.1 Micro Snyder Co1t Technique
Add another one or two -clean boiling chip. to the concentrator
tube and attach & two-ball micro Snyder col . Prsvec the
Snyder column by adding about 0.5 it of hexan. to th. top of
the colu 2. Place the t-D apparatus in a hot water bath (60C
to 65’C) so that the concentrator tub. is partially i er:ed in
the hoc water. Adjust the vertical position of the apparatus
and the water temperature u required to complete the
concentration in 5 to 10 minutes. At the proper rats of
distillation th. balls of the column will actively chatter but
the chanbers vi i ]. not flood with condensed solvent. When the
apparent volume of liquid reaches about 0.5 at, remove the K-D
apparatus from the water bath and allow it to drain for at
least 10 minutes while cooling. Remove the Snyder column and
rinse its flask and lover joint into the concentrator tube with
0.2 at of hexane. Adjust the final volume with hexane to 1.0
at (Florist].) or 2.0 at (analysis).
13.5.2 Nitrogen Evaporation Technique (taken from AST I Method D 3086).
13.5.2.1 Place the concentrator tube with an open micro
Snyder column attached in £ warm water bath (30’C to
PEST D-34 10/92
-------
35 ”C) and evaporate the solvent volune to ju.sc belov
1 or 2 L by blowing a gentle stream of clean, dry
nitrogen filtered through £ colut of activated
carbon above the solvent. Adjust the final volune
with hexane to 1.0 iL (FlorisLi) or 2.0 L
(analysis).
13.5.2.2 CAUTION: Gas lines froi the gas source to the
evaporation apparatus shall be stainless steel,
copper, or Teflon tubing. The internal wall of new
tubth.g shall be rinsed several tiises with hexane and
then dried prior to use. During evaporation, the
tube solvent level shall be kept below the water
level of the bath. DO NOT ALLOW THE EXTRACT TO GO
TO DRYNESS.
13.5.3 If the extract has not been put through Florisil yet, proceed
to !ect on 13.4 for extract cleanup. Otherwise, tran.sfer the
extract to a Teflon-lined screw-cap boctle and label the
bottle. Store at 4C (±2’C).
PEST D-35 10/92
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Another 12 hr a Last Sample
1st injection In strument Blank
past 12:00 hr.
2nd injection Performance Evaluation Mixture
o Sample
6
o Subsequent Samples
0
0
Another 12 hr. o Last Sample
1st injection Instrument Blank
past 12:00 hr.
2nd and 3rd Individual Standard Mixtures A and B
inJ ections
past 12 hr.
o Sample
0
o Subsequent Ss.mplas
a
0
etc.
NOTE: The first 12 hours are counted from injection #16 (the
Ins tru ent Blank at the end of the initial calibration sequence),
from injection #1. Samples may be injected until 12:00 hours haus
elapsed. All subsequent 12-hour periods are timed froa th. injection
of the instrument blank that brackets th. front end of the samples.
Because the 12-hour time period i. timed from injection of th.
instrument blank until the injection of the last sample, each 12-hour
period may be separated by the length of one chromatographic run, that
of the analysis of the last sample. Whil, the 12-hour period may not
be exceeded, the laboratory ru’ instrument blanks and standards
more frequently, for instance, to acco miodate staff working on 8-hour
shifts.
14.4 Included with the. subsequent samples in the analysis sequence are all
of the required method blanks and sulfur cleanup blanks. Tb.
Contractor may decide at what point in the sequence the method blanks
and sulfur cleanup blanks are to be analyzed.
14.5 Termination of Data Acquisition
After decachiorobiphenyl h is eluted from the CC column, the data
acquisition may be terminated fo that analysis.
15. DILU’TIONS
15.1 The sample or blank shall first be analyzed at the most concentrated
level (injection taken from the 2.0 aL final extract after the clean-up
steps).
15.1.1 If the response of any single component pesticide is greater
than the response of that analyce in the initial calibratton
high point standard, then the extract shall be diluted to have
PEST D-38 10/92
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the response of that analyt. between the initial calibration
low point and high point standard.
15.1.2 If the response of the largest peak in a multicomponent analyte
is greater than the most intense single component analyce
response in the initial calibration high point standard, thea
the response of the largest peak in a multicomponenc analyte
shall be diluted to have its response between the responses of
the initial calibration midpoint and high point standard of
that single component pesticide.
15.1.3 If a greater than 10 times dilution is needed (for example, 50
to 1 dilution), then a 10 times more concencrse dilution (5
to 1 dilution) also shall be analyzed.
15.2 When diluted, the chrowatographic data for the single component
pesticide shall be able to be reported cc greater than 10 percent of
full scale but less than 100 percent of full scale.
15.3 When diluted, multicomponene analyces shall be able to be reported at
greater than 25 percent of full scale but less than 100 percent of full.
scale.
15.4 If a chromacogram La reploceed electronically to meet these
requirement s, the scaling factor used shall be displayed on the
chromat ram. If th. chromatogrs.m of any sample need., to be reploteed
electronically to meet these requirements, both th. in.Lttil
chromacograa and the reploceed cbroisacogram(a) shall be submitted Lu
the data package.
15.5 Dilute the sample using the following procedure:
15.5.1 Calculate the extract dilution in order for the single
component pesticides to meet the requirement listed in Section
15.2.
15.5.2 Calculate the extract dilution in order for the mulcicomponene
analytea to meet the requirement listed in 14.3.
15.5.3 Dilute the sample extract vith hexane in a volumetric fla.ak.
16. IDEWrIflCATION 0? TARGET ANALTTZS
16.1 The laboratory will identify single component analyta peaks based on
the retention time windows established during the initial calibration
sequence. Single compcr enc .analyces are identified when peaks are
observed in the R,T window for the analyte on both CC column.,.
16.2 A set of three to five major peaks is selected for each multicomponent
an.alyte. Retention time windows for each peak are determined from the
initial calibration analysis. Identification of a multicomponent
analyce in the sample is based on pattern recognition in conjunction
PEST D.39 10/92
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17.8.2 During initial calibration, a set of three to five quancitacion
peaks was chosen for each ulticopOfleflC analyts. Calculate
the concentration of each of the selected Aroclor or Toxaphene
peaks individually using Equation D.32. Determine the mean
concentration for all of the selected peaks. The mean value is
reported on Form X (Exhibit B) for both CC columns.
17.8.3 For the single component pesticides. report th. lover of the
two values qu.antit.ated from the two columns of Form I. For the
multicomponent analytei. report th. lover of the two mean
values from the two columns on Form I.
17.8.4 The recoveries of the surrogates are calculated according to
Equation D.33.
EQ. D.33
Surrogate Percent Recovery — x 100
Where:
Q4— Quantity determined by analysis.
— Qu.antity added to sample/blank.
17.8.5 The percent difference is calculated according to Equation
D. 34.
EQ. D.34 ConcH COnCL
______________ x 100
C OnCL
Where,
ConcH — The higher of the two concentrations for the target
compound in question.
COflCL — The lover of the two concentrations for the target
compound in question.
Note that u.sin,g this equation viii result in percent difference
values that are always positive. Th. value viii also be
greater than a value calculated using the higher concentration
in the denominator, however, given the likelihood of a positive
interference raising the concentration determined on one CC
column, this is a con.servativo approach to comparing the two
concentrations.
18. TECHNICAL ACCEPTA2CZ C IT JcIA TOR SAXPII A (A.LTSIS
All requirements listed below apply independently to both CC column.s
and to all instruments used for these analyses.
18.1 Samples shall be analyzed under the CC/ECD operating condition., in
Section 9. The instrument shall have met all initial calibration and
PEST D42 10/92
-------
cilibracion vetificacicn technical acceptance criteria. Sample data
shall be bracketed at 12-hour intervals (or less) by acceptable
analyses of instrument blanks, Performance Evaluation Mixtures, and
Individual, Standard Mixtures A and 3, as described in Section 11.2.
.3.2 The sample shall be extracted and analyzed within the contract holding
ties.
.8.3 The LCS associated with the samples shall meet the LCS technical
acceptance criteria. The PES associated with the samples shall meet
the PES technical acceptance criteria. The method blank extracted with
the samples shall meet the method blank technical acceptance criteria.
if a sulfur cleanup blank is associared with the samples, that blank
shall eec the sulfur cleanup blank technical acceptance criteria.
18.4 The retention tue for each of the surrogates shall be within the
retention time window as calculated in Section 10.
18.5 The percent recovery for the surrogates shall be between 60.0 and 150
percent, .-inclu.sive.
18.6 No target analyte concentrations may exceed the upper limit of the
initial calibration (See Section 15.1.1 and 15.1.2) or else eZttact,
shall be diluted and reanalyzed.
A staxtd.ard for any identified multicomponene mnalyts shall be analyzed
on the same inatr .nt within 72 hours of its detection in a sample
within a valid 12 hour sequence.
18.8 The identification of single component pesticides by gas
chromatographic methods is based primarily on retention time data. The
retention tim. of the apes of a peak can only be verified from an on.
scale chromacogran. The identification of w .alcicomponent a.nalytea by
gas chro acographLc methods is based primarily on recognition of
patterns of retention times displayed on a chromatogram. Therefore,
the following requirements apply to all data prasaneed for single
component arid multicoaponent analytei.
18.8.1 When no analytes ire identified in a sample, the chromatogr
from the analyses of the sampl. extract shall use the same
scaling factor as was used for the low point standard of the
initial calibration associated with those analyses.
18.8.2 Chrow .atograms shall display singl, component pesticides
detected in the sample at less than full scale.
18.8.3 Cbromaeogram.s shall display the largest peak of any
multicomponent analyte detected in the sample at less than full
scale.
18.8.4 If an extract shall be diluted, chrom.atograms shall display
single component pesticides between 10 and 100 percent of full
scale.
PEST D-43 10/92
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20.2.4 Technical Acceptance Criteria for Sulfur Cleanup Blanks
20.2.4.1 All sulfur cleanup blanks shall be prepared and
analyzed at the frequency described in Section
20.2.2 using the procedure in Section 20.2.3 on a
CC/ECD system meeting the initial calibration and
calibration verification technical acceptance
criteria.
20.2.4.2 The concentration in the sulfur cleanup blank of the
target compounds in Exhibit C shall be Less than or
equal to the CRQL for each target compound.
20.2.4.3 The sulfur cleanup blank shall meet all sample
technical acceptance criteria in Section 18.
20.2.5 Corrective Action
20.2.5.1 If a gulfuZ blank does not meet the technical
acceptance criteria, the Contractor shall consider
the analytical system to b. out of control. It is
the ContractOra responsibility to ensure that
interferences cau.sed by contaminants in solvents,
reagents. glassware 1 and sample storage and
processing hardware that lead to discrete artifacts
and/or elevated baselines in gas chromatograis be
eliminated. If contaminetioft is a problem, the
source of the contamination shall be investigated
and appropriate corrective measures SHALL be taken
and documented before further sample analysis
proceeds.
20.2.5.2 Any sulfur blank that fails to meet the technical
acceptance criteria shall be reextracted and
reanalyzed at no additional cost. Further, all
samples (including LCS and PES) processed with a
sulfur blank that does not meet th. blank technical
acceptance criteria (i.e.. contaminated) will.
require reextraction and reanalysis at no additional
cost.
20.3 Instrument Blanks
20.3.1 Si .t ’i ry
An instrument blank is a volume of clean solvent containing the
surrogates that is analyzed to determine the extent of
contamination in the CC/ECD system.
20.3.2 Frequency
The first analysis after a 12-hour analysis sequence (see
Section 11.2) shall be an instrument blank. All groups of
acceptable sample analyses are to be preceded and followed by
PEST D-48 10/92
-------
acceptable instrument blanks. If wore than 12 hours have
elapsed since the injection of the instrument blank that
bracketed a previous 12-hour period. en instrument blank shall
be analyzed to initiate £ nev 12-hour sequence (see Section
11.2).
20.3.3 Procedure
20.3.3.1 Prepare the instrument blank by spiking the
surrogates into hexane or Lao-octane for a
concentration of 20.0 ng,/wL of Tetrachloro.s.xyl.ne
and Decachlorobipheny]..
20.3.3.2 Analyze the instrument blank according to SectIon 14
at the frequency listed in Section 20.3.2.
Calculate the results according to Section 17.
20.3.4 Technical Acceptance Criteria for Instrument Blanks
.20.3.4.1 All instrument blanks shall be prepared and analyzed
at the frequency described in Section 20.3.2 using
the procedure in Section 20.3.3 on a GC/ECD system
weeting the initial calibration and calibration
verification technical acceptance criteria.
20.3.4.2 The concentration in the instrument blank of each
target analyte in Exhibit C shall be less than or
equ.al to the CRQL for that analyt..
20.3.4.3 The Instrument blank shall weet all sample technical
acceptance criteria in Section 13.
20.3.5 Corrective Action
20.3.5.1 If analytes are detected at. greater than the CR I. or
the surrogate RTs are outside the RT vindove, all
data collection shall be stopped, and corrective
action xh fl be takes. Data for samples which were
run between the last acceptable instrument blank and
the unacceptable blank are considered suspect. An
acceptable instrument blank shall be rum before
additional data are collected. All samples which
wars run after ths last acceptable instrument blank
shall be reinjected during a valid rum sequence and
shall be repärted at no additional cost.
20.3.5.2 Analysts are cautioned that running an instrument
blank once every 12 hours (see Section 11) is the
ainimun contract requirewent. Late eluting peak.s
ay carry over frow one injection to the next If
highly ccwplex samples are analyzed or if the CC
PEST D49 10/92
-------
conditions are unstable. Such carryover is
unacceptable. Therefore, it way be necessary to run
instrument b1ank wore often to avoid discarding
data.
21. LABORATORY CONTROL 5A1’fPLZS (LCSI
21.1 SLITT ThJIry
The laboratory control sample (LCS) is an internal laboratory quality
control sample designed to assess (on an SDC-bySDC basis) the
capability of the contractor to perform the analytical method listed in
this Exhibit.
21.2 Frequency
The LCS shall be prepared, extracted, analyzed, and reported once per
Sample Delivery Group. The LCS shall be extracted and analyzed
concurrently with the samples in the SDG using the same inatrumentation
as the samples in the SDG.
21.3 Procedure
21.3.1 Measure a 1 liter aliquot of reagent water in a 1. liter
graduated cylinder and transfer the water to a continuous
extractor. Pipet 1.0 wI. . of the LCS spiking solution (Section
8.3.7) and 200 uL of the surrogate standard spiking solution
into the water and mix well. Extract and concent:ate the
sample according to Section 13.
21.3.2 Analyze the LCS per Section 2.4.
21.4 Calculation.s
21.4.1 Calculate the results according to Section 17.
21.4.2 Calculate individual compound recoveries of the LCS using
Equ.ation D.33, substituting LCS percent recovery for surrogate
percent recovery.
21.5 Technical Acceptance Criteria For Laboratory Control Sample Analysis
21.5.1 Th. LCS shall be analyzed at the freçuency described in Section
21.2 on a GC/ECD system meeting the initial calibration and
calibration verification technical acceptance criteria.
21.5.2 The LCS shall be prepared a.s described in Section 21.3.
21.5.3 The LCS shall meet all sample technical acceptance criteria in
Section 18.
21.5.4 The percent recovery for each of the compounds in the LCS shall
be within the recovery limits listed in Table D-14.
PEST D•50 10/92
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Table D-14
LABORATORY CONThOL SAMPlE RECOVERY LIMITS
COMPOUND % RECOVERY
56-123
Hepeichior epoxide 74-150
Dialdrin 33430
4,4 ’-DDE 50-150
Endrin 56-121
Endoaulfan sulfate 50400
ga a-Chlord.ane 33-130
NOTE: The recovery haLts for any of the coapound,, in the LCS
ay be expanded at any eLse during the period of performance if
SMO determthes that the lizaits are too restrictive.
21.6 Corrective Action
21.6.1 If the LCS technical acceptance criteria for the surrogates or
the LCS coa pound recovery are not act, check calculations 1 the
surrogate and LCS solutions, and instrument performance. It
aay be necessary to recalibrate the instruaeuc or take other
corrective action procedures Co aeec the surrogate and LC$
recovery criteria.
21.6.2 LCS technical acceptance criteria SHALL be act before data are
reported. LCS contamination froa laboratory sources or any LCS
analyzed not meeting the technical acceptance criteria will
require reextraction and reanalysis of the LCS me no additional
cost.
21.6.3 All samples prepared and analyzed in an SDC with an LCS that
does not meet the technical acceptance criteria will also
require reextraction and reanalysis at no addition.,], cost.
22. P!RYORMAYCZ EVAL ATIO SA ]1PIZS (P!S )
22.1 Sumnary
The PES is an external laboratory quality control sample prepa:ed and
designed to assess (on an SDC-by-SDG basis) the capability of the
contractor to perform the analytical method listed in this Exhibit.
22.2 Frequency
The Concraccot shall extract, analyze, and report the PES once per SDG,
if available. The PES shall be extracted and analyzed concurrently
with the samples in the SDC using the same instrumentation as the
samples in the SDC.
PEST fl-Si 10/92
-------
SECTION I V
DATA R.EPORT G POR.XS
B-45 10/92
-------
1LCD EPA SAMPLE NO.
DNC. WATER PESTICIDE ORCANICS ANALYSIS DATA SHEET —
ContraCt
:ode: — Case No.: — SAS No.: SDG No: ______
Sample ID: ______________ Date Received: __________
1e Volume: — (mL) Date Extracted: __________
ntrated Extract Volume: _______(uL) Date Analyzed:
‘ction Volume: — (uL) Dilution Factor:
ir Cleanup: (Y/N) — pH:
CONCENTRATION
CAS NO. COMPOUND (ug/L) Q
319—84-6 alpba—BHC _____
319—85—7 beta-BHC__________
319—36—8 -delta—BHC__________
L 53-89—9 gamma-BHC (Lindane)
5—44—8 Heptachior _____
D9—0O—2 A ld.riII_____________
£024—57—3 Heptachior epoxide_
959-98—8 EndoaUlfafl I________________
60—57—1 Dieldrifl
72—55—9 4,4 ‘—DDE
72—20—8 _____________________
3313—65—9 Endosulfafl II
72—54—8 —4,4’—DDD _____
1031—07—8 Endosulfafl sulfate__________
50—29—i 4,4’—D
72—43—5 MethoXyChlOr_
53494—70—5 Endrin ketone_______________ _____
7421—36—3 Endrin aldehyde
5103—71—9 _a lpha -chlOrdane_ _____
5103—74—2 ga maa- lordafle_ _____
8001—35—2 Toxaphefle_
12674—11—2 Aroc lor—101 6
11104—28—2 Aroclor— 122l
11141—16—5 Aroclor—12 32
53469—21—9 Aroc1orl2 42
12672—29—6 Aroclor—12 4 S
,1 1097—69—1 Aroc1or12S 4
11096—82—5 Aroc lor—1 26 O_
FORM I LCP 10/92
-------
2LCC
LOW CONC. WATER PESTICIDE SURROGATE RECOVERY
L ’ Name:_
Lab Code: _______
GC column(1);
ContraCt:
_____ SAS No.: ______
Case No.: —
_(mm) GC columri(2): -
TCX — TetraChlOrOmYle
DCB — DecaCh1OrObiP 1 Yl
# Co1um to be used to flag recovery values.
* Values outside of contract required QC limits.
D Surrogate diluted out.
page — of —
FORM II LCP
10/92
SDG No.: ______
— ID: ( m m .
TOT
OUT
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
EPA
TCX(1)
%REC 0
TCX(2)
%REC 0
SAMPLE NO.
- -
w- —
-
- -- --
DCB (1)
%REC 0
— a -
DCB (2)
%R.EC I
-
OTHER
(1)
(2)
QC LIMITS
%REC
(60—150)
(60—150)
-------
3LCC
C)W CONC. WATER PESTICIDE L 3 CONTROL SAMPLE RECOVERY
I.
Code: _______ Case No.:
Sample ID: _____________
Aliquot: ______ (uL)
:imtrated Extract Volume: _______(uL)
‘ction Volume: _____ (uL)
:ur Cleanup: (YIN) ___
EPA SAMPLE NO.
SM to.: — SOC No.: ______
LCS Lot No.: __________
Date Extracted: ________
Date Analyzed: __________
Dilution Factor: ________
pH: _____
:rument ID(l)
CC Column(l):
ID: ( mm )
COMPOUND
gamma-BHC (Lindane)_______
Heptachior epoxide
Di eldrin_________________
4 , 4’-DDE_________________
Endrin
Endosuif an sulfate________
ganuna—chiordanc
:rument ID(2)
CC Column(2):
-‘.umn to be used to flag recovery values with an asterisk.
Lies outside of QC limits.
ecovery:______ outside limits out of ______ total.
EN’TS:
Contract:.
COMPOUND
ID: ______ (mm)
gamma-BHC (Lindane)_______
Heptachior epoxide________
Die ldr in___________________
4,4 ‘—DDE_________________
Endrin
Endosuif an sulfata________
gamma-Chi ordane____________
AMOUNT
ADDED
(ng)
AMOUNT
RECOVERED
(ng)
%REC #
QC
LIXTS
•‘,- •• rrT
I r, /
-------
EPA SAXPLE NO.
4LCC
LOW CONC. WATER PESTICIDE METHOD DW(K SU)NARY
Nama:_ Contr&Ct:
b Code — Case No.: _____ SAS No.: —
te Extracted: — Lab Sample ID: —
te Analyzed (1): _________ Date Analyzed (2):
me Analyzed (1) ________ Time Analyzed (2):
strument ID (1): __________ Instrument ID (2):
Column (1): __________ ID: (mm) GC CO1U.mfl (2): —
ifur Cleanup: (1/N) —
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
Li
SDG No.: ______
ID:_____ (mm)
COMMENTS:
age — of
THIS METHOD BLANE AppLIES TO THE FOLLOWING SAMPLES AND LCS:
FORM I V LCP
10/92
-------
6LCD
. WATER PESTICIDE INITIAL CALIBRATION OF SINGLE COMPOWEN ANALITES
Contract:
Code: _______ Case No.: — SAS No.: — SDG No.: ______
-rument ID: __________ LevSl (x low): low — mid _____ high
..o lumn — ID: _(mm) Date(s) Analyzed:
RT 0? STANDARDS MZAN RT WINDOW
COMPOUND LOW MID HIGfl RT FROM TO
- - - - -- S - - ____ ____ ____ -
a1pha-B C ______ ______
beta-BHC — _____
delta-BHC__________
g mma—BHC (Lindane)_ ______ ______
Heptachior ______ ______ ______
Aidrin - _____
Heptach].or epoxide_ ______
Endosulfan I_______
Dieldrifl___________ ______
4,4’-DDE__________ _____ _____
Endrin_____________
Endosuif an II
4,4’—DDD _____
Endosulfan sulfate —
4,4’—DDT —
Methoxychior _____ _____
Endrin ketons______ ______
Endrin aldehyde — ______
aipha—chiordafle — ______
g ima—chlordans ______ ______ ______ ______
— - - ___ S - - -- ---
Tetrachloro-m-Xylefle
Decachlorobipheflyl_ ______
* Surrogate retention times are measured from md. Mix A analyses.
Retention time windows are ± 0.05 minutes for all compounds that
elute before HeptaChior epoxide, ± 0.07 minutes for all other
compounds, except ± 0.10 minutes for DecachlorobipheflYl.
FORM VI LCP—l 10/92
-------
6 LCE
CONC. WATER PESTICIDE INITIAL CALIBRATION OP SINGLE COMPONENT ANALYTES
Ham.:
Contract:.
Case No.: _____ SAS No.: ______ SDG No.: ______
_____ Level (x low): low _____ mid _____ high _____
ID: ( mm ) Date(s) Analyzed: ________
COMPOUND
ipha-BEC
eta-BEC
alta-BEC________
mn-BHC
eptachior__________
idrin_______
aptach.1 or
idosul ia.n ________
ieldrirz
,4’—DDE___________
drin______
dosulfan II
,4’—DDD__________
dosulZan sulfate
,4’—DDT_________
athoxychior______
.idrin ketone_____
drin aldehyde
1 pha—chlordane
mma— lordane
itzachloro—m—xyl en.
9cach.lorob iphenyl_
CALIBRATION
MID
FACTORS
HIGH
irrogate calibration factors are measured from md. Xix A analyses.
must be less than or equal to 20.0% for all compounds,
rogates, where %RSD must be less than or equal to 30.0%.
get compounds, but not surrogates, may have %RSD greater
less than or equal to 30.0%.
except the
Up to two
than 20.0%,
Code: _______
trument ID: ___
Column: _______
WV
AN
%RS D
(Lindane)_
epoxide_
I__________
FORM VI LCP-2
10/92
-------
6LC7
W CONC. WATER PESTICIDE INITIAL CALIBRATION 0? HULTICOMPONEW ANALYTES
Contract:.
CO4POIJND
Toxaphene
Aroclor 1254
Case No.:
ID: — ( )
AMOU1 T
- - - -
Aroclor 1260
* Denotes required peaks
RT
RT WINDOW
FROM TO
SAS No.: _____ SDG No.:
Date(s) Malyzed: _______ _______
PEAR
*1. _______ ______
*2 _______ ______
*3 _______ ______
4
5 ________ _______ ________ _______________
*1 _______ ______ _______ _____________
*2
*3 _______ _______ _____________
4 ________ ________ ________ _______________
5 ________ _______
*3 ______ ______ ____________
*3 _______ _______ _______ _____________
4 ________ ________ ________ _______________
5 ________ ________ ________ _______________
*1 _______ ______ _______ _____________
*2 _______ ______ ______ _____________
*3 _______ ______ ______ _____________
4 ________ _______ _______ ______________
5 ________ _______ _______ ______________
*1 _______ ______ ______ ____________
*2 _______ ______ ______ _____________
*3 _______ _______ _______ _____________
4 ________ _______ ________ _______________
5
*1 ______ ______ ______ ____________
*2
*3
4
5
‘1
*2
*3
4
5
*1 _______ ______ ______ _____________
*2 _______ ______ ______ _____________
*3 _______ ______ ______ _____________
4 ________ _______ _______ _______________
5
CALl BRAT ION
FACTOR
Code:
strument ID:
Column:
Aroclor 1016
Aroclor 1242
FORM VI LCP-3
10/92
-------
6LCG
LOW CONC. WATER PESTICIDE R.ESOUJTIOH CHECK SUXMAR (
Name:_________
Code: _______
______________ Contract:___________
Case No.: — SAS No.: ______
SDG No.: ______
:olumn (1):
Sample No.
3 Analyzed
01
02
03
04
05
06
07
08
09
___________ ID: _(mm)
(Standard 1):
(1): _________
Instrument ID (1): _______
Lab Sample ID (2): _________
Time Analyzed (1): _______
2olumn (2): _________ ID:
Sample No. (Standard 2):
3 Analyzed (2): ________
__tmm)
Instxi.imeflt ID (2): _______
Lab Sample ID (2): __________
Time Analyzed (2): _______
01
02
03
04
05
06
07
08
09
(%)
ANALYTE --
solution of two adjacent peaks must be calculated as a percentage cf the
!ight of the smaller peak, and must be greater than or equal to 60.0%.
(%)
ANALYTE -._--
RT_-
FOPJ( VI LCP-4
10/92
-------
7LCD
CONC. WATER PESTICIDE CALIBRATION VERI?ICATIOH SU) XARY
- a:
Code:
Column:
— Contract:__________
Case No.: _____ SAS No.: ______ SDG No.: ______
ID: ( mm ) mit. Calib. Date(s):_______ _______
Sample No. (PIBLX):
Sample ID (PIBLX) :_
Sample No. (PEN): —
Sample ID (PEN):___
Data Analyzed :
Time Analyzed :
Data Analyzed :
Time Analyzed :
—DDT % breakdown (1): _______
:!ned % breakdawn (1): _______
Endrin % breakdown (1): ________
%D of amounts in PEN must be greater than or equal to -25% and less
than or equal to 25.0%
4,4’-DDT breakdown must be less than or equal to 20.0%
Endrin breakdown must be less than or equal to 20.0%
Combined breakdown must be less than or equal to 30.0%
_CM.POUND
RT
RT WINDOW
FROX TO
CALC
AXOUNT
(ng)
...pha-BHC
ta—BEC__________________ ______ ______
mma-BHC (Lindane)_______ ______ ______
drin___________________ ______ ______
4’ —DDT__________________ ______
rychior
NON
AMOUNT
(ng)
FORM VII LCP—2.
10/92
-------
7 LCE
OW CONC. WATER PESTICIDE CALIBRATION VERIFICATION SUMMARY
.wDI VI DUAL MIX B
COMPOUND
wiw ow
FROM
TO
CALC
AMOUNT
(ng)
NON
AMOUNT
(ng)
Date Analyzed :
Tile Analyzed :
CALC NON
AMOUNT AMOUNT
(ng) (ng)
QC LIXITS: %D of amounts in the Individual Mixes must be greater than or
equal to —25% and less than or equal to 25.0%.
Name:
Code: _______
Column:
• Sample No. (PIBLX):
Sample ID (PIBLX):
• Sample No. (INDA):
• Sample ID (INDA):
Contract
_______ Case No.: — SAS No. ______ SDG No.:
ID: —___(m ) mit. Calib. Date(s):_______ _______
Date Analyzed :
Tile Analyzed :
Date Analyzed :
Time Analyzed :
WINDOW
FROM TO
INDIVIDUAL MIX A
COMPOUND
RT
•lpha-BHC
i nT a-BHC (Lindana)
.. _,.l,
;ndosul fanl_____________
i.ldr
ndr
A l_
•,-‘
A,
‘S •
t
.dtrachloro- 1xy1e1*
ecachl orob iphenyl
S l 3 No.(INDB):
Sample ID (INDB):
,eta-BHC_________
lalta-BHC________
Udrin________
eptach1or epoxide
,4’—DDE
ndosu1f an II
ndosulfafl sulfate________
ndrin ketons____________
nrin a].dehyde
alpha—C1 1lOrdane
;amma—C lOr0dafle
retrachlorO-m Ylefle
r cachlOrObiPhenYl
FORM VII LCP—2
10/92
-------
BLCD
LOW CONC. WATER PESTICIDE ANALYTICAL SEQUENCE
Contract:,
Case No.: _____ SAS No.:
ID: _____ m) mit. Calib. Date(s) _______ _______
S
1 ANALYTICAL SEQUENCE OP PERPORMANCE EVA.WATIOK MIXTURES, BLANXS,
SAMPLES, AND STANDARDS IS GIVEN 3ELOW:
TCX — Tetrachloro—m-xylene
DCB Decachiorobiphenyl
• Column used to flag retention
* Values outside of QC limits.
— of
QC LIMITS
(± 005 MINUTES)
(± 0.10 MINUTES)
time values with an asterisk.
Code:
Column: ___
tr’unent ID:
SDG No.:
MEAN SURROGATE RT PROM
TCX: DCB:
EPA
SAMPLE NO.
INITIAL CALIBRATION
LAB
SAMPLE ID
DATE
ANALYZED
TIME
TCX
DCB
ANALYZED
RT
•
RT I
-
—
01
02
03
04
05
06
07
08
-‘9
I0
.1.1
12
13
14
15
16
17
- 3
19
20
21
22
23
24
25
26
27
28
29
30
31
32
r PM V’IT LCP
10/92
-------
9 LCA
LOW CONC. WATER PESTICIDE FWRISIL CARTRIDGE CHECK
Contract:
SAS No.: SDG No.:
, Name:
Code: Case No.: —
risil Cartridge Lot Nunber: —
Colunn(1):
Date Analyzed:
.
ID: _( ) GC Colunfl(2).
COMPOUND
_p
alpha-BHC
gamina-BBC
Heptachior
Endosulfan I______________
Dieldrifl___________________
Endrin
4,4’—DDD
4,4’-DDT
Xethoxychlor
TetrachlOrO—n-Xylafle
Decachiorobipheflyl
SPIKE
ADDED
(ng)
SPIKE
RECOVERED
(ng)
REC 0
• Coluzn to be used to flag recovery with an asterisk
* Values outside of QC limits
QC
LIMITS
80—120
80—120
80—120
80—120
80—120
80—120
80—120
80—120
80—120
80—120
80—120
L’HIS CARTRIDGE LOT APPLIES TO THE FOLLOWING SAMPLES, BLANKS, AND LCS:
01
02
03
04
05
06
07
08
09
10
11
12
13
14
15
16
17
18
19
20
21
22
23
ID: _____(=)
ge — of —
FORM IX LC
1O/ 2
-------
lOLCA EPA SAMPLE NO.
LOW CONC. WATER PESTICIDE IDENTIFICATION SWIXARY ______________
FOR SINGLE COMPONENT ANALYTES
a:_______________________ contract
_______ Case No.: — SAS No.: ______ SDG No.: ______
Date(s) Analyzed: _______ ________
Instr .1 eflt ID (2): ________
____ GC column(2); ________ ____
___________ ID: _____ (ms)
COL RT
1 ________
2 _________
l ___ __
2 ___ __
1 ___
2 ________ ________
l ________ ________
2 ________ _________
2. ________ _________
2 ________ ________
1 ________
2 ________
2. ________
2 ________
1 ________
2 _________ _________
FORM X LCP—1
Code: _______
Sample ID
:ru.tnent ID (1):
Coluxnn(1):
ANALYTE
ID: ______ ( m m)
RT *j.ziuvw
FROM TO
CONCENTRATION
ge_of —
10/92
-------
1OLCB
LOW CONC. WATER PESTICIDE IDENTIFICATION SU?O(ARY
FOR MULTICOMPONENT ANALYTES
Name:__________________
Coda: _______ Case No.:
Sample ID : —
trument ID (1):
Colum.n(1): ____
EPA SAMPLE MO.
I I
least 3 peaks are required for identification of mu1tico portent analytes
FORI( X LCP-2
10/92
SDG No.:
Contract:________ _______________
SAS No.: —
Date(s) Analyzed: _______ ________
Instrument ID (2): _________
ANALYTE
1D: (m ) CC Column(2): _________ ID:
RT
RT WINDOW
FROM TO
--
( mm )
CONCENTRATION
NZAN
CONCENTRATION
COL.UHN 1
OLZThOi 2
PEAX
*1
*2
*3
4
5
*1
*2
*3
4
5
*1
*2
‘3
4
5
*1
*2
*3
4
5
•1
‘2
*3
4
5
‘1
‘2
*3
4
5
OLZThQ 1
OL JMN 2
p
oLmw 1
OL 2
of
-------
ATFACBMENT C.2
DETECTION LIMIT REQUIRE? {ENTS
Quantitation
Limits Water
PesticideslPCBs CAS Number (j&g/L)
1. alpha-BHC 319-84-6 0.003
2. beta-BHC 319-85-7 0.003
3. delta-BHC 319-36-8 0.003
4. gamma-BHC (Lindane) 58-89-9 0.003
5. Heptachlor 76-44-S 0.003
6. Aldri.n 309-00-2 0.003
7. Heptachlor epoxide 1024-57-3 0.003
8. Endosulfan I 959-98-8 0.003
9. Dieldrin 60-57-9 0.005
10. 4,4’-DDE 72-55-9 0.005
11. Endrin 72-20-8 0.005
12. Endosulfan II 33213-65-9 0.005
13. 4,4’-DDT 72-54-S 0.005
14. Endosulfan sulfate 1031-07-8 0.005
15. 4,4’-DDT 50-29-3 0.005
16. Mer .hoxychlor 72-43-5 0.03
17. Endrin ketone 53494-70-5 0.005
18. Endrin aldehyde 7421-36-3 0.005
19. alpha-Chlordane 5103-71-9 0.003
20. gamma-Chiordane 5103-74-2 0.003
21. Toxaphene 8001-35-2 0.3
22. Aroclor-1016 12674-11-2 0.05
23. Aroclor-1221 11104-28.2 0.10
24. Aroclor 1232 11141-16-5 0.05
25. Aroclor-1242 53469-21-9 0.05
26. Aroclor-1248 12672-29-6 0.05
27. Aroclor-1254 11097-16-5 0.05
28. Aroclor-1260 11096-82-5 0.05
9
-------
A11’ACHMENT C.3
CSF AUDIT FORMS
-------
LO CONCZ TRATIOH VATEI TOP ORCANICS CO)aLZTE SDG 71 12 (CST) fliVv ’roRT S !27
AI AT Y U* — CuT/STAll
CASE 10. ___________ G 10. ____________ G 10$. TO FOLLaJ __________ ___________ ___________
MO. _____
T2ACT NO. _____________________________________________________________ T) NO.
All documents delivered in the complete $DG file mu.st be original documents
where po sibls. (REFER CZ U4I3IT 3, SECTION II, PARAGRAPH 5, and SECTION III,
PARAGRAPH 16.)
PAGE HOe CRECX
FROM TO LAB EPA
Inventory Sheet (Form DC-2) (Do not number)
SDG Case Narrattv
Tr3fftc RepQr
! 2LiItiles Data
a. QC SLary
Surrogate Perc eat Recovery St ary (Form II LCV) ____ ____ _____ ________
Lab Control Saiiple Recovery (From III LCV) ____ ____ _____ _______
Method Blank SITT .T!ILrJ (Form IV LCV)
Tuning and Mass Calibration (Form V LCV) ____ ____ _____ _______
Sa2ple Data
TCL Results (Form I LCV)
Tent&tively Identified Compounds (Form I LCV-TIC)
Reconstructed total ion chroaatogram.I (P lC)
and Qu.antit.ation Reports for each saiple
Pot each sampi.:
Raw spectra and background-subtracted
mass spectra of target compounds identified
Mass spectra of all reported TICs with three
best library matches
c. Standards Data (AU Instruments)
Initial Calibration St T!I ary (Form VI LCV) _______
RICa and Quan Reports for all Standards _______
Continuing Calibration (Tori VII LCV)
RICa and Quant Reports for all Standards _______
Intarnal Standard Area and RT S”xy
(Tori V iii LCV)
d. QC Data
BFB
Blank Data
LCS Data
PES Data
e tvolatiles ‘Data
QC SummAry
Surrogate Percent Recovery Siimm nry (Form II LCSV)
Lab Control Sample Recovery (Tori III T.CSV)
Method Blank Suary (Form IV LCSV)
Tuning and Mass Calibration (Form V LCSV)
-..-..,, .‘,- , I
-------
LOW CONCENTRATION WATER 70& ORCANICS COKPLZTZ SDG TILE (CSV) fl !Wrl3aT SB!!? (Cont.)
____ 1
I — • TO FOLL 4 —
PAGE NOs CHECX
FROM TO LA5 EPA
5 L’wo1att1es Det (cont.)
b. Sazapl. Data
TCL Results (Form I LCSV)
Tentatively Identified Compounds (Form I LCSV-TIC)
Reconstructed total tort chrotnatogrw (RIC)
and Quantitatior% ReportS for each sample
For each sample:
Paw spectra and background SUbtraCt
mass spectra of TCI. COmPOUndS
Mass spectra of TICs vith three best library matches
GPC chroa.atogrw (if GPC performed)
c. Standards Data ‘(All Instruments)
Initial Calibration S”ry (Form VI LCSV)
RICa and Qua.n Reports for all Standardi
Continuing Calibration (Form VII LCSV)
RICa and Quart Reports for all Star.dard.s
Internal Standard Area and PT Swmi ’E7
(Form VIII LCSV)
d. QC Data
DFTPP
31a k Data
LCS Data
PES Data
Pest ctdei
a. QC S” ’-.ry ______
Surrogate Percent Recovery Su ry (Form II LCP)
tAb Control Sampla Recovery (Form III LCP)
Method 3laxik Sit?. Iiry (Form I V LCP)
b. Sample Data
TCL Results • Organic AnalysiS Data Sheet
(Form I LCP)
Chrow.atograa.s (Primary Colu i)
Chromatograms from second CC column confirmation
CC Integration report or data system printout and
calibration plots
Manual work sheets
For pesticides/Aroclors confirmed by CC/MS. copies
of raw spectra and copies of backgrOUfld5Ubtract mass
spectra of target compounds (samples & standards)
FORM DC-2-2
-------
.1 cONCZNTPATION VAT TOIL ORCANICS COXPLETE SDG FILE (CST) flWEZfIORT SHEET (Cont.)
CAU MO. MO. G .01. TO F0LL — — AS MO.
PACE NOs CHECK
FRC ( TO LAB EPA
Pesticidea . (cont.) -
c. Standards Data
tniti*l Calibration Data (Tori VI LCP)
Calibration Verification (Tori VII LCP)
Pesticides Analytical Sequence (Tori VIII.
LCP-l and -2)
PesticideFlorisil Cartridge Check (Tori IX , LCP) ________
Pestictde Identification (Tori X LCP)
Standard chro atograms and data system printout
for all Standards
For pesticides/A.roclors confir ed by CC/MS. copies
of spectra for standards used
d. QC Data
Blank Data
LCS Data
PES Data
dIsCell*neoU1 Data
Original preparation and analysis foru or copies of
preparation and analysis logbook pages
Internal sample and sample extract transfer
chain-of-cuatok’ records
Screening record..
AU inatru nent output, Including strip charts
frog screening .activitiea (describe or list) ________
EPA ThiDvtnaIRecetvtha oc ment3
Aizbillz (No. of ship ent.s _)
Chain-of-Custody Records
Sample Tags
Sample Log-In Sheet (Lab & DC1)
SDG Cover Sheet
Miscellaneous Shipping/Receiving Records
• (describe or list)
rn l tab Se vle Transfer Records md Trsc!’in2 Sheets
.e cribe or list)
y”P.l( DC.2-3
-------
LOW CONCENTRATION VATE1 VOL ORCANICS COXPLZTZ SX PXLE (CS?) INIENTORY SHEET (Cc .)
CA NO. G NO. wc . 70 F J . J — NO.
PAGE NOs CRECX
,IRON TO LAB EPA
Other Records (describe or list)
Telephone Counication Log ____ ____ _____ ________
Co enys :
p1etad by: ___________________________ ____________________________________ ____________
(CLP Lab) (Signature) (Printed Nazze/Title) (Date) —
u....ted by: _______________________ ________________________________ _________
(ZPA) (Signature) (Printed Na ze/?it1a) (bate)
FCRM DC2-4
-------
‘ . ib Jacis:
SAMPLE LOG4N SHEET
Reccivcd By
R eivod By
(Pruii ?4 ic):
(S n. curc):
Log-tn Dais:
Cmmbcr —
!a çlo Ddivu 7
1
SAS Nucther
CORR.ES POND !14G
F2A
SAMPLE
I
SAMPLE
TAG
I
ASSIGNED
LAB
0
COND OM
OF SAMPLE
SI MENT, ETC.
REMARKS:
1. Custody Scii(,)
2. Custody ScsU’tos.:
3. iis-o(-Cwtody
4. Tri cRzçxxu x
S. Aiz fl
7. S zç1oIqa
Siixçlc Tq
Nu bc s
2. S&mçLs Cto&aoa
P tejw/Abie
PccctiAbscrg
Airbill1 Iick.
Pre.scn i/Abac
LixodlN’X Usted
O
Custody
Intsa ’i3rokrAl
9. D xa i cXW& IO os
asitody re dj . In
rcpo 1s. &cd e tap
Ycjft4o
I1.T Reczived
Saa3pk Tra zfei
r
Arcai
B,-.
Os:
—
-
—
-
.
• Coat. SMO & d amath rca d oht.wIuUos
Rcvacwc4By:
—
L4, 2 book Ps c Ns:
B RM DC•Z
-------
EXHJJilT A
ATTACHMENT D
ANALYTICAL SPECIFICATION
FOR
TOTAL ORGANIC CARBON, TOTAL COMBUSTIBLE ORGANICS,
AND GRAIN SIZE IN SEDIMENT
-------
1. SCOPE
The analyses of Total Organic Carbon, Total Combustible Organics, and Grain Size
Distribution in soil, sediments, and waste solids is required to be performed by this
specification.
The laboratory must meet the required detection limits and prove those detection
limits with a recent MDL study.
2. PURPOSE
The data obtained through these analyses will be used to delineate contamination,
design remediation alternatives and/or to determine ecological risk.
3. DEFINITION OF WORK
Sediment samples are to be analyzed for Grain Size Distribution (ASTM D422-63),
and either Total Organic Carbon (TOC using the Lloyd Kahn method), or Total
Combustible Organics (TCO using ASTM D 2974-87) as instructed by M&E. The
chain of custody will indicate which samples are to be analyzed for TOC (low carbon
content) or TCO (high caibon content). M&E field personnel will determine which
analysis is appropriate.
4. SCTfl’IMJLE
Samples will be shipped daily as collected. Saturday delivery will be required.
Overnight delivery service will be used. Contacts for shipping and data delivery are
specified in Exhibit A, Attachment F.
Holding time:
Samples must be analyzed for all protocols within fourteen (14) days of
collection.
Delivery of Data:
Sample data must be delivered to M&E within thirty-five (35) days of
laboratory receipt of the last sample per sample delivery group of twenty
(20) samples or less.
5. ANALYTICAL REFERENCES (Attachment D.1)
1
-------
Total Organic Carbon: Lloyd Kahn Method for Determination of Total Organic
Carbon in Sediment. U.S. EPA, Region II. July 1986.
ASTM D2974 -87 July 1987
Standard Test Method for Moisture, Ash, and Organic Matter of Pear and Other
Organic Soils.
ASTM D 422-63 Nov. 1963 (R.eapproved 1990)
Standard Test Method for Particle Size Analysis of Soils.
6. SAMPLE PRESERVATION AND DETECTION LIMflS
A. Total Organic Carbon (TOC)
• Sample preservative: Cool to 4°C
• Holding time: Fourteen (14) days from time of collection to analysis
• Detection Limit Requirement: 100 mg/kg
B. Total Combustible Organics (TCO)
• Sample preservative: Cool to 4°C
• Holding time: Fourteen (14) days from time of collection to analysis
• Detection Limit: 100 mg/kg
C. Grain Size Distribution
• Sample preservative: Cool to 4°C
• Holding time: Not applicable
• Detection Limit: 0.1 mg (down to #200 mesh sieve), lowest
discernible gradation of the hydrometer
7. ANALYTICAL PROCEDURE
A. Total Organic Carbon (TOC)
1) Total Organic Carbon: Lloyd Kahn Method for Determination of Total
Organic Carbon in Sediment. U.S. EPA, Region II. July 1986.
2
-------
2) Perform the procedure as stated in the method (Attachment D. 1) with
the exceptions required below:
• If the sediment is less than 30% solids, a larger sample must be
analyzed in order to meet the reporting limit requirements. Determine
percent solids as per Method B ASTM D2974-87 in Attachment D. 1.
• Analytical procedures and instructions are provided in Attachment D.1.
• Each sample must be analyzed in duplicate. The RPD results must be
less than or equal to 20%. If the criterion is not met, reanalyze both
the sample and the duplicate. If the RPD criterion is still not met, flag
the sample and duplicate results with a “i”. Report both values the
average value in mg/kg on a dry weight basis.
• The date of preparation of each solution used in the analysis must be
clearly documented in the analyst’s logbook and provided in the fmal
data package.
• The standard calibration curve must contain a laboratory blank and five
(5) concentrations of standard solutions, which span the expected
concentration range. The lowest standard must be equal to the
reporting limit. The correlation coefficient must be greater than or
equal to 0.995 before the samples can be analyzed. If the criterion is
not met, generate a new standard curve and reanalyze the samples until
the criterion is met. If a sample falls outside of the calibration range,
either use less (no less than 50% of what method specifies) sample or
recalibrate using standards that span the desired range. Report the
source of the calibration standards.
• An EPA check standard (from a separate source than the calibration
standard), at a concentration of 200 mg/kg must be analyzed after the
standards and prior to blank and sample analysis, and after the last
sample in the analytical sequence. The recovery results must agree
within ±15% of the true value. If the check standard analyzed prior to
sample analysis does not meet the criterion, a new standard curve must
be generated. If the check standard analyzed at the end of the
analytical sequence dces not meet the criterion, reanalyze all samples,
blanks, and check standards. The check sample must meet the criterion
prior to sample analysis. Report the source of the check standard.
• A method blank must be analyzed prior to sample analysis after the
analysis of twenty (20) or fewer samples (including QC samples). The
blank is to be brought through the entire preparation and analytical
3
-------
cedure. If contamination is present at 50 mg/kg or greater,
determine the source of contamination, nd prepare and anaJyze a new
blank until the contamination is less than 50 mg/kg. This criterion
must be met prior to sample analysis.
• A matrix spike must be performed at a frequency of one (I) per SDG.
The sample indicated on the traffic report as the matrix spike sample
should be spiked such that the concentration in the spiked sample, at
the time of analysis, is at the mid-range standard concentration or at
twic the sample concentration, whichever is higher. Report the results
for the spiked and unspiked sample and the percent recovery (%R).
The %R must be within 80% to 120%. If this criterion is not met,
prepare and analyze a new spiked sample. If the %R is still outside the
limits, flag the matrix spike and unspiked sample results with a “#,‘.
• If a scrubber is incorporated in the instrumentation, the efficiency of
that scrubber must be measured daily before running samples. The
efficiency will be measured according to the manufacturer’s instructions
and the result reported along with each day’s run or with each sample
delivery group of twenty (20) samples or less.
B. Total Combustible Organcis (TCO)
1) Total Combustible Organics: ASTM D2974 - Standard Test Methods
for Moisture, Ash and Organic Matter of Peat and Other Organic Soils
2) Perform the procedure as stated in the method (Attachment D.l) with
the exceptions required below:
• ASTM Method D2974-87 uses several methods. Method B will be
used to determine moisture content. Method D will be used to
measure Total Combustible Organic content by combustion at
750°C.
• The sample size will be no less than 20 gms of dry, ground, and
homogenized soil. Any free water must be decanted and discarded.
If the moisture content of the soil is more than 50% then more soil
must be taken to insure that 20 gms of dry soil is used in ashing.
• The D2974-87 method does not stipulate the exact time to bring a
sample to air dryness or to constant ash weight. The air drying of
the sample is not necessary and the sample can be weighed directly
with the stipulation that is discussed in #2. The oven dried sample
must be brought to constant weight at a minimum of sixteen
4
-------
(16) hours at 105°C. The ashing time is also not stipulated in the
D2974-87 method. The minimum time at 750°C is two (2) hours
in the muffle furnace. This two (2) hours does not include the time
to bring the sample to temperature. Both temperatures must be
checked and if outside set limits the oven is readjusted.
Temperature limit must be met prior to sample analysis.
The amount of time the dishes are allowed to desiccate before
weighing must be constant from sample to sample and for all
blanks. A time between thirty (30) minutes and sixty (60) minutes
(but no more) is adequate for uniform cooling. The designated
desiccation time must be constant for all samples and must be
recorded for each sample in laboratory notebook.
• The analytical balance must be checked once per eight (8) hour
day. A method blank must be run on an empty drying dish and
must be performed for both stages, Method B and Method D. The
blank results for weight loss must be accounted for in the
calculation of sample results.
• Run each sample in duplicate. The RPD results must be less than
or equal to 30%. If the criterion is not met reanalyze the sample
and report all individual results. If the initial duplicate is within
30% RPD average the results and report. If the 30% criteria is not
met on reanalysis, report only the individual results. No average is
required.
C. Grain Size Distribution
1) ASTM D422-63 - Standard Test Methods for Particle Size Analysis of
Soil
2) Perform the procedure as stated in the method (Attachment D.l) with
the exceptions required below:
• Sieve analysis and hydrometer analysis are requested. Sieve
requirements as specified in Section 3.6 of the Method. For
quantitative detern ination of the distribution of particle sizes larger
than 75 jim, retained on the No. 200 sieve, follow the procedure
specified in Section 6.0 of the Method.
• The hydrometer portion of the analysis must be performed with a
ASTM approved hydrometer (3.3). The origin, model serial number,
5
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and manufacturer must be recorded on the data sheets. The hydrometer
must be corrected as per the Method.
The analytical balance used to determine the mass of each fraction must
comply with the requirements described in Section 3.1 of the Method.
The balance must be checked daily prior to weight determination with
class “S” weights and the calibration must be within the manufacturer’s
tolerance limits, or the balance must be recalibrated. The calibration
must be recorded and reported.
• Each sample must be analyzed (except sieve analysis) in duplicate. The
results must agree within 20% or another sample is run. If the results
agree within 20%, average the individual results and report this average
as well as the individual results. The grain size must be performed
down to the No. 200 sieve.
• Each sample for hydrometer analysis may be analyzed once.
• The thermometer must be certified accurate 1°F (0.5°C) and must be
checked daily.
• The water bath must be kept at constant temperature 20°C and the
temperature must be checked before and after the analysis of each
sample and recorded.
• The composite correction for the hydrometer reading must be
performed as in part 7 of the Method. The hydrometer must not be off
by more than 10% or another hydrometer must be used.
• The hydroscopic moisture must be measured as in part 8 of the
Method.
8. QUALITY CONTROL REQUIREMENTS
A. Total Organic Carbon (TOC)
Audits Required
Frequency of Audits
Limits
Corrective Actions
Standard Daily, prior to blank and Correlation Generate a new calibration curve
Calibration saiznle analysis Coefficient until a correlation coefficient of
Curve > 0.995 > 0.995 is achieved. Limits must
be met prior to sample analysis.
6
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Audits Required
Frequency of Audits
Limits
Corrective Actions
Continuing
Calibration
Check (Mid-
Range standard)
EPA Check
Standard
Matrix Spike
(Mid-Range
cone.)
CO: Scrubber
efficiency
1 per 10 analytical
samples and at end of
analytical run
Daily, prior to blank and
sample analysis, at
the end of the analytical
sequence
Daily, prior to sample
analysis I per 20
samples analyzed
Once per 8 hour day,
check prior to sample
analysis
Once per batch of
samples analyzed at the
same time
If outside limits, recalibrate
instruments and rerun samples
analyzed since last compliant
continuing calibration check.
If the criterion is not met for the
initial check standard, generate a
new standard curie and reanalyze the
check standard. The criterion must
be met prior to sample analysis. If
the final check standard is outside the
limits, reanalyze all samples
(including those analyzed since the
last acceptable check standard).
If the concentration is 50 mg/kg,
determine the source of
contamination, prepare and
analyze a new blank. All associated
samples must be reanalyzed. Repeat
until Criterion is met.
If the RPD is outside the limits,
repeat the analysis of both the sample
and duplicate. If the RPD is still
outside the limits, flag the results
with a ‘.
If the %R is outside the limits,
repeat the analysis. If %R is still
outside the limits, flag the matrix
spike and unspiked sample results
with a # .
Follow manufacturer’s instructions.
Limits must be met prior to sample
analysis.
Readjust oven. Limit must be
met prior to sample analysis.
Readjust furnace and rerun any
affected samples.
Method Blank
Duplicate
+10%
±15% of
true value
<50 mg/kg
RPD <
20%
80-120% R
No
response
Perform on every sample
1 per SDG
Daily
B. Total Combustible Organics (TCO)
Audits Required
Frequency of Audits
Limits
Corrective Actions
Oven
temperature
check
Muffle furnace
temperature
check
105°C ± 2°C
750°C ± 30
7
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Audits Required
Frequency of Audits
Limits
Corrective Actions
Method Blank
Balance Check
Duplicate
Once per batch of 10
analytical samples
Once per 8 hour day
All analytical samples
±50 tug
±0. 1 tug
±30%
Clean all ceramic ware and rerun
all affected samples.
Contact service representative.
Balance must be wjthj limit prior
to any weight determination.
Rerun the samples. Report
individual results.
C. Grain Size Distribution
Laboratory must submit sieve certification performed within six months prior
to sample analysis, complying with El 1 Section 2 of the Method.
Audits Required
Frequency of Audits
Limits
Corrective Actions
Duplicate
Balance Check
Hydrometers
151H, 152H
Check
All samples
Daily prior to sample
analysis
Daily prior to sample
analysis
± 20%
± manufact.
tolerance
±10%
If outside the limits, repeat the
analysis. If still outside limits,
flag the results with an asterisk
(U*U)
Check the balance for
malfunctioning, recalibrate.
Limits must be met prior to
sample analysis.
Check the temperature and insure
20°C and retest. If out, go to
new hydrometer and test. Must
meet specification prior to analysis
of samples.
9. ANALYTICAL DELiVERABLES
A. Total Organic Carbon (TOC)
• Narrative explaining all anomalies and corrective actions taken.
Included in the narrative should be a tabulation of the M&E sample
number with the corresponding laboratory sample number.
• A MDL study recently performed or a recent blank spiking study at a
concentration at or below the required detection limit. Ether study
must be no greater than six (6) months old.
8
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• Tabulated sample results; positive results and quantitation limits for
non-detected results. Report both TOC analysis results and the
average. All soillsediment results must be in dry weight, reported in
mg/kg.
• Laboratory analysis notebook pages or bench sheets; all sample raw
data such as preparation logs, analysis logbooks an all instrument strip
charts and printouts for all runs of samples and associated standards
and QC samples.
• Tabulated duplicate results (%D) and matrix spike analysis (%Rec),
tabulation of QC check standards (%Rec), EPA check sample results
(%Rec), calibration verification results, and blank results. The true
value and the actual concentration of spikes must be provided with the
percent recovery tabulation. Raw data, which is specified above, must
be provided.
• Standard curve raw data with instrument print outs and concentrations.
Plotted Standard Curves. Include linear regression equation.
• Examples of sample results calculations for each analysis. All
equations, dilution factors, and information required to reproduce the
laboratory results must be provided.
• Original signed chain of custody forms, sample tags and shipping
airbills. Copies of all telephone logs and communications between
M&E and the laboratory.
• The data package must be paginated and of good copy quality. The
data package must be as much like an EPA CLP package as possible.
• Copies of the sample log in sheets containing recorded cooler
temperatures and sample preservation checks, must be delivered with
the package.
B. Total Combustible Organics (TCO)
• A narrative explaining all anomalies and corrective actions taken.
Included in the narrative should be a tabulation of the M&E sample
number with the corresponding laboratory sample number. The
narrative must encompass all samples and field QC samples in the
sample delivery group.
• All moisture contents must be tabulated for samples and blanks.
9
-------
• All total combustible orga.nic contents must be tabulated for samples
and blanks.
• A record of balance calibration must be recorded in a notebook and
copied as a deliverable per eight (8) hour day.
• A record of the thermometer calibration must be recorded in a
notebook and copied as a deliverable per eight (8) hour day. The
temperature of the drying oven must be recorded per eight (8) hour day
in the notebook.
• A record of temperature calibration of the muffle furnace must be
recorded in a notebook and copied as a deliverable per eight (8) hour
day. The temperature of the muffle furnace must be recorded per eight
(8) hour day in the notebook.
• All weights must be recorded and tabulated.
• A sample calculation must be included with each day’s sample
tabulation.
• Results must be recorded in mg/kg dry weight basis for total
combustible organic content. Moisture content will be recorded in %
basis.
• All copies of laboratory notebook pages with raw data must be
included.
• All sample tags, airbills, and chain of custody sheets must be included.
Copies of any telephone logs for conversations between M&E and the
laboratory must also be included.
• The data package must be paginated and of good copy quality. The
data package must be as much like an EPA/CLP package as possible.
• Copies of the sample log in sheets that record cooler temperature and
sample preservation checks must be included.
C. Grain Size Distribution
• The report must include Sections 18.1.1, 18.1.2, 18.1.3.1, 18.1.3.2,
18.1.4, 18.1.5, 18.1.6 of the Method and all the hydrometer
deliverables.
10
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• Laboratory analysis notebook pages or bench sheets; all sample raw
data.
• Tabulated results of duplicate anaiyses and percent moisture results.
• Tabulated results of hydroscopic moisture of samples.
• Examples of sample results calculations for each analysis. All
equations and information required to reproduce the laboratory results
must be provided.
• Record of the water bath temperature before and after analysis of
samples.
• The following dated and signed originals must be included: chain of
custody forms, sample tags and shipping airbills. Telephone logs must
also be included.
• The data package must be paginated and of good copy quality.
• A case narrative explaining all anomalies and corrective actions taien.
Included in the narrative should be a tabulation of the M&E sample
number with the corresponding laboratory sample number. The
narrative must encompass all samples and field QC samples in the
sample delivery group.
• Copies of the sample log in sheets that record cooler temperature and
sample preservation checks must be included.
D. Complete Sample Delivery Group File (CSF) Audit
Due to the litigative nature of each Superfund site, Region I EPA requires that
all analytical data, quality control data, and tabulated raw or supporting data
be delivered with each sample delivery group (SDG). With each sample
delivery group, an EPA Region I Complete SDG File Completeness Evidence
Audit must be carried out. The CSF Completeness Evidence Audit Forms are
included in Attachment D.2 and must accompany each sample delivery group
(data package). The laboratory through these audit forms must demonstrate
that each piece of sample data, raw data, calibration data, and any other data
requirements of this specification is included by the laboratory in the data
package.
11
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The forms included in Attachment D.2 are for all types of data packages. For
this specification the laboratory will use the forms supplied to the best of their
ability where deliverable items are applicable.
10. EXCEPTIONS
If QC requirements or action limits are exceeded; or if samples are destroyed or lost;
or if matrix interference is suspected, contact:
Andrew F. BeliveaU
Metcalf & Eddy, Inc.
(617) 246-5200 ext. 4433
12
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ATTACHMENT D.1
ANALYTICAL PROCEDURES
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DErZRXD(ATIOU OF TOTAL Oat.&NIC CA2BO I SZDI XT
J ;} 1 3 9 3
P RE PARED BY: 7//O/(
Lloyd Liba, ( uilit7 jisurance Speci&list
A21ILLA TION: U.S. Zavtrocaefltal Protection Agency, Z.e ion U
InviroinentLI Services DivisiOn
MonitorL * XL@L$e eQt lranch
Idison, 1ev Jersey 08837
-------
D Tg&1(tXATI0 0V TOTAL OLCL?(IC C” O$ L I $ DIX )IT
1. Scop . and ApplictttOQ
1.1 This method describes protOCOlS for the determination of organic
carbon In ocean sediments.
1.2 Although the detection limit may vary vith procedure or Laatrijaent,
£ ainiiu r.portic.g value of 100 mg/kg vi ii be required for the
ocean dumping/dredging program.
1.3 Several types of determinatiofll, which are considered equivalent
are presented.
1.4 Data are reported in mg/kg on dry veight basis.
1.5 Wet combustion methods are not considered to be equivalent to the
pyrolytic methods herein described.
2. Su= ary of Xeth
2.1 Inorganic carbon from carbonates and bicarbon.ates is removed by
acid treatment.
2.2 The organic compounds are decomposed by pyro]ysLa in the presence
of oxygen or air.
2.3 The carbon dioxide that is formed is determined by direct non—
dispersive infrared detection, fla ionization gas chromatography
after catalytic conversion of the carbon dioxide to methane; thermal
conductivity gae chromatography, differential thermal conductivity
detection by sequential removal of vater and carbon dioxide; or
thermal. conductivity detection folloviag removal of vater with magnesium
perchiorats.
2.4 Water content in determined on a separate portion of sediment.
3. a ple aandlin and Preserv$tio !
3.1 Collect sediments in glass jars with Teflon or aluminum foil. Cool
and maintain at 4C. Analyze within 14 days.
4. Interferences
4.1 Volatile organics in th. sediments may be lost in the dec.arbonation
step resulting in a by bits.
4.2 3acterial decospoeitiOfl and volatilization of the organic compounds
are minimized by maintaining the sample at 4’C, analysing within the
specified holding time, and analyzing the vet sample.
-------
2.
5. 4pparatus
3.1 Drying oven aaiutsined &t 103 to 105’C.
5.2 A a1ytica1 Lnstru ient option..:
5.2.1 Perkin !leer Model 240C !len.ental Analyzer or equivalent.
5.2.1.1 In this in.tru eut, the siapie fr Section 7.2 is pyrolyled under
pure oxygen, veter is r .oved by a.tgns.iua percblorat. and the
carbon dioxide La r oved by ascarite. The decreas. In signal
obtained by differential therati conductivity detectors placed
betwen the co bustiOQ gas streaa before and after the ascent.
tube is £ aeasurs of the organic carbon content.
5.2.2 Carlo Erba Model 1106 C Analyzer, or equivalent.
5.2.2.1 In this apparatus, the staple is pyrolyzed in a induction typs
furnace, md the resultant c.arbou dioxide is cbrouatognaphic.ally
separated and analyzed by a differential therzs1 conductivity
detector.
5.2.3 tzco Models Wai.2, waIl2, or Cl—12 carbon deterainators, or
Models 600 or 800 CaI analyzers.
5.2.3.1 In the LZCO W2.—12, the sa.aple Li burned La high frequency induction
ma, the carbon dioxide is selectively adsorbed at rooe teaper—
ature in a eolecular sieve. It La subsequently released by beating
arid is aessured by a theraal conductivity detector. The Z—1l.2 is
an upgraded WR—12 eaptoying aicroprocessor electronics and a
printer to replace the electronic digital yo1 t.r.
5.2.3.2 In the LECO C1—12 carbon deteramnator, the staple ii c bust .d in
oxygen, aoiatur . and dust are reaovd by appropriate traps and the
carbon dioxide is aeasured by a ,.lectiy., solid state, infrared
dotector. Th, signal frog th. detector is then processed by a
aicroprocessor and the carbon content is displayed on a digital
readout mud recorded on an integral printer.
5.2.3.3 In the IICO CBX—600 and CEU—800 elezental analyzers, tb. staple is
burned under oxygen in a resistance furnace and the carbon dioxide
is peasured by a selective infrared detector.
5.2.4 Dohraan Model DC.35 Digital igb Teaperature TOC Analyzer.
5.2.4.1 In this instruaent, the siaple is burned in ra.ist.anài furnace under
oxygen, the interfering gases are reaoved by $ spazgen/scrubbisr
syat and the carbon dioxide is a asured by a non—disjensiv. infra-
red detector and shova on a digital display in concentration units.
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3.
5.3 Mo specific enelyaer is recoua.ended as superior. The above listing
is for inforaition only and is uot intended to restrict the s,
of other unlistsd instruaents capable of analyzing TOC. The iustr —
aents to be used ist have the following specifications:
3.3.1 A ccabustion boat which is heated in a stre of oxygen or air in a
resistance or induction—type furnace tO completely convert organic
subs acces to C o 2 and water.
3.3.2 A ans to physically or by aeasur sftt technique to separate water
and other mnterf.rants fros Co 2 .
3.3.3 A ans to quantitatively determine Co 2 with adequate sensitivity
(100 v.2Jkg), and precision (25Z at the 95 confidence level as deaou—
strated by repetitive aeasureaeuta of a well mixed ocean sediaent
sa. p1e).
5.4 A strip chart or other periauent recording device to doc ent
the analysis.
6. leagenta
6.1 Distilled water uaed in preparation of stzndarda and for dilution of
saaplei should be ultra pure to reduce the carbon concentration of the
blank.
6.2 Potaesiuz hydrogen phthalate, stock solutioø, 1000 ag carbon/liter:
Dissolve 0.2128 g of potaasiu hydrogen pbthalate (Primary Standard
Crade) Lu distilled vater and dilute to 100.0 ii.
NOTZ 2: Sodium oxalate and acetic acid are cot recc .i cded as stock
Solutions.
6.3 Pot issiuz hydrogen pbth.alate, standard solutions: Prepare standard
solutions fros the stock solution by dilution with distilled water.
6.4 Phosphoric acid solution, 1:1 by volume.
7. Proceduri
7.1 Vei gh the well mixed sample (up to 50O mg) into the coubustion boat
or cup. Add 1:1 phosphoric acid drop vise until effervescence
stops. fleet to 75C.
SOT!: This procedure will convert inorganic carbonates end
bicarbonate. to carbon dioxide and eliaicate it fros
the sample.
7.2 Analyu the residue according to the inatri eut manufacturer’s
instructions.
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J$ D2974
6.2.1 This calculation is used primarily for geotechnicai
purposes and the result should be referred to as the moisture
content as a percentage of oven-dried mass.
6.3 Take care to indicate the calculation method used.
7. Method B
7.1 This method should be used if pH, nitrogen content,
cation exchange capacity, and the like are to be tested.
7.2 Mix the sample thoroughly and select a 100 to 300 g
representative sample. Determine the mass of this sample
and spread evenly on a large flat pan. Crush soft lumps with
a spoon or spatula and let the sample come to moisture
equilibtiu with room air. This will require at least 24 h. S r
occasionaily to maintain maximum air exposure of the entire
sample. When the mass of the sample reaches a constant
value, calculate the moisture removed during air drying as a
percentage of the as-received mass.
7.3 Gnnd a representative portion of the air-dried sample
for I to 2 mm in a high-speed blender. Use the ground
portion for moisture, ash, nitrogen, cation exchange capacity
tests, and the like.
7.4 Thoroughly mix the air-dried, ground sample. Weigh
to the nearest 0.01 g the equivaierit of 50 g of test specimen
on an as-received basis. Determine the amount, in grams, of
azr-dricd sample equivalent to 50 g of as-received sample, as
follows:
Equivalent Sample Mz.s , g — 50.0 — ((50 X M)/100J
where:
M moisture removed in air drying. %.
7.5 Place the sample in a container as described in 5.1 and
proceed as in Method A.
8. Method B Cilcubtjo
8.1 Calculate the moisture content as fol!ows
Moisture Content, S — (50 — B) x 2
where:
B oven-dried sample, g.
Si.! This caiculation gives moisture content as a per.
cernage of as-received mass.
8.2 An alternative calculation is as follows:
Moisture Content, S — ((50 — B) x 100 )/B
8.2.1 This calculation gives moisture content as a per.
cenc.age of oven-dned mass.
9. Method C
ASH CO? ’I1tNT
9.1 Determine the ma.ssofa covered high-silica orporce.
lain dish.
9.2 Place a part of or all of the oven-dried test specimen
from a moisture determination in the dish and determine the
mass of the dish and specirneis.
9.3 Remove the cover and place the dish in a mume
furnace. Gradually bring the temperature in the furnace to
440C and hold until the specimen is completely ashod (no
change of mass occurs after a further period of beating).
9 4 Co er with the retained aluminum foil cover, cool in a
desiccator, and determine the mass.
9.5 This method should be used for all geotec
general classification purposes.
10. Method D
10.1 Determine the mass of a covered high.silj
celain dish.
10.2 PIaceacartofora1Jo(theovefldriedt
from a moisture determination in the dish and determine
mass of the dish and specimen.
103 Remove the cover and place the dish in a
furnace. Gradually bring the temperature in the
750C and hold until the specimen is completely as -
change of mass occurs after a further period of heatifl )
10.4 Cover with the retained aluminum foil Cover, co
a desiccator, and determine the mass.
10.5 This method should be used when peats axe b
evaluated for use as a fuel.
11. CalculatIon for Methods C and D
11.1 Calculate the ash content as follows:
Ash Content, S — (Cx 100)/B
where:
C ash, g, and
.8 — oven-dried test specimen, g.
12. Calculation
ORGANIC MAlTa
12.1 Determine the amount of organic matter by duff
ence, as follows:
whey
D — ash content, %.
Organic mailer, S — 100.0 — D
13. Report
13.1 Report the following information:
13.1.1 Results for organic master and ash content, to t&
nearest 0.1 %.
13.1.2 Furnace temperature used for ash content deterir
nations.
13.1.3 Whether moisture contents are by proportion
as-received mass or oven-dried mass.
13.1.3.1 Express results for moisture content as a p
cencage of as-received mass to the near 0J %.
13.1.3.2 Express results for moisture Content as a p
centage of oven.dried mass as toUows:
(a) Below 100 5 to the nearest I 5.
(b) Between 100 % and 500 % to the nearest S
(c) Between 500 5 and 1000 5 to the nearest 10 .
(d) Above 10005 to the nearest 205.
14. PrecisIon and BIu
14.1 The precision and bias of these test methods have cI
n determined. Data are being sought for use in devel
oping a precision and bias statement.
-------
D 2974
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• Designation: D 422 — 83 (Reapproved 199O) 1
Standard Test Method for
Particle-Size Analysis of Soils 1
This nindard u usund under the fiend deeijnanon D 422: the number immediately roBo,u ing the dce tsuon indiatci the w of
ong inai adopuon or. in the we o(rv ,uon. the yes, of La ‘ v’uon A number in perrnlhciej ,ndia SM ,w o(tan reapproy,] A
supcricnpc epiilcn (i) indicates in odztcnaj c an e nce the Isu re uaon or reapprovij.
Hurt—Section 19 was i ed nduoruily in September I9 .
1. Scope
I. I This test method covers the quantitative determina-
tion of the distribution of particle sizes in soils. The
distribution of particle sues larger than 75 jsm (retained on
the No. 200 sieve) is determined by sieving, while the
distribution of particle sizes smaiier than 7$ jsm is deter-
mined by sedimentation proce , using a hydrometer to
secure the necessary data (Notes I and 2).
Nort I—Separation may be made on the No. 4(4.75-mm). No. 40
( 425 -Mm), or No. 200 (75. ji ) sieve instead o(the No. 10. For wh.ue’rcr
sieve used, the sirs shall be indicated in the report.
Noit 2—Two types of dispersion devices are peovided (1) a
high-spred mecharucal stirrer. arid (2) a r dispersion. Estensi inv .i-
gallons indicate that air-dispersion devices produce a more pove
dispersion of pla ic soils below the 20-jim size and apprectably less
deg adauon on all sues when used iinth sandy soils. Because of the
definite advantages favonng air dispersion, its use is recommended. The
resuks from the two typ of devices diEter in magnitude, depending
upon soil type, leading to marked dsfl’crertois in paruck size disuibu-
tion. especially (or sizes finer than 20 jim.
2. Referenced Documents
2.1 ASTM Standards:
D421 Practice for Dry Preparation of Soil Samples for
Par icle-Sjze ArLaJysis arid Determination of Soil
Ccnstant.s 2
E 11 Specification for Wire-Cloth Sieves for Testing
Purposes 3
E 100 Specilication for ASTM Hydrometers 4
3. Apparatus
3.1 Balances—A balance sensitive to 0.01 g for weighing
the material passing a No. 10(2.00-mm) sieve, and a balance
sensitive to 0.1 % of the mass of the sample to be weighed for
weighing the material retained on a No. 10 sieve.
3.2 Stirring Apparatus—Either apparatus A or B may be
used.
3.2.1 Apparatus A shall consist of a mechanically oper.
‘Thu ice mcuiod ii under the juni4tct on OIASTM Commuter 0-1* on Sod
and Rock and u the direct r nub ,Iity of Subcommittee 01803 on Teetuie.
Ptaiticuy ‘‘4 )cnut Otarscscncii o(Sotls.
Currci t c4 uon appro nd No, 21. 963 Ongirafl) publuliod 1935. Rcpl.
0422 —62.
Annual Book e(2S77.d1 Vol 040*.
Ar aJ Book ofiSTM Sividards, Vol 14 02.
‘AriiiwJ Book (.LSTM Sgandards, Vol 14.03.
ated stirring device in which a suitably mounted e!e
motorturns a verticaJshaftata speedof not Iessthan 10,
rpm without load. The shaft shall l x equipped witi
replaceable stirring paddle made of metal, plastic, or ha
rubber, as shown in Fig. 1. The shaft shall be of such ler
that the stirring paddle will operate not less than Is In. (1
mm) nor more than 1½ in. (38.1 mm) above the bottoni
the dispersion cup. A special dispersion cup conforming
either of the designs shown in Fig. 2 shall be provided to 1
the sample while it is being dispersed.
3.2.2 Apparatus B shall consist of an air-jet dispersià
CUP’ (Note 3) conforming to the general details shown in
3 (Notes 4 and 5).
Nort 3—The amount o(au required by an air-jet dispersion c
of the order o(2 ft 1 /rnia: sonic small air compressors are nor capabte
supplying surncseni air to operate a cup.
Noi’z 4 —Another air-type dispersion device, known as
tube. developed by Ow and Davidson at Iowa State CoIlej —
shown to give results uivalent to those secured by the air-jet .
cups. When it is used, soaking of the sample ran be done i ,,th
sedimentation C tinder, thus eliminating the need for rrans(emng
slurry. When the air spersion tube is used, it shall be so indicatcç
the report.
.cra 3—Wa may condense in air kites when not in use. Thi
water mu be removed, either by using a water u p on the air line, o
b’owing the water out of the line before using any of the LC
dispersion purposes.
3.3 Hydrometer ASTM hydrometer, graduated IC
read in either spec ,— , ,. .‘ity of the suspension or grams
litre of suspension, .nd conforming to the requirements
hydrometers ISIH or l52H in Specifications E 100. Dimen-
sions of both hydrometers are the me, the scale being th
ordy item of difference.
3.4 Sedimenewon Cylinder—A glass cylinder essenti -
18 in. (457 mm) in height and 2½ in. (63.5 mm) in diameter
and marked for a volume of 1000 mL The inside diam ’
shall be such that the l000-mL mark is 36 ± 2 cm from
bottom on the inside.
3.5 Thermometer—A thermometer accurate to l
(0.5C).
3.6 Sieves—A series of sieves, of square-mesh woven. ’
cloth, conforming to the requirements of Specification E 1
A full set of sieves includes the foUowing (Note 6):
Detailed w’ortiiig di r ror tins cup yr available at a nomi
SM Amencan Socicty for bun; and Matenais. 1916 Race SL ?Pu
19103. Order Mjuncs No. 12.404220-00.
-------
0422
WGo’O,O49
CIwomI
.
0001
MmV c
0049
Eq d’ysisnta
0
¾
rmi
0
124
5.10
12.7
19.0
FIG. 1 Detail of Stimng Paddlea
3-io. (13-mm)
a. (3O.m a)
Vi’-rn. (37i -mml
1.40. (25.0 -mm)
40. (190 .mm )
-ia. (9.3-mm)
No. 4 (4. 7 5.mm)
-4n. ( 1 3.mm)
1 - o. (3 1 .3-mm )
l9 0 -mm)
-4 %. (9.3-mm)
No.4 (4J3 o m)
No. $ (26-mm)
No l0(2 .03-40m )
No. C850- am)
No.40 (42ham)
No.60 (230- &m)
No. 140 (lO6- m )
No. 200 (13 - imJ
Nmt 6--A iei of grnn uniform pacin; of point3 for the
graph. U requIred in Section (7, may be used ildedred. Thu set
of the foUowing s ev
3.7 Water Bath or Consia,u.Temperature Room—A
water bath or CoflstaflHernpeiature room for maintaining
the soil suspension at a constant temperature during the
hydrometer analysis. A satisfactory water tank is an insulated
tank that maintains the temperature of the suspension at a
convenient constant temperature at or ncai’ 68F (20’C).
Such a device is illustrated in Fig. 4. In cases where the work
is performed its a room at an automatically controlled
constant temperature, the wa r bath is not necessary.
3.8 Beaker—A beaker of 250-rn!.. capacity.
3.9 Timing Device—A watch or clock with a second
band.
4. Dispersing Agent
4.1 A o1utjo of sodium hexametaphosphate (sometimes
called sodium metaphosphate) shall be used in distilled or
dermrseralized water, at the rate of 4.0 g of sodium
hcxamctaphosphate/litre of solution (Note 7).
Nore 7—Sobjuons of .hh jt. if acidic. s ow)y re v1 c c hydrolyze
beck to the onhophosphate form witha zesultaot decrease 20
hCliOn. Solutions 1 uid be prepared frequcody (St )c2 * a mooth)
C l adjusted to pH of S or 9 by means of tedium corbenate Eoni
ClntaJfl flg soluuons should h.ave the date of pic ratian muted ca
them.
4 2 Al) u er used thai be either distilled or
— . . . te shall
No l6(I. )I .mm)
No )O(600*un)
No. 50 () - im)
No. 100 (150-tim)
No. 200 (75 -tim)
U. lc £ ai1i
It
2.6
3.75
IT ,,,
60
9 52
Dispsrvon Cups of App.ratus
be brought to the temperature that is expected to prevad
during the hydrotneter test. For example, ir the sedimenta-
tion cylinder is to be placed in the water bath, the distilled or
demineraiized water to be used shah be brought to the
tempcrature of the ccntioiled water bath; or, if the sedimen-
tation cylinder is used in a room with controlled tempera-
ture, the water for the test shall be at the temperature of the
room. The basic temperature for the hydrometer test is 68F
(20 ’C). Small variations of temperature do not introduce
differences that are of practical si sificance and do not
prevent the use of corrections derived as prescribed.
(a)
tb)
1.3
FIG. 2
-------
( 0422
FIG. 3 Atr$1OuflC Jp,OfApp1t1tt1B
5. Test Sample
5.1 Prepare the test sample for mechanical analysis as
outlined in Practice D42 1. During the preparation proce-
dure the sample is divided into two portions. One portion
contains only particles retained on the No. 10 (2.00-mm)
sieve while the other portion contains only particles passing
the No. 10 sieve. The mass of air .dried soil selected for
purpose of tests, as prescribed in Practice D421, shall be
sufficient to yield quanthies for mechanical analysis as
follows:
5.1.1 The size of the portion retained on the No. 10 sieve
shall depend on the maximum size of particle, according to
the foUowing schedule:
5.1.2 Thesizeofthe portion passingthe No. 10 sieve shall
be approximately 115 g for sandy soils and approximately 65
g for silt and clay soils.
5.2 Provision & made in Section 5 of Practice D 421 for
weighing of the air-dry soil selected for purpose of tests, the
separation of the soil on the No. 10 sieve by dry-sieving and
washng, and the weighing of the washed and dried fraction
retained on the No. 10 sieve. From these two masses the
percentages reiai - ’ed and passing the No. 10 sieve can be
calculated in acccrdance with 12.1.
Non 5—A ch k on the mass v,Ju and the thorou&hflCSl or
pulvcnzauon of the clods may be secured by weighing the portioo
pa.s ing the No. tO ijeve and adding this vaiue to the mass of the washed
and ovcn.dned pornon retained on the No. 10 sieve.
SIEVE ANALYSiS OF PORTION RETAINED ON NO.10
(2.00-mm) SIEVE
6. Procedure
6 I Separate the portion retained on the No. 10 (2.00-
mm) sieve into a senes of fractions using the 3-in. (75-mm),
Nominai Dsa cw o(
¼ (95)
V i (19.0)
I (25.4)
1½ (311)
2 (50.1)
306 -2)
Ap umaLL Miaimum
Ma o( Poruoa. g
500
2000
3000
4000
It
‘I .
1
Ma 1c EquiysIsi’
3 6’4
14
37
nrs
222
.4
78.2
1582
556
940
FiG. 4 kt*mMt*d Wats Bath
2-in. (50-mm), 1½-in. (37.5-mm), 1-in. (25.0-mm), ‘? i-i
(19.0-mm), ‘6-in. (9.5-mm), No. 4 (4.75-mm), and No.
sieves, 0’ as many as may be needed depending on
sample, or upon the specifications for the material under
test
6.2 Conduct the sieving operation by means of a lat¼
and vertical motion of the sieve, accompanied by a jarring
action in order to keep the sample moving continuously ov
the surface of the sieve. In no case turn or manipu1
fragments in the sample through the sieve by hand. Contirt t
sieving until not more than I mass % of the residue on
sieve passes that sieve during I mm of sieving. Wh
mechanical sieving is used, test the thoroughness of sievi
by using the hand method of sieving as described ab -
6.3 Determine the mass of each fraction on a
conforming to the requirements of 3.1. Al the —
weighing, the sum of the masses retained on all the sie’
used should equal closely the original mass of the quanz:t,
sieved.
doss s(cr
CLp I
I —
OP £
5 L
‘ S
C O .S SLCTO’
ci.. a
-------
HYDROMETER AND SIEVE ANALYSIS OF PORTION
PASSING TIlE NO. 10 (2.OO-a ui) SIEVE
7.1 Equations for percernages of soil remaining in suspen-
sion, as given in 14.), ire based on the use of distilled or
deminel’lJiZed water. A dispersing agent is used in the water,
howc ’er, and the specific gravity of the re5ulung liquid i.s
appreciably greater than that of distilled or demineraii.zed
water.
7.1.1 Both soil hydrometers are caiibrated at 68’F (20C),
a d variations in temperature from this standard tempera-
ture produce inaccuracies in the actual hydrometer readings.
e amount of the inaccuracy increases as the variation
from the standard temperature increases.
7.1.2 Hydrometers are graduated by the manufacturer to
be read at the bottom of the meniscus formed by the liquid
on the stern. Since it is not possible to secure readings of soil
suspensions at the bottom of the meniscus, readings nust be
taken at the top and a correction applied.
7.1.3 The net amount of the corrections for the three
items enumerated is designated as the composite corr ion,
and may be determined experimentally.
7.2 For convcnien a graph or table of composite
corrections for a series of 1 temperature difTerencs for the
range of expected test temperatures may be prepared and
used as needed. Measurement of the composite ccrrection.s
may be made at two temperatures spanning the range of
expected test temperatures, and corrections for the interme-
diate temperatures calculated assuming a straight-line rela-
tionship between the two observed values.
7.3 Prepare 1000 niL of liquid composed of distilled or
dcmincralized water and dispersing agent in the same
proportion as will prevail in the sedimentation (hydrometer)
lest. Place the liquid in a sedimentation cycinder and the
cylinder in the constant-temperature water bath, set for one
oIthc two temperatures to be used. When the temperature of
the liquid becomes constant, insert the hydrometer, and,
after a short interval to permit the hydrometer to come to the
temperature of the liquid, read the hydrometer at the top of
the meniscus formed on the stem. For hydrometer l5lH the
composite correction is the difference between this reading
and one; for hydrom 15211 ii is the difference between
the reading and zero. Bring the liquid and the hydrometer to
the o er temperature to be used, and secure the composite
correction as before.
8. Hygroseopic Moisture
8.1 When the sample is weighed for the hydrometer test,
weigh out an auxiliary portion of from 10 to IS gin a small
metal or glass container, dry the sample to a constant mass in
an oven at 230 ± 9 ’F(IlO ± S’C), and weigh again. Record
the masses.
9. Dispersion of Soil Simple
9.1 When the soil is mostly of the clay and silt sizes, weigh
out a sampl- of air-city soil of approximately 50 g. When the
soil is most ’ sand the sample should be approximately 100
9.2 Place the sample in the 250-mL beaker and co uj
125 mL of sodium hexametaphosphate solution (4C —)
Stir until the soil is thoroughly wetted. Allow to soak I L
least 16h.
9.3 At the end of the soaking perioci, disperse the sampk
further, using either stirring apparatus A or B. If sumng
apparatus A is used, transfer the soil - water slurry from thc
beaker into the special dispersion cup shown in Fig. 2.
washing any residue from the beaker into the Cup with
distilled or demineraliied waler (Note 9). Add distilled or
deminerajjzed water, if necessary, so that the cup is more
than half full. Stir for a period of I ruin.
Norr 9—A large size syringe is a ronvellient device (or handling t
waler in the wishing Operation. Other devic include the 5h ’w-ai
bonie and a hose with nozzle connected to a pr surized distilkd wa
Unk.
9.4 If stirring apparatus B (Fig. 3) is used, remove the
cover cap and connect the cup to a compressed air supply by
means of a rubber hose. A air gage must be on the line
between the cup and the control valve. Open the control
valve so that the gage indicates I psi (7 kPa) pressure (Note
10). Transfer the sod - water slurry from the beaker to the
air-jet dispersion cup by washing with distilled or
demineralized water. Add distilled or deminerajj j water, if
necessary, so that the total volume in the cup is 250 mL but
no more.
Nort 10—The initial air pressure oft psi is required to pre cnt the
soil - water mixture (mom entenng the air-jet chamber when the mixture
is transferred to the dispersion cup.
9.5 Place the cover cap on the cup and open the air
control valve until the gage pressure is 20 psi (140 kPa).
Disperse the soil according to the following schedule:
Disperaoo Penod.
Ptuucu) mdc i
Soils containing large percentages of mica need be dispersed
for only I mii i. After the dispersion period, reduce the gage
pressure to I psi preparatory to transfer of soil- water slurry
to the sedimentation cylinder.
10. Hydrometer Test
10.1 Immediately after dispersion, transfer the soil - water
slurry to the glass sedimentation cylinder, and add distilled
or deminerajized water until the total volume is 1000 mL.
10.2 Using the palm of the hand over the open end of the
cylinder (or a rubber stopper in the open end), turn the
cylinder upside down and back for a period of I mm to
complete the agitation of the slurry (Note II). At the end of
I mm set the cylinder in a convenient location and take
hydrometer readings at the following intervals of time
(measured from the beginning of sedimentation), or as many
as may be needed, depending on the sample or the specifica-
tion for the material under test: 2, 5, 15, 30, 60, 250, and
1440 mitt. ltthe controlled water bath is used, the sedimen-
tation cylinder should be placed in the bath between the 2-
and 5-mimi rcadinp.
Nm Il—The number of turn.s during this minute should be
approximately 60, counting the turn upside do n and back as two turns
)I 0422
7. DetermInation of Composite Correction for Hydrometer
Reading
Under S
6to O
5
i0
Is
&
-------
arithmetic scale as the ordinate. When the hydrometer
analysis is not made on a portion of the soil, the preparation
of the graph is optional, since values may be secured directly
from tabulated data.
18. Report
18.1 The report shall include the following:
18.1.1 Maximum size of particles,
18.1.2 Percentage passing (or retained on) each sieve,
which may be tabulated or presented by plotting on a graph
(Note 16),
18.1.3 Description of sand and gravel particles:
18.1.3.1 Shape—rounded or angular,
18.1.3.2 Hardness—hard and durable, soft, or weathered
and friable,
18.1.4 Specific gravity, if unusually high or low,
18.1.5 Any difficulty in dispersing the fraction passing the
No. 10 (2.00-mm) sieve, indicating any change in type and
amount of dispersing agent, and
18.1.6 The dispersion device used and the length of the
dispersion period.
NOTE 16—Thu tabulation of graph represenu the gradatioli o( the
sample tested. If PU1ICIeI larger than those contained in the m* re
removed before testing, the report shall so slate f,jblng the amount and
maximum size.
18.2 For materials tested for compliance with definite
specifications, the fractions called for in such specifications
shall be reported. The fractions smaller than the No. 10 sieve
shall be read from the graph.
18.3 For materials for which compliance with definite
specifications is not indicated and when the soil is composed
almost entirely of particles passing the No. 4 (4.75-mm)
sieve, the results read from the graph may be reported as
follows:
(I) GraveL pi ng 3-in. as d r io on No.4 neve
(2) SNo.4aandrrianicdonfl00ncve
(a) Coazic sand. passing No 4 sieve and rewned on
No Oiacve
fbI M ium sand. paa rgNo I0s eveindreuinedco
No.40 cve
(C) Fine sand, No.40 neve and rcumed on No.
(2) Sihsuc.0074soO0OSm
(4) Clay size. smaller than 0.003 m
C .wsaI than 0.00) m
18.4 For materials for which compliance with definite
specifications is not indicated and when the soil cor
material retained on the No. 4 sieve sufficient to requ
sieve analysis on that portion, the results may be reporter
follows (Note 17): U I ’
SIEVE ANALYSIS ire
Pawng
Thi Anwican Soc y l Tssjinq and MiliriilS 1** nO p03101 rSSPOCWV (hi vWIo ’Oy any fçhfa aswt.d .n coviec 0?
w,th wiy tin, mWIos vi LI1 stifldifd. USa Vt ma gbldhd WI I1D’*U ’ aCvi 5id U s c 0mvnsa g*, (hi vs4ty ci ’ any h
pizcv rçivz. and (hi rOt I1ü w.ms1 h içvrs. c i m ci.n t.spovssbity.
Tho stanalm b au0 .a to rwoo’i d aiiy DIII by d rswons’b’i tocMIcaI COIVTWtH *W nI4 ’ be ev,e,.ed . *y th . ,wi
I no iridSi. 141W tidXf owed 0’ wlhdtf*lt YOJ w,V1WU W I W IC 141W hi U Stlfl03fd 0’ # .ddR0iiIc$i
aI ahci d be .ddrss.zed to AS TM HsadQualf c i log ThT*!Z w 1e AI cai14i.( cci ccoi c a m.s&iq ( he
tichr al c Tvm1TM. wh h y may LflWId U yw feW t1 W yo.% convncfs hive n rci’ved a Ii, , hiannç you shcind mate ycit
,ewt knOwn (0 thi ASTU Con ,m,?Tee on SiifldIIdS. 19 16 Rica Sr. P’vlaae’pn a. PA 19I
T.r.u.gi.
IC
0422
TABLE 3 VaIu.s of K tot U.. In Equa on lot Compu n9 0(am.tsq of P.r cIi In Hydrom.tsr Analysis
245 2.50 2.35
260 2.65 2.70
275
260
285
16
17
18
19
20
001510
001511
00*492
001474
001456
0.0l
o.o ae
001467
001449
0.01431
0.01481
o.o’4 2
0.01443
001425
001406
0.01457
001439
001421
00I4
001356
001435
0.01417
001309
001352
001365
001414
0.01396
001375
001361
001344
001394
0.01376
0.01339
001342
001325
001374
001356
00*339
01323
001307
ooissi —
00*338
ooi i
g i
001259
21
22
23
24
25
001435
001421
001404
001355
001372
0.01414
001391
001381
001365
001341
0.01391
0.01374
0.01358
0.01342
001327
0.01369
001353
001337
001321
001306
001345
001332
001317
001301
001281
001321
001312
001297
001282
001267
001309
001294
001279
001264
001249
001291
001276
001281
001246
001232
0.01273
001256
001243
00l
0.01215
25
27
28
29
30
001331
00142
001327
001312
001296
001334
001319
001304
001290
001276
001312
001297
001283
001269
0.01256
0.01291
001277
001264
001249
001236
001272
001258
0012k
001230
001217
001253
0.01239
0.01255
001212
001199
001235
0.0132*
001206
001195
001182
001218
ooi o
001191
001178
001156
001201
001155
001hZ
001162
001149
S
S
S
‘ie
Sieve Size
3-in.
2.40.
P40.4 (4.75-mm)
No ID (2.00 .mm)
No.40 (425 . sm)
No.200 (7S . sm)
I.
HYDROMETER ANALYSIS . e
I s. ,
0074 mm
0005mm
000 1mm .-.
Nate 17—No. 1 (2.36-mm) and No. 50 (3OCijsm) sieves ma bR
substituted for No. 10 and No. 40 ss ves.
19. Keywords
19.1 grain-size; hydrometer analysis; hygroscopic mois
tare; particle-size; sieve analysis
-------
AflACHMENT D.2
CSF AUDiT FORMS
-------
LOW CONCENTRATION WATER FOR ORCANICS COMPLETE SDC FILE (CS?) INVENTORY SUZET (Cont.)
CAS IO. SOGNO. S OG .TOFOLL J SASMO.
PAGE NOs
FR ( TO
C11ECX
lAB EPA
c. Standard..s Data -
Initial Calibration Data (Fora VI LCP)
Calibration Verification (Fori VII LOP)
Pesticides Analytical Sequence (Fora VIII,
LOP-i and -2)
PesticideFlorisil Cartridge Check (Form IX, LOP)
Pesticide Identification (Form X LCP)
Stand.ard chromatograms and data system printout
for all Standards
For pesticides/Aroclors confirmed by GC/MS, copies
of spectra for standards used
d. QC Data
Blank Data
LOS Data
PES Data
Xlscellaneova Data
Original preparation and analysis forms or copies of
preparation and analysis logbook pages
Internal sample and sample extract transfer
chain-of-custody records
Screening records
AU instrument output, including strip charts
from screening activities (describe or list)
EPA Shi ilReceivina Documents
Airbills (No. of shipments )
Chain-of-Custody Records
Sample Tags
Sample Log-In Sheet (Lab & DCI)
SOC Cover Sheet
Miscellaneous Shipping/Receiving Records
(describe or list)
Internal teb $a ole Transfer Records end Trackin2 Sheets
(describe or list)
FOP.N DC-2 -3
Pesticides (cont.)
. o ‘°2
-------
CONCENTRATION VATER voa ORCANICS coMPLETE SDG PILE (CS?) INVENTORY SHEET (Cant.)
CA . _______ SOG MO. ________ G NOS. TO FOLLOJ _______ ________
PACE NOs CHECX
FROM TO LAB EPA
Other R ord3 (describe or list)
Telephone Co.inication Lag ________
C ent3 :
pleted by: __________________________ ___________
CLP Lab) (Signature) (Printed Name/Title) (Date)
__ rea by: _______________________ __________
:EPA) (Signature) (Printed Name/Title) (Date)
FORM DC-2-4
1 r /01
-------
SAMPLE LOG-IN SKEET
Lth Na c:
—
Cu. Numbcz
Swç4 . DcUvcq
Gr pNo.:
A Nu ber
R (ARXS:
. Ci&zcody Sc.iJ(s) Prc c . Abuu
foua/B okes
2. Cui ody Sc..1 Nos.:
3. Q is-o(-Ouwdy
L
4. Tra c Rz . u
Pac n 4 Un
5. Aizb fl AiZb I1/SIiCt
Pr ie t/Abmcr
6 Airb flNo.:
7- Tqa
S& çLc Tag L /NCC Liiwd
bcrz °
C-
S Sazz ,k CoQdiuos
Luking
9. D c x.. i
a. tody reazdj. trs c
rtpcxu, acd sa Ic tap
s c . . 7
10. jy 4u Lsb
II . Tinie Reccive&
Sacipk Tratufcr
Fiwios
-
Arts I:
B -
0.:
• Coota SMO a d snith reaxd o( rt3oIuUo
Renewed 2y
Dau:
Lo gbook No. —
Logbook Page ?4a
Lcg-u Data:
-r
OF SAMPLE
SHIPMENr, ETC
FORM DC-i
-------
APPENDIX D
REGION I LABORATORY PRE-QUALIFICATION
STANDARD OPERATING PROCEDURE
D-1
-------
REGION I LABORATORY PRE-QUALIF1CATION
STANDARD OPERATING PROCEDURES
15 March 1994
-------
10.5.3 Experience and References • 28
10.5.4 Participation in Performance Evaluation (PE) Programs . 29
10.5.5 Certifications 29
10.5.6 Method Detection Limit (MDL) Studies 30
10.5.7 Examples of Deliverables 31
11.0 SCORING OF RFP SUBMISSION FOR INDIVIDUAL COMPONENTS 31
[ 2.0 LABORATORY PRE-QUALIFICATION FINAL REPORTS 34
AUACHMENTS 38
U’PENDIX A UST OF CONTACTS FOR LABORATORY REGISTERS A-i
.PPENDIX B EXAMPLE ANAlYTICAL SPECIFICATIONS B-i
TOC-2
-------
Region I Laborazory Pre-Qualification SOP
Revision Number: I
Dale: 15 March 1994
Page 1 of 65
1.0 INTRODUCTION
1.1 Scope and Application
This Standnrd Operating Procedure (SOP) details the procedures recommended for
developing Requests for Proposals (RFPs) and evaluating Laboratory Quality Assurance
Plans (LQAPs) and Statements of Qualifications (SoQs) received from laboratories bidding
on analytical specifications, such as but not limited to:
• EPA Method 524.2 low concentration volatile organic compounds (VOC) in
drinking water
• TO-14, the determination of volatile organic compounds (VOCs) in ambient air’
using SUMMA passivated canister sampling
• Low level pesticides and PCBs in surface water
• Water Quality Parameters: (Alkalinity, Chloride, COD, Nitrate/Nitrate-N,
Phosphorous, Sulfate, TDS, TOC and TSS)
• Total Organic Carbon, Total Combustible Organics, Grain Size Distribution in
Sediments
The evaluation procedures detailed herein may be performed by Region I EPA personnel or
field sampling contractors obtaining analytical services for the Agency.
1.2 Purpose
The purpose of this SOP is to provide a standardized procedure and work products with
which to solicit and evaluate laboratozies to ensure that high quality, usable, and defensible
data are generated for the Agency. This SOP provides a mechanism for documenting the
review of pre-pialification submittals from responding laboratories using work sheets and’
standardized reporting procedures. The purpose of pre-qualifying laboratories on the basis of
technical ability is to identify those laboratories willing and capable of performing the work.
A determination of technical qualification should always be performed prior to reviewing any
analytical costs submitted by the responders.
A review of laboratory pre-qualification submittals should be performed prior to a pre-award
laboratory audit and is not meant to be performed in lieu of a complete laboratory audit.
-------
Region I Laboratory Pre-Qualificazion SOP
Revision Number: 1
Date: 15 March 1994
Page 2 of 65
Pre-qualitication may be combined with either an on-site audit or a performance evaluation
study to provide an entire pre-award evaluation assessment.
1.3 How To Use This SOP
Because pre-qualification of laboratories is time consuming, it should be performed on an
annual or semi-annual basis, and not left to just before a sampling event is scheduled. Pre-
qualification may cake as long as one month, depending upon the numbers of responding
labcratories, the complexity of the analytical specifications, and the quality of the REP
responses.
This Region I Laboratory Pre-Cualification Standard Operating Procedure (SOP) is divided
into two parts: 1) procedures for developing a Request For Proposal (RFP); and 2)
procedures for evaluating RFP responses.
Part 1 encompasses Sections 2.0 through 8.0. Section 2.0 provides guidance on selecting
laboratories for solicitation; Section 3.0 provides guidance for developing contracts between
field sampling contractors and laboratories; Sections 4.0 through 8.0 provide instruction on
compiling the technical portion of the RFP. Sections 6.0 through 8.0 may, in fact, be used
as the REP, with minor modification.
Part 2 encompasses Sections 9.0 through 12.0, and their numerous attachments. Sections 9.0
and 10.0 provide procedures for evaluating REP responses from laboratories; Section 11.0
illustrates how to establish a scoring scheme; Section 12.0 describes the Laboratory Pre-
Qualification Final Report and report distribution. The numerous attachments are provided
as work sheets for RFP evaluations. The field sampling contractor may include blank
evaluation worksheets in the RH’ package to illustrate how the bidder’s will be evaluated.
2.0 IDEN1WICATION OF LABORATORY COMMU1 ’flTY
To obtain an adequate but not burdensome response, between 10 to 30 laboratories should be
identified based upon the QAM’s knowledge of the laboratory community, and should take
into consideration the following:
• (3 ographic location
• Ability to perform the work required
• Current state and federal agency certifications
• Interest in performing the work
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• Laboratory size and staffing
• Reputation in the laboratory and environmental contractor community
The process of selecting laboratories for solicitation involves first defining the work required.
The specific analysis of an environmental medium may be performed by many laboratories or
by only a select few, depending upon the complexity of the analysis. An integral part of
defining the required work involves the development of an analytical specification and the
establishment of laboratory quality control criteria. The development of analytical
specifications is described later in Section 5.0.
The proximity of the laboratory to the site is important in terms of sample delivery and ease
of on-site laboratory auditing. Laboratories located in the same state as the site would also
be expected to be in compliance with the particular state requirements, i.e., for drinking
water and wastewater certification. Although the field sampling contractor should strive to
utilize laboratories within Region I, it is expected that analytical work will often have to be
done by a laboratory located outside of the Region. A number of lists may be consulted to
establish a base list from which to select laboratories for R.FP solicitation. Appendix A lists
sources from which to obtain the various laboratory registers.
Also impor ant is identifying laboratories both willing and capable of performing the
analytical specification. Four types of lists may be used to develop the laboratory solicitation
community:
• Contract Laboratory Program (CLP) This list of CL? participants include
those laboratories performing Routine Analytical Services.
• Specialty analytical services This list includes laboratories known for
performing specialty analyses such as low detection limit volatiles, low
concentration pesticidesfPCBs in various media, air analyses, fast turn-around
analyses, analysis of physical properties such as grain size distribution,
analyses of media using ASTM, ANSI, or other testing agency procedures,
and microscopic analyses such as asbestos fiber counting. Certain analytical
needs may require the contractor to look outside of Region I for services. For
example, Method TO-14 “Volatiles in Ambient Air” is not performed by
laboratories in New England on a regular basis, but is performed by
laboratories in California or those connected with incineration facilities testing.
The specialty laboratories group is chosen from laboratories who are known to
have successfully performed analyses for the connactor in an EPA Region I
program or some other governmental program.
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• State approved laboratory Lists This list includes all laboratories certified in
all New England states that perform water quality parameters such as those in
the WP/WS performance evaluation programs. These laboratories are certified
by the various state programs and perform those analyses on a reLlilar basis.
Each state department of environmental protection usually produces lists of
state approved laboratories, along with the methods that each laboratory is
certified to perform.
• WBEIMBE lists. Each state also provides lists of minority- and women-
owned business enterprises. These lists may also provide additional laboratory
information. WBE/MBEs may fulfill a set-aside requirement of a project.
Prior to solicitation, the pre-qualification evaluators may want to contact laboratories to
inquire about the laboratories’ interest in the proposed work. Many laboratories are not
interested in participating in programs with rigorous QA/QC requirements, whereas others
are interested and want to prove their technical ability. Contacting the laboratories prior to
solicitation should to narrow the field of laboratories for solicitation.
The process of identifying the laboratory community may take between one and four work-
weeks, depending upon the response of the agencies providing the certification lists. With a
prompt response, the process of identifying laboratories should take no more than two weeks.
Field sampling contractors that have previously generated CL? lists and state certification
lists may take less than one week to identify the laboratory community for solicitation.
3.0 LABORATORY CONTRACTS
The contracts that the field sampling contractor has with the laboratory should include the
following elements:
1. Analytical method including detection limits and holding times
2. Deliverable requirements
3. Overall data quality and specific quality control requirements
4. Number of samples
5. Anticipated schedule, including sample arrival dates and data due dates
6. Penalties for not meeting the requirements of the above items (optional)
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The contract should include the analytical method as the analytical specification. The
laboratory should be required to follow the analytical specification(s) exactly, using the
appropriate instrumentation, computer hardware, computer software, and reagent quality for
all chemicals. Data should be presented on tabulated forms similar to CL? required format.
All raw data should be submitted. A request for electronic deliverables in addition to bard
copy data is an option.
Quality control criteria specific to the analyses should also be defined in the contract scope of
services, as well as the corrective actions required when QC criteria are not met. For
example, the contract should specify that if surrogate recoveries are not within criteria, the
laboratory must perform a re-extraction of the sample. The contract should also detail how
long unused sample volumes, extract/digest sample volumes, and analytical data re to be
archived by the laboratory.
The contract should also specify the quantity of samples and anticipated schedule of sampling
and delivery. Under the contract, the laboratory should be required to analyze the specified
number of samples. If additional field samples are taken, the field sampling contractor
should make advance arrangements with the laboratory prior to shipment of the samples from
the field. The contract scope of services should be written to address the possibility of
additional samples, including the costs of any extra samples.
Samples should arrive at the laboratory within some pre-defined window. Potential changes
in the anticipaed schedule should also be addressed within the contract scope of services.
Furthermore, sample holding times and data turn-around times should be defined as part of
the contract scope of services.
Penalty clauses may be used to hold the laboratory to agreements in the contract. The
penalty clause should be enforceable, clearly stated and understood by all parties. Penalty
clauses should be used judiciously by the field sampling contractor as they may deter some
potential bidders from bidding. Depending upon the type and quantity of analyses, some
laboratories may not chance severe penalties if there is only a marginal profit in the analyses.
Alternatively, if there are many sample and a larger profit, the laboratory may not see the
potential penalty for reanalyzing a few samples as problematic.
Penalty clauses may be necessary when data are critical to the specific project being
undertaken andior re-sampling costs are expensive. Actions by the laboratory that cause the
rejection of data should incur some associated penalty. Examples of the most common
reasons for penalties include:
• Not analyzing all samples sent
• Missing sample holding times
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• Missing data turn-around times
• Missing required QC criteria
• Lack of delivery of required documentation
Penalties can include withholding payment or having the laboratory pay the field sampling
contractor for resampling and analysis (if time is available).
4.0 SUMMARY OF REQUEST FOR PROPOSAL COMPONENTS
Any Request for Proposal (RFP) for laboratory services should contain the following
documents and information:
• The analytical specification that includes: analytical method, quality control
requirements, detection limits and deliverable requirements
• Sampling schedule for the individual parameters associated with the analytical
specification
• Numbers and types of samples and field QC samples to be performed for each
analytical specification
• Example work sheets to be used by the pre-qualification evaluators (optional)
Note: The RFP should not include the name of the site.
Any RFP for laboratory services should require the responders to submit the following
documents and information:
• The laboratory’s method SOP that will be used to perform the analyses and/or
a clear narrative detailing how the bidder plans to accomplish the analytical
specifications
• Demonstration of an effective Quality Assurance Program including:
- A Laboratory Quality Assurance Plan (LQAP)
— Re iumes of personnel or team proposed to work on the analysis of
samples using the analytical specification
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— List of Evidentiary SOPs, including revision dates, that adhere to U.S.
EPA NEIC procedures for sample chain-of-custody, etc.
— List of all related technical and non-technical laboratory SOPs,
including revision dates, that will be used to support the performance of
the analytical specification including: sample receipt, glassware
cleaning, data mpnagement, data verification, completeness check, etc.
• A Statement of Qualifications (SoQs) relevant to the analytical specification
which includes; equipment inventory, facility description, analytical capacity,
experience refereflces. PE programs, certifications and deliverables, and
Method Detection Limit (MDL) studies (when required)
The following sections on RFP deliverable requirements for the LQAP, SOPs, resumes or
SoQs can be incorporated into any RFP that the field sampling contractor is writing. The
corresponding work sheets may also be included in the RFP package to provide prospective
laboratories with information on how their responses will be evaluated. Requirements for
pre-qualification submittals must be clearly detailed in the R.FP in order to get comparable
laboratory responses. Once the pre-qualification submittals have been evaluated and the
lowest cost most technically-qualified bidder has been identified, a pre-award laboratory audit
may be performed to confirm the information presented in the pre-qualification submittals.
The RFP should not take more than a few days to develop if standard requests for LQAPs,
SOPs, key personnel resumes, SOQs and standardized analytical specifications are used.
5.0 ANALYTICAL SPECIFICATIONS
The analytical specifications are the most important component of the RFP, and, as such
should be clear, comprehensive, and concise. They dictate the method of analysis, type of
instrumentation, detection limits, quality control criteria, corrective action measures,
sampling schedule, number of samples, communication contacts for sampling and technical
issues, and documentation and deliverable requirements. The essential technical elements of
an analytical specification include:
• Analytical procedure required, including analysis method, sample
preparationlextraction/digestion methods, sample extract clean-up methods, and
any special technical requirements to modify or deviate in any way from a
standard procedure. The analytical procedure should include all protocol
variations that may be used to alleviate sample matrix problems or
interferences. A copy of the analytical procedure must be attached to the
analytical specification; referencing a procecare is not adequate.
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• Detection/qiurntitation limits needed for specific parameters and sample
matrices, including concentration units.
• Quality control requirements, inchiding criteria for method/reagent blank
cont2minaton, precision and accuracy criteria for analytical/matrix spikes and
duplicate samples, initial and continuing calibration minimum response factors
and maximum %D/%RSDs, instrument tuning ion abundances and mass
assignments, instrument performance check recoveries, internal standard and
surrogate retention times and recoveries, and other method-specific criteria.
Corrective action procedures for non-compliant quality control results should
also be included.
• Specifications for the format and content of data package deliverables should
also be included. Deliverable requirements should be comprehensive, and
should be described in relation to CLP deliverables or in the most informative
format. Deliverables should be easy to read and validate. The analytical
specification should provide and/or request example deliverables where
applicable.
• Data mm-around times, sample preparation/extraction/digestion and analysis
holding times, and the preservation requirements needed for specific
parameters and matrices should be included in the analytical specifications.
The analytical specification may be based upon the U.S. EPA Region I Special Analytical
Services (SAS) requests (an example specification is provided as Appendix B of this
Laboratory Pre-Qualification SOP) The difference is that under this Laboratory Pre-
Qualification SOP, the EPA field sampling contractor is both the requestor and recipient of
the analytical data. The U.S. EPA Region I Regional Sample Control Coordinator (RSCC)
and EPA Sample Management Office are not involved in obtaining or receiving data.
However, the RSCC is involved in tracking the receipt of non-CLP data in accordance with
the Region I DAS Tracking Standard Operating Procedure .
The analytical specifications may be written in the form of an SOP using the following
format:
• Scope
• Purpose
• Definition of work
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• Schedule (optional, depending upon the project)
• Analytical reference(s)
• Sample preservation and detection limits
• Analytical procedure
• Quality control requirements, including corrective actions
• Analytical deliverables
• Exceptions (procedures for the contracted laboratory to follow if technical
andlor non-technical problems are encountered)
The development of an analytical specification may take up to 40 hours, depending on the
complexity of the analysis required and whether or not a similar analytical specification has
been generated and utilized previously. Analytical specifications previously written for the
U.S. EPA Region I SAS program should be used as a starting point for developing analytical
specifications for RFPs.
The R.FP should require that the responding laboratory explain in detail how they plan to
execute the analytical specification(s). The laboratory’s response to this requirement is
critical to the evaluation of RFP responses. The laboratory’s response should state that they
will either a) follow the analytical specification to the letter, or b) deviate in a defined
m2nner. Any deviation should be explained in detail and should result in an improvement to
the method accuracy, precision, data quality or detection limits. The deviation should not
change the required outcome or deliverables. The explanation may include details such as
sample size, special sample preparation and clean-up procedures, as well as use of dedicated
instruments, co lumnc, and computerized accessories. Alternatively, the explanation may be a
simple statement that the procedure wil1 be performed exactly as it is written in the analytical
specification. This response may be suspect if information in the LQAP, SOPs, resumes, or
SoQs is contradictory. All such discrepancies should be resolved prior to contract award.
6.0 QUALITY ASSURANCE PROGRAM REQUIREMENTS
The RFP should require documentation to demonstrate the existence of an effective quality
assurance program. This section describes the RFP pre-qualification deliverables including:
The Laboratory Quality Assurance Plan (LQAP), specific laboratory team member
qualifications, and analytical standard operating procedures.
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6.1 Laboratory Quality Assurance Plan (LQAP)
The. LQAP received by the field sampling contractor should, at a minimum, detail all
elements of the laboratory’s quality assurance program and establish that the
laboratory is able to generate high quality, legally defensible analytical measurement
data. The LQAP should describe the procedures that will be implemented to achieve
the following:
• Maintain data integrity, validity, and usability.
• Ensure that analytical measurement systems are maintained in an
acceptable state of stability and reproducibility.
• Detect problems through data assessment, establish corrective action
procedures to keep the analytical process reliable, and monitor
effectiveness of any corrective action(s).
• Document all aspects of the measurement process in order to provide
data which are technically sound and legally defensible.
The LQAP should present, in specific terms, the policies, organi7i tion, objectives,
functional guidelines, and specific QA and QC activities designed to achieve the data
quality objectives of the specific contact. Where applicable, SOPs pertaining to each
LQAP element described later in this section should be included or referenced as part
of the LQAP. SOPs pertaining to the analytical specification(s) should aiso be
included or referenced as part of the LQAP. The LQAP should be available during
on-site laboratory audits. Additional information relevant to the preparation of an
LQAP can be found in ASTM publications as well as in the U.S. EPA Contract
Laboratory Program (CLP) Routine Analytical Services (RAS) Statements of Work
(SOW) for organics and inorganics, OLMO1.9 and ILMO3.0, Exhibit E, Sections 3.0
and ill, respectively.
The responding laboratory’s LQAP should, at a minimum, contain the following
elements pertaining to the analytical specification bid:
A. Approvals page-signed by senior management and corporate QA Officer(s)
B. Statement of QA Policies and Objectives
C. Organi72tion and Personnel
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1. QA Management
a. - Organization
b. Assignment of QC and QA Responsibilities
c. Reporting Relationships (organizational chart; identify primary
contact for contact)
d. QA Document Control Procedures
e. QA Program Assessment Procedures
2. Personnel
a. Project Team (highlighting those persons involved in performing
the technical specifications)
b. Resumes (or references to a resume section)
c. Education and Experience Pertinent to this Contract
d. Training Programs
D. Facilities and Equipment
1. Instrumentation and Backup Alternatives
2. Maintenance Activities and Schedules
3. A Description of the Analytical Facility (simple floor plan may be
used)
E. Document Control
1. Laboratory Notebook Policy
2. Sample Tracking/Custody Procedures
3. Logbook Mainr nance and Archiving Procedures
4. Case File Organization, Preparation and Review Procedures
5. Procedures for Prepar don, Approval, Review, Revision, and
Distribution of SOPs
6. Process for Revision of Technical or Documentation Procedures
F. Analytical Methodology
1. Calibration Procedures and Frequency
2. Sample PreparationfExtraction Procedures
3. Sample Analysis Procedures
4. Standards Preparation Procedures
5. Decision Processes, Procedures, and Responsibility for Initiation of
Corrective Action
6. Procedures for Monitoring Effectiveness of Corrective Action
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G. Data Generation
1. Data Collection Procedures
2. Data Reduction Procedures
3. Data Verification and Completeness Check Procedures
4. Data Reporting and Authorization Procedures
H. Quality Control
1. Solvent, Reagent and Adsorbents Check Analysis
2. Reference Material Analysis
3. Internal Quality Control Checks
4. Corrective Action and Determinption of QC Limit Procedures
5. Designated Person(s) of Responsibility
I. Quality Assurance
1. Data Quality Assurance
2. Systems/Internal Audits
3. Performance/External Audits
4. Corrective Action Procedures
5. Monitoring Effectiveness of Corrective Action
6. Quality Assurance Reporting Procedures
7. Designated Person(s) of Responsibility
J. Safety Programs, Training and Documentation
K. Compliance with Environmental Regulations
1. Air Pollution Preventative Measures
2. Aqueous Effluent Disposal
3. Hazardous and Nonhazardous Waste Management Practices
4. Hazardous Waste Manifesting
The field sampling contractor should evaluate each LQAP and document the
evaluation in the Laboratory Pre-Quaiiflcation Final Report. Each laboratory LQAP
should be .evaluated in accordance with this SOP and graded acceptable or not
acceptable. Unacceptable LQAPs may need only slight revisions to be made
acceptable. If this is the case, the laboratory may be asked to amend and resubmit
the LQAP to comply with the requirements of the RFP. All LQAPs reviews should
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will be summarized utilizing the work sheets contained in the Attachments to this
SOP. All unacceptable LQAPs should be identified in the pre-qualificacion
documentation and a final report that details the reasons for an unacceptable score.
6.2 Resumes and Project Team
The LQAP should contain an organizational chart highlighting key management,
QAJQC personnel, and personnel responsible for producing the data for each
analytical specification. The LQAP should identify responsibilities of t im members
and should contain resumes for those key personnel performing the anaiytical
specification.
Resumes should contain the following information:
• Educational background, including the date and type of degree(s)
• Relevant experience in the field of expertise
• Years of experience (previous employment) - years employed by the
laboratory
• Experience with specific requested analytical specifications - include
years of experience operating specific analytical instrumentation
required in method
• Special tr2ining - courses, semii1 rs
• Publications, papers, awards etc.
The above required information should be easily ascertained from the submitted
resumes. The field sampling contractor will find that requiring a responder to submit
education and experience in a pecified format will aid in resume evaluation, although
it is not critical.
6.3 Laboratory Standard Operating Procedures Delivery Requirement
The laboratory should submit the following:
1. A complete copy of the method SOP for each analytical specification that the
laboratory is proposing to perform. The analytical specification SOP should
include: holding times, sample preparation, analyses, quality control criteria,
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corrective action measures, detection limits and deliverables format. (Refer to
Attachment 4b.)
2. A list of all other analytical and non-analytical SOPs, including revision dates,
that the laboratory will adhere to while performing work under the proposed
contract. These SOPs should include, but are not limited to:
• Sample Preparation
• Glassware Cleaning
• Calibration
• Other Analytical Procedures
• Maintenance Activities
• Analytical Standards
• Data Reduction Procedures
• Documentation Policy/Procedures
• Data Verification/Self Inspection
• Data Management and Handling
(Refer to Attachment 4 C.l)
3. A list of all evidentiary SOPs, including revision dates, that the laboratory will
adhere to while performing work under the proposed contract. These SOPs
should adhere to U.S. EPA NEIC guidelines and include the following:
• Sample Receiving
• Sample Identification
• Sample Security
• Sample Storage
• Sample Tracking and Document Control
• Computer-Resident Sample Data Control
• Data Package Orgpnization and Assembly
(Refer to Attachment 4 CJI)
SOPs prepared by the laboratory should be functional, clear, up-to-date, and
sufficiently detailed to permit duplication of results by qualified analysts. Additional
guidance for preparing SOPs may be found in Exhibits E and F of the U.S. EPA
CLP-RAS Statements of Work for Organics and Inorganics, OLMO1.9 and ILMO3.O.
All SOPs as presented to the field sampling contractor should reflect activities as they
are currently performed in the laboratory. In addition, all SOPs should be:
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S Subject to a document control procedure which precludes the use of
outdated or inappropriate SOPs. Controlled documents may be changed
only by those given the task under controlled conditions and
documented guidance.
• Consistent with current EPA regulations, guidelines, NEIC evidentiary
procedures, and as consistent with CLP requirements as possible.
• Consistent with instrument manufacturers’ instruction manuals.
• Available to the field sampling contractor during an on-site laboratory
audit. A complete set of SOPs should be bound together and available
for inspection at such audits. During on-site audits, laboratory
personnel may be asked to demonstrate the application of specific
SOPs.
• Written to ensure that all tasks required by and performed using the
analytical specification are fully recorded.
• Able to support determinations of data validity.
• Designed to describe the corrective action measures and feedback
mechanisms utilized when analytical results do not meet analytical
specification requirements.
• Reviewed regularly and updated as necessary when contract, facility, or
procedural modifications are made.
• Archived for future reference in useability or evidentiary situations for
stated period of time.
• Available at specific work stations as appropriate.
The format for SOPs may vary depending upon the kind of activity for which they are
prepared. Each SOP, however, should have the date of issue, date of revision, and
revision number clearly identified at the top of every page. In addition, at a
minimum, each SOP should have the following sections:
• Title Page or Designation
• Scope and Application
• Definitions (optional)
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• Responsibilities (optional)
• Procedures
• QC Limits
• Corrective Action Procedures, Including Procedures for Secondary
Review of Information Being Generated And Procedures For
Monitoring Effectiveness of Corrective Actions
• Documentation Description and Example Forms
• Miscellaneous Notes and Precautions
• References (pertinent known documentation)
• Safety Requirements
The field sampling contractor should use a standardized laboratory SOP evaluation
report (provided as an attachment and described later in this SOP) to evaluate
laboratory SOPs. The laboratory should compile an index of all laboratory SOPs
pertair ing to each analytical specification(s), listed by laboratory SOP I]) and/or title
and revision date. Laboratory SOPs may be listed for more than one category. The
format and content of each laboratory SOP should be evaluated for compliance with
this Pre-Qualification SOP and graded as acceptable or not acceptable. References to
portions of the current EPA SOWs are acceptable in laboratory SOPs, provided any
specifications and procedures not addressed in the EPA SOWs are included.
The laboratory SOP evaluation report (including work sheets) will be submitted by the
field sampling contractor to the U.S. EPA as part of the Laboratory Pre-Qualification
Final Report. The laboratory SOP evaluation report should document the reason(s)
for una ceptable scores.
7.0 STATEMENT OF QUALIFICATIONS (SoQs) REQUIREMENTS
The laboratory should be required to submit a statement of qualifications in conjunction with
the LQAP. The statement of qualifications should include the following information
pertinent to the analytical specification being bid:
• Equipment Inventory and Analytical Capacity
• Facility Description
• Experience and Professional References
• Participation in Performance Evaluation Sample Programs (results not over 9
months old)
• Certifications
• Method Detection Limit (MDL) Studies (not over 6 months old)
• Example of Deliverables
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Each of the above items should be addressed. The reports and work sheets described in
Section 10.4 of this SOP should be used, to the extent possible, in evaluating laboratory
responses. The laborator) should be allowed to add any pertinent information that enh2n es
its qualifications in a specific area of expertise.
7.1 Equipment Inventory and Analytical Capacity
The equipment inventory should contain a consolidated list of laboratory equipment
that is used for sample log-in, percent solid (or % moisture) determinations, sample
preparation, extract clean-up, sample analysis, data handling or any other important
function related to the analytical specifications being bid. The instrument list should
include manufacturers’ model numbers, instrument types, software revisions, and year
or age of the instruments.
The capacity to perform each analysis required in the RFP should be presented in
either a tabular or chart format. The capacity of the laboratory to analyze numbers of
samples over specific periods of time during the year should be known and presented
for each analytical specification bid. The numbers of instruments available and
number of personnel should be checked to verify laboratory capacity. The number of
samples that can be analyzed in a day, week, month, or year can be used to determine
the laboratory’s ability to perform the field sampling contractor’s analytical work in a
timely manner.
The equipment inventory description should list all attachments, accessories, or
ancillary equipment including associated computer hardware and software. Computer
descriptions should include data storage capacity, data handling capability, hard copy
output equipment and software revisions.
Inst ruments for each analytical specification to be bid should be described, including
but not limited to:
Gas Chromatograph (detector type)
Gas ChromatographiMass Spectrometer (GC/MS)
TOC/TOX Analyzer
UVIVisible Spectrophotometers
Titrators (automatic or manual)
Balances
Gel Permeation Chromatograph (GPC)
Flame Atomic Absorption Spectrophotometer
Furnace Atomic Absorption Spectrophotorneter
Mercury Analyzer (if a separate instrument)
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Inductively Coupled Plasma Spectrophotometer
Ion Chroniatograph
Regulated Water Baths
The equipment inventory submitted by the laboratory should include descriptions of
maintenance programs, repair records, and long term maintenance contracts for all
instruments to be used. The inventory should also identify backup instrumentation
and primary instrumentation. Redundancy of instrumentation should be a factor when
choosing technically-qualified laboratories.
Sampling equipment and accessories such as SUMMA canisters, critical orifices or
vacuum gauges used in ambient air sampling should be described in detail. SOPs for
cleaning/decontamination testing and canister certification should be listed in the
LQAP and should be referenced in the equipment inventory section of the laboratory
response. Alternatively, the LQAP may reference the equipment description section
which includes associated SOPs. Certificates of cleanliness and proof of leak testing
should be required with any type of air sampling equipment that may be used or
supplied for performance of any analytical specification.
7.2 Facility Description
A description of the laboratory facility should be included in the bidder’s submittal.
If a limited portion of the entire facility will be used to perform the analytical work,
then a description of that area should be submitted. Items such as total area (square
footage), lab areas, building age, building type and location are required. A
description of access routes for staff, equipment, and/or samples is required.
Electromechanical systems such as ventilation (including hoods), air conditioning, or
climate control should be described. The electrical source, clean water sources, and
clean air sources should be described. The following three items should be described:
• Water disposal options (holding tank s , septic/sewer)
• Solid waste handling methods
• Hazardous waste management practices
The responding laboratory may find it effective to supply a facility plan along with
the written description.
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7.3 Experience and References
Laboratory experience in performing each analytical specification for identified
projects or clients should be documented by the bidder. This documentation may be
submitted in the form of short paragraphs describing sample projects, including:
sample locations, number of samples, sample matrices, and client objectives. Each
project experience cited should include a client reference and the date(s) of service.
Client references should identify persons, companies, and agencies including proper
names, current addresses, telephone numbers and key contact persons. The bidder
should use short paragraphs to describe each client, project type, as well as type and
number of samples. The references chosen should be those for which moderate to
high volumes of work were performed. References and experience should be current
and pertinent to the analytical specification being bid. Historical experience can be
described but the most recent experience should also be included. Exerience
working for EPA CL?, Army Corps of Engineers, Department of Energy,
Department of Defense, state agencies, and local agencies should be highlighted. The
quality of responses received from a laboratory regarding references and experience
should be a major factor in determining the technical ability of the responding
laboratory.
7.4 Participation in Performpnce Evaluation Programs
Participation in performance evaluation programs for DOE, DOD, EPA, HAZWRAP,
and the Army Corps of Engineers generates especially important information. Copies
of the most recent results (no more than 9 months old) from performance evaluation
(PE) programs, such as the quarterly blind PE samples used to monitor CLP labs with
active contracts, EPA Water Supply, Water Pollution and/or NPDES DMR programs
or any non-EPA program should be submitted by the bidder. The laboratory PE
results should include the agency error allowances and should be pertinent to the
analytical specification being bKi. PE results provided by the laboratory should not be
from inactive programs. Historical performance in programs is not considered
relevant to the current evaluation of laboratory performance.
Single “blind” commercial performance evaluation sample programs may be submitted
by the bidder in lieu of participation in government agency programs. Laboratory PE
results and acceptance limits or nomin2l values should be provided by the bidder.
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7.5 Certifications
A list of active certifications, including the certificates that the laboratory currently
holds, should be submitted as part of the fre-qualification deliverables. The list may
include federal, state, or local programs as well as industrial programs such as the
Energy Producers Research Institute (EPRJ) and the American Association of
Laboratory Accreditation (A 2 LA).
7.6 Method Detection Limit (MDL) Studies
The analytical specification may or may not require a method detection limit (MDL)
study. If the bidder is required to deliver an MDL study, the deliverable will be
described in the analytical specification. If an analytical specification does not require
an MDL study, but the laboratory has one for that specification, then the responding
laboratory should submit that MDL study. The laboratory’s MDL studies should be
used to further evaluate laboratory qualifications. MDL studies should be current and
performed in accordance with 40 CFR Part 136, Appendix B, Revision 1.11.
7.7 Deliverables
An example of the entire deliverables data package relevant to the analytical
specification being bid should be provided as part of the bid package. The example
deliverable should include CLP forms (OLMO1.9, Exhibit B), or similar forms that
include laboratory name, DAS # (or other non-CLP #), field sample number,
laboratory sample number, matrix, low and medium levels, dilution factors, analytical
‘parameters, practical quantitation detection limits, instruments used, and dates of
sampling, sample receipt by laboratory, sample extraction and sample analysis. All
deliverables relating to QC analysis including method blanks, surrogate analysis,
initial and continuing calibrations, internal standard results, tuning results, and
laboratory control samples should also be required. Raw or supporting data
deliverables may not be required for the bid, but should be required whenever field
samples are analyzed.
8.0 SCHEDULE OF SAMPLING AND NUMBER OF SAMPLES
The RFP package should provide anticipated shipping dates of field samples for each
analytical specification. It should also identify requirements for sample shipping and
delivery, holding times, sample data delivery (including PE sample results), and field
sampling contact name(s) and address(es).
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The RFP should provide an estimated sample count, which conminc all samples and field
QC, for each analytical specification being solicited. If possible, the RFP should detail
numbers of samples (per matrix) to be shipped per day, per week, and over the entire project
schedule. Field QC should be included in the sample count.
9.0 Rfl EVALUATION TEAM
The qualifications of the RFP evaluation team are critical to the success of this activity.
Each RFP response should be evaluated by at least two qualified people, and one of those
evaluators should be the field sampling contractor’s Quality Assurance Manager (QAM). If
it is not possible for the QALM to be an evaluator, then the QAM should, at least, review the
work sheets and final reports prepared by the evaluators and verify their findings.
Each evaluator should have a B.S. in chemistry or a related physical science and have at
least five years of experience in the operation of an environmental laboratory or the
evaluation/validation of environmental data. The evaluators should have extensive knowledge
of laboratory analytical systems, quality assurance programs, and/or experience in one of the
analytical protocols and related instrumentation. The RFP evaluators should be familiar with
each analytical specification being bid, the Region I Laboratory Pre-Oualiflcation Standard
OiDeratin Procedure , and all associated work sheets to be used in the evaluation.
A mix of analytical specifications may arise out of the field sampling contractor’s work
assignments. The RFP may contain specialized analytical specifications that require different
qualified evaluators to review each submittal. In cases where the analytical specification is
unique there may be only one qualified person to evaluate the RFP response. In that case,
the qualified evaluator should evaluate all of the submittals pertaining to that analytical
specification.
Evaluation of the LQAP, resumes, and SOPs should be performed to ascertain that the
laboratory has effective operational controls in place to support the execution of the analytical
specification.
The QAM and evaluation team should establish a scoring scheme prior to RFP release. The
team should establish a total score that will be used to determine whether a laboratory is
technically-qualified. The scoring system should be well-defined so that each evaluator can
place an unbiased score on each eLement evaluated. The system for assigning a numerical
score to each element should be established and used universally to prevent biased
evaluations. Scoring is discussed further in Section 11.0 of this SOP.
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10.0 PRE QUALIFICATION EVALUATION OF RIP RESPONSES
The review of pre-qualification submissions may be performed in stages by the RFP
evaluation team. Each submission is to be checked for completeness using the work sheets
provided as the attachments. Three types of work sheets will be used: log-in; evaluation;
and summarizing report. The stages of the pre-qualification review are as follows:
1. Log-in sheet for laboratory submissions (Attachment 1)
2. Evaluation of Quality Assurance Program
• LQAP work sheets (Attachments 2a and 2b)
• Key project personnel work sheets (Attachments 3a through 3c)
• SOP work sheets (Attachments 4a through 4c)
• Overall comments and requests for clarification
3. Evaluation of Statement of Qualifications (SoQs)
• SoQs evaluation report (Attachment 5a)
• Work sheets for the eight (8) SoQ elements: equipment inventory;
facility description; analytical capacity; experience and references; PE
programs; certifications; deliverables; and MDL studies (Attachments
5b through 5g)
• Overall comments and requests for clarification
4. Scoring of submission for individual components
• Components/element weight
S Professional judgement scoring
5. Report on technical qualifications
• Justification of technically-qualified laboratories (Attachment 6)
• Cost analysis of technically-qualified laboratories
• Justification of technically-unqualified laboratories (Attachment 7)
Laboratory cost information should be separated and not made available to the technical
evaluation team. Laboratory submissions are evaluated to determine the group of
technically-qualified responders. Therefore, the responders’ bid prices are not factored into
the pre-qualiflcadon process until the group of technically-qualified responders is chosen. If
the bid price is prohibitive for a technically-qualified responder’s services, then another
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technically-qualified responder may be chosen for award. The technically-qualified
laboratory with the lowest bid price should generally be awarded the conttact.
The remainder of this section discusses work sheets that should be used by the evaluation
team to document the evaluation of REP responses. Section 11.0 provides a discussion of
overall scoring parameters.
10.1 Use Of Attachments
The log-in table, work sheets and evaluation reports should be used by the REP
evaluator to document the findings of the pre-qualification evaluation. The
attachments should be included with the REP to demonstrate the level of detailed
review to which the responders’ pre-qualificadon submittals will be subjected.
The log-in table for each laboratory is used to verify the analytical specifications
being proposed, as well as the timeliness and completeness of the bidder’s response.
Comments should be made on the log-in table if the response is incomplete.
Work sheets are used by the evaluator to document that all elements required in
Sections 5.0 through 7.0 are present and to assess the relative merits of those
elements. The evaluator is encouraged to make comments on the work sheets and, if
necessary, to add supplementary pages for comments.
Reports such as the LQAP evaluation report, SOP evaluation report, and the
professional qualifications report summarize the information contained on the
corresponding work sheets, which were used to evaluate the various elements.
The evaluation of a laboratory bid submittal (containing all elements of the LQAP,
SOPs, resumes, and SoQs) in the detailed manner described by this SOP may take up
to eight hours to complete.
10.2 Logging in Laboratory Pre-Qualification Submissions
Attachment 1 provides a mechanism for logging in laboratory submissions. It also
documents receipt of p: -qualification components within the requested time period.
The table ensures that, at first glance, required pre-qualification items have been
included in the package. If items are absent, then the laboratory should be contacted
for resubmission. Completion of the laboratory submission log-in table provides only
a cursory check. An in-depth check will be performed later during the detailed
evaluation process.
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10.3 Evaluation of Laboratory Response to Analytical Specifications
The work sheet ontained in Attachment 4b should be used to evaluate the bidder’s
analytical specification SOP, otherwise kiiown as the laboratory’s method SOP. The
laboratory’s method SOP for the analytical procedure may deviate from that of the
analytical specifications. Any deviations should be noted by the evaluators on the
work sheet. The laboratory should be required to amend their laboratory method SOP
to conform with the analytical specification to ensure that usable data is generated.
Failure to provide an acceptable laboratory method SOP or acceptable narrative that
describes how the analytical specification will be performed should result in automatic
disqualification.
Alternatively, the laboratory may submit data that show that all deviations from the
analytical specification will result in improved; data quality, sensitivity (detection
limits), precision and/or accuracy. The evaluator must review the submitted data to
determine method comparability and acceptability. The evaluator must be familiar
with the site Data Quality Objectives to correctly make this determination. Since
detection limits are key to obtaining usable data for risk assessment, the evaluator
should not allow modifications to the analytical specification that will impact needed
detection limits or compromise data quality.
10.4 Evaluation of Quality Assurance Program Deliverables
The following work sheets and reports are used to verify the adequacy of a bidder’s
Quality Assurance Program:
• Attachment 2a - LQAP Evaluation Report
• Attachment 2b - LQAP Work Sheet
•, Attachment 3a - Key Project Personnel Evaluation Report
• Attachment 3b - Key Project Personnel Resume Format Work Sheet
• Attachment 3c - Key Project Personnel Qualification Work Sheet
• Attachment 4a - SOP Evaluation Report
• Attachment 4b - Analytical Specification SOP Work Sheet
• Attachment 4c - General Laboratory SOP Work Sheet
These documents are used to verify receipt of the information requested in the RFP.
If a laboratory’s response is found to be inadequate after completion of the work
sheets, then the R.FP evaluator may request additional information from the
laboratory. A short time-frame, such as three days, should be allowed for re-
submittal.
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10.4.1 LQA.P Deliverables
The LQAP work sheet contained in Attachment 2b itemizes the individual
elements of the LQAP that should be evaluated. Each item listed on the
LQAP work sheet should be addressed in the bidder’s LQAP, but not
necessarily in the exact order provided on the work sheet. The bidder’s LQAP
may contain headings that differ from those present on the LQAP work sheet,
therefore, the evaluator will need to carefully review each section of the
bidder’s LQAP for content. Attachment 2a provides a report format
documenting the results of the LQAP evaluation. No other documentation is
necessary, but major deficiencies should be noted on this report. The
laboratory may be asked to correct certain deficiencies before their pre-
qualification submittal will be further evaluated.
10.4.2 Resumes and Project Team Deliverables
The review of key pr’ ject personnel qualifications should be documented on
Attachments 3a, 3b and 3c. Since resume formats differ from each laboratory,
the evaluator should be careful to consistently evaluate personnel
qualifications. The resumes should detail educational background, relevant
experience, years of experience, special training, and published papers and
awards. The resumes of key personnel should highlight the individual’s
experience performing the analysis described in the analytical specification.
Attachment 3b, Key Project Personnel Resume Format Work Sheet, combines
the evaluation of personnel qualifications with a checklist of required resume
elements. Each element should be reviewed in order to consistently evaluate
personnel from all responding laboratories. If a bidder’s response is found to
be inadequate utilizing this work sheet, an addendum may be requested.
Completion of the work sheet contaTled in Attachment 3b also provides the
evaluator an opportunity to identify and evaluate the entire project team that
will perform the analysis of the analytical specification.
Attachment 3c, Key Project Personnel Qualification Work Sheet, should
include the key personnel as well as other laboratory personnel that may be
involved in the analysis of samples as performed under the analytical
specification. The work sheets provided in this SOP can be modified to
include qualifications for personnel related to any analytical specification. The
level of expertise necessary to perform each individual analytical specification
may vary, thereby requiring amendment of the work sheets presented in
Attachment 3c.
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10.4.3 Laboratory SOP Deliverables
In addition to the complete laboratory method SOP which describes how the
analytical specification will be performed, the laboratory should be required to
submit a list of other applicable analytical and non-analytical laboratory SOPs,
including their revision dates. A list of evidentia.ry SOPs, including their
revision dates, should also be a required pre-qualification submittal.
The evaluation report provided in Attachment 4a should be used to document
results of the evaluators’ review of the analytical specification
SOPs/laboratory’s method SOP the list of the ancillaiy laboratory SOPs,
evidentiary SOPs, and the format of the laboratory’s SOPs. Evaluation of
analytical specification SOPs was described previously in Section 10.3 of this
SOP.
The laboratory’s lists of ancillary laboratory SOPs and evidentiary SOPs,
documented in Attachment 4c, indicates to what degree the laboratory has
contt-ol over all phases of their analytical and chain of custody systems. The
list of other laboratory SOPs required for submission is reviewed using
Attachment 4c - Sections I and H. Each SOP should follow the format
specified in the RFP and documented in Attachment 4c - Section ifi.
10.5 Evaluation of Statements of Qualifications (SoQs) Deliverables
S0Q deliverables are used for evaluating the laboratory’s overall capabilities,
experience, capacity to produce data, and professional reputation in the regulatory
community. Evaluation of laboratory participation in PE and certification programs
provides an overall view of the laboratory’s standing with respect to government
agencies and specific analytical programs. Evaluation of MDL study results provides
information on laboratory accuracy, precision and sensitivity for specific analytical
protocols. The SoQs Elements Work Sheet, which is presented in Attachment 5b, is
used to verify that all requirecPsubmittals are present for review. Attachment 5a,
SoQs Evaluation Report, is used to summarize the evaluation results for the individual
SoQs elements in accordance with this SOP.
Evaluation of the SoQs submittals may require more professional judgement than
evaluation of the LQAP. The work sheets contained in Attachments 5c, 5d, Se, 5f
and 5g encompass all of the SoQs elements and require comments to be made or
judgements to be formulated. The evaluator should decide if any elements will
negatively impact laboratory performance of the analytical specification. If more space
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is needed to document comments, additional pages should be attached to the work
sheets.
10.5.1 Equipment Inventory and Analytical Capacity
Major equipment to be used by the laboratory in performance of the analytical
specification should be provided by the bidder as a simple list containing
model numbers and age. Ancillary items such as ovens, muffle furnaces,
balances, and any specialized equipment used for sample preparation or clean-
up should also be highlighted on this list.
Attachment 5c provides an example of the equipment inventory work sheet to
be utilized by the evaluator. If, upon review of bidder’s pre-qualification
submittal, an instrument is found to be unacceptable for the intended purpose,
it should be noted on this work sheet. The equipment inventory should
indicate the laboratory’s capability to perform the analytical specification.
Insttument model numbers, age, analysis modes and software revisions should
all be checked for applicability to the analytical specification. The evaluator’s
score should reflect the amount and detail of equipment inventory information
received.
The capacity of a bidder to perform the numbers of analyses required by the
field sampling contractor during the specified period of time can only be
assessed if the laboratory presents the following information:
• Number of samples performed per year, per month, per week, per
day and a distribution chart showing how those samples are
distributed over the calendar year for a particular analytical
specification
• The number of instruments dedicated to a particular analytical
specification
• The number of personnel dedicated to a particular analytical
specification
These facts may not be sufficient to determine if the laboratory is under- or
over-utilized during the window that the field sampling contractor will be
shipping samples. The number of samples that the field sampling contractor is
planning to ship during a specific period of time should be compared to the
laboratory’s theoretical excess capacity with no regard whatsoever to other
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work the laboratory has in-house. If the laboratory has under-utilized capacity
during the field sample contractor’s sampling window, then the evaluator can
readily assess capacity. The combination of available instiiiment time, and
personnel, as well as the number of samples routinely analyzed by the
laboratory should give the evaluator enough information to assess capacity.
The laboratory should advise the field sampling contractor as to any potential
or known capacity problems at the time of the RFP bid, so that the field
sampling contractor can be assured that samples will be analyzed within
holding times and turnaround time. If the laboratory will be over-booked
during the scheduled sampling period, then the field sampling contractor
should either change the sampling schedule or use another laboratory. If the
evaluator is still uncertain, then the laboratory should be asked about their
capacity during the specific sampling window. The reputation of and
professional references provided by the laboratory should be taken into
consideration. Any laboratory incapable of analyzing samples during the
required period of time should be autoirfatically disqualified.
10.5.2 Facility Description
A facility description is generally provided by the bidder in the form of a
plan(s) showing entrances, exits, loading docks, gas storage, chemical storage,
and analytical laboratories. The area of the laboratory where the specified
preparation and analysis of samples is to occur should be highlighted or
provided in detail. The information relating to electromechanical equipment,
ventilation, climate control, electrical sources, water sources, and waste
harding is also important to the evaluator and should be adequately
documented by the bidder.
Alternatively, the laboratory may submit a completed Attachment 5d to
document the facility description or may describe the facility in a narrative
statement. The description of the facility required in this portion of the RH’
response is much more detailed than the simple description required in the
LQAP. The evaluator should score this element based upon the relative
quality and detail provided in all pre-qualification submittals.
10.5.3 Experience and References
References and experience, when combined, give the evaluator a clear picture
of the type and quality of work that has been performed by the bidder for
various clients.
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The responding laboratory should provide short paragraphs describing
particular projects, clients, number of samples, method(s) of analysis, date(s)
of service, and success rate (if appropriate). The breadth of historical and
current experience will be major factors in assessing this element. The cited
experience should be relevant to the analytical specification being bid. The
evaluators should use the work sheet provided in Attachment 5e to document
their review.
Each project experience cited should include a client reference. References
are persons, companies, and agencies who have used the laboratory’s services
and include proper address(es), telephone numbers and key client contacts. At
least three references should be checked by the evaluator, who should
document written comments on the work sheet provided in Attachment 5e.
10.5.4 Participation in Performance Evaluation (PE) Programs
PE sample results are a measure of a laboratory’s ability to accurately
quantitate and identify analytes. Laboratory participation in PE sample
programs is usually documented with score sheets produced by the agency or
testing group. If score sheets are submitted for review, they should include
the sample results as well as nominal values, acceptance windows, and
warning and action windows. The score sheets should also provide
information on target compounds which were missed (false negatives) as well
as non-target which were found (false positives). This information allows the
evaluator to ascertain whether laboratory results were acceptable or
unacceptable, and whether they were biased low or high. The evaluator should
assess how well the laboratory performs a specific analysis or analytical
specification using the information provided on the score sheets.
PE samples may not be available for specific methods or analytical
specifications. Also, PE samples do not encompass all compounds or
concentration ranges. PE samples designed for other methods, but containing
the analytes of interest, may be used as long as the concentration range is
within that of the analytical specification. Points should be awarded for both
participation in PE programs and for laboratory scores. The evaluators should
document their comments using the work sheets provided in Attachment 5f.
10.5.5 Certifications
Certifications are documented in the form of certificates or letters of
certification from the issuing agency or group. State departments of
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The first step in rating a laboratory is to determine what constitutes an acceptable overall
score and how individual RFP components will factor into that Score. This determination
should be documented prior to soliciting the RFP. If the team chooses, they may include in
the R.FP the attachment work sheets, reports, and tables along with the planned component
scoring weights. The project’s Data Quality Objectives should determir the analytical
quality requirements (precision, accuracy, sensitivity, etc.), which in turn should be used to
determine each component’s weight.
In determining what an overall acceptable score should be for an individual project, the
QAM and proposal evaluators may consider several items, in addition to the project’s DQO
and data requirements. One consideration is that, in the education system, 75/100 or 75%
has historically been considered “passing”. A second consideration is that, in the CL?,
several QC acceptance criteria for accuracy and reproducabiliry use 75 to 125, or 25%
relative percent difference (RPD) as “passing”. If a field sampling contractor can accept
75% of a total of 100% recovery for a spike and 25% difference in duplicates for laboratory
results, then the field sampling contractor should be able to accept 75% of the total points
when evaluating a laboratory deliverable.
Concurrent with determining an acceptable overall score, the evaluation team should assign
each component a portion of the total highest score. The points assigned to each individual
component depends upon the importance of the component to the project requirements. For
example, assume that the highest score achievable has been selected by the evaluation team
as 100, with a score of 75% indicating that a responder is technically qualified. If an MDL
study is very important to the project requirements, then the MDL study component should
be given the largest portion of the 100 possible points. Furthermore, it should be given
sufficient points so that any laboratory not providing an MDL study would be unable to reach
a score 75%, no matter what other pre-qualification requirements were met. In this case, the
MDL study component would need to be assigned 26 or more points.
Scoring schemes shduld be determined on a case-by-case basis. The evaluation team
determines a point score for every component and element from a pre-determined guideline
prior to the RFP solicitation.
In some cases, certain components or elements are applicable to a method, and therefore will
not be included in the scoring scheme. For example, there are no PE samples or
certifications awarded by any agency or org nh72tion for the analysis of grain size or total
combustible organics. The components for certifications and performance evaluation cannot
be factored into the scoring scheme for those analytical specifications. Therefore, no points
are assigned to these elements.
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The evaluation team not only needs to determine the overall maximum score, the score for
“technically qualifying”, and scores for RFP components, but also scores for each individual
element that makes up the larger components. An example breakdown of the 10 total points
for the “Experience and References” component follows:
• award 4 points for three comprehensive narratives pertinent to the analytical
specification
• award 2 points if the three experience narratives are related to projects which
were performed within the last six months
• award 2 points for references provided with full contact names, telephone
numbers, and addresses
• award 2 points if the references provide positive and complimentary
verification of the project
Table 1 provides examples of two scoring schemes to illustrate one evaluation team’s scheme
for scoring RFP responses. Other RFP evaluators may choose to weight the components
differently, and may choose a higher or lower total score for acceptance of a laboratory.
The scores provided in Table 1 are given in ranges as indicated. The evaluator may choose
to give zero points either due to the omission of the component or its unacceptable nature. If
a component or element of the component is omitted, the laboratory may be contacted to
submit that item within a specified time frame depending upon the number of responders and
the quality of their bid subinittals. If a responder fails to resubmit a requested item, then
zero points are assigned. The same process should be used for missing elements within a
component. No partial point scores, i.e., tenths of a point, should be awarded under the
scoring scheme.
Once a laboratory submittal has been reviewed, the total element points and the laboratory’s
overall score should be calculated by each evaluator. The laboratory’s final score is the
average of all the evaluators’ overall scores. The QAM should verify the scores resulting
from this process and check for large discrepancies between evaluators. Overall scores for a
laboratory should not deviate by more than 30% between evaluators. If large differences
exist between scores, the QAM should attempt to determine the cause of the difference and
whether further review of the bidder’s submittals is necessary.
Table 2 contains an example tabulation of laboratory scores. The total points for each
laboratory are snmmed and placed in the “Total Score” column of Table 2. The average of
each evaluator’s total score is used to determine the laboratories which are deemed
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thcally-qualifiedto perform the specific analytical specification (in this case, scores above
75 points).
The example provided in Table 2 shows that Laboratories B, C & D are technically-qualified
laboratories (when an MDL submittal is required). The evaluators should use Statement of
Technically-Qualified Laboratory(ies) Report, which is contained in Attachment 6, as the
final documentation of the review. Attachment 7 allows the evaluators to enumerate reasons
why a particular laboratory was deemed unqualified. For instance, in situations where a
laboratory did not submit a vital deliverable, and that deliverable would have potentially
increased their points score to within the acceptable range.
The Statement of Technically-Qualified Laboratoxy(ies) Report and score sheets should be
submitted to the field sampling contractors purchasing speciali r for comparison with cost
estimates. The laboratory with lowest cost from the list of technically-qualified laboratories
will be chosen and contractual arrangements will be made. The technical evaluators should
not know analytical bid prices when pre-qualifying laboratories.
12.0 LABORATORY PRE-QUA.LIFICATION ELNAL REPORTS
Completed Attachments 1 through 7 are considered to comprise the Laboratory Pre-
Qualification Final Report. If a pre-award audit is performed, then the Laboratory Pre-
Qualification Final Report should be attached to the Pre-Award Audit Final Report and filed
in the field sampling contractor’s project file. A copy of both should be sent to the Section
Chief of the Contracts Management Section, located in EPA’s Waste Management Division.
If a pre-award audit is not performed, then a justification expl iniT1g the reason why an audit
was not performed should be written. The justification and the Laboratory Pre-Qualification
Final Report should be filed in the field contractor’s project ñle. A copy of both should be
send to the Section Chief of the Contracts Management Section, located in EPA’s Waste
Management Division.
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TABLE 1. SAMPLE SCORING SCHEME USED IN DAS PILOT PROJECT
A. Scoring for analytical specification not requiring an MDL study
Oualitv Assurance Program
LQAP (less resumes) 0-15
SOPs 0-20
Resumes
Range/Total possible 50
SoOs
Equipment Inventory 0-4
Facility Description 0-4
Experience & References 0-10
Capacity 0-7
Example Deliverable 0-10
MDL Studies (nonspecific) 0-2
PE Programs 0-8
Certifications
Range/Total possible 50
Total possible points for analytical
specification not requiring an MDL study 100
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Region I Laboratory Pre-Quailfica jon SOP
Revision Number: 1
Date: 15 March 1994
Page 36 of 65
TABLE 1. SAMPLE SCORING SCHEME USED IN DAS PILOT PROJECT
(continued)
B. Scoring for analytical specification requiring an MDL study
Oualitv Assurance Program
LQAP (less resumes) 0-10
SOPs 0-15
Resumes 0-10
Range/Total possible 35
MDL Study
(Specific to analysis 0-35
with deliverables)
Range/Total possible 35
Sops
Equipment Inventory 0-2
Facility Description 0-2
Experience & References 0-5
Capacity 0-5
Example Deliverable 0-8
PE Programs 0-5
Certifications Q:
Range/Total possible 30
Total possible points for analytical
specification requiring an MDL study 100
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Region I Laboratory Pre-Qualificaiion SOP
Revision Number: I
Daze: 15 March 1994
Page 37 of 65
TABLE 2. SAMPLE LABORATORY COMPARISON SCORE CARD
QAP
SoQs
0
0. )
>
-a
0.)
C.
C I ,
0.)
E
C I ,
0)
lt
B
Laboratory
Name
“ -I
C l ,
0
C,,
0)
C.,
0.)
1
0)
C.
-a
C .)
0)
0.
0)
.0
I -.
0.)
0)
U )
0.)
U
0
2
0.)
—S
5
-a
C i
C .
0
C l ,
I-
C
I-
—S
0
0
C O
U
I-
0.)
0
Total
(100)
E ’ampleA
5
1
7
15
2
1
1
3
2
2
2
2
47
B
15
2
15
30
2
2
3
4
5
5
5
3
91
C
11
5
12
35
2
2
3
5
4
5
4
3
91
D
13
4
14
30
22
2
4
4
433
85
E
8
3
9
20
11
1
3
2
222
54
-------
ATI’ACEMENT 2b
LQAP WORK SH1 ET
Laboratory: __________ Analytical Specification(s):
Project Number: ____________ Date Reviewed:
Field Sampling Contractor: ____________ Reviewed By:
L
QA.P Evaluation
Acceptable
Not
Comments
Acceptable
3. Facility Description
Reference_(Sect.IID_No.)
E.
Document Control
1. Laboratory Notebook Policy Reference
(Sect.IID No.)
2. Sample Trac ng/Custody Procedures
Reference (Sect./ID No.)
3. Logbook Maintenance and Archiving
Procedures Reference (Sect.IJD No.)
4. Case File Organization, Preparation and
Review Procedures Reference
(Sect./ID No.)
5. Procedures for
Preparation/Approval/Review!
Revision and Distribution of SOPs
Reference
(Sect./ID No.)
6. Process for Revision of Technical or
Documentation Procedures Reference
(Sect./tD_No.)__________
42
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ATFACHMENT 2b
LQAP WORK SHEET
Laboratory: __________ Analytical Specification(s):
Project Number: _________________ Date Reviewed:
Field Sampling Contractor: ____________ Reviewed By:
LQA.P Evaluation
Acceptable
Not Comments
Acceptable
F. Analytical Methodology
1. Calibration Procedures and Frequency
Reference (Sect.IID No.)
2. Sample Prep/Extraction Procedures
Reference (Sect.IID No.)
3. Sample Analysis Procedures Reference
(Sect.IID No.)
4. Standards Preparation Procedures Reference
(Sect.ITD No.)
5. Decision Process Procedures/Responsibility
for Initiation of Corrective Action
Reference (Sect.IID No.)
6. Procedures for Monitoring Corrective
Action Reference
(Sect./ID_No.)___________
G. Data Generation
1. Data Collection Procedures Reference
(Sect.IID No.)
2. Data Reduction Procedures Reference
.
(Sect/ID No.)
3. Data Validation Procedures Reference
(Sect.TJD No.)
4. Data Reporting and Authorization
Procedures Reference
(Sect./ID_No.)_________
43
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ATTAChMENT 3c (continued)
PRE-QUALIFICATION KEY PROJECT PERSONNEL
QUALIFICATION WORK SHEET
Laboratory: Analytical Specification(s):
Project Number: __________________ Date Reviewed:
Field Sampling Contractor: _____________ Reviewed By:
Position
Requirements
Name
Education/Experience
Qualified (V/N)
Wet Chemistry
Operator
BS degree in chemistry/science/engineering
plus 1 year experience in wet chemistry OR
Inorganic Supervisor
BS degr e in chemistry/science/engineering
+3 yr ICP/AA experience, including 1 yr as
Inorganic Instrument
Operator
BS degree in chemistry/science/engineering
+ 1 yr ICP/AA experience OR 3 yrs
50
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ATTACHMENT 4a
SOP EVALUATION REPORT
Laboratory: ___________ Analytical Specification(s):
Project Number: _______________ Date Reviewed:
Field Sampling Contractor: ____________ Reviewed By:
Date submitted to Field Sampling Contractor ________________________
Comments on Analytical Specification SOPs (Laboratory’s Method SOP):
‘Comments on List of Ancillary Laboratory and Evidentiary SOPs:
Comments on SOP Format:
Verified by: _________ Date Verified:
51
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ATIACBMENT 5a
PRE-QUALIFICATION SOQS
EVALUATION REPORT
Laboratory: _________________ Analytical Specification(s):
Project Number: ______________ Date Reviewed:
Field Sampling Contactor: ____________ Reviewed By:
SoQs Evaluation:
Unacceptable SoQs:
Verified by: _________ Date Verified:
56
-------
ATFACEMENT Sb
SOQS ELEMENTS
WORK SHEET
Laboratory: _______________ Analytical Specification(s):
Project Number: ______________ Date Reviewed:
Field Sampling Contractor: ____________ Reviewed By:
SoQs DELiVERABLES ELEMENTS SUBMISSION
Yes No Date
1. Equipment Inventory and Analytical Capacity — _______
2. Facility Description — ______
3. Experience and Professional References
4. Participation in PE Sample Programs — ______
5. Certifications ______
6. Method Detection Limit (MDL) Studies — — _____
7. Examples of Deliverables — _______
57
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A1TACHMENT Sc
EQUIPMENT INVENTORY AND
ANALYTICAL CAPACITY
WORK SHJ* T
Laboratory: ________________ Analytical Specification(s): _____________
Project Number: _______________ Date Reviewed: _____________
Field Sampling Contractor: ___________ Reviewed By: _____________
Samples/Year
Samples/Month
Instrument Model or Type Year or Age Analysis Mode Samples/Day Acceptable (yes/no )
1.
2.
3.
4.
5.
6.
7.
8.
9.
10.
11.
12.
13.
14.
15.
16.
17.
18.
19.
20.
58
-------
AITACHMENT Sc (continued)
EQUIPMENT INVENTORY
ANALYTICAL CAPACITY
WORK ShEET
Laboratory: Analytical Specification(s): _____________
Project Number: ___________ Dare Reviewed: _________
Field Sampling Contractor: ____________ Reviewed By: _____________
Ancillary Equipment, Computerization. Software
Describe ancillary equipment, computerization, software packages used for the analysis of the particular
analytical specification:
Capacity Comments (identify laboratory’s ability to perform within the required window):
59
-------
ATrACHMENT Sd
FACILITY DESCRIPTION
WORK SIIFET
Laboratory: _________________ Analytical Specification(s): _______
Project Number: _______________ Date Reviewed: _______
Field Sampling Contractor: ____________ Reviewed By: _______
rflStrurflent Type Description Comments
1. Electrical source
2. Water source
3. Building type
4. Laboratory space sq.Ift.
5. Building age
6. Ventilation
7. Air conditioning
8. Climate control
9. Heating
10. Air handling/cleaning
11. Compressed gas storage
12. Chemical storage
13. Waste chemicals storage
14. Records storage
15. Waste disposal
16. Solid waste handling method
17. Hazardous waste management practices
18. Other
Facility Comments:
60
-------
AT ACBMENT Se
EXPERIENCE AND REFERENCES
WORK SHEET
Laboratory: _________________ Analytical Specification(s):
Project Number: _______________ Date Reviewed:
Field Sampling Contractor: ____________ Reviewed By:
SoQs: Experience and References
Client Reference
Relevant
Work
(yes/no)
Recent
Project
(date)
Date
Contacted
Acceptable
(yes/no)
Comments
1.
2.
3.
Additional Comments:
61
-------
ATrACHMENT Sf
PERFORMANCE EVALUATION PROGRAMS
AND CERTIIICATION REVIEW
WORK SHEET
Laboratory:
Project Number: ________
Field Sampling Contractor:
Analytical Specification(s):
Date Reviewed:
Reviewed By:
SoQs: PE Programs
Program Org2ni72tion
(providing PE sample)
Dare of PE
Matrix of
PE Sample
Score
Acceptable
(Y/N)
Comments
SoQs: Certifications
Program
Certifying
Orginization
Date of
Certificate
Date of
Expiration
Acceptable
(YIN)
Comments
62
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ATrACHMENT 5g
MDL STUDIES AND DELIVERABLES
WORK SHEET
Laboratory: ______ Analytical Specification(s):
Project Number: Date Reviewed:
Field Sampling Contractor: Reviewed By:
SoQs: MDL Studies
Analytical Fraction
Matrix Studied
Date
Results
Acceptable
(Y/N)
Comments on MDL Studies:
SoQs: Exirnples of Deliverables
Analytical Fraction
Matrix Studied
Acceptable
(YIN)
Comments
63
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AUACHMENT 6
TECHNICALLY-QUALIFIED LABORATORY(JES)
REPORT
The following laboratories are technically-qualified to perform analytical specification
Laboratory Name
1. ______________________________________________
2. ________________________________
3. _________________________________
Evaiuator Name Evaluator Si narure Date
Verified by: __________ Date Verified: ___________
Field Contractor:
Address:
64
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ATFACHMENT 7
COMMENTS ON QUALIIFICATIONS
The following laborazories were found to be unqualified for analytical specification
Laboratory Name
1. ______________________________________________
2. ________________________________
3. ___________________________________
Evaluator Name Evaluator Sizriature Date
Verified by: _________ Date Verified: _________
Field Contractor:
Address:
65
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Region I Laboratory Pre-Qualificazion SOP
Revision Nun*
Dare: ISMarck
Page 1 of Appenci.ixA
APPENDIX A
LIST OF CONTACTS FOR LABORATORY REGISTERS
To obtain RAS list:
U.S. EPA, Region I
JFK Federal Building (APE - CAN7)
Boston, MA 02203
For U.S. EPA Region I state lists:
Connecticut Department of Environmental Protection
165 Capitol Avenue, Room 113
Hartford, CT 06106
(203) 566-2110
Maine Department of Environmental Protection
State House, Station 17
Augusta, ME 04333
(207) 289-7688
Massachusetts Department of Environmental Protection
One Winter Street
Boston, MA 02108
(617) 292-5500
New Hampshire Department of Environmental Services
6 Hazen Drive
Concord, NH 03301
(603) 271-3503
Rhode Island Department of Environmental Management
9 Hayes Street
Providence, RI 02908
(401) 277-2771
Vermont Department of Environmental Conservation
103 S. Main Street
Waterbury, VT 05676
(802) 244-8731
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Region I Labor zory Pre-QualificaLion SOP
Revision Number: 1
Daze: 15 March 1994
Page 1 of Appendix B
APPENDIX B
EXAMPLE ANALYTICAL SPECIFICATIONS
Analytical Specification for Method 524.2
Analytical Specification for EPA Method TO-14
Analytical Specification for TOC, TCO, and Grain Size in Sediment
-------
APPENDIX E
REGION I LABORATORY AUDIT
STANDARD OPERATING PROCEDURE
E-1
-------
REGION I LABORATORY AUDIT
STANDARD OPERATING PROCEDURE
15 March 1994
-------
PREFACE
The Region I Laboratory Audit Standard Operating Procedure was developed by the Region I
Quality Assurance Office. The document is provided as guidance and may be used by any
EPA or contractor personnel responsible for obtaining analytical services for EPA.
I
-------
TABLE OF CONTENTS
1.0 SCOPE AND APPLICATION
2.0 PURPOSE
3.0 USE OF THIS SOP
4.0 DEFINITIONS AND ACRONYMS
1
.1
2
3
5.0 AUDITTEAM
5.1 Quality Assurance Manager (QAM)
5.1.1 QAM professional requirements
5.1.2 QAM duties and responsibilities
5.2 Auditor
8
9
10
10
11
11
12
13
13
14
15
16
16
17
18
19
19
20
21
21
22
22
22
4
4
4
6
6
6
7
5.2.1 Auditor professional requirements
5.2.2 Auditor duties and responsibilities
6.0 ON-SITE LABORATORY AUDITS AND EVALUATIONS
6.1 Prior To The Facility Visit
6.2 Pre-award Pre-Facility Audit Meeting
6.2.1 Analytical Specification Discussions
6.2.2 Quality Assurance Practices
6.2.3 The Laboratory Quality Assurance Plan
6.2.4 Organization and Personnel Summary
6.2.5 Technical Communications
6.3 Post-award Pre-facility Audit Meeting
6.4 Problem Resolution Pre-Faciity Audit Meeting
6.5 Laboratory Facility Audit
6.5.1 Sample Receipt, Log-In, Storage, and Security Areas
6.5.2 General Facilities
6.5.3 Organic Sample Preparation Areas
6.5.4 stndards Preparation anti Storage
6.5.5 Sample Analyses and Instrumentation
6.5.5.1 Instrument Performance
6.5.5.2 CalibratiOn
6.5.5.3 Instrument Documentation and Usage
6.5.5.4 Instrument Maintenance
6.5.5.5 Auditing of Organic SOPs
6.5.5.6 GC Extractable Analysis
6.5.6 Data Handling and Review
11
-------
TABLE OF CONTENTS
(CONTINUED)
6.5.7 Quaiity Assurance Practices • 23
6.5.8 Data Verification and Completeness Check 23
6.6 Post-Facility Audit Meeting
6.6.1 Pre-award Post-facility Audit Meeting 23
6.6.2 Post-award Post-facility Audit Meeting 24
6.6.3 Problem Resolution Post Audit Meeting
7.0 AUDITING DOCUMENTATION 26
8.0 LABORATORY AUDIT FINAL REPORT 27
9.0 CHECKLISTS 27
U i
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Region I Laboratory Audit SOP
Revision Number: I
Date: 15 March 1994
Page 1 of 77
1.0 SCOPE AND APPLICATION
Pre-award on-site laboratoiy evaluations, or laboratory audits, may be used to verify that a
laboratory has the instnjnients, standard operating procedures, personnel and Quality
Assurance/Quality Control (QA/QC) program(s) presented in its pre-qualification submissions
or bid packages. Contracts should be awarded to laboratories based on technical
qualifications (see associated Region I Laboratory Pre-Qualification Standard Operating
Procedure ) and bid price. After a laboratory has been pre-qualifled as the most technically
qualified low bidder, a pre-award audit may be included as an additional pre-qualification
requirement to ensure technical ability. The decision of whether or not to perform a pre-
qualification audit should be made based on numerous factors including, but not limited to:
the laboratory’s satisfactory participation in CLP or other analytical program, number of
samples to be analyzed, geographical location of laboratory, complexity of analytical
specification, quality and type of pre-qualification information received from bidders, and
data quality objectives for the sampling events.
Alternatively, a post-award audit may be used to verify that the chosen laboratory is
conforming to the analytical specification or method, has implemented effective corrective
actions andlor has sufficient sample capacity to accommodate projected work. Post-award
audits may be initiated by the field sampling contractor’s Quality Assurance Manager (QAM)
to resolve specific technical or delivery problems and are then termed problem resolution
audits.
This Standard Operating Procedure (SOP) for auditing can be adapted for use with all types
of laboratories performing organic, inorganic (metals), wet chemical parameters, and
physical analysis and testing. This SOP evaluates and eicompasses the entire organic
laboratory analytical system from the point the sample enters the laboratory to the point that
the analytical testing data is released as hard copy or electronic information to the client.
Attachment A includes the EMSL Audit Guidelines for inorganic sample preparation and
analysis to supplement this audit SOP.
2.0 PURPOSE
The purpose of this SOP is to standardize the laboratory auditing process, including audit
team qualifications, the audit procedures used, auditing documentation (i.e., checklists) and
final audit report. Laboratory audits are performed to ensure technical capability and sample
capacity of a laboratory and to resolve technical and logistical problems.
Prior to a pre-award audit, laboratories are pre-qualifled using procedures documented in the
Region I Laboratory Pre-Oualification Standard Operating Procedure . Once the set of
technically-qualified laboratories has been determined, bid prices are ex rriined, and then the
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Region I Laboraxory Audit SOP
Revision Number: I
Daie: 15 March 1994
Page 2 of 77
lowest priced, technically qualified laboratory is determined. This laboratory may then be
audited to verify specific information supplied by the bidder or to obtain additional
information from the bidder. In this case, the audit is the final step in pre-qualifying the
laboratory.
The post-award audit is performed after a laboratory has been awarded the contract. A post-
award audit may be performed to verify that all corrective actions required during the pre-
qualification phase have been implemented. The laboratory may also be audited to ascertain
that it is conforming to the analytical specification, that sufficient analytical capacity exists to
perform the work, and to determine if the key project personnel are working on the project.
The post-award audit is a check on the laboratory to determine and verify its technical
abilities, and also to establish communications with key personnel. If, during a post-award, a
laboratory is determined to be technically unqualified or if it is determined that the laboratory
does not have sufficient capacity to perform the work, then action should be taken against the
laboratory.
The problem resolution audit is performed to resolve analytical or non-technical problems
that result in failure to produce compliant data. Non-compliant data may result when quality
control criteria are exceeded, required corrective actions are not implemented, or when data
is late. Problem resolution audits are generally focussed on specific laboratory problems
rather than on the entire laboratory analytical system. Problem resolution audits are typically
the result of the laboratory not resolving the problems on their own through in-house
corrective action measures.
This SOP can be used for laboratory audits that encompass any type of analytical procedure,
although it must be adapted to those procedures. Careful and complete documentation of
what was audited, how it was audited, and what criteria were used to audit is recommended.
Laboratory audit documentation should be filed with the associated project file and a copy
should be submitted to the Agency.
3.0 USE OFTHIS SOP
This Laboratory Audit Standard Operating Procedure (SOP) is organized to present:
1) qualifications of the audit team; 2) procedures for performing on-site audits of
laboratories; 3) preparation of the on-site audit report; and 4) example checklists for
documenting the audit(s).
Section 4.0 lists the acronyms and abbreviations used throughout this procedure. Sections
5.0, 6.0, and 7.0 define the requirements for audit team qualifications; describe actual audit
procedures; and present the process of audit documentation and final reporting. Section 8.0
describes filing requirements for a Laboratory Audit Final Report. Example checklists to be
used during the audit are provided in Section 9.0.
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Region I L3boratory Audit SOP
Revision Number: 1
Date: 15 March 1994
Pa’e 3 of 77
4.0 DEFINITIONS AND ACRONYMS
The following acronyms and abbreviations are used throughout this report:
BNA Base/Neutral-Acid Extractables
CLP Contract Laboratory Program
CCC Chain of Custody
CRQL Contract Required Quantitation Limits
DAS Delivery of Analytical Services
ECD Electron Capture Detector
EPA Environmental Protection Agency
EPTOC Extraction Procedure Toxicity Characteristics
ESD Environmental Services Division
GC Gas Chromatography
GC/FID Gas Chromatography/Flame Ionization Detector
GC1PID Gas ChromatographylPhotoionization Detector
GC/MS Gas ChromatographyfMass Spectroscopy
GPC Gel Permeation Chromatography
HAZWRAP I-T27 ardous Waste Remedial Action Program (DOD/DOE)
IDL Instrument Detection Limit
LIMS Laboratory Information Management System
LQAP Laboratory Quality Assurance Plan
MDL Method Detection Limit
mg Milligram
mg/kg Milligrams per Kilogram
mg/L Milligrams per Liter
NBS National Bureau of Standards
NPDES National Pollutant Discharge Elimination System
PCBs Polychiorinated Biphenyls
PE Performance Evaluation
QAIQC Quality Assurance/Quality Control
QAM Quality Assurance Manager
QAO Quality Assurance Officer
QAPP Quality Assurance Program Plan
QAPjP Quality Assurance Project Plan
RAS Routine Analytical Services
RRF Relative Response Factor
RSD Relative Standard Deviation
SAS Special Analytical Services
SDG Sample Delivery Group
SOP Standard Operating Procedure
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Region I Laborazory Audit SOP
Revision Number: I
Daze: 15 March 1994
Page 4 of 77
TDS Total Dissolved Solids
TOC Total Organic Carbon
TSS Total Suspended Solids
j gJL Micrograms per Liter
zg/kg Micrograms per Kilogram
VOC Volatile Organic Compounds
VOA Volatile Organics Analysis
5.0 AUDIT TEAM
An audit team qualified to evaluate the laboratory procedure(s) to be audited should be
assembled. The team should be made up of an auditor who is experienced with the type of
analytical specification being audited, and a Quality Assurance Manager (QAM), the team
leader. If the QAM is not present, the auditor with seniority will be the team leader. The
auditor performs the audit and documents the audit findings; the QAM reviews and approves
the audit documentation. The qualifications and duties of each of these professionals is
described in this section. In some cases, the QAM and auditor may be the same person. In
this case, the field sampling contractor’s program mpnager approves audit documentation. In
other cases, several auditors may be required to review different analytical specifications
performed in one laboratory.
5.1 Quality Assurance Manager (QAM)
5.1.1 QAM professional requirements
The QAM should have a B.S. degree in chemistry or a related physical science and be a
professionally trained analytical chemist with at least ten years of broad laboratory
experience in the field of analytical chemistry. The QAM should have performed five
laboratory audits covering multiple analytical techniques and should have at least eight
years of experience in environmental analysis of the following parameters in various
matrices:
• Organics, including volatiles, semivolatiles, pesticides, herbicides, PCBs, dioxins,
oil/PAH fingerprinting, and water-soluble organic compounds
• Inorganics, including metals, cyanide, anions, and sulfide
• Organic carbon, including TOC, TCO, COD, and BOD
• General organics such as total petroleum hydrocarbons, MBAS, and oil & grease
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Region I Laboratory Audit SOP
Revision Number: I
Date: 15 March 1994
Page 5 of 77
• Physical testing, including grain size, Attenburg limits, compactability, particle size,
and asbestos identification
Other expectations of the QAM include extensive knowledge of and/or expertise with:
• Operations of the instrumentation used in all analytical specifications.
A solid working knowledge of the limitations and problem resolution procedures for
all analytical instrumentation should be required. The QAM is not required to have
hands-on experience operating each instrument, but should be familiaz with the
theoretical operation.
• Development, and preparation of analytical specifications, especially SAS requests.
This would include experience with: CLP SOWs - organic, inorganic, low
concentration, dioxin; SW 846 methods; CWA 500 Series methods; Methods of
Chemical Analysis of Water and Wastes; Standard Methods for Exaruinatjon of
Water and Wastewater ; and Compendium of Methods for the Determination of Toxic
Organic Compounds in Ambient Air .
• Application of quality assurance/quality control requirements to the methodologies
described above.
These analytical and QC requirements should be clearly delineated in each analytical
specification.
• Validation of analytical data according to the Region I Functional Guidelines .
The QAM should understand validation requirements, and be able to validate various
types of data to determine whether or not the chemical data are valid.
• Interpretation of environmental data to draw legally defensible conclusions.
This is accomplished by evalu ting the validity of analytical data in light of problems
originating from sampling notes, site history, and site conditions.
• Development of statistically-based DQOs and the deterrniration of whether those
objectives have been achieved.
• Effective communication with laboratories in an informed manner .
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Region [ Laboratory Audit SOP
Revision umber: I
Daze: 15 March 1994
Page 6 of 77
The QAM should be familiar with all areas of laboratory operations, including types
of deliverables, data systems, capabilities, and documentation. The QAM should be
able to translate this knowledge into clearly written analytical specifications.
In summary, the QAM should be experienced in all aspects of laboratory auditing
environmentai sampling, and analysis and data evaluation. In addition, the QAM should
be familiar with all contract requirements and penalties for non-compliance in the
contract.
5.1.2 QAM duties and responsibilities
The QAM should be present at all audits and is the Auditing Team Leader. The QAM can
be both auditor and author of all the audit documentation, or can be part of a larger audit
team. In either case, the QAM is responsible for overseeing the entire audit process. The
QAM is responsible for: 1) determining if a pre-award, post-award, or problem
resolution audit is necessary; 2) developing the audit procedure, checklists, and
documentation requirements for the audit; 3) training the auditor(s) on audit procedures
(sequence of events), what to look for, and how to properly document the audit results; 4)
reviewing and approving the audit report, including all checklists, comments, meeting
notes, post-facility audit debriefing report, final report, and any corrective action reports;
5) following-up on corrective action requests made by the auditor and determining if
corrective actions have been implemented properly by the laboratory; 6) determining if a
laboratory is able to produce analytical data in the required manner described in the
analytical specification; and 7) submitting Laboratory Audit Final Reports to the EPA in
accordance with Section 8.0.
Based on the evaluation of pre-qualification documentation and the audit verifying
documentation, the QAM makes the final decision as to which laboratories are technically-
qualified. The QAM approves the final auditing report, and verifies that all review
comments have been addressed. The QAM also verifies that appropriate corrective
actions were implemented by the laboratory prior to sample analysis and documentation of
sample analysis. A successful audit followed by implementation of proper corrective
actions should elimin2te the need for corrective actions during the analysis and data
reporting phase.
5.2 Auditor
5.2.1 Auditor professional requirements
The laboratory auditor should have a B.S. degree in chemistry or a related physical
science and should have at least two years experience as an analytical chemist operating
the particular instrumentation system to be audited. The auditor should have performed at
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Region I Laboratory Audit SOP
Revision Number: 1
Date: 15 March [ 994
Page 7 of 77
least two audits satisfactorily in the presence of the QAM or another experienced auditor
prior to conducting an independent audit. More than one auditor may be required if
several instrument systems are to be audited. The auditor should be fully versed in the
requirements of the method or analytical specification. The auditor should understand the
physical, electronic, and chemical properties of the analytical instrumentation; chemical
properties of the analytical instrumentation; chemical properties of the analytes; quality
assurance/quality control requirements of the methods; and their interdependence.
Familiarity with each step of the analytical procedures is required in order for the auditor
to pose appropriate questions about the various instrumental accessories (such as columns,
detectors, temperature programs, etc.). The auditor should have a complete understanding
of other related auxiliary laboratory functions in order to evaluate the overall laboratory
operation.
5.2.2 Auditor duties and responsibilities
The auditor’s duties are to: 1) prepare for the audit, as described in Section 6.1 of this
SOP; 2) conduct a pre-faciliry audit meeting, as described in Section 6.2 of this SOP; 3)
complete the audit checklists, noting all correct procedures as well as any deficiencies or
non-compliant procedures found; 4) conduct a post-facility audit debriefing session with
laboratory personnel; and 5) document the audit in its entirety, using both checklists and
written report. In the case of special audits where the auditor is the only analytical
specialist, the auditor will develop the checklist in conjunction with the QAM. The auditor
should be familiar with the method or analytical specification. The
communications/contact route between the laboratory and the field sampling contractor
should be established at the debriefing and be clearly understood by both parties.
To conduct an audit, the auditor should have a detailed checklist encompassing each
laboratory area or function that could be used to perform the analysis of samples for a
method or analytical specification in order to guide them through the audit process.
During the post-facility audit meeting (debriefing), all deficiencies, discrepancies or
unancwered questions should be discussed and corrective actions agreed upon and a time
frame established. The auditor should document and notify the laboratory personnel of all
deficiencies found during the audit, or during the pre-qualification review of laboratory
documents, that need to be corrected. The laboratory should be allowed a pre-determined
and agreed upon amount of time to correct all deficiencies. The implementation of
laboratory corrective actions should also be documented by the auditor prior to laboratory
receipt of samples.
If the labcratory does not satisfactorily correct deficiencies noted during a pre-award
audit, the laboratory should be determined “not qualified”, and the contract should be
awarded to another laboratory. In the case of a post-award audit, the laboratory should not
be sent samples until corrective actions have been implemented. Alternatively, the field
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sampling contractor could take allowable contract action against the laboratory. In the case
of a problem resolution audit where the laboratory may be receiving samples or have
samples in house to analyze, the QAM should use professional judgement in deciding
whether or not to allow the laboratory to continue analysis.
Contract non-compliance and failure to implement effective corrective action should be
dealt with directly. The exact nature of the laboratory contract will determine the
required action. Laboratory disqualification during the pre-award phase is a decision by
the auditor (with concurrence with the QAM) that the laboratory is not technically-
qualified or is no longer qualified.
The auditor is responsible for documentation of the audit and compilation of the
Laboratory Audit Final Report. The auditor should submit the audit checklists and final
report to the QAM for review and approval.
6.0 ON-SITE LABORATORY AUDITS AND EVALUATIONS
Pre-award laboratory audits are performed to confirm that the laboratory systems, as
documented in the pre-qualification deliverables, exist and are performing properly to
produce data of high quality. Post-award audits are performed to verify that corrective
actions have been implemented and that samples are being analyzed in accordance with the
analytical specification or method. Problem resolution audits are performed to investigate
and resolve a specific analytical problem. Prior to the on-site audit, the auditor should have a
predetermined approved checklist(s) that encompasses the analytical specification(s) or
protocol(s) as well as all other procedures that the analytical samples will undergo during
processing. These protocols include:
• Sample receipt, storage, and security
• General facilities, including safety, glassware cleaning, and laboratory waste disposal
• Sample preparation
• Standards preparation
• Sample analysis and instrumentation, (i.e., instrument performance, calibration, sample
analysis, and instrument maintenance)
• Data handling and review
• Quality assurance practices
• Data verification, completeness and technical review of data
This list can be expanded to include any specialty items that the particular analytical
specification may require.
Laboratory functions can be broken down into various categories such as: organic, inorganic
(methods), wet chemical, air methods, biological, physical testing, radiological, microscopic,
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etc. Due to the nature of the U.S. EPA Superfund (CERCLA) program, the areas of
analysis most commonly used are organic, inorganic, and sometimes wet chemicai analysis.
Air methods, radiological, biological, physical analyses and microscopic analysis, while not
routinely performed on environmental media, may be required for a specific site. This
Laboratory Audit SOP focuses on organic analyses, but the procedure may be adapted to
inorganic, wet chemical analysis and physical parameter testing and other analytical
protocols. See Attachment A for additional auditing guidance.
Two items common to laboratory audits of all methods and protocols are laboratory
personnel and laboratory equipment. Actual laboratory equipment in use should be recorded
during the audit and matched to the pre-qualification deliverables, see Region I Laboratory
Pre-Oualification Standard Operating Procedure . During the audit, the qualifications of the
laboratory’s personnel should be verified with the information supplied in the pre-
qualification submittal. This can be accomplished either during an interview with the
personnel or during the pre-facility audit meeting. Verification of pre-quali.ficadon
information should be recorded on the checklists. The actual organizational plan should aiso
be checked to ascertain if the reporting structure exists as stated in the pre-qualification
submittal. The details associated with auditing laboratory personnel and equipment are
incorporated in Sections 6.2 through 6.5 of this SOP.
6.1 Prior To The Facility Visit
The person performing the audit, auditor or QAM, should contact the laboratory at least
two weeks prior to an audit. The laboratory should be informed as to the type of audit that
will be performed (pre-award, post-award, problem resolution), and the procedure(s) or
protocol(s) to be audited. The laboratory should have the analysts who will perform the
analyses on-hand for the audit. The auditor may send an agenda to the laboratory to plan
the day(s) of the audit. At least one full day should be planned for a complete laboratory
audit and half a day for more focussed audits of specific operations.
Also prior to the pre-award audit, the auditor should prepare the audit checklist and
carefully evaluate the laboratory’s Quality Assurance Program. The laboratory’s Quality
Assurance Program should include a Laboratory Quality Assurance Plan (LQAP),
laboratory organii ation including restimes and project team definition, and laboratory
standard operating procedures. (For further information on each of these items, refer to
Section 7.0 of the Region I Laboratory Pre-Qualification Standard Operating Procedure. )
The QAM should, prior to the audit, compile all checklists to be used during the audit and
brief the auditor on the goals of the audit. The QAM may need to prepare some new
checklists, depending upon the analytical specification(s) being audited. If the QAM is not
the auditor and the auditor is a specialist, then the auditor should help the QAM prepare the
checklists.
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6.2 Pre-award Pre-Facility Audit Meeting
The purpose of the pre-faciity audit meeting for a pre-award or post-award audit is
essentially the same, the auditor (QAM or auditor) will establish agenda, purpose, and
communications for the -audit. The purpose of a pre-facility audit meeting for a problem
resolution audit depends on the specific problem to be resolved.
Upon arrival at the laboratory, the auditor (QAM or designated auditor) should meet with
the laboratory personnel that will perform the analytical specification. During the pre-
facility audit meeting, four major subjects should be discussed: 1) analytical specifications;
2) quality assurance practices; 3) the LQAP; 4) organization and personnel summary; and 5)
QA/QC personnel interactions. The laboratory team should include the project manager,
the analysis team, the responsible QAJQC person, or Quality Assurance Officer (QAO), and
the responsible manager or director of the laboratory section. The meeting should be held
informally allowing for introductions and for the auditor to get to know each person on the
laboratory team. The meeting should last no more than two hours. The schedule for the
laboratory tour should be established and a time for the post-facility audit meeting should be.
agreed upon.
6.2.1 Analytical Specification Discussions
The first important item to be discussed at the pre-fadility audit meeting is the analytical
specification. The laboratory and the auditor should clarify each detail and step of the
analytical specification item by item. The analytical specification should contain any and all
special precautions to be taken during the analysis of the project samples. The auditor and
chemists may discuss refinements to the analytical specifications necessitated by variations
in analytical instrumentation or sample preparation, extraction or clean-up equipment. Any
concerns about sample preparation, clean-up, extraction and analysis should be discussed,
and if not specifically addressed in the analytical specification, the auditor should clarify
how to handle non-routine samples while staying within the specification. Because an
analytical specification can not cover every variable, the RFP should require the laboratory
to communicate all non-routine problems to the QAM. The QAM will decide what action
should be taken based on the Data Quality Objectives of the project. All analytical
refinements/agreements should fall within the scope of the contract and analytical
specification. Variations in instrumentation and equipment are allowed but the final sample
analytical data should meet the requirements of the analytical specification.
During the meeting, the auditor will review the QC criteria specified in the analytical
specification. The laboratory analytical team should understand the criteria, and the
subsequent corrective action that are necessary when criteria are not met. The penalties, if
any, for not performing corrective action should be discussed and understood.
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All other evidentiary, technical and non-technical laboratory SOPs that will be used to
support the performance of the analytical specification should be identified. For additional
guidance on laboratory SOPs, refer to Region I Laboratory Pre-Oualiflcatjon Standard
Operating Procedure , Section 6.3.
6.2.2 Quallty Assurance Practices
The next important item to be discussed in the pre-fadilicy audit meeting is the quality
assurance practices of the laboratory. The following are general quality assurance practices
adhered to by the laboratory which the auditor should check to ensure that the laboratory
does in fact have a quality assurance program.
The laboratory Quality Assurance Officer (QAO) should be part of the laboratory
organizational chart reporting only to the most senior management level. The QAO should
be independent of the analytical production laboratory. The QAO should periodically
introduce blind performance evaluation (PE) samples into each separate laboratory for
analysis. Double blind PE samples can be brought in from outside sources in such a
manner as to also test the entire laboratory system including sample logging, tracking,
preparation, analysis and data reporting. If internal double blind or single blind PE samples
are used, the nominal values or aczepcance ranges for the blind PE samples and the
laboratory results should be posted for all laboratory employees to see how they performed.
The QAO should document any corrective action necessary due to poor performance on the
PE samples. The QAO should also maintain control charts for each type of routine analysis
QC sample spiking results. The results of precision and accuracy measurements from
spiking studies make up the control charts. These control charts should be sufficiently
detailed to track at least six months of QC data and should be available to the U.S. EPA or
any client needing proof of laboratory performance.
The QAO should be the final reviewer of all QC data and associated sample data that is
approved by the laboratory manager for final release. Evidence of QAO approval of final
QC data should be evident.
6.2.3 The Laboratory Quality Assurance Plan
Prior to the audit, the auditor should examine the Laboratory Quality Assurance Plan which
was received as part of the pre-qualification deliverables. The LQAP should contain the
quality control requirements, including procedures for ensuring precision, accuracy,
representativeness, and completeness. The precision and accuracy criteria should be stated
for each set of analyses that will be performed. The representativeness and completeness of
data may be stated as goals or in an explanatory narrative as to how the laboratory wifi
ensure representativeness and completeness. The LQAP presented during pre-qualification is
usually not a site- or project-specific document. Certain projects may require special QC
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according to the analytical specification or method. If special QC criteria are required by
the project, the laboratory may need to produce an addendum to the LQAP that states
specific QC criteria and corrective actions to be taken if the criteria are not met for the
project.
The LQAP should address the following elements related to QA and QC:
• Personnel - duties of QA personnel
• Facilities and equipment
• Operation of instruments
• Documentation of QC criteria requirement in all procedures
• Preventive ni intenance
• Reliability of data
• Data self-validation
• Feedback and corrective action
• QA/QC self-inspection
For additional guidance, refer to Region I Laboratory Pre-Oualiflcation Standard Operating
Procedure , Section 6.1.
The LQAP should detail both general laboratory procedures used as well as specific
practices that will be used for the project. The LQAP should be a current and controlled
document that is periodically reviewed and updated, when necessary or according to a pre-
determined schedule, by approved and qualified personnel. Outdated portions should be
removed and archived for historical reference.
Each analytical method and analytical specification has QC criteria requirements such as
surrogate recovery spikes, matrix spikes, laboratory fortified blanks criteria, etc. These
elements should be documented in each analytical method and also be incorporated into the
LQAP by reference. The auditor should e amine those elements that relate to the project
analytical specification being audited as well as any other elements that directly control the
quality of the data produced on the specific sample analyzed. The LQAP should encompass
all QC criteria associated with all aspects of the laboratory system. During the facility audit,
the auditor should check specific items in the LQAP which relate to the analytical
specification such as standards preparation or calibration sequences, to ensure that the
laboratory follows the LQAP.
6.2.4 Organization and Personnel SllmTrniry
Prior to the audit, the auditor should review the organization of the laboratory and
individual resumes of key personnel. When the audit is scheduled, the auditor should
identify the key personnel who should attend the initial pre-fadility audit meeting. At the
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meeting, the auditor should confirm that key personnel are qualified as stated in the pre-
qualification submittals. Key personnel should be asked to sign an attendance list. The
auditor should document all issues discussed during this meeting. Any key personnel not in
attendance in the meeting should be contacted and should be employed at the time of the
audit and during the ftitute analysis. If qualified personnel are not in attendance or are not
employed at the time of the meeting and during the analysis, the auditor may decide to
suspend the audit and determine whether the laboratory is not, or no longer, technically-
qualified. The analytical team should meet the analytical specification requirements as
previously documented in the pre-qualification submittals. Any changes in the analytical
team should be documented and personnel replacing the original personnel should meet or
exceed the requirements of the project specifications. A laboratory personnel checklist
should be used to determine if the correct team is in place (Checklist IX).
6.2.5 Technical Communications
Discussions with project personnel that reflect uncertainty as to the understanding of the
project should be noted and clarified. The meeting should be amicable, and the auditor
should establish avenues of communication between the analytical team, laboratory project
m niger and the field sampling contractor. The lines of communication should be clearly
defined for the field samplers and laboratory sample receipt personnel or the laboratory
project manager. Communication requirements between the field sampling contractor lead
chemist/project chemist and the laboratory project manager should be identified during the
pre-faciity audit meeting. Any problems, logistical or technical, should be communicated
between the field sampling contractor and the laboratory in a timely manner to prevent any
loss in sample integrity.
Any potential changes in scope (#‘s of samples, schedule, turnaround time, or matrix
differences) should be discussed at this initial, pre-facility audit meeting to determine how
they will be resolved. If project schedules change, the protocol for handling unexpected
Circumstances is established by the auditor and noted in the audit report.
6.3 Post-award Pre-fadility Audit Meeting
A post-award audit is performed after a laboratory has been awarded a contract. The post-
award audit is performed to verify that a laboratory is adhering to the analytical
specification andlor has implemented required corrective actions noted during evaluation of
the pre-qualification submittais or during a pre-award audit. It may also be performed to
assess laboratory capacity and to interview key personnel.
The post-award pre-facility audit meeting is similar to the pre-award pre-faciity audit
meeting in that the analytical specification, quality assurance practices, the LQAP,
organization and personnel summary and QAIQC personnel interactions may be all
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discussed. This discussion is to ensure that the laboratory is adhering to the analytical
specification and has sufficient capacity to handle projected work. Since post-award audits
may be performed to verily that corrective actions have been implemented, the laboratory
should describe all required corrective actions that have been implemented. If personnel are
the focus of the audit, the field sampling contractor should notify the laboratory that certain
key personnel should attend the meeting. Key personnel should provide resumes to the field
sampling contractor at this time.
Whether the post-award pre-facility audit meeting is to discuss the performance of the
analytical specification, corrective action responses, general requirements, or capacity,
similar rules apply as with the pre-award pre-fadility audit meeting. The auditor should
notify the laboratory in writing prior to the audit as to the reason and the purpose of the
audit.
6.4 Problem Resolution Pre-Fadility Audit Meeting
The problem resolution audit is usually triggered by a poor performing, non-compliant
laboratoiy. lii an effort to resolve a problem, several discussions should take place
between the QAM and the laboratory before a problem resolution audit is scheduled. The
problem resolution pre-facility audit meeting focusses on the resolution of specific
deficiencies. Key personnel responsible for the non-compliance may be the only laboratory
personnel present at the meeting and should explain any technical analytical problems,
repeated failure to meet QC criteria, failure to meet detection limit requirements, lateness of
data or other non-compliant deliverables.
The entire problem resolution audit may consist of only a pre-facility audit meeting. A
facility audit may not be necessary if the laboratory instrumentation system is compliant.
Also, in the case of capacity problems, lateness of data or other clerical deliverable issues,
a facility audit may not necessary.
The auditor or QAM should notify the laboratory in writing prior to the audit as to the
focus and the reasons for the audit. All other pre-award discussions and attendance
requirements may also apply to the problem resolution pre-facility audit meeting.
Resolutions for corrective actions should be agreed upon and documented. A timeframe for
implementation should also be determined and the effectiveness of the corrective action
should be monitored by both the laboratory and the field sampling contractor.
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6.5 Laboratory Facility Audit
During the task of auditing a laboratory for any analytical specification or method, there are
several laboratory areas and functions common to any type of analysis that should be
ex2mined. The procedures listed in Section 6.0 for auditing include the following common
areas:
• Sample receipt, log-in, storage, and security (Checklist I)
• General facilities, including safety, glassware cleaning, and laboratory waste disposal
(Checklist 11)
• Sample preparation (Checklist III)
• Standards preparation and storage (Checklist IV)
• Sample analysis and instrumentation, including instniment performance, calibration,
sample analysis, and instniment maintenance (Checklist V)
Checklists 111 to V are specific to organic analyses but may be adapted to inorganic and
other types of analyses. The analytical laboratory performs the specified protocol/method
or analytical specification using instrumentation and the physical facility. The auditor
should check every detail described in Sections 6.5.1 through 6.5.5. The auditor should
also examine the ancillary analysis functions such as:
• Data handling and review, including electronic data management practices and data
deliverable archiving
• Data verification and technical review of data
• Quality assurance practices, including implementation of corrective action (CA) and
effectiveness of CA
• Adherence to NEIC evidenxiaxy guidelines and correct documentation of data
These items are very important to the auditor’s overall assessment of the orgar1i7 ton In
determining the effectiveness of the Laboratory’s quality assurance policies and the level of
technical exnertise of key personnel. The following questions should be asked: How does
the laboratory review the data prior to releasing the data? Or who is responsible for the
data review, internal data validation, data release and possible fumre third-party validation
questions or the resulting corrective actions? (QAO or Laboratory Manager). These
questions and others should be answered as part of the audit. Ability to produce valid,
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defensible data is not limited to equipment and technical expertise alone. A proven and
working QAJQC program is essential in assuring that the laboratory can produce valid data.
The auditor will audit these iten:Is during the pre-facility audit meeting, and will verify the
existence of a dynamic QA/QC program during the laboratory facility tour. Data handling
and review audit checks are described in Section 6.3.6. Audit details for quality assurance
practices were discussed in Sections 6.2.2 through 6.2.4, and are amplified in Section
6.3.7.
6.5.1 Sample Receipt, Log-In, Storage, and Security Areas
The audit of the sample receipt, storage and security areas should encompass all sample
types and include items such as; area security, the presence of appropriate SOPs, sample
custodians (hours and person) and back-up sample custodians, ventilation, safety, sample
log-in, recordkeeping, laboratory chain of custody, sample checks (temperature and
preservation), etc. The sample receipt area should have limited access, should be secure at
all times and should not be left unattended without being locked. Laboratory security
should be investigated by the auditor and noted on Checklist I. The entire laboratory,
offices, data management and support areas (glassware/chemical storage) should be secure.
Pertinent SOPs should be available and all paperwork should be neat, legible and in order.
SOPs such as sample custody, sample labeling and marking, sample tracking, sample
storage, sample log-in, sample integrity, and sample disposal should be available in the
sample receipt area. The status of any sample should be accessible at any time. The
temperature in storage refrigerators should be monitored and corrective action SOPs posted
for temperature excursions. Checklist I contains the checklists to be used by the auditor to
document the findings in the Sample Receipt, Storage, and Security Areas.
6.5.2 General Facilities
The general laboratory facilities should be examined during the laboratory tour to determine
if, overall, the laboratory is kept clean, has adequate space for each worker, is safe for
work, and constructed of materials applicable to their function. All the laboratory facilities
should be spotless, uncrowded, environmentally safe, free of safety hazards and constructed
for long lasting use. Checklist II contains a checklist to document for this purpose.
All areas of the laboratory should have adequate safety apparatus including fire
extinguishers, fire blankets, neutralization kits, spill control pillows and related apparatus.
Signs for each should be visible as well as fire exit signs and emergency routes to safety.
A site safety plan should be accessible by visitors and personnel at all times.
Disposal practices of analysis-related wastes should be checked by the auditor, noting any
effluent permits and laboratory waste disposal SOPs. The auditor should also check
whether or not the facility is in compliance with federal, state, and local waste storage and
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disposal regulations, as documented by notices of violation, notices of deficiency, or other
agency correspondence.
The auditor should confirm that project samples are held for the period of time required and
that they are disposed of properly.
Storage areas for chemicals, sample containers, and field-related equipment should be
checked. These areas should be lit, safe, and have good ventilation. Chemicals should be
stored in the proper cabinets to protect the chemist and to ensure chemical integrity.
Storage areas for data (electronic and hard copy) should be inspected to determine if data
integrity may be compromised. These areas should be environmentally stable, with
controlled temperati.ire and humidity, and should be secure.
6.5.3 Organic Sample Preparation Areas
Organic preparation areas, inorganic preparation areas, wet chemical analysis areas have
some common elements, but their individual nature requires separate audits and checklists.
Refer to Attachment A for specific inorganic and wet chemistry checklists and auditing
guidance.
The preparation and analysis of volatile organic samples should be strictly separated from
semivolatile/pesticide (extractable) preparation and analysis areas due to cross contamination
of extraction solvents. The checklists in Checklist III identify items to be used for
documentation of auditing laboratory preparation areas.
I Volatile organic preparation areas include both water and soillsolid samples. The areaS
should be very clean and have adequate venting with either fume hoods or smaller
ultra-clean vented enclosures similar to those used in bacterial.analysis. The
preparation rooms should be on separate ventilation systems from all other rooms.
The VOA prep rooms should have refrigerators for short-term sample storage and
storage in separate refrigeration units of calibration standards, surrogates standards,
matrix spike standards.
• Semivolatile/pesticide/PCB prep ration areas include liquid/liquid extraction areas,
separatory funnel extraction areas, sonicator hoods, soxhlet extraction areas, and
extract concentrator areas. The areas should be vented with adequate hood space,
have numerous glassware apparatus racks and have adequate solvent storage facility.
Solvent storage in separately vented safety cabinets is required. The glassware
cleaning apparatus may be in this area or may be in its own separate area. A gel
permeation chromatography (GPC) apparatus may also be present in this area and
should be in good order, clean and uncontaminated. Evidence of the ability to
perform florisil clean-ups, alumina clean-ups, sulfur clean-ups, or any additional
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required clean-up s should be visible. All of the above items should be documented on
the checklists.
• Key factors in the general auditing of organic preparation areas are cleanliness of the
work space, ventilation and hooded areas, storage and cleanliness of glassware,
reagent con ol, and storage and dating of solvents and standards.
• Sample weights are critical to sample integrity, and therefore, balances should be
accurate. Monthly calibration with Class “S” weights should be performed and
•logged. Routine m2intenance of balances should be performed and recorded.
• Key factors in auditing organic preparation paperwork are the presence of SOPs,
preparation logs, analysis run logs and standard logs in accordance with NEIC
guidelines. All the logs should be up-to-date and signed by the chemist and
supervisor. All logs should be stored away from the chemical storage areas and actual
preparation benches.
6.5.4 Standards Preparation and Storage
Standards should be traceable to a verified and validated source. Standards can be procured
from U.S. EPA approved sources with accompanying documentation of purity studies. All
standards documentation and purity studies should be archived by the laboratory for
historical reference. The purity studies should be performed on the same numbered lots of
standards currently used by the laboratory. The auditor should check that the purity studies
correspond to standards being used.
Standards for all organic analysis fractions (VOA, BNA, Pest) should be prepared and
stored in a mpnner to ensure their integrity over a specified and controlled period of time.
Standards, including calibration standards, internal standards, surrogates, and matrix spike
standards, should be protected from cross-cont miriation, evaporation or any other action or
operation that would otherwise alter the ultimate concentration or components. For this
reason, primary standards cannot be used routinely. A secondary standard, made from the
primary standard, is to be used on a routine basis. Whenever the primary standard is used,
care should be taken by the chemist to use only what is needed and mark the standard’s vial
to show the actual level of fluid left in the standard. At the same time, the analyst should
enter a notation in the preparation log to show that the standard was used, on a specific
date, and also note the volume of the remaining standard. Standards that have lost volume
or evaporated since their last use should be discarded.
Standards should be stored in an environment that protects their integrity. Normally
refrigeration is used to protect standards integrity. There are some chemicals that require
freezing to prevent sample los . Standards are usually individual neat compounds or
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mixtures of neat compounds, packaged in very small volumes. Standards require very
exacting procedures for weighing and aliquoting to produce a primary standard.
The auditor should check on the standard storage, standard labeling, standard use logs and
the age of each standard: If any of the above parameters are outside good laboratory
practice guidelines, then the auditor should note that fact on the checklists and discuss this
item at the post-facility audit meeting. This is an area where corrective action is important
and should be enforced.
Worksheets for standards preparation area audit and for documenting the findings of the
audit in the sample storage areas are provides as Checklist IV.
6.5.5 Sample Analyses and Instrumentation
The accurate analysis of environmental samples by the tuned and calibrated instrumentation
is dependent upon; the condition of the sample and matrix or sample extract, sample
preparation technique, and the overall integrity of the sampling program that produced the
sample. The auditing of the sample analysis areas should be performed after the auditing of
the sample receipt, sample preparation, and sample clean-up areas. The audit of
instrumentation and analysis areas should be performed by persons that are familiar with the
instruments, how the instruments operate, and what causes instruments to operate
improperly. The auditor should have a pre-approved (by the QAM) standard checklist that
follows the method or pre-qualification analytical specification to verify adherence to the
analytical specification.
This portion of the audit encompasses instrument performance, calibration, sample analysis,
and instrument maintenance. This audit SOP contains checklists for organic sample analysis
and instrumentation only; the procedure may, however, be adapted to other analytical
protocols. Refer to Attachment A for specific inorganic and wet chemistry checklists and
auditing guidance. Checklists to document the VOA and BNA sample analysis and
instrumentation portion of the audit are provided as Checklist V. Checklist VI may be used
for documenting the audit of GC extractables sample analysis and instrumentation.
6.5.5.1 Instrument PerformanceS
The analysis of environmental samples for organic constituents has been traditionally
performed using gas chroniatographs with various detectors, gas chromatograph/mass
spectrometers and, in some cases, high performance liquid chromatograpbs. In all cases,
the analytical instruments should be checked to determine if they are performing properly.
The first check of the gas chromatograph is to determine if the operating conditions are
optimized. Those conditions, as stated in CLP SOW OLMO1.9 D-39 Pest are an example
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of setting instrument conditions. Chrotnatographic performance is checked by determining
if the target analytes are eluting properly in terms of sequence and resolution. For
example, during a pesticide/PCB initial calibration sequence, (OLMO1.9 D-42), a
resolution check mixture is used to inspect the resolution of peaks on both COlllmn . DDT
and endrin breakdown are measured in the performance evaluation mixtures to determine
column performance. Absolute retention times for single component compounds are also
checked. These elements are part of the initial sequence as well as part of the calibration
sequence. Total instrument performance is measured by the resolution check mixtures,
breakdown characteristics and retention time windows. The auditor should review records
for documenting column resolution and performance.
GCIMS instruments use tuning as a measure of instrument performance. A tuning
compound, such as DFJ’PP or BFB, is analyzed to confirm accurate resolution by the
mass spectrometer within a specified AMU range, correct ion abundance criteria, and
specified peak shape covering only one AMtJ. Tuning criteria should be met prior to
analysis of standards, blanks or samples. Each analytical instrument, no matter what the
type (organic or inorganic analysis), should have standard procedures to check how well
the instrument is performing. Acceptance criteria as provided in the analytical
specification or method should be adhered to and corrective action implemented when
limits are exceeded. The auditor should review records for evidence of corrective action.
6.5.5.2 Calibration
Analytical instruments are calibrated using multiple concentration standards. The
standards can be mixtures of many components or of only a few components.
Calibrations for volatile and semivolatile fractions are generally performed using five
point calibrations whereas pesticides, PCBs, herbicides, and other extractable organics
may use only three calibration points or other means of measuring calibration. Inorganic
ins uments may use two or more standards.
The analytical specification or method being performed by the laboratory should be
reviewed by the auditor to check the step-wise process of tuning, calibration, and other
instrument performance parameters. The laboratory’s documentation of tuning,
instrument performance, calibradon , etc. should be evident in the run logs for each
instrument. Each of these items should be checked and documented by the auditor.
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6.5.5.3 Instrument Documentation and Usage
Instrumentation and proper analysis rely on such items as instrument maintenance,
instrument type and configuration, instrument accessories, and quality assurance and
quality control of the analysis. The analytical specifications, methods and SOW’s detail
the method QA/QC required. The auditor should check each of the individual steps of the
analysis and related QC as written in the laboratory SOP and document what is being
performed in the laboratory. The auditor should also check the documentation produced
for each of these analytical steps. The instrument logs, and data output logs should
conform with the requirements of the laboratory SOP and adhere to NEIC evidentiary
guidance.
Each instrument should have a run-log kept in the vicinity of the instrument. The run log
should be kept up to date and signed by the instrument operator and countersigned
regularly (within a few days of entry) by the section supervisor.
The auditor should be familiar enough with the instrumentation to recognize “out of
control” situations for particular instruments and how “out of control” situations should be
documented in the run logs. The notations in the run logs should be obvious and identify
to any observer both “out of control” situations and “in control” situations. The run logs
should chronicle all instrument performance measures such as calibration, continuing
calibration, QC samples, blanks, and performance evaluation (PE) samples. Any
corrective actions by the laboratory personnel should also be noted on the run logs and a
report written by the QA officer or the laboratory supervisor.
The laboratory’s initiation of corrective actions, and types and frequencies of problems
addressed, should be audited. The checklists in Section 9.0 document these items for
organic analysis.
6.5.5.4 Iustrwnent Maintenance
In order to keep an instrument operating properly, all instruments require m2intenance.
Maintenance can be categorized as daily maintenance or scheduled preventive maintenance
(PM). Daily maintenance shculd b e recorded in a log. Preventive maintenance may be
performed by a technician in the laboratory and involves changing certain parts and/or
checking alignments and electronic measurements. It may be performed as part of a
maintenance contract with the instiiimenx manufacturer. In this case, the manufacturer
comes on a schedule and performs the required adjusunents and checks. Either type of
maintenance is acceptable but both should be recorded in a log. A report of any out-of-
specilication repair(s) made should be kept in the laboratory.
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Daily maintenance and scheduled preventive maintenance usually will prevent
breakdowns. If breakdowns do occur, then repair of the instrument should be recorded in
a repair log as well as the maintenance log. The logs should be readily available and the
auditor should physically examine these logs to determine if required maintenance is being
performed. All logs and documentation should be signed and dated by the instrument
operators and the supervisor of the laboratory. Note that the instrument should be re-tuned
and re-calibrated before sample analysis can be continued.
6.5.5.5 Auditing of Organic SOPS
There are numerous items to be evaluated in each area audited. Detailed questions on
CC, CC/MS (VOA) and CC/MS (BNA) are listed in Checklists V and VI. Laboratory
Standard Operating Procedures for each area should be available in the appropriate
laboratory area and these procedures should be adhered to. The SOP adherence is a
common question the auditor may pose to all analysts. The auditor should document the
existence of quality control checks for either CC or CC/MS.
6.5.5.6 GC Extractable Analysis
Organic extractable analysis by gas chromatography has similar characteristics to the
CC/MS area but the instrumentation, sample preparation, sample clean-ups and analysis
parameters are quite different. Checklist VI provides checklists for the auditor to use in
the evaluation of CC analysis and associated quality control procedures. These checklists
are divided into similar groupings as for GCIMS with the addition of aluniiiia equivalency
checks, florisil column checks, institiment performance checks, and quality control
requirements.
6.5.6 Data Handling and Review
Data produced in the laboratory should be checked first by the analyst to determine if the
particular sample or sample run meets QC criteria. Other items such as; low percent solids
determinations, results outside the range of the calibration curve, poor peak resolution, poor
surrogate recoveries, and poor reproducibility, can cause the analyst to investigate the
analytical system to determine if corrective action is necessary. Sample data and QC data
calculated by the analyst or by the computer system should be spot-checked by a second
person or supervisor prior to final input into the laboratory information management system
(LIMS). The second check allows for timely corrective action measures to be implemented.
The laboratory should document and define data review and the approval chain of command
as part of a written data review SOP. The auditor should look for the proof (a signature or
initials) of secondary review of data throughout the analytical system. Signatures (or
initials) of supervisory approval should be evident on all laboratory output. The auditor
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should investigate the computerized data systems to determine the adequacy of data
processing software and data processing equipment to handle a large workload. If the
system is inadequate, then the laboratory should find a way to increase the capacity or the
samples should go to another laboratory.
Checklist VU provides a mechanism for documenting this portion of the audit.
6.5.7 Quality Assurance Practices
Quality assurance practices that require auditing have been described previously in Sections
6.2.2 through 6.2.4. Most of this documentation should have been reviewed prior to arrival
at the facility and during the pre-fadiity audit meeting. During the laboratory tour, the
auditor will want to verify that written procedures are being followed. Checklist V is
provided to document the quality assurance practices audit components.
6.5.8 Data Verification and Completeness Check
Complete analytical data packages should go through a final review process called data
verification and completeness check. The completed package should be examined against a
checklist that is established by the laboratory and documented in the LQAP and a laboratory
SOP on data verification and completeness. The verification and completeness check may
be performed by a dedicated reviewer or a person intimately familiar with the analytical
instrumentation. The review should be signed, either on the checklist or on the data
package.
The au litor should look for evidence of data verification and completeness check by
qualified personnel on a data package that the laboratory is preparing to send out. The
auditor should also check the qualifications of the reviewer.
6.6 Post-Facility Audit Meeting
A post-facility audit meeting, or debriefing, is held at the end of a pre-award, post-award or
problem resolution audit to discuss audit findings, answer questions, identify corrective
actions that are needed, and set a schedule for implementation of the corrective actions.
6.6.1 Pre-Award Post-Facility Audit Meeting
After the auditor has examined each section of the laboratory relating to, or associated with,
the analytical specification or method and analysis of samples, a post-facility audit meeting
should be conducted to discuss any deficiencies found.
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Deficiencies should be resolved at this meeting to keep the project on schedule. The
laboratory should be given the opportunity to respond to all deficiencies, and to correct the
problem(s). A schedule for agreed-upon corrective actions should give the laboratory a
reasonable amount of time to correct any deficiencies while also accommodating the project
schedule. If a laboratory refuses to implement corrective actions, the auditor may
determine that the laboratory is not technically-qualified to perform the analytical
specification. The final decision to disqualify a laboratory from contract consideration
should be made by the QAM at the earliest possible time. The laboratory should not be
disqualified without due notification and the chance to respond. All corrective actions should
be documented by the laboratory to the satisfaction of the auditor and the field sampling
contractor QAM before the contract is awarded.
In most cases, deficiencies are minor and can be corrected by simple changes in the
laboratory’s mode of operation. There will be cases where the laboratory cannot
immediately produce control charts or compliant performance evaluation data. In those
cases, it is left to the discretion of the auditor and the QAM to determine the required
corrective action.
The laboratory may suggest improved techniques for the analysis of the project samples.
The auditor may agree to those changes if they do not modify the technical analytical
specification or method, or compromise data quality, detection limits, or turnaround time.
Proposed changes to the analytical specification should not routinely occur at this time
because the laboratory was given the opportunity during the pre-qualification phase to
propose alternate methods. Any improvements should be agreed upon by the QAM and
should be proven to benefit the analysis.
The post-facility audit meeting should conclude with resolution of all deficiencies, corrective
action schedules, and agreement on answers to all questions on both sides. If agreements
have to be postponed to a later date, due to a resultant corrective action measure, then this
fact should be documented and a date for final resolution should be set.
6.6.2 Post-AwaEd Post-Facility Audit Meeting
A post-award post-facility audit meeting is held to discuss deficiencies and develop
corrective actions. All deficiencies found during a post-award audit should be addressed
immediately by the laboratory to ensure that the field sampling contractor can meet project
schedules. The auditor will set the schedule for corrective actions during the post-facility
audit meeting. If deficiencies are minor the corrective action may be performed quickly to
meet project schedules. If the deficiencies are potentially recurrent, the auditor may require
a monitoring and reporting program to ensure effectiveness of corrective action (see Section
6.6.3.).
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If laboratory capacity is a problem, then the laboratory’s analytical schedule should be
investigated thoroughly to ensure that the laboratory has the capacity to produce data during
the project period. The capacity of the laboratory may not be large enough and alternative
laboratory services should be obtained by the field sampling contractor to meet the
analytical demand. The laboratory capacity is a pre-qualification review item that should
have been checked before the contract award. A capacity problem may be resolved by
rescheduling of priorities within the laboratory and flexibility in the project schedule.
If the laboratory is resistant to ccrrecting non-compliances, the auditor should get direction
from the QAM and the field sampling contractor project mpnager as to what action should
be taken against the laboratory. In all cases, the laboratory should be given a reasonable
amount of time to resolve minor deficiencies, so long as project schedules are met.
If the laboratory is unable to produce data that meets EPA Data Quality Objectives, then
action against the laboratory should take place as soon as possible with concurrence with the
QAM or field sampling contractors’ program manager. Action against a laboratory may
result in serious schedule problems, and the field sampling contractor may be required to
obtain alternate analytical services.
6.6.3 Problem Resolution Post Audit Meeting
The purpose of the problem resolution audit is to achieve a resolution for a technical or
non-technical problem that has impacted data quality and usability. A problem resolution
audit should be focussed and should result in corrective actions that will take place
immediately or shortly after the audit. These corrective actions should be monitored over
time to ensure that corrective actions are effective.
The post audit meeting should be used to summarize the following: 1) the source of the
problem 2) laboratory and auditor concurrence on problem resolution 3) development of a
schedule for implementation of corrective actions and demonstration of effectiveness.
During this meeting, the laboratory should explain such things as why holding times,
detection limits and/or quality control criteria were not met and should present remedial
approaches. Problems such as equipment failures, poor instrument performance or poor
instniment design may require long-term corrective actions. If the findings of the problem
resolution audit indicate that there is no timely resolution to the problem and the laboratory
is unable to produce data that meets the data quality objectives, then action against the
laboratory may be required. If action is taken, a cont agency plan for sample analysis in
progress should be developed by the field sampling contractor.
The effectiveness of the corrective action may be monitored internally by the laboratory
Quality Assurance Officer which may include daily, weekly or monthly progress reports to
the field sampling contractor depending on project objectives. The monitoring program
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Revision Number: I
ctu CKLLST I Date: 15 March 1994
SAMPLE RECEIPT, STORAGE, AND SECURITY AREAS Page 30 of 77
(Continued)
LAB
CODE:
iTEM YES NO COMMENT
1.20. If a sample custodian available 24 hours a day -
Monday through Friday?
1.21. Is a sample custodian available on Saturday and
Sunday?
1.22. Is there evidence of a secondary review of all
documents and logbooks by someone other than
the sample custodian (person generating the
documents)?
1.23. Is the log-in process linked by computer to the
main laboratory facility through a UMS?
Note additional comments below:
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Type of Audit: Pre-awazd _Posr-award_Problein Reso1ucon _
CHECKLIST II
GENERAL FACILnLiS
L B
CODE:
rrEM YES NO COMMENT
11.1. Is the laboratory maintained in a clean and
organized manner?
11.2. Does the laboratory appear to have adequate
work space (6 linear feet of unencumbered bench
top per analyst)?
11.3. Are laboratory benches and flume hoods made of
suitable impervious materials or are they covered
with absorbent materials?
11.4. Are there adequate fire extinguishers, fire
blankets, sprinklers available in case of fire?
Are chemical spill pillows and spill kits readily
available?
11.6. Are there signs showing emergency equipment
and emergency exits?
11.7. Are there adequate hoods and are they
functional?
11.8. Is there adequate lighting?
11.9. Is there adequate ventilation?
11.10. Does the lab have an SOP for disposal of lab-
related waste?
Does each lab have separate waste drums for
each waste stream?
• Are records available of waste disposal and
past waste disposal practices?
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Region I Laboratory Audit SOP
Revision Number: I
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Type of Audit: Prc-award ____Post-award_ •• ..3roblem Resolution____
CHECKLIST V
SAMPLE ANALYSIS AND INSTRUMENTATION:
VOA & BNA
ITEM
GCIMS OPERATIONS AND MAINTENANCE
V.1. Are manufacturer’s operating manuals readily
available to the operator?
V.2. Does the laboratory purchase a service contract
for instruments?
V.3. Are extensive in-house replacement parts
available?
V.4. Does the laboratory perform regular preventive
maintenance on the instruments used?
V.5. Is a prepared schedule for maintenance of the
instruments available for inspections?
V.6. Is a permanent service record maintained in a
logbook?
V.7. Are the instruments properly vented or are
appropriate traps in place?
V.8. Have the instruments been modified in any way?
MAGNErIC TAPE STORAGE OF GC/MS ELECTRONIC
DATA
V.9. Is raw data, including quantitation output files
and libraries, archived on magnetic tape?
V.10. Is a log of the contents of the raw data magnetic
tapes available?
YES NO COMMENT
LAB
CODE:
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Revision Number: 1
Date: 15 March 1994
CHECKLIST V Page 39 of 77
SAMPLE ANALYSIS AND INSTRUMENTATION:
VOA & BNA
(Continued)
L B
CODE:
iTEM YES NO COMMEN’r
GCIMS VoIAnus 1) BNA ANALYSIS
V.11 Does the laboratory have the necessary
equipment to perform volatile organic analyses or
BNAs?
V.12 Can the laboratory document the use of three
separate calibration curves for volatile sample
analysis (water, low soil, medium soil)?
V.13 Are volatile holding blank results available for
inspection? (One per case)
V.14 Are VOA samples stored and analyzed in an area
isolated from the extraction area?
V.15 Does the laboratory have instrumentation
dedication to volatile analysis?
V.16 Is the MDL study for project-specific methods
available for review by the auditor?
V.17 Has the lab compared the calculated MDL with
the contract-required detection limits (CRQL)
required by the client?
V.18 Is the lab employing the method indicated
columnc?
V.19 Does the laboratory have an updated NBS or
other library?
V.20 Is sufficient dedicated glassware ot sample
containers to meet project needs?
V.21 Can verifications be made for column changes in
source cleaning?
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Revision Number: 1
Date: 15 March 1994
ct [ ECKLJST V Page 42 of 77
SAMPLE ANALYSIS AND INSTRUMENTATION:
VOA & BNA
(Continued)
LAB
CODE:
ni M YES NO COMMENT
V.40 Are control charts for calibration standards
maintained?
Note additional comments below:
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Type of Audit: Pre-award _____Post-award___Problem Resolution_____
CHECKLIST VI
SAMPLE ANALYSIS AND INSTRUMENTATION:
GC EXTRACTABLES
LAB
CODE:
YES NO COMMENT
GC, GCIMS OPERATION AND MAINTENANCE
VI. 1. Are manufacturer’s operating manuals readily
available to the operator?
VI.2. Does the laboratory purchase a service contract
for instruments used?
VI.3. Are extensive in-house replacement parts
available?
VI.4. Does the laboratory perform regular preventive
maintenance on the instruments?
VI.5. Is a prepared schedule for m2intenance of the
instruments available for inspections?
VI.6. Is a permanent service record maintained in a
logbook?
VI.7. Are the instruments properly vented or are
appropriate traps in place?
VI.8. Have the instruments been modified in any way?
ALUMINA EQuIv 1 uir cy CBECK
VL9. Is the percent recovery of all single component
pesticides greater or equal to 80% except for
endosulfansuifate which should be greater than or
equal to 60% and endrin aldehyde which should
not be recovered?
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CHECKLIST V I Daze: 15 March 1994
SAMPLE ANALYSIS AND INSTRUMENTATION: Page 44 of 77
GC EXTRACTABLES
(Conthiued)
LAB
CODE:
YES NO COMMEN’I
VI. 10 Has the laboratory- analyzed a diluted
tribomophenol standard to verif ’ its retention
time and noted its absence join the alumina
equivalency GC chromatograms?
INSTRUMENT PERFORMANCE CHECKS
VI. 11 Do the analysts perform and record column
resolution and tailing performance checks?
INSTRUMENT PERFoRMANCE CHECKS
VI. 12 Is the appropriate portion of the SOP available to
the analyst at the Pesticide analysis area?
VL13 Do the analysts record all GC injections in a
bound or serially numbered logbook?
VI.14 Are the GC injection logbooks completed in a
manner consistent with the laboratory’s SOP?
VI. 15 Is there evidence of a secondary review of all
documents and Iogbooks by someone other than
the person generating the documents?
INSTRUMENTATION
VI. 16 Does the laboratory have the MDL study for GC
method for review of the auditor?
VI.17 Does the calculated MDL meet the required
CRQL of the analytical specification?
VI.18 Is the laboratory employing the method indicated
GC detectors and coliimn c?
VL19 Have the instruments been modified in any way?
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Type of Audit: Pre-award ____Post-award Problem Rc.so!ution_ Region I Laboratoty Audit SOP
Revision Number: I
CHECKLIST VI Daze: 15 March 1994
SAMPLE ANALYSIS AND INSTRUMENTATION: Page 45 of 77
GC EXTRACTABLES
(Continued)
CODE:
YES NO COMMENT
V1.20 Can verifications be made for septum changes,
column changes detector maintenance?
SAMPLE ANALYSIS
VL21 Are laboratory specific SOPs developed for the
analytical method specification present in the
laboratory?
VI.22 Are all samples routinely analyzed within 40
days VSTR?
VI.23 Are blanks routinely run following the analysis of
a highly conr2min ted sample to assess carry
over?
VI.24 Are QC samples labeled and is a copy of the
labeling system available to each analyst?
VI.25 Does the GC laboratory have a separate
refrigerated storage area for PCBIpest samples?
Is this separate from standards storage?
VI.26 Are the analysts initials on the chromatograms
and grant? Are reports consistent with the run
log and traceable to the individual actually
performing the analysis?
VL27 Are control charts for calibration standards
maintained?
VI.28 Does the lab reanalyze samples when surrogates
are not within recovery limits?
VL29 Does the lab keep a record of retention time
studies in the area? Does the laboratory calculate
standard detention of three absolute retention
times for the retention time windows?
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Revision Number: I
CJiI CKLIST VI Date: 15 March 1994
SAMPLE ANALYSIS AND INSTRUMENTATION: of 77
GC EXTRACTABLES
(Conthiued)
LAB
CODE:
YES NO COMMENT
VL3O GC/ECD confirmation perfonned on evexy
sample, standard and blank?
Note additional comments below:
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Date: 15 March 1994
Page 47 of 77
Type of Audit: Ftc-award _Post -award_ProbIcui Resolution____
CUECKLIST VU
DATA HANDLING AND REVIEW
LAB
CODE:
ITEM YES NO
VII. 1 Was a written data review SOP available for review?
VII.2 Are data calculations spot-checked by a second person?
VIL3 Do records indicate that appropriate corrective action has
been taken when analytical results fail to meet QC criteria?
VII.4 Do supervisory personnel review the data and QC results
prior to submission?
VII.5 Is data verification per formed and recorded?
Is the person performing the data verification qualified? ______
Is there evidence of data verification in the final data
packages?
VII.6 Does the laboratory maintain adequate data processing
equipment and software for the electronic submission of
analytical results? (Diskette Deliverables)
Additional Comments:
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Daic: 15 Marth 1994
Page 48 of 77
Type of Audit: Pre-award _Post-award Problem ResoIu on____
CLu CKLIST V I II
QUALITY ASSURANCE PRACTICES
lAB
CODE:
ITEM YES NO
QuAlrry AsSURANCE OFF icER
Vfl1.1 Does the Laboratory Quality Assurance Officer report to senior
management levels?
Vffl.2 Can the Quality Assurance Officer document the analysis of blind
laboratory QA samples?
VUI.3 Does the Quality Assurance Office maintain records of laboratory
performance, such as precision and accuracy charts of laboratory
spikes?
QAO Comments:
LABORATORY QUALiTY ASSURANCE PLAN CHECKLIST
VHL4 Does the laboratory mpintain a project-specific Quality Assurance
Plan?
Vffl.5 Are outdated portions of the LQAP properly archived?
Vl]L6 Does the LQAP address the importanx elements of a QA program,
including the following?
a. Personnel?
b. Facilities and equipment?
c. Operation of instruments?
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Revision Number: 1
Ci{ECKLIST VU! Daze: 15 March 1994
QUALiTY ASSURANCE PRACTICES Page 49 of 77
(continued)
L B
CODE:
ITEM YES NO
d. Documentation of QC criteria requirement in procedures?
e. Preventive maintenance?
f. Reliability of data?
g. Data validation?
h. Feedback and corrective action?
1. QAJQC self-inspection
Quality Control Manual Comments:
ORGANIZATION ANI) PERSoNNEL SuMi u Y
(See Key Personnel List, Checklist IX)
VUL7 Do personnel assigned to this project have the appropriate
educational background to successfully accomplish the objectives
of the program?
V1IL8 Is the organiz:tion adequately staffed to meet project commitments
in a timely manner?
V [ LL9 Were all ke’, personnel available?
List those not available in the comments section.
Organi72tional & Personnel Comments:
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Revision Number: 1
CaECKLIST VIII Date: 15 March 1994
QUALiTY ASSURANCE PRACTICES 1’ e 50 of 77
(continued)
LAB
CODE:
iTEM YES NO
G LtL
VILL1O Do responses to the evaluator indicate that project and supervisory
personnel are aware of QA/QC and its applications to the project?
VIII. 11 Do project and supervisory personnel place positive emphasis on
QA/QC?
Vifi. 12 Have responses with respect to QAIQC aspects of the project been
open and direct?
VIII. 13 Has a cooperative attitude been displayed by all project and
supervisory personnel?
VIII. 14 Have corrective actions recommended during previous evaluations
been implemented? If not, provide details below.
Additional Comments:
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Date: 15 March 1994
Page 51 of77
Type of Audic: Pre-award ____Post-awaid_Problem Resolution____
CHECKLIST IX
LABORATORY PERSONNEL AND EQUIPMENT
I. Key Personnel List Lab Code
List the personnel assigned to the following functional
positions. -
POSITION
Q
UNQ
GCIMS Laboratory Manager
Name:
Requires BS chemistry/physical science + 3 yrs lab experience
including 1 year as a supervisor.
GC/MS Operator
ame:
Name:
Name:
Requires BS chemistry/physical science ÷ 1 yr GCIMS/DS
experience or 3 yrs GCIMS/DS experience.
GC/MS Spectral Interpretation Specialist
Name:
Requires BS in chemistry/physical science + a training course in
mass spectral interpretation + 2 yrs experience
GC Laboratory Supervisor
Name:
Requires BS in chemistry/physical science +3 yrs lab experience,
including 1 year as a supervisor.
Pesticide Residue Analyst Expert
Name:
,Name:
Requires BS in chemistry/physical science + 2 years experience in
oerating/maintaining Gcs and interpreting chrornatograms.
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Revision Number: I
CHECKLIST IX Date: 15 March 1994
LABORATORY PERSONNEL AND EQUIPMENT Page 52 of 77
(continued)
I. Key Personnel List Lab Code
List the personnel assigned to the following functional
positions. -
POSITION
Q
UNQ
Sample Preparation Laboratory Supervisor
Name:
Requires BS chemistry/physical science + 3 yrs lab experience,
including 1 year as supervisor.
Extract.ionlConcentration Expert
Name:
Name:
Requires High School diploma and a knowledge of general chemistry.
Backup Chemist
Name:
Requires BS chemistry/physical science + 1 yr lab experience in
GCTMS operation, MS interpretation, Extraction, and Pesticides
analysis.
Project Manager
(Responsible for overall aspects of U.S. EPA contract, Primary
contact to EPA HO)
Name:
Sample Custodian
(Responsible for receiving U.S. EPA samples)
Name:
NOTE:
Q - indicates that the individual is qualified for this position.
UNQ - indicates that the individual lacks the minimum qualifications for the position
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Type of Audit: Pie-award ____Post-award Prob1e n R so!ution____ Region I Laboratoiy Audit SOP
Revision Number: 1
CHECKLIST IX Date: 15 March 1994
LABORATORY PERSONNEL AND EQUIPMENT Page 53 of 77
(continued)
I. Key Personnel List Lab Code
List the personnel assigned to the following functional
positions.
POSITION
Q
IJNQ
Data Reporting and Delivery Officer
(Responsible for all aspects of data deliverables: organi7 tion,
packaging, copying, arid delivery)
Name:
Quality Assurance Officer
(Responsible for overseeing quality assurance aspects of the data)
Name:
-
NOTE:
Q - indicates thzt the individual is qualified for this position.
UNQ - indicates that the individual lacks the minimum qualific3LiotIs for the position
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Revision Number: I
CHECKLIST IX Date: 15 Mardi 1994
LABORATORY PERSONNEL AND EQUIPMENT Page 54 of 77
(conthiued)
LI. Sample Preparation Equipment Lab Code:
iTEM
ADEQ
INADEQ
Sonicator Manufacturer and Model Number:
GPC Manufacturer and Model Number:
Number of Continuous Liquid/Liquid Extractors Available:
tEl. Semi-Volatile Analysis GCIMS Lab Code:
Instrumentation
Lab Manufacturer Model Software! Date Installed
ID# Revision
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Type of Audit: Pre-award ____Post-award____Problem Resolution____ Region I Laboratory Audit SOP
Revision Number: I
ciu CKLJST J Date: 15 Maith 1994
LABORATORY PERSONNEL AND EQUIPMENT Pa’e 55 of 77
(continued)
IV. Volatile Analysis GCIMS Lab Code___
Instrumentation
Lab Manufacturer Model Software! Date Other
ID# Revision Installed Notations
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Revision Number: 1
Date: 15 March 1994
Page 56 of 77
ATTACHMENT A
EMSL Guidelines
1. Sample Preparation (Inorganic)
All inorganic distillations and extractio s are performed in the Inorganic Sample Preparation area. This portion of the laboratory
should be separate from the analytical areas and the work should be performed within properly functioning fume hoods. The
areas should be clean and appropriate for trace level work. A sample preparation person should be identified and they should
meet the education and experience requirements of the program. That person should be made available for discussions on the
procedures followed within the area. Current SOPs should be readily available within the area. These SOPs should include
sample preparation techniques, glassware washing, and standards preparation (if appropriate).
An auditor examines the sample preparation analyst’s logbooks or bench sheets for prcper records of each technique, including
dates carried out, solvents used, initial and final volumes and weights used. This can be performed by reviewing the paperwork
associated with the sample(s) that are being tracked through the laboratory. An example of a preparation bench sheet is shown
on page 58. The personnel are asked to demonstrate or discuss their preparation techniques. The procedures followed for the
area should be evaluated according to the items listed in the check list shown on pages 60 through 63 of this section. Overall,
the auditor should evaluate the procedures for adequate millimi7MiOn of sample conurniii, rion, appropriate sample transfer,
adequate spiking technique, adequate monitoring of digestion and distillation conditions, and appropriate documentation and
communication. Items specific to the preparation area that should be evaluated are:
The sinks for glassware washing should have a washing SOP posted near the sink, as well as having it in an SOP. Clean
glassware is vital to sample integrity, the auditor should also examine glassware storage facilities ensuring that glassware
stored away from possible areas of contln’inMion. If conr minarion was noted as a constant problem through previous
EMSL-LV data reviews or regional reviews, then improper cleaning of glassware may well be the problem.
If standards preparation is performed within this area, an SOP and a standards tracking, log should be available. An example
of a standards tracking log sheet is shown on page 59. The expiration dates on the standard solvents are checked, as are any
dates of opening that the preparation analyst may have marked on the bottles. It should be noted who prepares the various
standards. Some laboratories allow only the analysts to prepare standards, other laboratories allow the preparation staff to
prepare some of the standards. It is required by the contract that fresh standards be prepared daily for GFAA standards, as
they degrade quickly. ICP standards and other standards that are at higher concentrations may be stored longer. The
laboratory should have established procedures in place for standards holding times and verification of standards integrity over
time. The auditor, through observation and interviews, should evaluate the procedures used by the standards preparation
analyst(s). For example, are the laboratory personnel checking standards before use? Are they correctly labelling standards?
And are they using proper techniques when preparing the standards? Another source of error can be through the use of
automatic pipertes (e.g., Eppendorf). Routine calibrations of automatic pipettes should be performed and tracked.
Another very important item that should be examined by an auditor is the type of internal review employed by the laboratory.
Does the supervisor routinely review the documentation generated by the preparation area. Also, the type of training program
performed in this area for new personnel is important. Is there an effective corrective action procedure in place?
Accurate weights axe also vital to sample preparation, hence analytical balance calibrations (using class S weights) should be
routinely performed and logs kept for penisal by an auditor. Also the area where balances are housed is examined to be sure
there are no drafts in the area.
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Region I Laboratory Audit SOP
ATrACHMENT A Revision Number: 1
EMSL Guidelines Date: 15 March 1994
(continued) Page 57 o177
Lines of communication within the laboratory are of utmost importance. The auditor should establish how the standards and
sample preparation personnel communicate with the analysts. This is to en.sure that the analysts know, in a time(y rn nner,
when samples will be ready for analysis.
It is important to ensure that the calibration standards for the mercury analysis are prepared with the samples, since that is a
method requirement. Also, check and see if the pH of the samples are being checked and that information is being written on
the preparation log.
In preparing for an on-site evaluation of the Inorganic Sample Preparation area there are sonic common indicators found in data
audits and other monitoring information that would lead the on.site auditor to believe that there were problems in this area.
Some of those indicators are listed below and may help the student when preparing to evaluate this laboratory area:
• Frequent lateness of data and delays in preparation of samples may be the result of poor communication between sample
receipt and the preparation laboratory. Long delays in analysis after preparation may indicate poor communication and
coordination between the sample preparation and analysis areas.
• Chronic reporting of spikes and duplicates outside of criteria may be an indication of poor preparation and spiking
technique. Consistendy poor spike recoveries may also indicate a poorly prepared or out-of-date spiking standard.
• Chronic reporting of low level contamination in the preparation blanks may indicate poor glassware cleaning techniques,
poor sample transfer technique, or contaminated work areas.
• Deviations from laboratory procedures and program requirements and poor documentation of preparation information may
be an indication of a lack of understanding of the procedures, of poor training, and a lack of QA oversight.
Once the auditor is satisfied that all his or her questions arc answered in this area, they move on to the Inorganic Analysis areas.
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Region I Laboratozy Audit SOP
ATFACUMENT A Revision Number: 1
EMSL Guldellnei Date: 15 March 1994
(continued) Page 58 of 77
W.B. Goode LaboratoriesMetals Digestion Preparation Benchshect
Date: 8/5/91 Client: EPA
Method: ICP Case: 10000 SD-G: ?vfBCl23
Client Initial Final
Sample Sample pH Vol/Wt. Vol. Color Clarity Texture Artifacts
Blank NA iCY) ml 100 ml NA NA NA NA
LCS LCS NA lCd) nil 100 mi WA NA NA NA
W8! MBCJ23 < 2 100 nd 100 mi Colorless Clear NA NA
W8JS MBC1235 < 2 100 mid ICY) mid Colorless Clear NA NA
W82 MBCJ24 < 2 ICY) ml ZOO ml Colorless Clear NANA
W82d MBCJ24D < 2 iCY) ml ICY) ml Colorless Clear NA NA
Blank Blank NA 1.00 g lCd) ml NA NA NA NA
LCS LCS NA 1.00 g iCY) ml NA NA Sandy NO
P183 MBCJ2S NA 1.02 g 100 ml NA NA Sandyd
W83S MBCJ2SS NA 1.01 g 100 mid NA NA Sandy
None
P 184 MBCJ26 NA 1.04 g 100 ml NA NA Sandy
None
W84d MBCJ26D NA 1.03 g 100 ml NA NA Sandy
Digested by I. Baker Date 815/9 !
Received by M. Jones Date 317191 Reviewed by Date
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ATFAC1IMENT A
EMSL Guidelines
(cüiil lnued)
gion1 Laborawry Audit SOP
Revision Number: 1
Date: 15 March 1994
Page 59 of 77
ABC Laboratory, Inc.
Inorganic Standards Tracking Log
Notebook No. 910187 Cant. from Page .7... Notebook No. 910187 Cant. from Page j_
line
No.
Description
Supplier
Lot/Batch
No.
Received
Opened
Expires
Out of
Service
Recipient
Lab ID
No.
1
Co 10,000 ppm
Acme
C-2C0
26-JUL-91
29-JUL-91
30-JUL-92
.1. Smith
91018708
1
2
Cr 10,000 ppm
u
B-2CR
26-JUL-91
29-JUL.-91
30-JUL-92
J. Smith
91018708
1
3
Cu 10,000 ppm
B2-MD
26-JUL91
29-JUL-91
30-JUL-92
J. Smith
91018708
1
4
EPA ICV-].
0690
04-AUG-91
30-AUG-91
29-AUG-92
J. Smith
WBG123
5
EPA ICV2
0590
04-AUG-91
30-AUG-91
29-AUG-92
3. Smith
1480124
6
EPA ICV-3
1190
0390
04-AUG-91
04-AUG-91
30-AUG-91
30-AUG-91
29-AUG-92
29-AUG-92
3. Smith
3. Smith
WB0125
WBG126
Read and Understood By
Read and Understood By
Date Signed
Date Signed
Signed
Date Signed
Date
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Region I Laboraioty Audit SOP
ATTACHMENT A Rcvisio Number: 1
EMSL Gu1deUn Daze: 15 March 1994
(continued) Page 60 of 77
LABORATORY SYSTEMS AUDIT FORM
IV. Sample Prepa ntion for TCP, GFAA. and Hg
IV a. Facilities
ITEM YES/NO Comment
Is the sample preparanon laboratory
maintained in a clean and organized
manner that is appropriate for trace
level analysis?
2. Are the boods functional?
3. Is an adequate dzying oven available
with a temperature measurement device?
Is the temperature being monitored?
4. Is there an adequate amount of equipment
and glassware to prepare the required
volume of samples?
IV b Personnel
ITEM YES/NO
COMMENTS
Are sample preparation specialist
identified?
Name
Name
2. Do the persons identified meet the
education and experience requircmen ?
(High school diploma and college level
course in chemisuy and 1 yr experience
with microwave digestion, if microwave
technique used).
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Region I Laboratory Audit SOP
ATrACUMENT A Revision Number: I
EMSL Gu1deIIn Date: 15 March 1994
(continued) Page 61 of 77
LABORATORY SYSTEM AUDIT FORM
iv. Sample Preparation for ICP, GFAA. and Hg
Procedures ITEM YES/NO COMMENT
I. Are written SOPs dcvclopcd for preparañon of samples?
2. Do the SOPs meet the requirements for content and format? If no, see Attachment B.
3. Can it be documented that analyte-free water is available and used for the preparation of standards and blanks.
4. Is the conductivity of the analyte-free waier checked and documented in a logbook?
5. Are the analytical balances located away from drafts and areas subject to rapid temperanire change?
6. Have the balances been calibrated and checked within one year by a certified technician?
7. Are the analytical balances checked daily with the approptiale class S weights and the results recorded?
8. La there a documented procedure for quality, use, and inventomy of reagents?
9. Are spiking standards preparatior. and tineking logbooks maintained?
10. Can the laboratory document the traceability, purity, and procedure for the preparation of standards?
11. Are fresh analytical standards prepared at the frequency consistent with the lab sops?
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Region I Laboraroty Audit SOP
ATTACHMENT A Revision Numbcr I
EMSL Guldellnei Dale: 15 March 1994
(continued) Page 62 of 77
LABORATORY SYSTEMS AUDIT FORM
IV Sample Preparation for ICPI GFAA. and Hg
IV c. Procedures (continued )
ITEM YES/NO CO vQvfEZTr
12. Are reference standards properly labeled
with concennations, daze of
preparation, and the identity of the
person preparing the standard andfor is
a aeeabIe reference code number used?
13. Is work scheduled and arc employees
no fied of work in a systematic manner?
14. Dotheana1ystsrecordbcnchda jna
neat and accurate manner?
15. Is the pH of the samples checked and
recorded in the preparation
documentation?
16. Is there evidence of a secondaiy review
of all documenta and logbooks by someone
other than the person generating the
documents?
17. Are the standards stored separately from
sample digestazes?
18. Are the SOPs for glassware posted at the
cleaning stanons?
19. If microwave digestion is to be used, s
an adequate microwave oven (progrnmmahle
power settings up to 600 wa minimum)
available?
20. Are the appropriate portions of the SOPs
available to the laboratory stafi?
21. Does the SOP prescribe an adequate
amount of acid ueanncnt of the
g ssware?
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Region I Laboratory Audit SOP
ATrACHMENT A Revision Number 1
EMSL Guidelines Date: 15 March 1994
(continued) Page 63 of 77
LABORATORY SYSTEMS AUDIT FORM
IV. San,yle Preparation for ICP. GFAA. andj
fll.c. Procedures (continuedi
rIEM YES/NO COMMENT
22. Are p dures and docunien tion
performed in a manner consistent with
the laboratory SOPS?
23. Do the SOPs mcet the requirenien of the
SOW?
Observations:
IV d. Sample Preparation Problems Noted Since Last Visit (Audits, Customer
Comments )
Noted Problems:
ITEM YES/NO CO v1ENT
1. Are analysts and supervisory staff aware
of problems noted?
2. Has there been documented corrective
action taken to resolve the problems?
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Region I L.aboracoiy Audit SOP
ATTACHMENT A Revision Number: 1
EMSL Guidelines Date: 15 March 1994
(continued) Page 64 of 77
2. ICP Analysis Area
Analysts of samples by inductively coupled plasma atomic emission spectioscopy (ICP) is performed in this area. Other analysis
techniques zany be found within the same analytical area. Sample preparation should be performed in a separate area from the
analytical area to prevent contamination and to prevent corrosion of the instruments. The analysis aieas should be clean and
maintained in a manner consistent with trace level work. The required number of instruments should be available, Fjnctional,
and properly maintained. An ICP Spectroscopist and an ICP operator should be identified and they should meet the educanort
and experience requirements for their positions. Both persons should be made available to the on-site audit team. The laboratory
personnel should be interviewed to evaluate whether their technique is consistent with SOPs and compliant with program or
method requirements. This evaluation of the ICP procedures, personnel, and analytical laboratory should be performed
consistently with the check list shown on pages 65 through 68. Items specific to this area are shown below:
• ft should be determined if the laboratory is performing long terra performance monitoring of the ICP(S) through
tracking of instrument calibration intensities in a log.
• Does the analyst properly correct for interfererits and do they know how to recognize interference problems? Some
laboratories have stated that since they are using sequential ICPs, that interference correction is unnecessary. The
laboratory should demonstrate that such a claim is accurate through an evaluauori of the analytical wavelengths while
analyzing high concenuations of interfering metals.
• Run logs and raw dam documentation should be evaluated for compliance with the program requirements and 012.
The personnel should also be evaluated for a general knowledge of problems in their area that arc specific to ther performance
in the program for which the auditor is evaluating. ft is important for the analysts to be aware of project problems and involved
in the resolution and corrective action. Such an involvement is an indication of a strong and proactive QA program.
En preparing for an on-site evaluation of the ICP area, there are some common indicators found in data audits and other
monitoring information that would lead the on-site auditor to believe that there were problems in this area. Some of those
indicators arc Listed below and may help the student when preparing to evaluate this laboratory area:
• Long delays in analysis after preparation may indicate poor communication and coordination between the sample
preparation and analysis areas. Non-compliance with special project requirements may indicate a lack of
communication with sample receipt and project management personnel.
• Chronic reporting of analytical spikes outside of criteria may be an indication of poor analytical or spiking
technique. Consistently poor spike recoveries may also indicate a poorly prepared or out .of- .iaxe spiking standard.
• Chronic reporting of low level contamination in the analytical blanks may indicate poor sample analysis technique,
con n n d solvent water, or cont minated work areas.
• Chronic reporting of over or under correction of the interference check solution (ICSA). may be an indication of
improper interference correction of the instrument
• Chronic reporting of serial dilution results outside of criteria may be an indication of poor technique or unusual
nebuther and torch conditions.
Deviations &ocn laboratory procedures and program requirements and poor documentation of analysis information
may be an indication of a lack of understanding of the procedures, of poor training, and a lack of QA oversight
• Chronic reporting of poor CR1 standard results (low level standard at twice the CRDL) may be an indication of
instability in the instrument at or acar the detection limit or an indication of a poorly prepared standard.
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Region I Laboratory Audit SOP
ATFACEMENT A Revision Number: 1
EMSL Guidelines Daze: 15 March 1994
(continued) Page 65 of 77
LABORATORY SYSTEMS AUDIT FORM
V. IC ?
V.a. Facilities - Requirements are one ICP spectiomctcr for 200 or 300 sampLes/month capacity and two ICP spcc ometcrs
for mare than 300 samples/month capacity .
Installation
Manufacturer Model
SpecU ometer
ID#
Data System
Specti ometer
ID#
Data System
ITEM YF-517V0 COMMENT
I. Is the laboratory maintained in a clean
and organized manner?
2. Does the laboratory appear to have
adequate work space?
3. Are contamination-free work areas
provided for ace level analytical
work?
4. Arc manufacturer’s operating manuals
readily available to the operator?
5. Does the laboratory have service
contracts for the IC? instruments?
6. Are appropriate in-house replacement
paita available?
7. Does the laborator ; perform regular
preventive maintenance on the ICP
insmunents?
8. Are prepared maintenance schedules
available for inspection?
9. Arc permanent service records main iaed
I in a logbook?
10. Are the instruments vented to outside
the l acthty?
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Region I Laboratory Audit SOP
ATrACHMENT A Revision Number: 1
EMSL Guidelln Daze: 15 Mazth 1994
(coiitinued) Page 66 of 77
LABORATORY SYSTEMS AtJDIT FORM
V. ICP
V b. Persormel
ITEM YES/NO Comment
1. is an ICP spectroscopist identified?
Name
2. Does the ICP spectroscopist meet the
educaijen and experience requirements?
(BS or BA in science, 1 yr ICP
experience, 3 yrs additional experience
in lieu of the education requirement).
3. Is an ICP operator identified?
Name
4. Does the IC? operator meet the education
and the experience rcquirementi? CBS or
BA in science, 1 yr IC? experience, 3
yrs additionai experience in lieu of the
education requirement).
V.c. Procedures: Ask the analyst to describe their procedures. The fol1owin item.i should be addressed .
YESJNO COZY 1ENTS
Are writren SOPs developed for
inductively coupled plasma (ICP)?
2. Do the SOP(S) meet the requirements of
the SOW for content and format? If no,
see Attschincnt B.
3. Are the appropriate portions of the SOPs
available to the laboratory staff?
4. Are the analysts notified that samples
are available for analysis and are
analyses SCheduled in a systematic
manner?
5. Does the laboratory maintain a sample
injection logbook?
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Region I Laboratory Audit SOP
ATrACEMENT A Revision Nunaber: I
EMSL Gu1delln Dale: 15 March 1994
(continued) Page 67 of 77
LABORATORY SYSTEMS AUDfl FORM
V IC
V c. Pmcedures (coniinued
rr YESINO COM ? 4T
6. Do the analysts understand and perform
the proper analyocai sequence for each
method?
7. Arc calibration results kept in a
permanent record?
8. Arc terelement correction oc cicnts
determined prior to analysca (ICP)?
9. La an initial calibration verification
standard (ICVS) run after initial
calibration?
10. Is the ICVS uaceabte to a NIST standard
or other certified and indcpcndcnt
standard?
11. Are continuing calibration verification
standards (CCVS) run with each batch of
samples?
12. Arc interference check s dards
analyzed every 8 hours?
13. Are samples dilated, when required, to
get a u et element within the
quantitanon range?
14. Are analytical spikes performed when
required?
IS. Arc b lanb analyzed with every s npIc
batch?
16. Are blank c ptanen criteria clearly
established and understood by the
cb &
17. Ate mathx spike samples analyzed to
demoosirate recovery e ciency?
18. Are duplicates analyzed to demons tce
pteci3ion?
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Region I Laboratory Audit SOP
AT ACUMENT A Revision Number: 1
EMSL Guidelines Date: 15 Maidi 1994
(continued) Page 68 of 77
LABORATORY SYSTEMS AUDIT FORM
v rc
V c Procedur (continued )
ITEM YESWO COMMENT
19. Arc conuol limit for accuracy and
precision results stiictly observed?
20. Are laboratory contiol samples analyzed?
21. Are out of crjterii QC events documented
and followed up with corrective action?
22. Are limits of detection determined and
reported in an acceptsble manner?
23. Werc.the procedures described by the
analyst consistent with the SOP? If not,
please note below?
V.d. ICP QC Problems Noted Since Last Vi jt
Problems
rr YESiNO COMMENTS
Are sts.ff aware of above problems?
2. Has there bean documented corrective
action tsken?
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Region I Laboratory Audit SOP
ATrACmvIENT A Revision Number: 1
EMSL Guidelines Daze: 15 March 1994
(continued) Page 69 of 77
3. AAArea
Analysis of samples by graphite furnace atomic absorption spectroscopy (GFAA), by flame atomic absorption
spectroscopy (FAA), and by mercuzy cold vapor atomic absorption spectroscopy (CVAA) is performed in this area.
Other analysis techniques may be found within the same analytical area. Sample preparation should be performed
in a separate area from the analytical area to prevent contamination and to prevent corrosion of the instruments. The
analysis areas should be clean and maintained in a manner consistent with trace level work. Tie required number of
instruments should be available, functional, and properly maintained. AA operators should be identified and they
should meet the education and experience requirements for their positions. These persons should be made available
to the on-site audit team. The laboratory personnel should be interviewed to evaluate whether their technique is
consistent with SOPs and complete with program or method requirements. This evaluation of the AA procedures,
personnel, and analytical laboratory should be consistent with the check list shown on pages 70 through 73. Items
specific to this area that should be ei rnined include:
It should be determined if the laboratory is performing long term performance monitoring of the AA(s) through
tracking of instrument calibration absorbances in a log.
It should be determined if appropriate matrix modifiers are in use for the graphite furnace AA analysis. There
is no requirement for modifiers in the method, but it is useful to ,assess the analyst’s knowledge of their use and
purpose.
The analyst’s knowledge of the CLP decision tree for determining if method of standard additions is necessaiy
for graphite furnace AA should be evaluated. This de ision is somewhat complex and often confuses new
analysts.
Run logs and raw data documentation should be evaluated for compliance with the program requirements and
GLP.
The personnel should also be evaluated for their hnowledge of identified problems in the AA area that are specific
to the auditor’s program. ft is important for the analysts to be aware of project problems and involved in the
resolution and corrective action. Such an involvement is an indication of a strong and proactive QA program.
In preparing for an on-site evaluation of the AA area 1 there are some common indicators found in data audits and
other monitoring information that will help the on-site auditor in his or her knowledge of this area. Some of those
indicators are listed below and may help the student when preparing to evaluate this laboratory area
• Missed holding times for mercury and long delays in analysis after preparation may indicate poor
communication and coordination between the sample preparation and analysis areas. Non-eompliance with
special project requirements may indicate a lack of communication with sample receipt and project
rnnn2gement personnel.
• Chronic reporting of low level COflthmin tiofl in the analytical blanks may indicate poor sample analysis
technique, contaminated solvent water, or cont2minaied work areas.
• Deviations from laboratory procedures and program requirements and poor documentation of analysis
information may be an indication of a lack of understanding of the procedures, of poor training, and a lack
of QA oversight.
• Chronic reporting of poor CRA standard results (low level standard at twice the CRDL) may be an indication
of instability in the instrument ax or near the detection limit or an indication of a poorly prepared standard.
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Region I Laboratory Audit SOP
ATFACBMENT A Revision Number: 1
EMSL Guideilnes Date: 15 March 1994
(continued) Page 70 of 77
LABORATORY SYSTEM AUDIT FORM
YL Atomic Absorption S ectroscopy (AA )
via. Facilities - Requirenien are two GFAA spectrometers for 200 samples/month Capacity and four GFAA spectrometers
for more than 300 samples/month capacity. Reqwremcnta for mercury analyzers are two mercury cold vapor AAs required
for 200 and 300 samples/month capacity.
Installation
GFAA Manthcnirer Model ID#Date
Spectrometer
Data System
Spectrometer
Data System
Mercury
Spectrometer
Mercury
Spectrometer
ITEM YES/NO COI Q T
I. Is the laboratoiy maintained in a clean
and organized manner?
2. Does the laboratory appear to have
adequate work space?
3. Are contamination-flee work areas
provided for trace level analytical
work?
4. Are manthctuxer’s operating manuals
readily available to the operator?
S. Does the laboratory have service
contracts for the atomic absorption (AA)
instruments?
6. Are appropriate in-house replacement
parts available?
7. Does the laboratory perform regular
preventrve maintenance on the AA
instruments?
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Region I Laboratoxy Audit SOP
Afl ’ACBMENT A Revision Number: 1
EMSL Guiddines Date: 15 March 1994
(continued) Page 71 of 77
LABORATORY SYSTEMS AUDfl FORM
VT. Atomic Absorption Spectroscopv (AA )
V1.a . Facilities (continued)
rr EM YES/NO COMMENT
8. Are prepared maintenance schedules
available for inspection?
9. Are permanent service records maintained
in a logbook?
10. Are the instruments vented to outside
the facility?
VI.b. Personnel
ITEM YES/NO COMM&V7
1. Are GFAA operators identified?
Name
Name
Name
2. Is a mercury analyst identified?
Name
3. Do all analysts meet the education and
experience requirements for their
positions? (BS or RA in science, 1 yr
experience for each of the following AA
techniques appropriate for analysts
responsibilities: flame, graphite
furnace, and cold vapor, 3 yrs
additional experience in lieu of the
education requirement).
V.c. Procedures (Ask the analysts to describe their procedures. The following items should be addressed.)
ri-EM YES/NO COMMENTS
I. Are-written SOPs developed?
2. Do the SOP(S) meet the requirements of
the SOW for content and format? If no,
see Attachment B.
3. Are the appropriate portions of the SOPs
available to the laboratory staff’?
4. Are the analysts notified of arrival of
samples and are analyses scheduled in a
systematic manner?
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Region I Laboratory Audit SOP
ATTACHMENT A Revision Number: 1
EMSL Gu1deiln Date: 15 March 1994
(continued) Page 72 of 77
LABORATORY SYSTEMS AUDIT FORM
VI. Atomic Absorption Spectroscopy (A.
VT c. Procedures (con tinued
ITEM YESiNO COMMENT
5. Does the laboratory main in a sample
injecuon logbook?
6. Do the analysts underatand and performed
the proper analyncal sequence for each
method?
7. Are 4-point initial calibrations
performed daily for GFAA? Are
calibration standards for GFM. prepared
for each daily ron?
8. Is ax least a 5-point calibration curve
prepared with each mercwy preparanon
batch?
9. Are initial calibrations within the
0.995 correlation coc cient criteria?
10. Is an iniual calibration verification
standard (ICVS) run afcer initial calibration?
I I. IsthcICVStraccabletoaNIST dardor
other certified and independent stondards?
12. Axe continuing calibration verifications
performed every 10 samples?
13. Are continuing calibrauon verifications
within the 90-110% recoveiy criteria?
14. Are calibration resulta kept in a permanent record?
15. Is spectral intcrfcrencc correction performed (AA)?
16. Am samples diluted, when required, to get a
target element within the quantitation range?
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Region I Laboratory Audit SOP
ATTACHMENT A Revision Number: I
EMSL Guidelines Date: 15 March 1994
(continued) Page 73 of 77
LABORATORY SYSTEMS AUDIT FORM
Vi Atomic Absorption SDeCtrOSCODV (AA )
VLc. Procedures ( continued)
ITEM
17. Are blanks analyzed with every sample batch
18. Are blank acceptance criteria clearly established and understood by the chemists ?
19. Arc ma spike samples analyzed to demonstrate recovery efflciencv ’
20. Are duplicates analyzed to demonstrate precision ?
21. Are control limits for accuracy and precision results strictly observed ?
22. Are laboratory control samples analyzed ?
23. Are out of criteria QC events documented I and followed un with corrective action ’
24. Are limits of detection determined and reported in an acceptable manner ?
25. Are procedures and documentation performed in a manner consistent with the laboratory SOPS? If not, note
discrepancies below .
Observations
YES/MO COMMENT
‘ lid. AA OC Problems Noted Since Last Visit
Problems
r i -EM YES/MO COMME? TtS
1. Are staff aware of above problems ?
2. Has there been documented corrective action taken ?
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Region I Laboratory Audit SOP
AITACBMENT A Revision Number: 1
EMSL Guidelines Date: 15 March 1994
(continued) Page 74 of 77
4. W Chemistry Area
Preparation and analysis of samples for cyanide by wet chemistry techniques is performed in this area. The
preparation and analysis areas should be clean and maintained in a manner consistent with trace level work. The
required number of spectrometers should be available, functional, and properly maintained. Wet chemistry personnel
should be identified and they should meet the education and experience requirements for their positions. These
persons should be made available to the on-site audit team. The laboratory personnel should be interviewed to
evaluate whether their technique is consistent with SOPs and compliant with program or method requirements. The
evaluation of the procedures, personnel, and analytical area assigned to wet chemistry should be consistent with the
check list shown on page 75 through 77. Items specific to this area that should be examined include:
• A CL? laboratory is required to have six distillation apparatus in operation, this should be verified. The
requirement is necessary to ensure the laboratory has enough preparation capacity for their contract.
• Checking the samples for pH, sulfides, and oxidants is important to verify that the samples were preserved
correctly and that they are free of sulfide and oxidant interference. Sulfides may cause the formation of
thiocyanates or react with the color reagents used in the analysis and oxidants can also be interferents in the
calorimetric process.
• It should be verified that the laboratory is titrating their stock cyanide guard against a verification standard to
monitor degradation of the cyanide standard.
• All data audits and the analyst’s procedures should be thoroughly reviewed for indications of problems in
calculation of results. All highest occurrence of calculation problems in the inorganic CL? arises in the wet
chemistry area for cyanide analysis.
The personnel should also be evaluated for knowledge of identified problems in the Wet Chemistry area that are
specific to the auditor’s program. It is important for the analysts to be aware of project problems and involved in
the resolution and corrective action. Such an involvement is an indication of a strong and proactive QA program.
In preparing for an on-site evaluation of the this analytical area, there are some common indicators found in data
audit.s and other monitoring information that will help the on-site auditor in his or her evaluation of this area. Some
of those indicators are listed below and may help the student when preparing to evaluate this laboratory area:
• Missed holding times for cyanide analysis may indicate poor communication and coordination between the
analysis and the sample receipt personnel. Noncompliance with special project requirements may also indicate
a lack of communication with sample receipt and project management personnel.
• Deviations from laboratory procedures and program requirements and poor documentation of analysis
information may be an indication of a lack of understanding of the procedures, of poor training, and a lack of
QA oversight.
-------
Region I Laboratory Audit SOP
ATTACHMENT A Revision Number: I
EMSL Guidelines Daxe: 15 March 1994
(continued) Page 75 of 77
LABORATORY SYSTEMS AUDIT FORM
VII. Wet Chemiswv (Cyanide )
VILa. Facilities - Requirements for cyanide are twelve distillation apparatus + one photometer for 200 and 300
samples/month capacity.
Installation
Manufacturer Model Date
Spec ometer
ITEM YES/NO COMMENT
I. Is the laboratory maintained in a clean
and organLzed manner?
2. Does thc laboratory appear to have
adequate work space?
3. Are contamination-free work areas
provided for uacc level analytical
work?
4. Arc sufficient cyanide disnl!ation
apparatus available to routinely analyze
all samples within the requu ed holding
period?
VIib. Personnel
ITEM YFSINO COMMENTS
I. Is a wet chemistry analyst identified?
Name
2. Does the analyst meet the education and
experience requirements of the connact?
(BS or BA in science, I yr experience; I
yr experience with automaxed analyzer,
if used; 2 yr additional experience in
Lieu of the educanon requirement)
-------
Region I Laboratory Audit SOP
ATrACEMnIT Revision Number: 1
EMSL Guidelln Date: 15 March 1994
(ctlnued) Page 76 of 77
LABORATORY SYSTEMS AUDrI’ FORM
VI I Wet Chemisav (Cyanide )
VUc. Procedures (Ask the analysts to descaibe their procedures. the foUowing-items should be
ITEM YES/NO
COMMENTS
1. Arc written SOPs developed for wet chernisury ’
2. Do the SOP(S) mcet the requirements of the SOW for content and format? If no, see Attachment B .
3. Are the appropriate portions of the sops available to the laboratory staff?
4. is there a documented procedum for quality, use, and invernorv of reagents ?
S. Are fresh analytical standards prepared at a frequency consistent with good OC ?
6. Arc reference materials properly Iabclcd with cancentations, date of preparation, and the identity of the person
p re aring the standard?
7. Is documentation of standards preparation maintained ?
8. Are standard curves documented ?
2. Ared:n calculations documented ?
10. Are calculations spot checked by a second person ?
11. Do supervtsory personnel review the data and OC results ?
12. Are samples diluted, when required, to get a.4arget compound within the quantitation range?
-------
Region I Laboratory Audit SOP
ATTACHMENT A Revision Number: 1
EMSL Guidelln Date: 15 March 1994
(continued) Page 77 of 77
LABORATORY SYSTEMS AUDIT FORM
VII Wet Chemisn (Cyanide )
Procedures ( continued )
ITEM YE ?1O COMMENTS
13. Are blanks analyzed with every sample
batch?
14. Are blank acceptance criteria clearly
established and understood by the
cheznis ?
15. Are matrix spike samples analyzed to
demonstrate recovery e ciency?
16. Are duplicates analyzed to demonstrate
precision?
17. Are method detection limit studies
performed? (note at what frequency)
18. Will samples be checked for the presence
of sulfides?
19. Are procedures and documentation
performed in a manner consistent with
the laboratory SOPS? If not, note
discrepancies below.
Observations:
Vii d. Wet Chemistry QC Problems Noted Since Last Visit
Problems:
ITEM YF IO
COMMENTS
I. Are staff aware of above problems?
2. Has there been documented corrective
action taken?
-------
APPENDIX F
REGION I DAS TRACKING
STANDARD OPERATING PROCEDURE
F-i
-------
REGION I DAS TRACKING
STANDARD CPERATING PROCEDURE
January, 1994
-------
TABLE 0? CONTEIiTS (cent’ d)
PAGE $
DUE ON... ....13
TAT..... ..
CCS R.ECVD.. ... .14
CSF R_EC!VD. •.s........ 14
DATA VALIDATION COMPLETE 14
VALIDATION CODE......
REVIEWER . . . . . . . . . . . . . . . . . 15
DV SUBCON’I’RAC’I’OR. . . . . . . . . • . . . . . . . 15
WMD CO ’Q1EN rS . . . . . . . . . 15
DATA EN’I’RY SCREEN. • • . . . . . . . . . . . . . . 1.6
DATA PACKAGE NUMBER (DPN) . 16
MATRIX, PARAMETER, NUMBER OF
SANPLES................. 36
RE PORTS . . . . . . . . . . . . . . . . . . . . . . . . . • • . . . . . . . 17
OUTSTANDING ANALYSIS REPORT..... . . ..17
OUTSTANDING DATA VALIDATIONS REPORT......17
SUMMARY OF ALL DATA PACKAGES REPORT 18
QA/QC TRACKING REPORT...... . 18
LAB PERFORMANCE WITH WMD CO!’2 ENTs REPORT. 18
DAS ACTIVITY REPORT......... . .. ..... . . . .1g
DATA RECEIPT NOTIFICATION FORM & INSTRUCTIONS
SITE LOOK-UP REPORT
CONTRACTOR LOOK-UP REPORT
T.ZB tOOK_TIP REPORT
FULL LAB NAME LIST
MATRIX LOOK-UP REPORT
PAJ(ETER LOOK-UP REPORT
OUTSTANDING ANALYSIS REPORT
OUTSTANDING DATA VALIDATIONS REPORT
SUMMARY OF ALL DATA PACKAGES REPORT
QA/QC TRACKING REPORT
LAB PERFORMANCE WITH WMD CO NTS REPORT
DAS ACTIVITY REPORT
WEEKIX DAS REQUEST FORM
WMD DATA ENTRY SCREEN
VALIDATION CODES
SAMPLE DATA ENTRY SCREEN
6.2.1.15
6.2. 1.16
6. 2. 1. 17
6 .2. 1. 18
6. 2. 1. 19
6. 2. 1.20
6. 2. 1.21
6. 2. 1.22
6.2.1.23
6.2.2 SAMPLE
6.2.2.1
6.2.2.2
6.3 STATUS
6.3.1
6.3.2
6.3.3
6.3.4
6.3.5
6.3.6
7.0 ATTACHMENTS
ATTAOHMENT 1:
ATTACBI1ENT 2.
ATTACMM T 3:
ATTAcHMENT 4:
ATTACHMENT 5:
ATTACHMENT 6:
ATAcHMENT 7:
ATTACHMENT 8:
ATTACHMENT 9:
ATTACHME 1.0:
ATrACHMENT 11:
ATTACHMENT 12:
ATTACHHEN’T 13:
ATTACHMENT 14:
ATTACHMENT 15:
ATTACHM 1.6:
ATTAcHMENT 17:
-------
FIGURE 1
DAS SAMPLE TRACKING FLOW CHART
1 ARCS, ste. biforms RSCC a’ sampling event
on Wednesday of th. week prior to eampung (Input to CLPSTS)
Notifies HSCC of laboratory code, etc.
2. ARCS, etc. sends sampl.sto LAB
Q ARCS, eta. send. COCa to RSCC wIthin 2 week. of # I
‘J . (input toCLPSTS)
5 Data Receipt Form sent from ARCS, etc. to RSCC within one day
of data package receipt (Input to CLPSTS)
6. DV Repoit sent to ES!) and WMD from ARCS, etc. withIn 21 days
of data package receipt (input to CLPSTS)
I cIpst
RSCC 4
4 iat sends data package to ARCS, etc. within TAT
-------
DAB Tracking SOP
Revisjo Number: 1.
Date: 31 January 1994
Page 15 of 19
When data are not validated, due to
various reasons, the field sampling
contractor is responsible for providing
written notification and justification
to EPA so that the appropriate
validation tier code can be entered.
When data are not validated, the RSCC
enters tier code as “N” and enters the
reason why the data were.not validated
in the WMD Comments field. Refer to
Attachment Sixteen for a list of
appropriate codes.
6.2.1.21 REVIE 4ER
The Reviewer field contains the first
initial and last name of the person who
validated the data package for the field.
sampling contractor.
The reviewer is identified in the data
validation memorandum.
6.2.1.22 DV SUBCONTRACTOR
The DV Subcontractor field contains the
subcontractor that the field sampling
contractor used to validate the data
package. If no subcontractor was used,
this field is left blank.
The DV Subcontractor is identified in
the data validation memorandum.
6.2.1.23 WMD COZ ENTS
The WND Comments contains any comments
that were listed on the DV cover sheet
of the data validation memorandum that
might have prevented the memorandum from
being sent to the Region on time. Also
included in this section are brief
comments which provide additional
information regarding
problems/deficiencies with the
laboratory analysis procedures.
-------
DAB Tracking SOP
Revision Number: 1
Dat&: 31 January 1994
Page 16 of 19
6.2.2 SAMPLE DATA ENTRY SCREEN
Attachment Seventeen contains the data entry
screen for the sample data ,thich are
containe4 in each data package and are
received by the field sampling contractor.
The sample data for each data package is
contained in the Parameter/Sample portion of
the CLPSTS. This sample data portion differs
from the Total No. Samples field (Section
6.2.1.8) because it lists the number of
samples analyzed for a specific matrix and
parameter. Since there may be more than one
parameter contained in each data package, the
number of samples listed for each parameter
may not equal the total number of samples
listed in section 6.2.1.8. The
Parameter/Sample portion is accessed by
pressing the F5 function key when at the WMD
data entry screen (Attachment Fifteen). Each
field is described in the sections that
follow.
6.2.2.1 DATA PACKAGE NUMBER (DPN)
The Data Package is the internal
tracking number used by the RSCC, see
section 6.2.1.1. When the number is
entered into this field the Site field
is automatically entered.
6.2.2.2 MATRIX, PARAMETER, NUMBER OF
SAMPLES
Entered in the sample data screen,
Attachment Seventeen, is specific sample
information for each Data Package
Number. The sample information is
obtained from the data provided on the
DAS Data Notification Receipt Form
(Attachment One #14). Parameter and
matrix codes are found in their
respective Look—Up Tables, Attachments
Six and Seven.
The total number of samples submitted
for analysis for each parameter and
matrix is entered. For example, if both
-------
DAB Tracking SOP
Revision Number: 1.
Date: 32. anuary 1994
Page 19 of 2.9
just DAB labs that pertain to a specific field
sampling contractor.
This report will be used by the field sampling
contractor to initiate appropriate corrective
action measures with the laboratory. Refer to
Attachment Twelve for an example of the report.
6.3 • 6 DAB ACTIVITY .REPORT
The DAB Activity Report is generated and submitted
to each field sampling, contractor on a monthly
basis. It lists the matrices and parameters
requested for each site during a specified time
frame. The report for each field sampling
contractor contains DAB information for that field
sampling contractor only.
This report will be used by the field sampling
contractor to monitor the level and type of DAB
activities for each site. Refer to Attachment
Thirteen for an example of the report.
-------
REGION I WEEKLY DAS REQUEST FORM
REQUESTS FOR THE WEEK OF:
DAS U/LABCODE/TAT
Site Name/Location
Operable Unit
No. of
Samples
Matrix
Parameter
QC Sample
Numbers
.
Contractor
DAS#:
LAB:
TAT:
SITE:
UNIT:
CITY.
STATE:
DAS#:
LAB:
TAP:
SITE:
UNIT:
CITY:
STATE:
.
DAS#:
LAB:
TAT:
SITE:
UNIT:
CITY:
STATE:
.
DAS#:
LAB:
TAT:
SITE:
UNIT:
CITY:
STATE:
COMMENTS:
-------
ATTAC} ENT ONE
-------
INSTRUCTIONS FOR FILLING OUT RECEIPT FORN
These are instructions for filling out the DAS Data Recej t
Notification form. This form is to be filled out and sent to the
RSCC, via facsimile, when a data package has been received.
Look-ufl Tables have also been provided to ensure that the correct
ccdes are entered on the form.
1. This is the site where the sampling event occurred for this
data package. The exact Site name as present on the lcok-u
table must be entered. If the site does not exist on the
look—up table, contact the RSCC for instructions.
2. The contractor code designates the sam 1ing cCntrac or
(M&E=Metcalf & Eddy, etc.), the contract (Al=ARcsj, T6=TES6,
etc.) and the suffix “DAS”. This segregates the data
packages from the RAS and SAS analytical work.
3. The DAS is soecific for each sampling event and. sampling
contractor. This number is a four digit number followed by
the sampling contractor’s assigned letter (M=Metca lf & Eddy,
etc.). This number is assigned sequentially by the
contractor.
4. The lab code signifies which laboratory performed the
analysis for the data package. The exact lab name as
present on the look-up tables must be entered with the
prefix “DAS”.
5. The SDG is to be assigned by the sampling contractor a d is
the lowest number in the list of am le numbers received
with the data package.
6. The number of samples that are included in the data packace.
This e uals the total number of DAS sample numbers and is
derived from the number of unique sample locations included
in the specific sampling event. This number will not
necessarily equal the total number of samples in item 14
(below). In the examol form (attached), the total number
of samoles is 10 ( aqueous and 5 soils) but each Cf the l
samples was not analyzed for only one parameter.
7. 11]. DAS sample numbers must e listed to dazarm e w i: :
samples were included in the data package.
. The DAS samole numbers f or the equi ment blanks and tnt
blanks are listed. The samole number should be followed b ,
an “E” if an equi;ment blank arid a “T” if a trio blank.
9. The DAS sample numbers for the field duplicates are to be
listed in pairs with a slash (I) separating th cain.
-------
10. The DAS sample numbers for the PE samples are to be 1: tad
if PE samples were shipped to the lab and are includ in
the data package.
11. The date that the last sample was shipped to the laboratory
for this data package.
12. The date that the sampling contractor received the da:a
package from the laboratory.
13. The date of receipt from the laboratory of all origir.ai.
documentation associated with the data package. c-enerall.y,
the date should be identical to the Data Package Rece t
Date.
14. List the total number of samples that were submitted f:r
analysis for each parameter. They should be listad
separately by matrix and parameter. For example, if th
water and soil sam les were to be analyzed for both lc t
concentration VOC and low concentration semivoC, there
should be four entries in this section of the form:
• The number of acuecus sam les for low ccncentr tj
‘foci
• The number Cf aqueous samples for low concen atj:n
semiVOC,
• The number of soil samples for VOCs plus additional
compounds,
• The number of soil samples for semiVOCs plus a iziona.
compounds.
-------
DAS DATA RECEIPT NOTIFICATION
Site Name: _1___
Contractor: 2
DAS: 3
Lab Code: 4
SDGNo.: 5
Number of Samples: 6
DAS Sample Numbers: 7
Blanks: ____B____________________________________
Duplicates: _9_____________________________________
PE Samples: 10
Ship to Lab Date: _______ 11
Data Package Receipt Date: 12
CSF Receipt Date: 13
Matrix Parameter Sample Count
14 ____________ _______________
-------
ATTAcHJ NT TWO
-------
CL? Sample Trackir’. System ,9/O9’ :3 RL :
Site LookUp Report 14:22:00 Page
(All)
Ordered by: S_NAME+S_STATE+S_CIT’I
Site Name State City
A.C. LAWRENCE CO. ME SOUTH PARIS
A.H. NILSON MACHINE CO CT SHELTON
ACCURATE BRAZING COMPANY CT NEWINGTON
AERO FAB INC. ME SANFORD
AEROFAB MUNICIPAL AIRPORT ME SANFORD
AKIN ENGINEERING CT WINDHAH
ALLING INDUSTRIAL PARK VT WILLISTON
AMSTAR CT SPRAGUE
ASHLAND CHEMICAL CT BETHEL
ATLAS TACK SITE MA FAIRHAVEN
ATTLEBORO DYING MA ATTLEBORO
AUBURN ROAD LANDFILL NH LONDONDERP.Y
AUGAT INC. ME SANFORD
BAIRD & MCGUIRE MA HOLBROOK
BALL & ROLLER BEARING CO. CT DANBURY
BANGOR AROOSTOCK RAILROAD CO ME BANGOR
BAR1Q AMSTED LANDFILL CT NEW HARTFORD
BARTON ELECTRIC DEPT VT BARTON
BEACON HEIGHTS LANDFILL CT BEACON FALLS
BEEBE ROAD DUMP VT DERBY LINE
BENNINGTON MUNICIPAL SANITARY LANDFILL VT BENNINGTON
BETHEL LATEX CT BETHEL
EFI SANITARY LANDFILL (ROCKINGHAN) VT ROCKINCHAM
BOLIDEN METECH, INC RI PROVIDENCE
BRICKYARD POND DISPOSAL RI BARRINGTON
BRIDGEPORT BRASS CT SOUTH NORWALK
BRISTOL COMPANY CT WATERBURY
BROWN COMPANY ME PORTLAND
BRUNSWICK NAVAL AIR STATION ME BRUNSWICK
BURGESS BROTHERS LANDFILL VT WOODFORD
BURGESS LANDFILL CT SOUTH WINDSOR
BURT COMPANY ME PORTLAND
CAMBRIDGE PLATING MA BELMONT
CANNON ENGINEERING (CEC) MA BRIDGEWATER
CAPITAL CITY PRESS VT BERLIN
CEDAR GROVE REDEVELOPMENT CT NEW LONDON
CEECO, INC. MA DORCHESTER
CENTRAL LANDFILL RI JOHNSTON
CHARLES-GEORGE LANDFILL MA TYNGSBOROUGH
CHEM WASTE STORAGE, INC. ME NORTH BERRICK
CHZ3HIRE ASSOCIATES PROPERTY CT CHESHIRE
CHESTER LANDFILL CT CHESTER
CIBA GEIGY RI CRANSTON
CLEAN HARBORS MA BRAINTREE
CLINTON MUNICIPAL CT CLINTON
-------
CLP Sample Track-jri System O$/O9/ 3 RIJ:_
Site LockUp Report 14:2 :Oi) Page
(All)
Ordered by: S_NAME+SSTATE+S_CITY
Site Name State City
COAKLEY LANDFILL NH NORTH HAMPTON
CONNECTICIJT DOT CT ROCKY HILL
CONSOLIDATED HYDRO INC. ME SANFORD
CORNING ROAD MUNICIPAL LANDFILL CT NORWICH
CORNWALL DOT GARAGE CT WEST CORNWALL
CROOKER & SONS ME TOPSHAM
CULBRO INDIAN HEAD FARM CT EAST GRANBy
DANIELSON DOT GARAGE CT KILLINGLy
DARLING HILL DUMP VT LYNDON
DAVIS (GSR) LANDFILL RI GLOCESTER
DAVIS LIQUID WASTE RI SMITHFIELD
DAVISVILLE NAVAL CONSTRUCTION BAT. CENT. RI NORTH KINGSTOWN
DECART VT HORRISVILLE
DEEP RIVER TOOL AND DIE CT DEEP RIVER
DEPT. OF TRANSPORTATION CT ROCKY HILL
DEPT. OF TRANSPORTATION LAB CT ROCKY HILL
DERBY LINE DUMP VT DERBY LINE
DIP AND STRIP CT NORWALK
DOVER MUNICIPAL LANDFILL NH DOVER
DURHAM MEADOWS CT DURHAM
E & D CHUCK CT MEWINGTON
EAGLE INDUSTRY ME SANFORD
EAST GRANBY LANDFILL CT EAST GRANBY
EAST HAMPTON LANDFILL MA EAST HAMPTON
EKTO MANUFACTURING ME SANFORD
ELECTRO POWER CT WOLCOTT
ELECTROLUX CT SEYMOUR
FAIRFIELD MUNICIPAL CT FAIRFIELD
FLETCHER’S PAINT NH .“IILFORD
FORT DEVENS HA AYER
FORT DEVENS/SUDBURY TRNG. MA SUDBURY
G TECH RI N. SMITHFIELD
GALLUP’S QUARRY CT PLAINFIELD
GEER BROTHERS SEPTIC CT ATERFORD
GREAT NORTHERN ME MILLINOCKE:
GRODEL MANUFACTURING CT WATERBURY
GROVELAND WELLS MA GROVELAND
H L DIEHL CT SOUTH WINDEAM
HAMILTON STANDARD CT WINDSOR LOCKS
HANDCR.AFT TEXTILE PRINTS CT PLAINVIEW
HARTFORD BALL CT ROCKY HILL
HARVEY RUBBLE CT NEW TOWN
HAVERHILL MUNICIPAL LANDFILL 1A HAVERHILL
HOCOMONCO POND MA WESTBOROCGH
-------
CLP Sample Tracking System 09/09/93 RL J_SI
Site LookUp Report 14:22:00 Page
(All)
Ordered by: S_NAME÷S_STATE+S_CITY
Site Name State City
HOLLYHOCK ISLAND CT NORWICH
HOLTOM CIRCLE GROUND WATER CONTAMINATION NH LONDONDERRY
HUBBARD HALL CT WATERBURY
HUDSON WORSTED LAGOON HA HUDSON
I B H VT ESSEX JUNCTION
INDUSTRI-PLEX MA WOBURN
IRON HORSE PARK HA BILLERICA
JARD CO VT BENNINGTON
JEFFERSON GARDENS APTS CT NEW LONDON
JOHNSON & DIX VT NORTH SPRINGFIELD
JONES & LAUGHLIN STEEL CT WINDHAX
KEARSARGE METALLURGICAL NH CONWAY
KEEFE ENVIROMENTAL SERVICES NH EPPING
XELLOGG—DEERING WELL FIELD CT NORWALK
KENDALL COMPANY CT WINDRAM
KILLINGSWORTH MUNICIPAL LANDFILL CT KILLINGSWORTH
LANDFILL & RESOURCE RECOVEY, INC. (L&RR} RI NORTH SMITHFIELD
LAUREL PARK, INC. CT NAUGAT JCK
LINCOLN SITES RI LINCOLN
LINEMASTER SWITCH CORP. CT WOODSTOCK
LISBON DOT GARAGE CT LISBON
LORING AIR FORCE BASE ME LIMESTONE
LYDALL INC CT MANCHESTER
H H RHODES INC CT AVON
H S CHAMBER & SON CT SPRAGUE
MASS BAY iNDUSTR iAL WASTE RI NARRAGANSETT
MCKIN CO. ME GRAY
HEG UIER AND JONES HE SOUTH PORTLAND
MOSS AMERICAN CT NORTH HAVEN
MOTTOLO PIG FARM NH RAYNOND
NAUGATUCK TREATMENT CT NAUGATUCE
NEW BEDFORD SITE MA NEW BEDFORD
NEW ENGLAND WOOD RI WARWICK
NEW ENGLAND WOODCRAFTING CT VERNON
NEW HAMPSHIRE PLATING CO. NH MERRIMACK
NEW LONDON SUBMARINE BASE CT GROTON
NEW LONDON TEXTILE PRINTS CT PORTLAND
NEW SITE M i BOSTON
NEWPORT NAVAL EDUCATION & TRAINING CENT. RI NEWPORT
NIKE INDUSTRIES SANFORD
NORTH END DISPOSAL CT W. TERBURY
NORTHEAST UTILITIES CT WALLINGFORI
NORWALK POWDERED METALS CT NORWALK
NORWOOD PCB MA ORWOO
-------
CL? Sample Trac in System 09/O9/ 3 RLU_5t
Site LookUp Report 14:22:00 Pate
(All)
Ordered by: S_NAME+S_STATE+S.CITY
Site Name State City
NUTMEG VALLEY ROAD CT WOLCOTT
NYANZA CHEMICAL WASTE DUMP MA ASHLAND
NYANZA SITE III MA ASHLAND
NYMAN MANUFACTURING. RI EAST PROVIDENCE
O’CONNOR COMPANY ME AUGUSTA
OLD SOUTHINGTON LANDFILL CT SOITHINGTON
OLD SPRINGFIELD LANDFILL VT SPRINGFIELD
OLSON BROTHERS CO CT PLAINVILLE
OTIS AIR NATIONAL GUARD BASE/C. EDWARDS MA FALMOUT}(
OTTATI & GOSS NH KINGSTON
P. F. INDUSTRIES CT WOLCOTT
PAPISH INC. CT DANBURY
PAR FINISHING CT WOLCOTT
PARKER LANDFILL VT LYNDON
PEASE AIR FORCE BASE NH PORTSMOUTH/NEWINGTON
PERKIN ELMER CORP CT WILTON
PETERSON PURITAN RI CUMBERLAND
PETERSON/PURITAN, INC. RI LINCOLN
PICILLO FARM RI COVENTRY
PILOT STUDY MA WOBURN
PINE STREET CANAL VT BURLINGTON
PINETTE’S SALVAGE YARD ME WASHBURN
PLYMOUTH HARBOR/C NON ENG.CORP MA PLYMOUTH
POHFRET DOT GARAGE. CT BROOKLYN
PORTLAND SAND PIT CT PORTLAND
PORTSMITH MELVILLE DUMP CT PORTSMITH
PORTSMOUTH NAVAL SHIPYARD ME KITTERY
POWNAL TANNERY T POWNAL
PRECISION PLATING coa . CT VERNON
PSC RESOURCES MA PALMER
PUTNAM DOT GARAGE CT PUTNAM
QUALITY NAME PLATE CT LASTONBeRy
R P OLSON & SON CT OUTHINGTON
RAYEX ‘T PLAINVILLE
RAYMARK INDUSTRIES CT STRATFORD
REFUSE GARDENS LANDFILL CT ELLINGTON
RESOLVE INC. NA DARTMOUTH
REVERE TEXTILE PRINTS CT STERLING
RONCARI TRAP ROCK QUARRY CT EAST GL N3Y
ROSE DISPOSAL PIT IFT) MA LANESBORO
ROSE HLI. LANDFILL RI SOUTH KINGSTOWN
ROSE?. TANNERY CT GLASTONBURY
ROSS IGNOL SKI ME PORTSMOUTH
ROYCE ALUMINUM TAUNTO\
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CL? Sample Tracking System 09/O9/ 3 RLU_s:
Site LookUp Report 14:22:00 Page
(All)
Ordered by: S_NAME+S_STATE÷S_CITY
Site Name State City
RUMFORD AVENUE LANDFILL MA NEWTON
RYE STREET SITE CT EAST WINDScR
S.D. WARREN ME WESTBROOK
SACO MUNICIPAL LANDFILL HE SACO
SACO TANNERY WASTE PITS ME SACO
SALEM ACRES MA SALEM
SANFORD MUNICIPAL AIRPORT HE SANFORD
SAVAGE MUNICIPAL WATER SUPPLY NH HILFORD
SEYMOUR BRASS TURNING CT SEYMOUR
SHPACK LANDFILL MA NORTON/ATTLEBORO
SILRESIH CHEMICAL CORP. MA LOWELL
SIHSBURY TOWN LANDFILL CT SIMSBTJR Y
SOLVENTS RECOVERY CT SOUTHINGTON
SOMERSWORTH SANITARY LANDFILL NH SOMERS WORTH
SOUTH MUNICIPAL W. S. NH PETERBQ orj
SOUTH PORTLAND SHIPYARD ME SOUTH PORTLAND
STAFFORD MUNICIPAL LANDFILL CT STAFFORD
STAMINA MILLS, INC. RI NORTH SMITHFIELD
STERLING DOT CT STERLING
STEVE’S CT THOMASTON
STRATFORD SITtS CT STRATFORD
SULLIVAN’S LEDGE MA NEW BEDFORD
SYLVESTER NH NASHUA
TANSITOR ELECTRONIC VT BENNINGTON
TEXACO—NEW HAVEN CT NEW HAVEN
THOMASTOM AVENUE DUMP CT WATERB URY
THOMpSON DOT GARAGE CT THOMPSON
TIBBETTS ROAD NH BARRINGTON
TINK}IAM GARAGE NH LONDONDEg Y
TOWN OF MANCHESTER CT MANCHESTER
TRAVERS STREET GRAVEL PIT ME BIDDEFORD
TREMBLAY BAREL HATFIELD
TRUK-MJAY INC
TURCHIN JUNK YARD NH TILTO’;
UNION CHEMICAL COMPANY ME SOUTH HOPE
UNITED CLEANING CENTER ME HOULTc :
VERPLEX co. CT ESSEX
VITEK CT SHELTON
W.R. GRACE & CO INC. HA ACTON
WATERBURY PLATING CT WATERBURY
WAUCANTUCK MILLS CT UXBRZDGE
WELLS G & H MA WOBTJRN
WEST GREENWICH TOW’ LANDFILL RI WEST GREEN ; H
WEST KINGSTOWN DUMP! DISPOSAL AREA RI SOUTH KINGSTQWN
-------
CLP Sample Tracking System 09/09/93 :L_ :
Site Look p Report 14:22 OO Page
(. 11)
Ordered b7: S_NAME+S_STATE+5_CITY
Site Name State City
WESTERN SAND & GRAVEL Rt BURRILIVILLE
WHITCOMB CONSTRUCTION’ NH WALPOLE
WHITNEY BLAKE Co VT ROCKINGHA 4
WIL} INSoN CHEMICALS CT NORTH HAVEN
WILLINGTQN DOT GARAGE CT WILLINGTON
WINTHROP LANDFILL 1E WINTHROP
WOLCOTT MUNICIPAL LANDFILL CT WOLCOTT
YANKEE ELECTRONIC SERVICES CT BETHEL
YAWORSKI WASTE LAGOON CT CANTERBUSY
YORK MFG. ME SANFORD
-------
ATTACI*IENT THREE
-------
CLP Sample Tracking System 09/09/93 RL CO
Contractor LockUp Report 14:29:47 Pate
(All)
Ordered by: CONTRACTRS
Contractor Name
ADL/Al
.ATK
CD fF/A1
CDMF/RCRA
CD 1F/T5
ESD
ESI/Al
1&E
f&E/Ai.
H&E/A1 DAS
NUS/Al
RFW / Al
TRC/Al
TRC/T6
-------
ATTAC} ENT FOUR
-------
CLP Sample Track-inz System 09I09/ 43 RLL_L
Lab Look-Up Report 14:30:20 Page
(All)
Ordered by: LABS
Lab Name
AA LA B
AATS
AATSLA
AB B
ABC
ACC RED
AC CU
ACNC
ACZ
ADL
ADTT
AETEST
AICORP
AIRTOX
ALDEN
ALl
ALLIED
ALTA
AMANAL
ANTECH
AM WEST
ANACON
ANAJJYT
ANAMET
ANLAB
APPL
AQ S URV
AQUAI
ARDL
ARI
ASI
ASTECO
ATAS
ATEC
All
ATIWA
ATL
BALAZS
BARRIN
BATPNW
BATTEL
BCA
BEC
BELMNT
BETZ
-------
CLP Sa nt1e Trackin System 0 /0 /93 R _L
Lab Look1ip Report 14:30:20 Paze
(All)
Ordered by: LABS
Lab Name
B ET Z P A
BIONO 1
BONNER
BRAW’(
BSK
BSPHER
BURLNG
CALH 20
CAMBRG
CANON
CARTER
CDS
CEIHIC
CENREF
CENTEC
GENTRY
CENTST
CEP
CH2HAL
CH2XS
CH 1
CHE 1EX
CHEHW
CHEN
CLAYCA
CLAYTN
CLEAN
CLEAN 2
COAST
COLUIB
CO 1ON
COHPtJ
COORS
CORECA
CORECO
CORETX
CO REWY
COS PER
CSE RVE
CSU
CTCIN
I-fl• —
‘. L.
CTM
-------
CLP Sample Trackir.g System 0 /O9/93 RL _LA
Lab LookUp Report 14:30:20 Page
(All)
Ordered by: LABS
Lab Name
DANDF
DASAI RTOX
DASAQUAI
DATAC
DATACO
DAVY
E3 1
EAENG
EAGLE
EAI
EA LA B
EANDE
EARTH
EARTHA
EAS
EAT L
ECAL
ECOTEK
ECS
EEAST
EERCO
EHRT
El RA
EMPIRE
EMS CA
EMS I
EMSIN
EMS MO
EMS NJ
EHSTI
ENCOT
ENS ECO
ENS R
ENS RMA
ENS RT:c
ENV
ENVRTE
ENVSYS
ENVTST
EP L
EPS
ERC
ERI
ESA
-------
CLP Sample Tracking System R
Lab LookUp Report 14:30:20 P. e
(All)
Ordered by: LABS
Lab Name
ESE
ES ECO
ESERTI
ESICA
ETC
ETC-CA
ETCOH
ETCTOX
ETS
EUREKA
EWI
FGL
FIRST
FLOWER
GALSON
GARDEN
GASCOY
GENTST
GLOBAL
G PENV
GRACE
GULF
GYNNUR
H 2 l LAB
HAGER
HARD LA
HAS
HAZ EN
HAZ LAB
HAZ LET
H I ThAN
HUFF
MW L?. 1
H L;.
LC 1
I EA
IEACT
IEANJ
IEAVT
lIT
IN DUST
I NPO L
INTECH
I Q J A
-------
CLP Sample Trackiri System Q /O9/I 3 RL L.A
Lab Looktjp Report 14:3 :2O Page 5
(All)
Ordered by: LABS
Lab Name
IT
ITKNOtv
ITMO
ITNJ
ITOH
ITPA
ITSTU
JHA
JTC
KCSE
KEYPA
KEYTX
LANCAS
LANGST
LANL
LAUCKS
LEN L
LRI
MAC K
HATER
MCCOY
MC LA RN
MC RON E
MDSPEC
H ED LAB
H E DTOX
HETA
METCHM
METCHW
MICROB
HPELI
fRI
YANCO
AT ION
NCOAST
N EA
N EAST
NET
NFT
NLE
NO LAKE
NSL
Ni.IS
-------
CLP Sample Tracking S -stem 0 /09/ 3 RLU.LA
Lab LockUp Report 14:30:20 Pa!e
(All)
Ordered by: LABS
Lab Name -
NUSTX
NYSDH
NYTEST
OBG
OLI
OREGON
ORS
ORTEK
PACE
PACECA
PACEKS
PACENY
PACEPA
PACIF
PART
PBSJ
PDCLAB
PDL
PDP
P El
P ERFR 1
PNELI
PRECIS
PRINCE
PRIOR
QTI
RADIANC
RADIANN
RADIANT
RAIN
REC 1D
RECNY
RE SAN
RE VET
RXC
R fT
ROSS
S3
SAl
SAIC fD
SCTECH
SEQUOI
SIERRA
SILVER
-------
CLP Sample Tracking System 09/09/93 RLU_LA
Lab LookUp Report 14:30:20 Page 7
(All)
Ordered by: LABS
Lab Name
SKINER
SOEAST
SORI
SPCTRM
SPECTE
SPL
STDTST
STILSN
SWOK
SWRI
TAI
TCH LAB
TECI
TELEDY
TELEIL
T EXAM
THERHO
TIOAK
THA
TMAARL
THAEBR
T.’IS
TRI
TRICtL
TRILAB
TRILABX
TRUDAL
TTL
TWIN
TWININ
UE&C
USTCWA
USTEST
TJVNE
UVV’(
VEGAS
VERESM
VERSAR
VGELE
WADS
¶‘iADS P A
t iANCO
WANTEC
WCAS
-------
CLP Sample Tracking System 09/09/93 RL ..
Lab Lookrjp Report 14:30:20 Page S
(All)
Ordered by: LABS
Lab Name
WESCA
WESTEC
WESTON
WESTONG
WEYER
WGULF
WILSON
WRI
YRC
-------
ATTAC ENT FIVE
-------
AATS American Analytical and Tec nica1 services
(Ok1aho a)
AATSLA Anerican Anaivtica]. and Tec injcaj Services
(Louisiana)
ABB Coast to C ast Analytical Services, Inc. (Maine)
ABC
AC ZD
ACCU Accurex
ACNC
ACZ ACZ Labs (Stea cat, Colorado)
AOL Arthur 0. Little
ADT
AET ST
AICORP
AIRTOX Air Toxics Limited
ALD
ALl Associated Laboratories, Inc.
ALTA ALTA Analytical Laboratory, Inc.
A ANAL
AMTECH
AMWEST
ANACCN Contest Analytical
ANALIT Analvti.¼em (New Jersey)
AMAXET Anametrix, Inc.
AMI B
APFL
AQSURV
AQUAI Acuatec, Inc.
ARDL ARDL, Inc
AflI Analytical Resources, Inc.
ASI
ASTECO
ATAS American Tac .nical and Analytical Services
ATEC ATEC Associates, Inc.
ATI
ATIWA
ATL
BALAZS
BARRIN Barringer Labs (Go..den, Colorado)
EATPNW Battelle, Pacific Northwest
BATEL Battalle (Duxbury, !assachusetts)
BCA
EEC
BEL T Bel .ont Labs
BETZ BETZ Laboratories (Texas)
BETZPA BETZ Laboratories (Pennsylvania)
BIONOM
BONNER
ERAUN
ESPHER
B LNG
-------
ALH2O Cal Water Labs
CA RG NET/Cambrid e Division
CANON Carincrie
CART S
CDs
CEI fIC Cei ic Ccr oratiori
C R.EF
C TEC
C TRY
CENTST Century Testina Laboratcries, Inc
CE
CH2MAL CH N (Hill, Alabama)
CH2MSE
C iemtec i Consulting Grou
CHE L
CHE’!EX Analytical Technologies, Inc.
CW1W Chem West
CHEN
CLAYCA Clayton Environmental Consultants (Ca1jfo ja)
CLAYTN Clayton Environmental Consultants (Michigan)
CLEAN Clean Harbors (Braintree)
CLEAN2 Clean Harbors (Bedford)
COAST
COLtThiB Columbia Analytical Services, Inc.
COMMON
CO U Com uchem Laboratories
COORS Coors Spectrolytics (Golden, Colorado)
CORECA Core Labs (California)
CORECO Core Labs (Colorado)
CORETX Core Labs (Texas)
COREWY Core Labs (Wyoming)
COSP LR
CSL VE Chemserve (New Hamos iire)
Cs
CTCI T Coast to Coast Analytical Services, . (India na)
cTcThS TNS Analytical Services***
CTE
CTM CTh Analytical Laboratories, LTD.
DANDF Davis & Floyd, Inc.
DATAc Datachem Laboratories, Inc.
DATACO
DAVY
E31 E31 (Massachusetts)
EXENG HA Laboratories
EAGLE Eagle—Pitcher Envircrimental Services
HAl Eastern Analytical
EALAB
EANDE Ecology & Environment, Inc.
EARTH
EARTEA
EAS Environmental Analytical Services, mc.
E.ATI. ENSECO Inc. Air Toxics Laboratory
EC. LL ENSECO-Cal Laboratory
-------
ECOTEX ECCT i.aboratcry Services, Inc.
ECS
EL ST ENSECO East
E CO iSECO—ERCO
Environmental Health, Research and Taszjnc
EI EIP A (Louisianrla)
IRE
EMSCA S Labs (Cali crnia)
sI
SIN S/Heritage Laboratory, Inc.
SMO EMS Labs (Missouri)
E SNJ EMS Labs (New Jersey)
EMSTX Environmental Monitoring Services, In:
ENCOT ENCOTEC
ENSECO ENSECO
ISR ENSR
ENSRNA ENSR (Massachusetts)
ENSRTX ENSR (Texas)
TCT - St Louis
ENVRTE EAS Laboratories
ENVSYS Envirosystems, Inc.
ZN VT ST
EPL
EPS
Elemental Researc 1, Inc.
ESA Environmental Services Agenc (!ed ord,
Mass acbusat:s)
ESE Environmental Science and Enaineerin , Inc.
(Florida)
ESECO Environmental Science and Engineering, Inc.
(Coicrado)
ESEP TI
ES I CA
ETC Environmental Testing and Cerifica:.:n
ETC-CA Environmental Testing and
(California)
ETCOH Environmental Testing and Cerificaticn (Ohio)
ETCTOX Environmental Testing and Certificatior. (Louisiana)
ETS ETS Analytical Services
EtR A EURE
-------
HAGL
HARD LA
EAS
M.AZEi
EAZL
HA Z LIT
HITh.AN
hVFF
MW L 3 1
MW L 2
IL;
IZACT
I EANJ
I EAVT
lIT
INDUST
INPOLL
INTEC
IOWA
IT
IT OW
Imo
ITNJ
ITc:-
IT?A
ITSTtI
KC!I
I CAS
L? NGST
LANL
LAL7 ZS
L 1L
LRI
MACX
.‘tATL
: ccc’z
a — -
McRONZ
MDSPIC
MEDL
MEDTOX
MITc-
— Cerrj:os (Ca1i c: ja)
( Cnoxvil1e)
(Missouri)
(Ne’d Jersey)
(Ohio)
— Ex ort (PY1;a ia)
T c
b.a._ — I •
Macer Labs (Cclo:adc)
Ha: iz g La ison Associates
Eazen Reseerch (C 1orado)
3iono ics Laboratory, Iflc.
Hazletort E. virc enzal Services, In:.
HITt?.N E3ASCO
Hu an
Indus ::ial Cor sion Mana e en
Indusz:ial E.nvi:cn ental Analysts, ( c: :
Carolina)
Industial Ez1vircn ental Analvszs, Inc.
(Conziec :ic t)
Industial E wir:r. anzal Analysts, L :. ( e Thrsev)
Industial L vir:r. ental ?.na].yszs, In:. (7 : : -
Inze: o1l Laboratories, Inc.
Laboratory Resources, Inc. (Intech Divisjcn)
University of Iowa
IT Analvticaj. Services
IT Analytical Services
IT Analvcic,al Services
IT Analytical Services
IT Analytical Services
IT Analytical Services
ITAS / Kno villa
ansas Ci:: Scientific
Aeyszone Las
C es :er La .ne: -
Lancaster L oratories. Inc.
Lanc zon La s
Lauo s Tes:inc
La Inviro ental a:icnal a.cra::”
ay.an: o :ral Sar-;ic
— r- ———— —— •,—
-------
ICRO
ETL/> id-?aci i Envircnmen:al Lab
Mid ast P esearcn Institute
NANCO NANCC
NATION
NCOAST
NZA C’iasz r Labnet - Portland
NL ST orzneasz La o:a -cry Serv.ces
NET NET idwasz, Inc.
N T
NLE CCCSZ t C ast Analyz .cal Services, In:. (Indiana)
NOI X1
NSL
NUS Ealliburtcn NtJS Enviror enzal C:r .
NVSTX NUS (Texas)
NYSDH Ne J York State De arz ent c Eealt .
N TEST MYTEST Envirn ental, Inc.
OEC-
CLI Orlando Laboratories
ORE 3N
ORS
ORTL
PACE Pace, Inc. — Minnea o1is
PACECA Pace Laboratories (California)
PAC S Pace Laboratories (Kansas)
PAC ? Pace, Inc. — Wappingers Falls
PACEPA Pace Laboratories (Pennsylvania)
?aci ic Analytical, Inc.
FART
F!! & J Envircr ental Labs
P DC - .B
PDL
PD? PD? a1yzical Services
PU
? ?
:;:-.L: , aci :c :3rz : asz fir:nzanzai a:
PR1CIS Precision Analytical Laboratcry, Inc.
PRINCE Prin atcn Testing Laborazcry
PRIOR
QTI
Radian (Norz . Carolina)
RADL.NN Radian
RAIN
P.IC A Envirr. antzl, :-. . ( a:;La
P ICV R CRA Envircn en:al, Inc. (New Ycr ,
Pace, New Encland (Resaurca Analysts;
RIV R Z Enviror ental and Anal’ ical Lab
R C Rtc Invircr . entaJ. Services, Inc.
ROSS Ross Analytical Services,
SA l LAIC Cali ::nia)
SAC D SA:: aryland)
S
-------
SEQtJQI S cucia A a1vica1
SIERRA Sierra Tec ni ai Services
SILV SVZ. ;. a1y ica1, Inc.
S IN TNA / Skinz er and Sherman Lass, Inc.
SCEAST Souz eascern Ana1v ica1 Ser,icas, Inc.
SORI
SPCT M
SP!CT Sceczralytix, Inc.
SPL
STDTST
STILSN
SWOK Soutn zest Labs cf Qklahoza
SWRI Sc :n est Research Znszi: ze
Til
TECI
TELEDY Teladvrie
TELEIL
TEXAM Texas A & M t.7niversizv
Envi:cr. enta1
Therr.o Analytical / ERG
TILAB T.I. La oratcries, Inc.*it
TIOAX
TMP TM.k Lass
TMAARL TY...k Labs
TMAEBR ThA Labs
T S
TRI
TRICL. . Labs
TRILA .B Triancle Laboratories ( ort Carolina)
TRIL2X Triancle Laboratories of Houston, Inc.
TRUD 4 L
TTL
TWIN Twin City Testing Cortoration
TWIN IN
TLTE & C
USTCWA US esz (Wasningzon)
USTEST US Test (New York)
UVNE
UvWY
VEGAS Vecas Analytical Labs, Inc.
VL .ESI
V S .AR VERS La :a::ries, Inc.
VGELI
WADS Wa. crt / Alert Lar:ries, :n:.
WADSPA Wa wo:t I Alert L c:a:cr:es, Inc. (Pennsyl-;ania
WAMCO
WANTIC WAN ‘ecb.nolc ies
WCAS West Coast ?jtal’rcical !er,ices
WESCA Roy Weszcn, Inc. - St z:n
WE ST C
WESTON Z. Weston - Licnvll e
WZSTCNG
e:naeuse Analrt:cal £ stinc Sar .:as
-------
ATTAC C1ENT L IX
-------
CL? Sample Tracking System O /O /93 RLU_ L .
Matrix LookL T p Report 14:34:32 Page
(All)
Ordered by: MAT_SHORT
Matrix Matrix
Code Name
AQ WATER
AR AIR
DW DRINKING WATER
Fl FISH
Or OIL
St SLUDGE
SO SOIL
WT WASTE
-------
ATTACmCNT SEVEN
-------
CLP Sample Tracking System 10/13/93 RL
Parameter LookUp Report 08:55:47 Page
(All)
Ordered by: PARA_SHORT
Parameter Parameter
Code Name
1290D DIOXINS/FURANS 12/90 SOW ANALYSIS
130.1 HARDNESS - COLORINETRIC, AUTOMATED
130.2 HARDNESS — TITRIMETRIC, EDTA
1311 TCLP EXTRACTION METHOD
160.1 TOTAL DISSOLVED SOLIDS (TDS)
160.2 TOTAL SUSPENDED SOLIDS (TSS)
2320.B BICARBONATE
300.OC CHLORIDE - IC (EPA METHODS)
300. OS SULFATE
305.1 ACIDITY
310.1 ALKALINITY
325.2 CHLORIDE, AUTOMATED, FERRICYANIDE
325.3 CHLORIDE, TITRIMETRIC, HGNO3
335.2 CYANIDE, TITRIHETRIC, SPECTROPHOTOM
340.2 FLUORIDE
350.1 AMMONIA — COLORINETRIC, AUTOMATED
350.2 AMMONIA-COLoR. ,TITRI. ,POTEN.—DISTIL
350.3 AMMONIA - POTENTIOMETRIC
351.2 TKN, COLORIMETRIC, S 1IAUTOMJtTED
351.3 TKN, MANTJAL, COLOR., TITR., POTEN.
352.1 NITRATE, COLORIXETRIC, BRUCINE
353.1 N-N03/NC2 - COLORIMETRIC, AUTOMATED
354.1 N-N02 - SPECTROPHOTONITRIC
3540 TOT.RECOV.PET.HYDROCARB. - SOXHLET
365.2 T-P - COLOR., ASCORBIC ACID, 1 REAG
365.3 T-P - COLOR., ASCORBIC ACID, 2 R.EAG
365.4 T-P - COLORIIIETRIC, AUTOMATED
370.1 SILICA
375.1 S04 — COLORIMETRIC, AUTOMATED
375.4 S04 — TURBIDIMETRIC
376.1. SULFIDE
403 BICARBONATE
405.1 BOD
410.1 COD - TITRIMETRIC, MID-LEVEL
410.2 COD - TITRINETRIC, LOW-LEVEL
410.4 COD - COLORINETRIC, AUTO OR MANUAL
4110 ANICNS
413.1 OIL AND GREASE (O&G) — GRAVIMETRIC
413.2 OIL AND GREASE (O&G) — IR SPEC.
415.1 TOC - COMBUSTION OR OXIDATION
415.2 TOC - LOW LEVEL, tJV PROMOTED
418.1 TPH - PETROLEUM HYDROCARBONS.
504 EBD & DBCP
507 BOD - STD. METH. 16TH EDITION
-------
CLP Sample Tracking System 10/13/93 RLUPA
Parameter LockUp Report 08:55:47 Page 2
(All)
Ordered by: PARA_SHORT
Parameter Parameter
Code Name
5210 BOD — STD. METH. 17TH EDITIOW
524.2 VOA LOW DET LIMITS - DRINXING WATER
525 BASE/NEUTRAL/ACID EXT. — LOW QL
601 VOLATILE ORGANICS — HALOCABBONS
602 VOLATILE PURGEABLE AROMATICS
680 PCB’S
7196 HEXAVALENT CHROMIUM
8 015 2-METHOXYETHANOL
8021A HALOGENATED,AROMATIC VOC, GC/EC/PID
8080 PCBSS
8140 ORGANO—PHOSPHOROUS PESTICIDES
8150 CHLORINATED HERBICIDES
8270 S 4IVOLATILE ANALYSIS
8280 DIOXIN/FURANS
9020 TOX — TOTAL ORGANIC HALIDES
9030 ACID SOLUBLE & INSOLUBLE SULFIDES
9057 CHLORIDE — IC (STANDARD METHODS)
ALK ALKALINITY
ANTIMONY ANTIMONY BY GRAPHITE FURNACE 204.2
AROT AROCLOR/TOXAPHENE - HIGH CONC SOW
ASBESTOS ASBESTOS BY TRANS. ELECT. MICRO.
ASTN2974 TCOC - TOT COMBUSTIBLE ORG CONTENT
ASTMD422 GRAIN SIZE ANALYSIS
ASTMD S13 CARBONATE, BICARBONATE, IN WATER
AVS ACID VOLATILE SULFIDES
BNA RAS BNA, LOW/MED CONC.
BNA+CPDS S 1IVOLATILES PLUS ADD. COMPOUNDS
BNAL 00 0N LOW CONCENTRATION SEMIVOLATILES
CADMIUM CADMIUM BY GRAPHITE FURNACE 213.2
CN RAS, CYANIDE
DIOXIN PCDD/PCDF ANALYSIS DFLMO1.0
DMET DISSOLVED METALS
DM N,M-DMF — MOD. METHOD 8000 (NPD)
MET RAS METALS, LOW/MED CONC.
MET+CPDS METALS PLUS ADDITIONAL ANALYTES
METCN PAS METALS & CYANIDE, LOW/MED CONC.
METCNLC LOW CONCENTRATION METALS & CN
METLOCON LOW CONCENTRATION METALS
MICROPRT MICROPARTICULATES
P/P PA! PEST/PCB, LOW/MED CONC.
P/P+CPDS PESTICIDES/PC3’S + ADD. AROCLORS
P/PLOCON LOW CONCENTRATION LOW PEST/PCB
PAH’S PAH ANALYSIS - CC/MS/SIN MODE
-------
CLP Sample Tracking System 10/13/93 RLU
Parameter LockUp Report 08:55:47 Page 3
(All)
Ordered ty: PARA_SHORT
Parameter Parameter
Code Name
TBT TR.IBUTYLTflr, ANAL.CHEN. 1988, 60,696—
TCLPBNA BNA BY TCLP EXTR?tCTION
TCLPMCN METALS & CN BY TCLP EXTRACTION
TCLPP/P P/P BY TCLP EXTRACTION
TCLPVOA VOA BY TCLP EXTRACTION
TO-i VOC - AIR, TENAX TUBES
TO- I A VOC - AIR, SUMMA CANISTERS
TO-2 VOC - AIR, CARBON MOLECULAR SIEVE
TOCLK TOC ANALYSIS BY LLOYD KAHN METHOD
TOCWB TOC BY WALIa EY-BLACK METHOD
VOA RAS VOLATILE ORGANIC ANALYSIS
VOA+C PDS VOA PLUS ADDITIONAL COMPOUNDS
VOA.LOCON LOW CONCENTRATION VOLATILES
-------
ATTAC ENT EIGHT
-------
O1/2 f94 I4:43 3 PaRQ
CLP Samp]e Tracking System — U8ez . Defined Report
H&E DAS Outatanding Aria1y i8 Report (CKLASICI)
Index: CLP MAST->CASE NUM+CLP_HAST->LAI3
Ship Date Lab Caae No. # Samp1e Contractor Due Date
* Site IRON HORSE PARK
09/14/93 DASABB 000 IM/ 26 M&E/A1DAs 10/19/93
09/17/93 DASABE (JOU1MI 6 H&E.’A lDAS 10/22/93
09/22/93 DASABB uooinf .19 H&E.’A lDAS 10/27/93
-------
ATTACIflIE IT NINE
-------
Page 1
01/26/94 10:08:03
C].JP Sample Tracking System - User Defined Report
i& DAS Outstanding Data V 8 1id tt0 (AL.EE)
Index: CL12MAST-)SITE+CLP .HAST_>CASE MUH
Case No. contractor Lub No. Samp. D Reed
* Site CHARLES-GEORGE LANDFILL
000ZM/ M& /A1DAS DASHORRI 13 ti/10/93
0002H1 M&E/A IDAS DASMORfU 18 t1/1O.’93
* Site DOVER MUNICIPAL LANDFILL
000314/ M&E/A1DAS DASMATIU 10 1.1/19/93
* Site IRON HORSE PARK
000114/ M&E/AIDAS DASABD 26 / /
000114/ M&E/A1DAS DASCAMBR 14 10/12/93
000114/ M& /AiDAS DASABB 0 / /
000114/ M&E/AIDAS DASABE 19 1 /
-------
ATTAC1 ENT T
-------
01/26/91 0 :J1:25
CL F’ Sample Tracking System - Uzer Defined Report
H&E DAS Sumrnazy ot 11 Data ?acka ea (ALEE)
Index; CLPNA5T- SITEpcT.,p NAST- CASE.JIUH
Contractoz Case # SDG No. Date Shipied D?ite DP Reed Date DV
* Site CHARLES-GEORGE LANDFILL -
L b DASCAI4BRG
M&E/AIDAs 0002H/ DAM5O1 10/01/93 10/22/93 01/19/94
* Lab DASHORRIS
H&E/A1DAS 0002M1 DAM5 O3 09/28/93 11/10/93 / /
1&E/A1VAS 0002M/ DAM5O9 09/29/93 11/10/93 / /
M&E/A1DAS 000ZM/ DAM523 10/01/93 11/10/93 / /
* Site DOVER MUNICIPAL LANDFILL
* Lab DASHATRIX
H&E/A11)As 0003H/ DAM6O1 10/15/93 11/19/93 / /
* Site iRON HORSE PAR C
* Lab DASABB
M&E/A IDAS 0001M/ 09/14/93 / / / /
* Lab DASCAMBRG
H&E/A1DAS 0001H/ DAM OO4 09/20/93 10/12/93 12/10/93
?4&E/A1DAS 000Uf/ DAMU46 09/20/53 i0/iZ/93 12/10/93
H&E/A1DAs 0001H/ DAHO8 O 09/22/93 1 (3/12193 / /
* Lab DASABB
H&E/AIDAS 0001 )1/ 09/17/93 / / / /
)f&E/A1DAs oooini 09/22/93 / / / /
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ATTAC ENT ELEVEN
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01/26/94 08:37:47 Page
CL I ’ Sarnp1 TracJcj System - User Defined Report
DAS GA/OC TRACKING REPORT (CKLASKI)
Index: CL? MAST-SITE+CLPHAST_>CASENU 1
CASE/SAS # SDG LAB MATRIX # SAMPLES
* SITE CHARLES-GEORGE LANDFILL
BLANKS -- None ——
* DUPLICATES -- none —-
0002H/ DM1503 DASMORRIS SO 4
0002H/ DAMSO3 DASMORRI5 SO
000211/ DAM539 DASMORRIS SO 7
000211/ DM1509 DASMORRI5 50 6
000211/ DM1523 DASMORRIS SO 10
0002 i/ DA?1523 DASMORPrS SO 8
* SITE IRON HORSE PARK
BLANKS -— None ——
* DUPLICATES DAMO59/60,DA 1068/69
000111/ DM1045 T)ASCAM RG AQ 14
000111/ DM1045 DASCAMBRO AQ 14
DUPLICATES -- None ——
000111/ DASABB AQ 6
* BJ.ANXS flAIIO93E
* DUPLICATES DA lO34/o 5
000111/ DAMOO4 DASCAMBRG AG 20
000111/ DAMOO4 DASCANDRG AG 20
* BLANKS DAMO99E
* 1)UPI ICATEs DM10841087 ,DAMO8O/085
000111/ DM1080 DASCAMBEG AQ 14
* BLANKS -- Nonc -—
“ DUPLICATES DAMO1O/li.
000111/ DASABB AG 10
* BLANKS DAHOO9E
* DUPLiCATES DM10841087 ,DAMO8O/Q85
000] 1’1/ DAI 108O DASCAMBRO 14
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CL F.II L T.
01/26/94 08:37:47 Pare 2
amp1e Tracktng System - User Defined Roport
QA/QC TRACKING REPORT (CKLASKI)
index: CLPMAST SITE+C MT_> NUH
CASE/SAS SDG LAB HATRIX * SAMPLES
SITE IRON HORSE PARK (Continued)
* BLANKS -- None -— (Continued)
* DUPLICATES DM1010/li i entinued)
0 0 0XH/ DASABD AQ 26
* BLANKS DAHO9 E
4 DUPLICATES -- Nonc - -
00 01H/ DASABB AQ 19
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ATTA ENT TWELVE
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LP Sample Tracking System 12/09/93 REPESD s
SD Special: Lab Performance with WMD Comments 13:26:17 Page
A1l Inorganic/Organic/Other Analysis Shipped to Lab between 09/01/93 and io,
Ordered by: LAB+MATRIX+PARAMETER
Matrix Parameter Rated TAT Case SDG
Number
* Lab: AATS’
AQ DIOXIN 29 8037A/ SA1941 ** No WMD Comments
AQ MET 39 20786/ MACP21
> RESUBMITTED CCS RECEIVED 11/5/93
SO DIOXIN 29 8037A/ SA1941 ** No WMD Comments
SO MET 39 20786/ MACP21
> RESUBMITTED CCS RECEIVED 11/5/93
* Lab: AATSLA
AQ CN 57 20782/ MABS25 ** No WMD Comments
AQ MET 57 20782/ MABS2S ** No WMD Comments
AQ MITCN 57 20782/ MABS25 ** No WND Comments
* Lab: AQUAI
AQ SNA 18 20781/ ADY47 ** No WMD Comments
AQ P/P 18 20781/ ADY47 ** No WMD Comments
* Lab: CH
AQ MET 16 20942/ MACPS]. ** No ?Th!D Comments
AQ MET 28 2083 1/ MADH29 ** No WIlD Comments
AQ MET 18 20733/ MABN76 ** No WIlD Comments
AQ MET 17 20787/ MADGZ6 ** No WIlD Comments
SO MET 16 20942/ MACP52 ** No WIlD Comments
SO MET 17 20787/ MADG66
> RESUBMITTED CCS RECEIVED 11/4/93
* Lab: COMPU
AQ BNA 19 20832/ AFS62 ** No WIlD Comments.
AQ ENA 17 20787/ A1F37 . ** No WIlD Comments
AQ P/P 14 20698/ AFM75 ** No WIlD Comments
AQ P/PLOCON 15 8019Q/20798 SA2642 ** No WIlD Comments
SO P/P 14 20698/ A1M63 ** No WMD Comments
SO P/P 14 20698/ AFMS ] . ** No WMD Comments
* Lab: DANDF
AQ BNA 26 2 0782/ ADY O2 ** No WIlD Comments
* Lab: EANDE
AQ BNA 35 20696/ ADQ38 ** No WMD Comments
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ATTACHMENT THIRTEEN
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. • - L
91/26/94 10:54:45
Sample Tracking Sy L m — User Defincd Report
ACTIViTY (CKLASKI)
Index: CLP_MAST_>CONT)(ACTOR+5AMPLE)PARAMETER C1JP MAST CASE .NUt
SAS No. Ship Date Matri. SDG No. Samp1e
‘ Contractor H&E/A1DAS
* Parameter 310.1
* Site IRON HORSE PARK
000 IM/ 09/20/93 AQ DAHO45 14
00 01M/ 09/20/93 AQ DAHOO4 20
000IH/ 09/22/93 DM1080 14
* P ramoter 415.1
* Site IRON HORSE PARK
00 01M/ 09/20/93 AQ DAHO45 14
0001H/ 09/20/93 AQ DAMOO4 20
0 0 0 IH/ 09/22/93 AQ DM1080 14
* I’aramctcr 624.2
Site IRON MOR$E PAR C
0 0 01M/ 09/14/93 AQ 10
* s DOVER MUNICIPAL LANDFILL
0003M/ 10/15/93 AQ DAH6O1 10
4 Parameter ASTH2Q74
* Site C1 ARLES-CEORGE LANDFILL
00 02M/ 09/28/93 50 DAM5O3 1
000ZM/ 09/29/93 80 DAH5O9 0
0002M/ 10/01/93 SO DAHS23 8
* Parameter ASTHD422
* Site CHARrJES-cEQRGE LANDFILL
0002M/ 09/28/93 So DAMGO3 4
0002M/ 09/29/93 50 DA 1f509 7
0002M/ 10/01/93 so DM1523 10
L’ararnet r ‘/I’LOCON
site IRON HORSE PARK
0 0 01H/ 09/17/93 AQ 8
09/14/93 AO 20
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CLP Sam 1e Trackinz System 12/08/93 REPSAS
ESD SDecja].: SAS .kctivity 10:17:49 Page
(All Inorganic/organic/other Analysis Shipped to Lab between 08/01/93 and
Ordered by: CONTRACTOR+SITE+CASE_NUM
SAS Ship
Number Date Matrix/Parameter
Contr.2ctor: ADL/A1.
* Site: BFI SANITARY LANDFILL (ROCKINGHAM)
7804A/20674 08/29/93 AQ/524.2
8019Q/20673 08/26/93 AQ/BNALOCON
8056A/ 08/27/93 AQ/METCNLC
Site: OTTATI & GOSS
7945A/ 08/09/93 SO/TOCLK
7945A/ 08/09/93 AQ/TOCLK
7988A/20692 08/23/93 Fl/MET
7988A/20692 08/24/93 Fl/MET
* Contractor * SAS = 6 Method 5
** Grand Total ** SAS 6 Method 5
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CLP Sainole Tracking System 12/08/93 REPSAS
Special: s. s . ctjvit 10:18:52 Pa’e
Inorganjc/Orzanjc/Other Analysis Shi ed to Lab between 08/01/93 arid 08/30/
red by: COMTRACTOR+SITE+CASE_NUM
SAS Ship
Number Date 1atrix/Parameter
* Contractor: CD 1F/A1
Site: FORT DEVENS
7572Q/20602 08/20/93 AQ/BNALOCON AQ/P/PLOCON
7804A/20499 08/12/93 A0/524.2
7804A/20601 08/21/93 AQ/524.2
80190/20500 08/05/93 .AQ/BNA AQ/P/P
8019Q/20500 08/11/93 .4Q/BNALOCON .- /P/PLOCON
* Site: FORT DEVENS/SUDBURY TRNG.
7 720/2CdO5 08/25/93 ..\Q/BNALOCON AQ/P/PLOCON
7804A/20497 08/10/93 AQ/524.2
7804A/20604 08/25/93 AQ/524.2
80190/20498 08/04/93 AQ/B IA AQJP/P
Site: IRON HORSE PARK
7798A/20560 08/12,’93 .AQ/353.1
8049A/ 08/12/93 A0/418.1
C “ ntractor * = SAS 11 Hethod = 11
Grand Total ** th S. S = 11 Slethod 11
:******************
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ATTACI CIT TO CJRTEEN
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REQUEBTB FOR THE WEEK OF:
REGION I WEEKLY DAB REQUEBT FORM
DAS #
LAB
TAT
SITE NAME
LOCATION
COMNENPS
I OF
SAMPLES
MATRIX
PARAMETER
CONTRACTOR
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ATTACHMENT FIFTEEN
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DDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDLrD 7
Contract Lab Program - Sample Tracking System W 1D Data
DDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDPDDVDDDDDDDDDDDDDDDDDDDDDDDDDDDDDL’nD
Data Package Mo.:( - ] Case/SAS No:( /
actor..: ( iSite. . :1
Rated: [ 1 S.D.G.:f 1
No. Samples.: [ 0]
)DDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDD000DDDDDDDDDD 6
E?A Sample Nos......:( 1
:1 1
1anks.
Duplicates:
Spikes. . . .
Ship to Lab (09/08193)<—Days
Data Package Recd EPA....:( / / )
CCSRecd .:( / I
CSF Recd .( / / )
Data Validation Complete.:( / /
Since
Due
on
TAT
0)
(10/13193)
( 35)
0)
eviewer. .: [ 1 DV Subcontractor.: [
8
HD 3 3
omments..:3 3
0)
0)
T
Validation Code: ( 1
)DDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDDD =
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ATTACI*tENT SIXTEEN
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CLP Sample Tracking System 09127/93 RLU 0?
Data Pa ckage Validation Code Lookup Report 16:36:19 Page — 1
(All)
Ordered by: PVCODE
Code Description
1 TI l
2 TIER2
3 TI 3
N O VALID T
P PARTIAL T3
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ATTAC1 iT SEVENTEEN
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Add Santple Data
IDDDDDDDDDDDDDDDDDDDDDDDDQDDDDDDDDDDDDDD
Data package
Site:
1atriX
Pararneter
Nun ber of Sa p1eS 0
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