SOP HW-36A
Revision 0
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Hazardous Waste Support Section
SOP No. HW-36A Revision 0
SOM02.2
Pesticide Data Validation
Approvals:
J
Russeft Arnone
Chemist. Hazardous Waste Support Section
C (j
/Sc/s
Date
2, ArC
Cocifzza
Chief hazardous Waste Support Section
XJai/o
Date
Jon/Gab^
Chief, Hazardous Waste Support Branch
/ /?
Date
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NOTICE
The policies and procedures set forth here are intended as guidance to the United States
Environmental Protection Agency (hereafter re 1 erred to as USRPA) and other governmental
employees. They do not constitute rule making by I 'Sl'PA, and may not be relied upon to create
a substantive or procedural right enforceable by any other person. The Government may take
action that is at variance with the policies and procedures in this manual.
The guidance for data validation set forth in the quality assurance project plan (QAPP) for the
project associated with the data in question will always take precedence over the data validation
guidance listed herein.
Validators should note that their professional judgment supersedes any guidance listed in this
document.
Government contractors to the USFPA using this document to validate data should not hesitate
to contact their Contracting Officer Representative with any questions regarding data validation
or data package completeness.
This document can be obtained from the l!STPA's Region 2 Quality Assurance website at:
http://www.eDa.gov/reaion2/qa/documents.htm
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tabu; ok com cm s
NO TICK I
tabu: ok com km s 2
US 1 OI* I AB K K S 3
AC RON V MS ,4
DATA Ql ALIKIKR DKKINITIONS 7
DATA PACKAGK INSPKCHON 7
IIWSS DATA VALIDATION PROCESS 8
PRELIMINARY REVIKW 9
Preservation 10
Gas Chromatograph with Klectron Capture Detector (GC/KCD) Instrument
Performance C heck 12
Initial Calibration 15
Continuing Calibration Verification (CCV) 18
Blanks 20
Surrogate Spikes 23
Matrix Spike/Matrix Spike Duplicates (MS/MSDs) 25
Laboratory Control Samples (LCSs) 26
Horisil ( artridge Performance Check 28
Gel Permeation Chromatography (GPC) Performance Check.................................. 29
Target Compound Identification 30
Gas Chromatograph/Mass Spectrometer ((iC/MS) Confirmation 32
Compound Quantitation and Reported Contract Required Quantitation Limits (CRQL.s)
33
Kield Duplicates 34
Overall Assessment of Data 35
APPKNDIX A: GLOSSARY 36
APPKNDIX B: ORGANIC DATA KXECLTIVK NARRATIVE TEMPLATE 39
APPKNDIX C: SAMPLE ORGANIC DATA SAMPLE SUMMARY 40
APPKNDIX I): KLI C I RONIC DATA DELIVERABLE TEMPLATE 41
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LIST OK TABLKS
Table 1.1 lolding Time Actions for Pesticide Analyses ......... 11
Table 2. Gas Chromatograph with 1 Electron Capture Detector (GC/KCD) Instrument Performance
Check Actions 11
Table 3. Concentration Levels of Calibration Standards.. 15
Table 4. Initial Calibration Actions for Pesticide Analyses 17
Table 5. Continuing Calibration Verification (CCV) Actions for Pesticide Analyses 19
Table 6. Blank Actions for Pesticide Analyses 22
Table 7. Surrogate Actions for Pesticide Analyses 24
Table 10. Pesticides Laboratory Control Sample (I.CS) Spike Compounds and Recovery Limits
26
Table 11. Laboratory Control Sample (LCS) Recovery Actions 27
Table 12. Florisil Cartridge Performance Check Actions 28
Table 13. Gel Permeation Chromatography (GPC) Performance Check Actions 29
Table 14. Action on Qualifying Positive Pesticide Result 31
Table 15. Gas Chromatograph/Mass Spectrometer (GC7IV1S) Conllrmation Actions 32
Table 16. Percent Moisture Actions for Pesticide Analysis For Non-Aqueous Samples 33
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ACRONYMS
%l)
Percent Difference
%RSD
Percent Relative Standard Deviation
A KG
A roc lor
ASH
Analytical Services Branch
BIB
Bromofl uoroben/.ene
CCS
Contract Compliance Screening
CCV
Continuing Calibration Verification
CI
Calibration Factor
C'LP
Contract 1 .aboratory Program
CLP PO
Contract 1 .aboratory Program Project Officer
CRQL
Contract Required Quantitation Limit
(SI
Complete SDG file
DART
Data Assessment Rapid Transmittal
DA 1
Data Assessment Tool
DCH
Decaehlorobiphenyl
1,1 rp V
Decafluorolriphenylphosphine
DMC
Deuterated Monitoring Compound
DQA
Data Quality Assessment
DQO
Data Quality Objective
KDI)
Electronic Data Deliverable
Kl) M
EXES Data Manager
LSAT
Environmental Services Assistance Team
IX IS
Electronic Data eXchange and Evaluation System
GC
Gas Chromatograph
GC/FXD
Gas Chromatograph/Electron Capture Detector
GC/MS
Gas Chromatograph/Mass Spectrometer
GPC
Gel Permeation Chromatography
nwss
1 la/ardous Waste Support Section
IN DA
Individual Standard Mixture A
INDB
Individual Standard Mixture B
IN DC
Individual Standard Mixture G
I.CS
Laboratory Control Sample
MS
Matrix Spike
MSI)
Matrix Spike Duplicate
OSRTI
Office of Superfurtd Remediation and Technology Innovation
PC lis
Polychlorinated Biphenyls
pi:
Per form ance E v aluation
PLM
Performance Evaluation Mixture
QA
Quality Assurance
QAC
Quality Assurance Coordinator
QAPP
Quality Assurance Project Plan
QC
Quality Control
RAS
Routine Analytical Services
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RIC
Reconstructed Ion Chromatogram
RIM)
Relative Percent Difference
RRK
Relative Response factor
RRF
Mean Relative Response f actor
RR'I
Relative Retention Time
RSCC
Regional Sample Control Center Coordinator
RSI)
Relative Standard Deviation
RT
Retention Time
SAP
Sampling and Analysis Plan
SC P
Single Component Pesticide
SIM,
Sample Delivery Group
SIM
Selected Ion Monitoring
SMO
Sample Management OHice
SOP
Standard Operating Procedure
SOW
Statement of Work
TCL
Target Compound List
K LP
Toxicity Characteristics 1 .eachale Procedure
IC X
Tetrachloro-m-xylene
TIC
Tentatively Identified Compound
TO PO
Task Order Project Officer
TR/COC
Traffic Report/Chain of Custodv Record
US EPA
United States Knvironmental Protection Agency
liV
Ultraviolet
VISR
Validated Time of Sample Receipt
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INTRODUCTION
This document is designed to offer the data reviewer guidance in determining the validity of
analytical data generated through the I SI PA Contract Laboratory Program {("I P) Statement of
Work (SOW) for Multi-Media, Multi-Concentration Organics Analysis (SOM02.2), and any
future editorial revisions of SOM02.2, hereinafter referred to as the SOM02.2 SOW. This
guidance is somewhat limited in scope and is intended to be used as an aid in the formal
technical review process.
The guidelines presented in the document will aid the data reviewer in establishing (a) if data
meets the specific technical and QC criteria established in the SOW, and (b) the validity and
extent of bias of any data not meeting the specific technical and QC criteria established in the
SOW. It must be understood by the reviewer that acceptance of data not meeting technical
requirements is based upon many factors, including, but not limited to site-specific technical
requirements, the need to facilitate the progress of specific projects, and availability for re-
sampling.
The reviewer should note that while this document is to be used as an aid in the formal data
review process, other sources ofguidance and information, as wel 1 as professional judgment,
should also be used to determine the ultimate validity of data, especial 1)' in those cases where all
data does not meet specific technical criteria.
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DATA Ql ALII II R DKI INH IONS
The following definitions provide brief explanations of the national qualifiers assigned to results
in the data review process.
u
The analyte was analyzed for, but was not detected above the level of the reported
sample quantitation limit.
J
The result is an estimated quantity. The associated numerical value is the
approximate concentration of the analyte in the sample.
J+
The result is an estimated quantity, but the result may be biased high.
J-
The result is an estimated quantity, but the result may be biased low.
NJ
The analysis indicates the presence of an analyte that has been "tentatively
identified" and the associated numerical value represents its approximate
concentration.
LI J
The analyte was analyzed for, but was not detected. The reported quantitation limit
is approximate and may be inaccurate or imprecise.
R
The data are unusable. The sample results are rejected due to serious deficiencies in
meeting Quality Control (QC) criteria. The analyte may or may not be present in the
sample.
C
T his qualifier applies to results when the identification has been confirmed by Gas
Chromatograph/Mass Spectrometer (GC/MS)
X
This qualifier applies to results when GC/MS analysis was attempted but
unsuccessful
DATA PACK AG 1*1 INSPECTION
For data obtained through the Contract Laboratory Program (CLP), the HXLS Data Manager
(LDM) is a useful tool in the data review process. I'or more information about LDM, please refer
to the following Sample Management Office (SMO) website:
httpsi/zepasmoweb. fedcsc.com/help/uuides/Submit" o2()and°o2()lnspect0 o20Datan o20Quickno20G
uide%20°o28LXLS" o29.pdf
LDM will identify an}' missing and/or incorrect information in the data package. The CLP
laboratory may submit a reconciliation package for any missing items or to correct data.
If there are any concerns regarding the data package, contact the CLP Project Oflker (CLP PO)
from the Region where the samples were taken. For personnel contact information, please refer
to the following CI P website:
http://w\vw'.epa.gov/supeiTund/programs/clp/contacts.htrn
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IIVYSS DATA VALIDATION PROCESS
Alter downloading the data package from I DM, the data validator will use the recommendations
in this SOP as well as their own professional judgment to validate the data.
All data is initially marked as "reportable" (Y) in EDM before validation is begun. Sometimes,
due to dilutions, re-analyses, or SlM/scan runs all being performed, there will be multiple results
for a single analyte from a single sample. The following criteria and professional judgment are
used to determine which result should be reported:
The analysis with the lower CRQL
The analysis with the better QC results
The analysis with the higher result
The analyte values and their respective CRQI.s are then transferred into a single sample run. The
runs that are not to be used are updated as "not reportable" or (N) in KDM.
The data will be saved in the following location, under the appropriate case number folder:
t.i: DESADIV IIWSS DM A VALIDATION
The file naming conventions will consist of
A. case number i.e., 12345
B. SDG name i.e., BXYI2
C. level of validation performed i.e., S3VL
Examples: 12345JiXYl 2_S3VE.xls
12345 li\YI2 S3VI.M.\Is
When data validation is completed, the data package is uploaded for the client to download from
the I iWSS data delivery website:
The completed data package includes the Executive Narrative (see Appendix B for template), the
Sample Summary Report (see Appendix C for example), and the Electronic Data Deliverable
(EDD) (see Appendix I) for a list of the column headers included in this document).
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PRKLIMINARY UK VIEW
This document is for the review ofanalytical data generated through the SOM02.2 SOW and any
future editorial revisions of SOM02.2 for TSTPA Region 2. To use this document effectively,
the reviewer should have an understanding of the analytical method and a general overview of
the Sample Deliver}' Group (SDG) or sample Case at hand. The exact number of samples, their
assigned numbers, their matrix, and the number of laboratories involved in the analysis are
essential information.
It is suggested that an initial review of the data package be performed, taking into consideration
all information specific to the sample data package [e.g.. Modi lied Analysis requests, Traffic
Report/Chain of Custody (TR/COC) documentation, SDG Narratives, etc.].
The reviewer should also have a copy of the Quality Assurance Project Plan (QAPP) or similar
document for the project for which the samples were analyzed. The criteria for data validation
outlined in the QAPP supersede this Standard Operating Procedure. The reviewer should contact
the appropriate Regional Contract Laboratory Program Project Officer (C I P PO) to obtain
copies of the QAPP and relevant site information. This information is necessary in determining
the final usability of the analytical data.
The SDGs or Cases routinely have unique samples that require special attention from the
reviewer. These include Held blanks and trip blanks. Held duplicates, and Performance
Evaluation (PI:) samples which must be identified in the sampling records. The sampling records
(e.g.. TR/COC records. Held logs, and/or contractor tables) should identify:
1. The Region where the samples were taken,
2. The Case number,
3. The complete list oI'samples with information on:
a. Sample matrix;
b. Field blanks (i.e., equipment blanks or rinsate blanks) and trip blanks:
c. Field duplicates;
d. Field spikes;
e. QC audit samples;
f. Shipping dates;
g. Preservatives; and
h. Laboratories involved.
The TR/COC documentation includes sample descriptions and date(s) of sampling. The reviewer
must consider lag times between sampling and start of analysis when assessing technical sample
holding times.
T he laboratory's SDG Narrative is another source of general information. Notable problems with
matrices, insufficient sample volume for analysis or reanalysis, samples received in broken
containers, preservation, and unusual events should be documented in the SDG Narrative. The
reviewer should also inspect any email or telephone/communication logs detailing any
discussion of sample or analysis issues between the laboratory, the CLP Sample Management
Office (SMO). and USHPA Region 2.
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Prcsen ation
Action;
1. Qualify aqueous sample results using preservation and technical holding time
information as follows (see Table 1):
a. If there is no evidence that the samples were properly preserved (T ^ 4CC ±
2°C), and the samples were extracted or analyzed within the technical
holding times [seven (7) days from sample collection for extraction; 40 days
from sample collection for analysis], qualify detects as estimated (J) and non-
detects as estimated (UJ).
b. If there is no evidence that the samples were properly preserved (T - 4rC ±
2r'C), and the samples were extracted or analyzed outside the technical
holding times [seven (7) days from sample collection for extraction; 40 days
from sample collection for analysis], qualify detects as estimated (J) and non-
dctects as estimated (UJ).
c. If the samples were properly preserved, and were extracted and analyzed
within the technical holding times [seven (7) days from sample collection for
extraction; 40 days from sample collection for analysis], no qualification of
the data is necessary.
d. If the samples were properly preserved, and were extracted or analyzed
outside the technical holding limes [seven (7) days from sample collection
for extraction; 40 days from sample collection for analysis], qua lily detects
as estimated (J) and non-detects as estimated (UJ). Note in the Data Review
Narrath e that holding times were exceeded and the effect of exceeding the
holding time on the resulting data,
2. Qualify non-aqueous sample results using preservation and technical holding time
information as follows (see Table 1):
a. If there is no evidence that the samples were properly preserved (T - 4CC ^
2CC), and the samples were extracted or analyzed within the technical
holding time [14 days from sample collection for extraction; 40 days from
sample collection for analysis], qualify detects as estimated (J) and non-
detects as estimated (UJ).
b. If there is no evidence that the samples were properly preserved (T - 4 C =
2CC), and the samples were extracted or analyzed outside the technical
holding time [14 days from sample collection for extraction; 40 days from
sample collection for analysis], qualify detects as estimated (J) and non-
detects as estimated (UJ).
c. If the samples were properly preserved, and were extracted and analyzed
within the technical holding time [14 days from sample collection for
extraction; 40 days from sample collection for analysis], no qualification of
the data is necessary.
d. If the samples were properly preserved, and were extracted or analyzed
outside the technical holding time 114 days from sample collection for
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extraction; 40 days from sample collection for analysis], qualify detects as
estimated (J) and nun-detects as estimated (UJ). Note in the Data Review
Narrative that holding times were exceeded and the effect of exceeding the
holding time on the resulting data.
3. Whenever possible, the reviewer should comment on the effect of the holding time
exceedance on the resulting data in the Data Rev iew Narrative.
4. Use professional judgment to qualify samples whose temperature upon receipt at the
laboratory is either below 2 degrees centigrade or above 6 degrees centigrade,
5. If technical holding times are grossly exceeded, use professional judgment to qualify the
data.
6. Note, for Contract Laboratory Program Project Officer (CLP PO) action, when technical
holding times are exceeded.
Table I. Holding Time Actions for Pesticide Analyses
Matrix
Preserved
Criteria
Action
Detected
Associated
Compounds
Non-Detected
Associated
Compounds
Aqueous
No
< 7 days (for extraction)
< 40 days (for analysis)
J
UJ
Nu
> 7 days (for extraction)
> 40 days (for analysis)
J
I 1
Yes
1 7 days {for extraction)
< 40 days (for analysis)
No qualification
Yes
> 7 days (for extraction)
> 40 days (for analysis)
J
UJ
Yes/No
Grosslv F.xceeded
Use professional judgment
Non-Aqueous
No
£ 14 days (for extraction)
< 40 days (for analysis)
J
UJ
No
> 14 days (for extraction)
> 40 days (for analysis)
J
UJ
\ es
< 14 days (for extraction)
i 40 days (for analysis)
No qualification
Yes
¦> 14 days (for extraction)
> 40 days (for analysis)
J
UJ
Yes No
Grossh I Acceded
Use professional judgment
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Gas Clirom;uograi)h with Electron Capture Detector ((rC/'ECl)) Instrument Performance
Check
Action:
1. Resolution Check Mixture
a. The resolution between two adjacent peaks in the Resolution Check Mixture
must be greater than or equal to 80.0% for all analytes for the primary column
and greater than or equal to 50.0° o lor the confirmation column in order to use
one Individual Standard Mixture (C). The resolution between two adjacent
peaks in the Resolution Check Mixture must be greater than or equal to 60.0%
if two Individual Standard Mixtures (A and B) are to be used, irresolution
criteria are not met, the quantitative results may not be accurate due to
inadequate resolution. Qualitative identifications may also be questionable if
coelution exists.
i. Qualify detects lor target compounds that were not adequate!} resolved
as tentatively identilied (NJ) (see Table 2).
ii. Qualify non-detected compounds as unusable (R).
2. PHM
a. If PHM analysis is not performed at the required frequency (see Pesticides
Organic Analysis, of SOM02.2 NFG), qualify all associated sample and blank
results as unusable (R).
b. The resolution between any two adjacent peaks in the initial calibration and
continuing calibration verification PHMs must be greater than or equal to 90% on
each GC column. If PHM resolution criteria are not met. the quantitative results
may not be accurate due to inadequate resolution. Qualitative identifications may
be questionable if coelution exists.
i. Qualify detects as tentatively identified (NJ).
ii. Qualify non-del eels as unusable (R).
c. If4,4'-DDT breakdow n is greater than 20.0%:
i. Qualify detects for 4.4'-l)I) f as estimated (J).
ii. Qualify detects for 4,4'-DDD and/or 4,4'-DI)H as estimated (J).
iii. If4,4'-I)D H was not detected, but 4.4'-I)DD and/or 4.4'-l)I)H were
detected, qualify non-detects for 4.4'-I)I)T as unusable (R). and qualify
delects for 4.4'-!)!)!) and/or 4,4'-DDH as presumptively present at an
approximated quantity (NJ).
d. 1 f Hndrin breakdown is greater than 20.0%:
i. Qualify detects for Hndrin as estimated (J).
ii. Qualify detects for Hndrin aldehyde and/or Hndrin ketone as estimated (J).
iii. If Hndrin was not detected, but Hndrin aldehyde and/or Hndrin ketone
were detected, qualify the non-detects for Hndrin as unusable (R), and
qualify detects for Hndrin aldehyde and/or Hndrin ketone as presumptively
present at an approximated quantity (NJ).
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e. If the combined 4,4'-DI)T and Kndrin breakdown is greater than 30.0%. the
review er should consider the degree of individual breakdown of4„4'-DDT and
Kndrin and apply qualifiers as described in this section.
Mid-point Individual Standard Mixtures (A and R) or (C)
a. If mid-point Individual Standard Mixture analysis is not performed at the required
frequency (see Pesticides Organic Analysis, of SOM02.2 NFG), quality all
associated sample and blank results as unusable (R).
b. The resolution between any two adjacent peaks in the mid-point concentration of
Individual Standard Mixtures (A and B) in the initial calibration and continuing
calibration verification must be greater than or equal to 90.0% on each column.
The resolution between any two adjacent peaks in the mid-point concentration of
Individual Standard Mixture (C) in the initial calibration and continuing
calibration verification must be greater than or equal to 80.0°6 for the primary
column and greater than or equal to 50.0% for the secondary column. If mid-point
Individual Standard Mixtures (A and B) or (C) resolution criteria are not met, the
quantitative results may not be accurate due to inadequate resolution. Qualitative
identifications may be questionable if coelution exists.
i. Qualify detected target compounds that were not adequately resolved
tentatively identified (NJ).
ii. Qualify non-detecls as unusable (R).
Note in the Data Review Narrative the potential efleets on the sample data resulting from
the instrument performance check criteria. Notify the Contract Laboratory Program
Project Officer (CLP PO) if the laboratory has repeatedly lai led to comply with the
requirements for linearity, resolution, or 4,4'-DD 1'I 'ndrin breakdown.
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Table 2. Gas Chromatograph with Klectron Capture Detector (G( 7K( 1>) Instrument
Performance Check Actions
Criteria |Individual
Standard Mixtures
( A and li)|
Criteria (Individual Standard
Mixture C)
Action
Resolution Check
Mixture
°0 Resolution <60.0%
Resolution Check Mixture
% Resolution <80.0% (primary
column)
% Resolution <50.0% (secondary
column)
Detects; Ml
Non-detects: R
PKM °o Resolution <90.0%
Detects: NJ
Non-detects: R
PKM: 4,4'-DDT °o Breakdown >20.0% and 4,4'-DDT is
detected
Detects for 4.4'-DI)T: J
Detects for 4,4'-DDD: .1
Detects for 4,4'-DDI:: J
PKM: 4.4'-DDT % Breakdown -'20.0% and 4.4'-f)I)i is not
detected
Non-detects for 4.4'- DDT: R
Detects for 4.4'-I)I)l): NJ
Detects for 4.4'-DDI-:: NJ
PEM: Kndrin % Breakdown >20.0% and Kndrin is detected
Detects for Tndrin: J
Detects for Kndrin aldehy de: J
Detects for Kndrin ketone: J
PKM: Kndrin % Breakdown >20.0% and Kndrin is not
detected
Non-detects for Kndrin: R
Delects for Kndrin aldehyde: NJ
Detects for Kndrin ketone: NJ
PKM: Combined °o Breakdown >30°o
Apply qualifiers as described
above considering degree of
individual breakdown.
Mid-point Individual
Standard Mixtures (A
and B)
% Resolution <90.0%
Mid-point Individual Standard
Mixture (C)
% Resolution <80.0% (primary
column)
Mid-point Individual Standard
Mixture (C)
% Resolution <50.0% (secondary
column)
Detects: NJ
Non-detects: R
PKM analysis not performed at the required Frequency (see
Pesticides", ofSOM02.2 NFG)
All results: R
Mid-point Individual Standard Mixtures analysis not
performed at the required frequency (see Pesticides, of
SOM02.2 NFG)
All results: R
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Inilial Calibration
Table3, Concentration Levels of Calibration Siaiulards
( (impound
Concern ration (n«/mL)
CS1
CS2
CS3
CS4
CSS
alpha-BHC
5.0
10
20
40
80
gamma-BHC
5.0
10
20
40
80
Heptachlor
5.0
10
20
40
80
Hndosulfan I
5.0
10
20
40
80
Dieldrin
10
20
40
80
160
Hndrin
10
20
40
80
160
4.4-1)1)1)
10
20
40
80
160
4.4'-!)l) 1
10
20
40
80
160
Methoxvchlor
50
100
200
400
800
beta-BI-IC
5,0
10
20
40
80
delta-BHC
5.0
10
20
40
80
Aldrin
5.0
10
20
40
80
1 leptachlor-epoxide
5.0
10
20
40
80
4,4'-DDH
10
20
40
80
160
Hndosullan 11
10
20
40
80
160
Hndosulfan sulfate
10
20
40
80
160
Hndrin ketone
10
20
40
80
160
Hndrin aldehvde
10
20
40
80
160
alpha-Chlordane
5.0
10
20
40
80
gamma-C'hlordane
5.0
10
20
40
80
Tetrachloro-m-xvlene
5.0
10
20
40
80
Decaehlorobiphenyl
10
20
40
80
160
Toxaphene
500
1000
2000
4000
8000
Action,:
NOTES: At least one chromatogram from each of the Individual Standard Mixtures (A and
B) or (C) must yield peaks that give recorder defections between 50-100% oi"full
scale.
Hither peak area or peak height may be used to calculate the Calibration Factors
(CTs) that are, in turn, used to calculate °oRSl). However, the type of peak
measurement used to calculate each Cl; lor a given compound must be consistent.
For example, if peak area is used to calculate the low-point CF lor Hndrin,, the
mid-point and high-point CFs for Hndrin must also be calculated using peak area.
1. If the proper initial calibration sequence is not performed, or the steps of the initial
calibration are not followed in the proper sequence, use professional judgment to evaluate
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the effect on the data and notify the Contract Laboratory Program Project Officer (CLP
PO) (see Table 4). This is especially critical for the low-level standards and non-detects.
2. If RT Windows are not calculated correctly, recalculate the windows and use the
corrected values for all evaluations.
3. If the chroniatogram display (recorder deflection) criteria are not met, use professional
judgment to evaluate the effect on the data.
4. If the standard concentrations listed in Table 3 are not used, use professional j udgment to
evaluate the effect on the data and notify the CLP PO. This is especially critical for the
low-level standards and non-detects.
5. The Percent Relative Standard Deviation (%RSD) of the CPs for each of the single
component target compounds must be less than or equal to 20.0%, except for alpha-BHC
and delta-BI IC. The %RSD of the CFs for alpha-BHC and delta-BHC must be less than
or equal to 25.0° o. The %RSD of the CFs for each of the Toxaphene peaks must be £
30% when 5-point ICAL is performed.The %RSD of the CFs for the two surrogates
(tetrachloro-m-xylene and decachlorobipheny 1) must be less than or equal to 30.0%. If
the %RSD criteria are not met, qualify detects as estimated (J) and use professional
judgment to qualify non-detected target compounds.
6. If the %RSD criteria are within allowable limits, no qualification of the data is necessary.
7. At the reviewer's discretion, and based on the project-specific data quality objectives,
consider a more in-depth review using the following guidelines:
a. If any pesticide target compound has a %RSI) greater than the maximum
criterion, and if eliminating either the high or the low-point of the curve does not
restore the %RSI) to less than or equal to the required maximum:
i. Qualify detects for that compound(s) as estimated (J).
ii. Qualify non-detected pesticide target compounds using professional
judgment,
b. If the high-point of the curve is outside of the linearity criteria (e.g.. due to
saturation):
i. No qualifiers are required for detects in the linear portion of the curve.
ii. Qualify detects outside oflhe linear portion of the curve as estimated (J).
iii. No qualifiers are required for pesticide target compounds that were not
detected.
c. If the low-point oflhe curve is outside of the linearity criteria:
i. No qualifiers are required for detects in the linear portion oflhe curve.
ii. Qualify low-level detects in the area of non-linearity as estimated (J).
iii. For non-detected pesticide compounds, use the lowest point of the linear
portion of the curve to determine the new quantitation limit.
8. Note in the Data Review Narrative potential effects on the sample data due to problems
with calibration. Notily the CLP PO if the laboratory has repeated!)' failed to comply
with the requirements for frequency, linearity, RT. or resolution.
9. Quality data for Toxaphene sharing the same RT Window with any Single Component
Pesticide (SCP) in any Individual Standard Mixture using professional judgment.
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Tahle4. Initial Calihralion Actions for Pesticide Analyses
Criteria
Action
Detected Associated
Compounds
Non-Detected
Associated Com pounds
Initial calibration is not performed or not performed
in the proper sequence
Use professional judgment and notify CLP PO
°oRSD exceeds allowable limits*
J
Use professional
judgment
0c»RSI) within allowable limits*
No qualification
* %RSD 2_20.0°'o for single component target compounds except alpha-BIlC and delta-B!!('.
{, oRSI) <25.0% for alpha-Bl IC and delta-BUC.
%RS1) <30.0? o for Toxaphene peaks.
" uRSI) <_30.0% for surrogates (letrachloro-m-xvlene and decachlorobiphenyl).
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Continuing Calibration Verification (C'C'V)
Action;
1. The RT Windows are used in qualitative identilleation. If the standards do not fall
within the R I Windows, carefully evaluate the associated sample results (see Table 5).
All samples injected alter the last in-control standard are potentially affected.
a. For non-detected target compounds in the affected samples, check to see if the
sample chromatograms contain any peaks that are close to the expected RT
Window of the pesticide of interest.
i. If no peaks are present, consider non-detected values to be valid and no
qualification of the data is necessary.
ii. If any peaks are present close to the expected R I Window of the
pesticide of interest, use professional judgment to qualify the non-detects
as presumptively present fNJ).
b. For detected compounds in the affected samples, if the peaks are within the RT
Window, no qualification of the data is necessary. However, if the peaks are
close to the expected RT Window of the pesticide of interest, the reviewer may
take additional effort to determine if sample peaks represent the compounds of
interest.
For example, the reviewer can examine the data package for the presence of
three or more standards containing the pesticide of interest that were run within
the analytical sequence during which the sample was analyzed. If three or more
such standards are present, the RT Window can be re-evaluated using the Mean
Retention Times (RTs) of the standards.
i. If the peaks in the affected sample fall within the revised window, qualify
detects as tentatively identified (NJ).
ii. If the reviewer cannot do anything with the data to resolve the problem of
concern, qualify all non-detects as unusable (R).
2. For the P1:M, if the Percent Difference is not within ±25.0° o, qualify associated detects
as estimated (J) and non-detects as estimated (UJ).
3. For the Calibration Verification Standard (CS3), if the Percent Difference is not within
±25.0°o, qualify associated detects as estimated (J» and non-detects as estimated (UJ).
4. If 4,4'-DDT 0..Breakdown is - 20.0%, qualify detected 4,4'-DDT, 4,4'-DDD, and 4,4'-DDE as
estimated (J). When 4.4-DDT is not detected, but 4,4'-DDD and 4.4'-DDH are detected, qualify
non-detected 4,4'-DDT as unusable (R) and detected 4,4'-DDD and 4,4 -1)1)1. as presumptively
present with estimated concentration (NJ).
If Endrin %Breakdo\vn > 20.0%. qualify detected Endrin, Endrin aldehjde and Hndrin ketone as
estimated (J). When Endrin is not detected, but Endrin aldehyde and Endrin ketone are detected,
5. qualify non-detected Endrin as unusable (R) and detected Endrin aldehyde and Endrin ketone as
presumptively present with estimated concentration (NJ). If more than 14 hours has elapsed
from the injection of the instrument blank that begins an analytical sequence (opening
(TV) and the injection of either a PI: VI or mid-point concentration of the Individual
Standard Mixtures (A and B) or (C). qualify all data as unusable (R).
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6. 11" more than 12 hours has elapsed from the injection of the instrument blank that begins
an analytical sequence (opening CCV) and the injection of the last sample or blank that
is part of the same analytical sequence, qualify all data as unusable (R).
7. H" more than 72 hours has elapsed from the injection of the sample with a Toxaphene
detection and the Toxaphene Calibration Verilocation Standard (CS3), qualify all data as
unusable (R).
8. If the Percent Difference, time elapsed, and R Is are within acceptable limits, no
qualification of the data is necessary.
9. Note in the Data Review Narrative potential effects on the sample data due to problems
with calibration.
Fable 5. Continuing Calibration Verification (CCV) Actions for Pesticide Anahses
Criteria
Action
Detected Associated
Compounds
Non-Detected
Associated Compounds
RT outofRT window
Use professional judgment
°oD not within limits*
J
rj
Time elapsed is greater than acceptable limits**
R
°oD, time elapsed, and R f are within
acceptable limits
No qualification
PEM: 4.4'-DDT ^.Breakdown >20.0% and 4.4'-
DDT is detected
j for 4,4'-DDT. 4,4'-
1)1)1). and 4.4'-l)l)E
No qualification
PKM: 4,4'-I)DT % Breakdown --20.0% and 4,4'-
I)D I is not detected
R lor 4.4 -1 )[> I
\.I lor 4.4-1)1)1) and
4,4'-f)f)i;
PKM: Endrin %Breakdo\\n -"20.0% and Hndrin is
detected
j for Endrin,
Endrin aldehyde, Endrin
ketone
No qualification
PEM: Endrin "'((Breakdown ""--20.0% and Endrin is
not detected
R for Endrin
NJ for aldehyde and
Endrin ketone
See Actions 2 and 3
See Actions 5, 6, and 7
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Blanks
Action:
NOTES: The concentration of non-target compounds in all blanks must be less than or
equal to 10 j.ig/1,.
The concentration of each target compound found in the method or Held blanks
must be less than its CRQL listed in the method.
Data concerning the Held blanks are not evaluated as part of the CCS process. If
field blanks are present, the data reviewer should evaluate this data in a similar
fashion as the method blanks.
NOTES: "Water blanks, "drill blanks", and "distilled water blanks" are validated like any
other sample and are not used to qualify data. Do not confuse them with the other
QC blanks discussed below.
All Held blank results associated with a particular group of samples (may exceed
one per case) must be used to qualify data. Blanks may not be qualified because
of contamination in another blank. Field blanks must be qualiiied for system
monitoring compounds, instrument performance criteria, and spectral or
calibration QC problems.
Analytes qualiiied "U" for blank contamination are treated as "hits" when
qualifying for calibration criteria.
Samples taken from a drinking water tap do not have associated field blanks.
When applied as described in Table 6 below, the contaminant concentration in the
blank is multiplied by the sample dilution factor.
Action regarding unsuitable blank results depends on the circumstances and origin of the
blank. In instances where more than one of the same type of blank is associated with a given
sample, qualification should be based upon a comparison with the associated blank having the
highest concentration of a contaminant. Do not correct the results by subtracting any blank
value.
1. If a target SCP or Toxaphene is found in a method blank, but not found in the sample, no
qualification of the data is necessary (see 'fable 6).
2. If a target SCP or Toxaphene concentration in a method or Held blank is less than the
CRQI. and:
a. the sample concentration is less than the CRQI.. report the CRQI. value with a
"IT.
b. the sample concentration is greater than or equal to the CRQL, no qualification is
required.
3. If a target SCP or Toxaphene concentration in a method or Held blank is greater than the
CRQL mid:
a. the sample concentration is less than the CRQI., report the CRQL value with a
"ir.
b. the sample concentration is greater than or equal to the CRQL, and less than or
equal to the blank concentration, report the concentration of the compound in the
sample at the same concentration found in the blank and qualify with a "IP,
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c. the sample concentration is greater than or equal to the CRQL and greater than the
blank concentration, no qualification is required.
4. if a target SCT or Toxaphene concentration in a method or field blank is equal to the
CRQLand:
a. the sample concentration is less than or equal to the CRQL, report the CRQL
value with a "lr,
b. the sample concentration is greater than the CRQL, no qualification is required.
5. If gross contamination exists (i.e., saturated peaks, "hunip-o-grams", "junk" peaks), raise
the CRQL to the level of the blank contamination and report the associated sample data
below this level as CRQL-U, Non-detected pesticide target compounds do not require
qualification unless the contamination is so high that it interferes with the analyses of
non-detected compounds.
6. If contaminants are found in the field blanks, the following is recommended:
a. Review the associated method blank data to determine if the contain inant(s) was
also present in the method blank.
i. If the analyte was present at a comparable level in the method blank, the
source of the contamination may be in the analytical system and the action
recommended for the method blank would apply.
ii. If the analyte was not present in the method blank, the source of
contamination may be in the storage area, in the field, or during sample
transport. Consider all associated samples for possible cross-
contamination.
7. If method blank data are unavailable, the reviewer may use professional judgment or
substitute field blank data for missing method blank data.
NOTE: There may be instances where little or no contamination was present in the
associated blanks, but qualification of the sample is deemed necessary. If the
reviewer determines that the contamination is from a source other than the
sample, they should qua lily the data. Contamination introduced through dilution
water is one example. Although it is not always possible to determine, instances
of this occurring can be detected when contaminants are found in the diluted
sample result, but are absent in the undiluted sample result.
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Table 6. Blank Actions for Pesticii
e Analyses
Blank Type
Blank Result
Sample Result
Action for Samples
Method. Sulfur
Cleanup,
Instrument
Field,
TCLP/SPLP
Detects
Not delected
No qualilication required
- C'RQI.
C'RQI.
Report C'RQI. \alue with a U
C'RQi.
No qualification required
C'RQI.
C'RQl.
Report C RQI. value with a U
C'RQI. and .
blank concentration
Report blank value lbr sample
concentration w ith a t"
C'RQi and
blank concentration
No qualilication required
C'RQI.
IA
r
O
Report C'RQI value with a U
C'RQI.
No qualilication required
Gross
contamination
Detects
Report blank value lor sample
concentration with a U
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Surrogate Spikes
Action:
If either surrogate spike recover} is outside the acceptance limits, the reviewer must consider
the existence ofcoelution and interference in the raw data and use professional judgment to
qualify data, as surrogate recovery problems may not directly apply to target analytes.
1. For any surrogate recover)1 greater than 150% (see Table 7):
a. Qualify detected target compounds as biased high (J+).
b. Do not quality non-detected target compounds.
2. If both surrogate recoveries are greater than or equal to 30%, and less than or equal to
150%, no qualification of the data is necessary.
3. For any surrogate recovery greater than or equal to 10%. and less than 30%:
a. Qualify detected target compounds as biased low (J-),
b. Qualify non-detected target compounds as approximated (UJ).
4. For any surrogate recover}1 less than 10%, the reviewer should examine the sample
chromatogram to assess the qualitative validity of the analysis. If low surrogate
recoveries are from sample dilution, professional judgment should be used to determine if
the resulting data should be qualified. If sample dilution is not a factor:
a. Qualify detected target compounds as biased low (J-),
b. Quali ly non-detected target compounds as unusable (R).
5. In the special case of a blank analysis with surrogates out of specification, the reviewer
must give special consideration to the validity of associated sample data. The basic
concern is whether the blank problems represent an isolated problem with the blank
alone, or whether there is a fundamental problem with the analytical process. For
example, if one or more samples in the batch show acceptable surrogate recoveries, the
reviewer may choose to consider the blank problem to be an isolated occurrence. Note,
for Contract I.aboratory Program Project Ofticer (CLP PO) action, analytical problems
even if this judgment allows some use of the affected data.
6. If surrogate RTs in PI {Ms, Individual Standard Mixtures, samples, and blanks are outside
of the R I' Windows, the reviewer must use professional judgment to qualify data.
7. If surrogate RTs are within R I windows, no qualification of the data is necessary.
8. If the two surrogates were not added to all samples, MS/MSDs, standards, FCSs, and
blanks, use professional judgment in qualifying data as missing surrogate analyte ma}1 not
directly apply to target analytes.
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Table 7. Surrogate Actions lor Pesticide Analyses
Action*
Criteria
Detected Target
Non-detected Target
Com pounds
Compounds
%R> 150%
J+
No qualillcation
30% < %R < 150%
No qualification
10°o < °0R < 30°o
J-
UJ
%R < 10% (sample dilution not a factor)
J-
R
°oR < 10% (sample dilution is a factor)
Use professional judgment
RT out of RT window
Use professional judgment
RT within R 1 window
No qualification
Use professional judgment in qualifying data, as surrogate recovery problems may not
directly apph to target analytes.
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Matrix Spike/Matrix Spike Duplicates (MS/MSI)s)
Action;
NOTES: Data lor MS and MSDs will not be present unless requested by the Region.
Notify the Contract Laboratory Program Project Officer (CLP PO) if a Held blank
was used for the MS and MSI), unless designated as such by the Region.
NO IT.: Lor a Matrix Spike that does not meet criteria, apply the action to only the field
sample used to prepare the Matrix Spike sample. If it is clearly stated in the data
validation materials that the samples were taken through incremental sampling or
some other method guaranteeing the homogeneity of the sample group, then the
entire sample group may be qualified.
1. No qualification of the data is necessary on MS and MSI) data alone. However, using
professional judgment, the validator may use the MS and MSI) results in conjunction
with other QC criteria and determine the need for some qualification of the data.
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Laboratory Control Samples 1 LCSs)
Table 10. Pesticides Laboratory Control Sample (LCS) Spike Compounds and Recovery
Limits
LCS Spike Compound
Recovery Limits (%)
gamma-BI IC
50 - 120
Heptachlor epoxide
50 - 150
Dieldrin
30-130
4,4"-DDl:
50 - 150
Lndrin
50 120
F.ndosullan sulfate
¦ji
0
1
to
o
trans-Chlordane
30 - 130
I etrachloro-m-xy 1 ene (surrogate)
30 - 150
Deeachlorobiphenyl (surrogate)
30 - 150
Action:
NOTES: The recovery limits for any of the compounds in the l.CS may be expanded at any-
time during the period of performance if USLPA determines that the limits are too
restrictive.
All samples prepared and analyzed with an LCS that does not meet the technical
acceptance criteria in the method will require re-extraction and re-analysis.
If the ICS criteria are not met, laboratory performance and method accuracy are in question. Use
professional judgment to determine if the data should be qualified or rejected. The following
guidance is suggested for qualifying sample data for which the associated LCS does not meet the
required criteria.
1. If the LCS recover}' criteria are not met, use the 1 .CS results to qualify sample data for
the specific compounds that are included in the ICS solution (see Table 11).
a. If the LCS recovery exceeds the upper acceptance limit, qualify detected target
compounds as estimated (J). Do not qualify non-detected target compounds.
b. If the LCS recovery is less than the lower acceptance limit, qualify detected
target compounds as estimated (J) and non-detects as unusable (R).
c. Use professional judgment to qualify data for compounds other than those
compounds that are included in the l.CS.
d. l-se professional judgment to qualify non-1 .CS compounds. Take into account
the compound class, compound recovery efficiency, analytical problems
associated with each compound, and comparability in the performance of the
LCS compound to the non-LCS compound.
2. If the LCS recovers- is within allowable limits, no qualification of the data is necessary.
3. Note, for Contract Laboratory Program Project Officer (CLP PO) action, if a
laboratory' fails to analyze an LCS with each Sample Delivery Group (SDG), or if the
reviewer has knowledge that a laboratory consistently fails to generate acceptable LCS
recoveries.
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Tahle 11. Laboratory Control Sample (LCS) Recovery Actions
Action
Criteria
Detected
Non-Detected
Associated
Associated
Compounds
Com pounds
°oR > Upper Acceptance Limit
J+
No qualification
°oR < Lower Acceptance Limit
J-
R
Lower Acceptance Limit < °oR < Upper
Acceptance Limit
No qualification
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Florisil Cartridge Performance ( heck
Action;
NOTE: Florisil cartridge cleanup is mandatory for aU extracts.
1. If the Florisil Cartridge Performance Check criteria are not met, examine the raw data
for the presence of polar interferences and use professional judgment in qualifying the
data as follows (see Table 12):
a. I f the Percent Recovery is greater than 120% for any of the pesticide target
compounds in the Florisil Cartridge Performance Check, qualify detected
compounds as estimated (J). Do not quality non-detected target compounds.
b. If the Percent Recover)1 is greater than or equal to 80% and less than or equal to
120% for all the pesticide target compounds, no qualification of the data is
necessary.
c. If the Percent Recover}' is greater than or equal to 10% and less than 80% for any
of the pesticide target compounds in the Florisil Cartridge Performance Check,
qualify detected target compounds as estimated (J) and non-detected target
compounds as approximated (UJ).
d. If the Percent Recovery is less than 10% for any of the pesticide target
compounds in the Florisil Cartridge Performance Check, qualify detected
compounds as estimated (J) and qualify non-detected target compounds as
unusable (R).
e. If the Percent Recovery of 2,4,5-trichlorophenol in the Florisil Cartridge
Performance Check is greater than or equal to 5%. use professional judgment to
qualify detected and non-detected target compounds, considering interference on
the sample chromatogram.
2. Note in the Data Review Narrative potential effects on the sample data resulting from
the Florisil Cartridge Performance Check analysis not yielding acceptable results.
Table 12. Morisil Cartridge Perfor mance Check Actions
Action
Criteria
Detected Associated
Non-Detected
Compounds
Associated Compounds
%R > 120% (pesticide target
compounds)
J
No qualification
80% < °oR < 120%
No quali
ication
10% < %R -'80°o (pesticide target
j
UJ
compounds)
%R < 10% (pesticide target compounds)
J
R
%R > 5% (2,4,5-trichlorophenol)
Use professional judgment*
Check sample chromatogram for interferences.
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(.el Permeation Chromatography (GPC) Performance Check
Action;
NOTE: GPC cleanup is mandatory for all soil samples.
1. If GPC criteria are not met, examine the raw data for the presence of high molecular
weight contaminants; examine subsequent sample data for unusual peaks; and use
professional judgment in qualilying the data. Notify the Contract Laboratory Program
Project Officer (CLP PO) if the laboratory chooses to analyze samples under
unacceptable GPC criteria.
2. If the Percent Recovery is less than 10% for the pesticide compounds and surrogates
during the GPC calibration check, the non-detected target compounds may be suspect.
Qualify detected compounds as estimated (J) (see 'fable 13). Qualify all non-detected
target compounds as unusable (R).
3. If the Percent Recover}' is greater than or equal to 10% and is less than 80% for any of
the pesticide target compounds in the GPC calibration, qualify detected target compounds
as estimated (J) and non-detected target compounds as approximated (L"J).
4. If the Percent Recovery is greater than or equal to 80% and less than or equal to 120% for
all the pesticide target compounds, no qualification of the data is necessary.
5. If high recoveries (i.e., greater than 120%) were obtained for the pesticides and
surrogates during the GPC calibration check, qua lily detected compounds as estimated
(J). Do not qualify non-detected target compounds.
6. Note in the Data Review Narrative potential effects on the sample data resulting from the
GPC cleanup analyses not y ielding acceptable results.
Table 13, Gel Permeation Chromatography (GPC) Performance Cheek Actions
Action
Criteria
Detected Associated
Non-Detected
C om pounds
Associated Com pounds
%R 10% (pesticide target compounds)
J
R
10%-%R -- 80%
J
UJ
80%i£%R^ 120%
No quali
1 cat ion
%R 120°o (pesticide target compounds)
J
No qualilication
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In met Coin pound Identification
Criteria:
1. The Retention Times (RTs) of both of the surrogates and reported target compounds in
each sample must be within the calculated RT Windows on both columns. Tetrachloro-
m-xylene (TCX) must be within ±0,05 minutes of the Mean RT ( RT ) determined from
the initial calibration and Decachlorobiphenyl (DCB) must be within ±0.10 minutes of
the RT determined from the initial calibration.
2. The Percent Difference (°oD) for the detected mean concentrations of a pesticide target
compound between the two Gas Chromatograph (GC) columns must be within the
inclusive range of ^25.0.
3. When no analytes are identified in a sample, the chromatograms from the analyses of the
sample extract must use the same scaling factor as was used for the low-point standard of
the initial calibration associated with those analyses.
4. Chromatograms must display Single Component Pesticides (SCPs) detected in the sample
and the largest peak of any multi-component analyte detected in the sample at less than
full scale.
5. If an extract must be diluted, chromatograms must display SCPs peaks between 10-100%
of full scale, and multi-component analytes between 25-100% of full scale.
6. For an>' sample, the baseline of the chromatogram must return to below 50% of full scale
before the elution time of alpha-BHC, and also return to below 25% of lull scale after the
elution lime of alpha-BHC and before the elution time of DCB.
7. If a chromatogram is replotted electronically to meet these requirements, the scaling
factor used must be displayed on the chromatogram, and both the initial chromatogram
and the replotted chromatogram must be submitted in the data package.
Action:
1. If the qualitative criteria for both columns were not met, all target compounds that
are reported as detected should be considered non-detected. The reviewer should
use professional judgment to assign an appropriate quantitation limit using the
following guidance:
a. If the detected target compound peak was sufficiently outside the pesticide RT
Window, the reported values may be a false positive and should be replaced
with the sample Contract Required Quantitation Limits (CRQL) value.
b. If the detected target compound peak poses an interference with potential
detection of another target peak, the reported value should be considered and
qualified as unusable (R).
2. If the data reviewer identifies a peak in both GC column analyses that falls within
the appropriate RT Windows, but was reported as a non-detect, the compound
may be a false negative. Use professional judgment to decide if the compound
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should be included. Note in the Data Review Narrative all conclusions made
regarding target compound identification.
3. If the Toxaphene peak RT windows determined from the calibration overlap with
NCI's or chromatographic interferences, use professional judgment to qualify the
data.
4 If target compounds were detected on both GC columns, and the Percent
Difference between the two results is greater than 25.0%, consider the potential
for coelution and use professional judgment to decide whether a much larger
concentration obtained on one column versus the other indicates the presence of
an interfering compound. 1 f an interfering compound is indicated, use
professional judgment to determine how best to report, and if necessary, qualify
the data according to the guidelines in Table 14 below.
5. If Toxaphene exhibits a marginal pattern-matching quality, use professional
judgment to establish whether the differences are due to environmental
"weathering" (i.e., degradation of the earlier eluting peaks relative to the later
eluting peaks). If the presence of Toxaphene is strongly suggested, report results
as presumptively present (N).
Table 14, Action on Qunlit'ving iVsithe Posticicle Result
Percent Differences
Qualifier
0°o - 25°o
No qualification
26° o - 200%
Professional judgment
1010o — 200% (interferences detected)*
JN
- 50°o (pesticide value < CRQL)**
U
>200%
R
When interferences are detected on either column, qualify the data as "JN".
When the pesticide value is below CRQL and °ol) > 50%. raise the value to CRQL and
qualify "IT undetected.
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Gas Chromalograph/Mass Spec!rometer ((.C'/iVIS) Confirmation
Action;
NOTE: This confirmation is not usually provided by the laboratory. In cases where it is
provided, use professional judgment to determine if data qualified with "*C can
be salvaged if it was previously qualified as unusable (R).
1. If the quantitative criteria for both columns were met (> 5.0 ng/pf for SCPs and > 125
tig/pf, for Toxaphene), detemiine whether GC7MS confirmation was performed. If it
was performed, qualify the data using the following guidance (see Table 15);
a. If GC'/MS confirmation was not required because the quantitative criteria for
both columns was not met, but it was still performed, use professional
judgment when evaluating the data to decide w hether the detect should be
qualified with "C '.
b. If GC/MS confirmation was performed, but unsuccessful for a target
compound detected by GC/TiCD analysis, qualify those detects as "X".
Table 15. (,as Chronialo^aph/.Ylass Spectrometer ((.(VMS) Confirmation Actions
Criteria
Action
SCP/Toxaphene was confirmed by GC/MS
Detects C
SCP/Toxaphene was not con tinned by GC/MS
Detects X
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Compound Quantitation and Reported Contract Required Quantitation Limits (CROl.s)
Action:
1. When a sample is analy/ed at more than one dilution, the lowest CRQLs are used unless
a QC exceedance dictates the use of the higher CRQLs from the diluted sample. Replace
concentrations that exceed the calibration range in the original analysis by crossing out
the "ir and its corresponding value on the original Form 1 and substituting the data from
the diluted sample.
2. Results between the MDL and CRQL should be qualiiled as estimated (J).
3. Results less than the MDL should be reported at the CRQL and qualified (U). MDLs
themselves are not reported.
4. For non-aqueous samples, if the percent moisture is less than 70.0%. no qualification of
the data is necessary. If the percent moisture is greater than or equal to 70.0% and less
than 90.0° o, qualify detects as estimated (J) and non-detects as approximated (UJ). If the
percent moisture is greater than or equal to 90.0°o, qualify delects as estimated (J) and
non-detects as unusable (R) (see Table 16).
5. If any discrepancies are found, the Region's designated representative may contact the
laboratory to obtain additional information that could resolve any differences. If a
discrepancy remains unresolved, the reviewer must use professional judgment to decide
which value is the most accurate. Under these circumstances, the reviewer may determine
that qualification of data is warranted. Note in the Data Review Narrative a description of
the reasons for data qualification and the qualification that is applied to the data.
6. Note, for Contract I.aboratory Program Project Officer (CLP PO) action, numerous or
significant failures to accurately quantify the target compounds or to properly evaluate
and adjust CRQLs.
Table 16. Percent Moisture Actions for Pesticide Anahsis For Non-Aqueous Samples
Action
Criteria
Detected Associated
Non-detected Associated
Compounds
Compounds
% Moisture 70.0
No qualification
70.0 ^ °o Moisture 90.0
J
UJ
% Moisture > 90.0
J
R
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Field Duplicates
Action;
NOTE: In the absence of QAPP guidance lor validating data Irom field duplicates, the
following action will be taken.
Identity which samples within the data package are Held duplicates. Hstimate the relative percent
difference (RPD) between the values for each compound. If large RPDs (> 50%) is observed,
confirm identification of samples and note difference in the executive summary.
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Overall Assessment oI'Daia
Action;
1. Use professional judgment to determine if there is any need to quali I'v data which were
not qualified based on the Quality Control (QC) criteria previously discussed,
2. Write a brief narrative to give the user an indication ofthe analytical limitations ofthe
data. Note, for Contract Laboratory Program Project Officer (CLP PO) action, any
inconsistency ofthe data with the Sample Delivery Group (SDG) Narrative. If sufficient
information on the intended use and required quality ofthe data is available, the reviewer
should include their assessment ofthe usability ofthe data within the given context. This
may be used as part of a formal Data Quality Assessment (DQA).
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APPENDIX A: GLOSSARY
Analytc — The element of interest, ion, or parameter an analysis seeks to determine.
Analytical Services Branch (ASH) — Directs the Contract Laboratory Program (CLP) from
within the Office of Superfund Remediation and Technical Innovation (OSRTI) in the Office of
Solid Waste and Emergency Response (OSWHR).
Analytical Sample — Any solution or media introduced into an instrument on which an analysis
is performed excluding instrument calibration, Initial Calibration Verification (ICV), Initial
Calibration Blank (ICR). Continuing Calibration Verification (CCV), and Continuing Calibration
Blank (CCB). Note that the following are all defined as analytical samples: undiluted and diluted
samples (USHPA and non-US FP A); Matrix Spike samples; duplicate samples; serial dilution
samples, analytical (post-digestion/post-distillation) spike samples; Interference Check Samples
(ICSs); Laboratory Control Samples (LCSs); and Preparation Blanks.
Associated Samples -- Any sample related to a particular Quality Control (QC) analysis. For
example, for Initial Calibration Verification (ICV), all samples run under the same calibration
curve. For duplicates, all Sample Delivery Group (SDG) samples digested/distilled of the same
matrix.
Blank — A sample designed to assess specific sources of contamination. See individual
definitions for types of blanks.
Calibration -- The establishment of an analytical curve based on the absorbance, emission
intensity, or other measured characteristic of known standards. The calibration standards are to
be prepared using the same type of reagents or concentration of acids as used in the sample
preparation.
Calibrat ion Blank — A blank solution containing all of the reagents in the same concentration
as those used in the analytical sample preparation. This blank is not subject to the preparation
method.
Calibration Curve -- A plot of instrument response versus concentration of standards.
Calibration Standards -- A series of known standard solutions used by the analyst for
calibration of the instrument (i.e., preparation of the analytical curve). The solutions may or may
not be subjected to the preparation method, but contain the same matrix (i.e.. the same amount of
reagents and/or preservatives) as the sample preparations to be analyzed.
Case -- A Unite, usually predetermined number of samples collected over a given lime period
from a particular site. Case numbers are assigned by the Sample Management Office (SMO). A
Case consists of one or more Sample Delivery Groups (SDGs).
Contract Compliance Screening (CCS) — A screening of electronic and hardcopy data
deliverables for completeness and compliance with the contract. This screening is performed
under USLPA direction by the Contract Laboratory Program (CLP) Sample Management Office
(SMO) contractor.
Continuing Calibration Verification (CCV) -- A single parameter or multi-parameter standard
solution prepared by the analyst and used to verify the stability ofthe instrument calibration with
time, and the instrument performance during the analysis of samples. The CCV can be one ofthe
calibration standards. I lowever, all parameters being measured by the particular system must be
represented in this standard and the standard must have the same matrix (i.e.. the same amount of
reagents and/or preservatives) as the samples.
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Contract Laboratory Program (CLP) ~ Supports the USLPA's Super fund effort by providing
a range of state-of-the-art chemical analytical services of known quality. This program is
directed by the Analytical Services Branch (ASB) of the Office of Superlund Remediation and
Technical Innovation (OSRTI) of USf.PA.
Contract Laboratory Program Project Officer (CLP PO) — 1 ho Regional I SI PA official
responsible for monitoring laboratory performance and/or requesting analytical data or services
from a CLP laboratory.
Contract Required Quantitation Limit (CRQL) — Minimum level of quantitation acceptable
under the contract Statement of Work (SOW).
Duplicate - A second aliquot of a sample that is treated the same as the original sample in order
to determine the precision oflhe method.
Field Blank — Any sample that is submitted from the Held and identified as a blank. A Held
blank is used to check for cross-contamination during sample collection, sample shipment, and in
the laboratory. A field blank includes trip blanks, rinsate blanks, bottle blanks, equipment blanks,
preservative blanks, decontamination blanks, etc.
Field Duplicate — A duplicate sample generated in the Held, not in the laboratory.
Holding Time — The maximum amount of time samples may be held before they are processed.
Contractual - The maximum amount oftime that the Contract I.aboratory Program (CLP)
laboratory may hold the samples from the sample receipt dale until analysis and still be in
compliance with the terms of the contract, as specified in the CLP Analytical Services Statement
of Work (SOW), t hese times are the same or less than technical holding times to allow for
sample packaging and shipping.
Technical — The maximum amount of time that samples may be held from the collection date
until analysis.
Initial Calibration -- Analysis of analytical standards for a series of different spec i lied
concentrations to define the quantitative response, linearity, and dynamic range of the instrument
to target analvtes.
Initial Calibration Verification (ICV) — Solution(s) prepared from stock standard solutions,
metals, or salts obtained from a source separate from that utilized to prepare the calibration
standards. The ICV is used to verify the concentration of the calibration standards and the
adequacy of the instrument calibration. The ICV should be traceable to National Institute of
Standards and Technology (NIST) or other certified standard sources when USKPA ICV
solutions are not available.
Internal Standard — A non-target element added to a sample at a known concentration after
preparation but prior to analysis. Instrument responses to internal standards are monitored as a
means ofassessing overall instrument performance.
Matrix — The predominant material of which the sample to be analyzed is composed, for the
purposes of this document, the matrices are aqueous/water, soil/sediment, wipe, and filter.
Matrix Spike — Introduction of a known concentration of analyte into a sample to provide
information about the effect ofthe sample matrix on the digestion and measurement
methodology (also identified as a pre-distillation/digestion spike).
Method Detection Limit (.MDL) ~ The concentration of a target parameter that, when a sample
is processed through the complete method, produces a signal with 99 percent probability that it is
different from the blank, for 7 replicates ofthe sample, the mean value must be 3.14s above the
blank, where "s" is the standard deviation ofthe 7 replicates.
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Narrative (SI)G Narrative) -- Portion of the data package which includes laboratory, contract,
Case, Sample Number identification, and descriptive documentation of any problems
encountered in processing the samples, along with corrective action taken and problem
resolution.
Office of Solid Waste and Emergency Response (OSWER) - The I SI l'A office that provides
policy, guidance, and direction for the E'SEPA's solid waste and emergency response programs,
including Siiperfund.
Percent Difference (%D) — As used in this document and the Statement of Work (SOW), is
used to compare two values. The difference between the tw o values divided by one of the values.
Performance Evaluation (PE) Sample — A sample of known composition provided by I ;SEPA
for contractor analysis. Used by USE PA to evaluate C ontractor performance.
Preparation Blank — An analytical control that contains reagent water and reagents, which is
carried through the entire preparation and analytical procedure.
Relative Percent Difference (RPD) — As used in this document and the Statement of Work
(SOW) to compare two values, the RPD is based on the mean of the two values, and is reported
as an absolute value (i.e., always expressed as a positive number or zero).
Regional Sample Control Center Coordinator (RSCC) -- In I Si PA Regions, coordinates
sampling efforts and serves as the central point-of-contact for sampling questions and problems.
Also assists in coordinating the level of Regional sampling activities to correspond with the
monthly projected demand for analytical services.
Relative Standard Deviation (RSD) — As used in this document and the Statement of Work
(SOW), the mean divided by the standard deviation, expressed as a percentage.
Sample — A single, discrete portion of material to be analyzed, which is contained in single or
multiple containers and identified by a unique Sample Number.
Sample Delivery Croup (SDC) - A unit within a sample Case that is used to identify a group
of samples for delivery. An SI)G is defined by the following, whichever is most frequent:
a. Each 20 field samples [excluding Performance F;valuation (PH) samples] within a
Case; or
b. Each 7 calendar day period (3 calendar day period for 7-day turnaround) during
which field samples in a Case are received (said period beginning with the receipt
of the first sample in the SIXi).
c. Scheduled at the same level of deliverable.
In addition, all samples and/or sample fractions assigned to an SIXi must be scheduled under the
same contractual turnaround time. Preliminary Results have no impact on defining the SIX3.
Samples may be assigned to SDGs by matrix (i.e., all soil/sediment samples in one SIXi. all
aqueous/water samples in another) at the discretion of the laboratory.
Sample Management Office (SMO) -- A contractor-operated facility operated under the SMO
contract, awarded and administered by the USEPA. Provides necessary management, operations,
and administrative support to the Contract Eaboratory Program (CEP).
Statement of Work (SOW) — A document which specifies how laboratories analyze samples
under a particular Contract Eaboratory Program (CEP) analytical program.
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APPENDIX B: ORGANIC DATA EXECUTIVE NARRATIVE TEMPLATE
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION 2
DESA/HWSBJHWSS
2890, Wood bridge Avenue, Edison, NJ 08837
EXECUTIVE NARRATIVE
Case No.:
S ite:|
Number of Samples:
Analysis:
SDG No.:
Laboratory:
Sampling dates:
QAPP
HWSS ft
Contractor Document #:
SUMMARY:
Critical: Results have an unacceptable level of uncertainty and should riot be used for making decisions
Data have been qualified "R" rejected.
Major: A level of uncertainty exists that may not meet the data quality objectives for the project A bias
is likely to be present in the results. Data has been qualified "J' estimated.
Minor: The level of uncertainty is acceptable. No significant bias in the data was observed.
Critical Findings:
Major Findings:
Minor Findings:
Reviewer Name(s):
Approver's Signature:
Name:
Affiliation:
Date:
USEPA/R2i'HWSBiHWSS
Page 1 of 3
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AIM'KNDIX C : SAM PLC ORCANIC DATA SAM I'll SUMMARY
f.1-r-NV OQOCi
Contract:
SDGNo- • -
laHCod? ocooi
sample Nuj.tbei
BA!X'<
M.-tho-J
V>iln\ veil
MA Number:
Sainpl-1 ocation
pll S 2
Saittpb Drtr i- *
Sain] k» Time 13 'JJ
"o Mos^mre
:£• r>
~i Willi*
Analyte Name
Result Units
Dilution Factor
Lab Flag
Validation
Reportable
Validation Level
2.4.5-T
ir,
ug kg
1,0
i;
r
Ycv
S5YEM
J " ^-T? i Mb. c\<
-Y"
ug kg
1,0
IT
U
Yes
S3YEM
- —t-
59
15 L" k 2
i.O
u
u
\ C>
S3YEM
; 4-rm
39
»k, kj
1.0
u
r
Ye>
ViYF.M
Dal1!'' it.
97
WL 1 J
u
u
Y«
DiCarib1
•' re kg
i
Yes
•vVf-M
liy kj
[ •
\ e*
\ATN!
Dm^eb
1L ] nuLj
u
u
Yes
VYfcM
Mi. PA
:*-> )
kj
u
UJ
Yc-
S.iYEM
Mt PP
ug'ke
r
o
Yes
SJYEM
Pwiit whk'ij|ii ai
ol
3,9
lit. U
iT
u
Yc-
S.;VEM
4-\ns^j'i cnoi
39
HC 1'4
1,0
u
u
Yes
ViVfM
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APPENDIX I): 1LEC TRONIC DATA DELIVERABLE TEMPLATE
DATA PROVIDER
1 AB MA I RIX CODI
RIST LI UNI I
SYS SAMPLH CODE
ANAL I OCA DON
DETECTION LIMIT UNIT
SAMPLE NAME
BASIS
ITC RETENTION TIME
SWUM ! MA I RIX CODE
CONTAINER ID
RI.SUI 1 COMMLN'I
SAM PI E. TV PI- CODE
Din iton LAcroR
QC ORICilNAI. CONC
SAMPI I- SOl.RCT.
PRI'P METHOD
QC SPIKE ADDED
PAREN r SAMPI I-: CODE
PREP DATE
OC SPIKE' MEASURED
SAMPLE 1)1'I. (iROl.'P
LLACflATL METHOD
OC SPIKE RECOVERY
SAMPI i . DA IT.
1J-ACHATE date:
QC DUP ORKilN \I. CONC
SYS l,OC CODI
1 AB NAME. CODI
OC DI P SPIKE ADDET)
STAR!' DEPTH
QC LEVEL
QC DUP SP1KI Ml \SI RI D
end i)i-;i'ni
LAB SAMPLE ID
OC Dl P SPIKI REX'OVE'RY
DEPIII CM 1
PERCENI MOISTURE
OC RPD
CHAIN ()l- Cl'SIODV
SLBSAMPi.E AMOl NT
OC SPIKE I CL
SI N 1 iO I AM PA it:
SI BSAMPLI AMOENI UNIT
OC SPIKE UCL
SAMPI I RECEIPT DA IK
ANALYST NAME:
OC RPD CL
SAMPI. I. R
INSTRUMENT ID
OC SPIKE: STATUS
SAMPI.INC.! COMPANY CODE
COMMENT
OC DUP SPIKE S I A 1 I S
SAMPI INC) REASON
preservative:
OC RPD SI A IT'S
SAMIM INC I K 11NlOt !
TINA! YOLl ME
BREAK 2
I ASK com-:
TINA I VOl I Ml. UNI 1
sys sample: code:
COI I.I CI ION Ql.'ARITR
CAS RN
I AB AM. ME 1 HOD NAME
COMPOSIIE YN
CI 1EMICAI NAME
A N AI YSIS DA IT
COMPOSI I 1 DI SC
RISLEI valt e:
TOTAL OR DISSOLVED
SAMPLE CLASS
re:sult error delta
COLUMN NUMBER
CUSTOM FIELD 1
result type: code:
TEST TYPE
CUSTOM FIELD 2
REPORTABLE RESULT
TEST BATCH TYPE
CI SIOM ITI I D
DEI LCI T1 .Ati
TEST BATCH ID
COM Ml-NT
LAB 01 A.I ITII RS
CASE
BREAK 1
VA1 IDA TOR 01 A1 IT 1! RS
CONTRACT NUM
SYS SAMPLE CODE
INTERPRE 1 ED QUAI 1M1 RS
SCRIBE SAMPLE. ID
1 AB ANI. ML I I101) NAME
ORdANIC YN
sample: time
ANALYSIS DA IT
METHOD DEI! (,'TION 1 IMI I
T'RAC ITON
TOTAL OR DISSOLVED
REPOR 1 INti DETECTION LIMIT
Pll
con mn number
QUANTITATION 1 IMI T
DATA YAL LABEL
TEST TYPE
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