SOP HW-31
Revision 6
September 2016
Hazardous Waste Support Section
SOP NO. HW-31, Revision 6
Analysis of Volatile Organic Compounds in Air Contained in Canisters by
Method TO-15
PRO^
Approvals:
( W-8-Zo \L
Narendra Kumar Date
Chemist, Hazardous Waste Support Section
fl/f/'/C
iifip Cocuzza // Date
ihief. Hazardous Waste Support Section
Jon Otibry . Date
Chief, Hazardous Waste Support Branch
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NOTICE
The policies and procedures set forth here are intended as guidance to the United States
Environmental Protection Agency (hereafter referred to as USEPA) and other governmental
employees. They do not constitute rule making by USEPA, 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 with provided justification supersedes
any guidance listed in this document.
This document can be obtained from the USEPA's Region 2 Quality Assurance website at:
http://www.epa.gov/region2/qa/documents.htm
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TABLE OF CONTENTS
NOTICE 2
TABLE OF CONTENTS 3
LIST OF TABLES 4
ACRONYMS 5
INTRODUCTION 6
DATA QUALIFIER DEFINITIONS 7
DATA PACKAGE INSPECTION 7
HWSS DATA VALIDATION PROCESS 8
PRELIMINARY REVIEW 9
Sample Integrity and Preservation 10
Gas Chromatograph/Mass Spectrometer (GC/MS) Instrument Performance Check 123
Method Detection Limits 14
Initial Calibration 14
Continuing Calibration Verification (CCV) 18
Blanks 20
Laboratory ControL Samle/Laboratory Control Sample duplicate 23
Internal Standards 24
Standards Data 26
Target Compound Identification 27
Tentatively Identified Compounds (TICs) 28
Compounds Quantitation and Reported Contract Required Quantitation Limits
(CRQLs) 29
Field Duplicates 30
System Performance 31
Regional Quality Assurance (QA) and Quality Control (QC) 32
Overall Assessment of Data 33
APPENDIX A: GLOSSARY 34
APPENDIX B: ORGANIC DATA EXECUTIVE NARRATIVE TEMPLATE 37
APPENDIX C: ELECTRONIC DATA DELIVERABLE TEMPLATE 38
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LIST OF TABLES
TABLE 1. CANISTER LEAK TEST ACTIONS FOR TO-15 ANALYSIS 10
TABLE 2. CANISTER CONTAMINATION ACTIONS FOR TO-15 ANALYSES 11
TABLE 3. HOLDING TIME ACTIONS FOR TO-15 VOLATILE ANALYSES 12
TABLE 4. TO 15 VOLATILE COMPOUNDS LIST 15
TABLE 5. INITIAL CALIBRATION ACTIONS FOR TO-15 ANALYSES 18
TABLE 6. CONTINUING CALIBRATION VERIFICATION (CCV) ACTIONS FOR TO-15
ANALYSES 19
TABLE 7. BLANK ACTIONS FOR TO-15 ANALYSES 21
TABLE 8. FIELD/TRIP BLANK SUITABILITY BASED ON CANISTER
CONTAMINATION 22
TABLE 9. LCS/LCSD ACTIONS FOR TO-15 ANALYSIS 23
TABLE 10. INTERNAL STANDARD ACTIONS FOR TO-15 ANALYSES 25
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ACRONYMS
%D
Percent Difference
%RSD
Percent Relative Standard Deviation
ASB
Analytical Services Branch
BFB
Bromofluorob enzene
CCV
Continuing Calibration Verification
CF
Calibration Factor
CRQL
Contract Required Quantitation Limit
DAR
Data Assessment Report
DAT
Data Assessment Tool
DQA
Data Quality Assessment
DQO
Data Quality Objective
EDD
Electronic Data Deliverable
ESAT
Environmental Services Assistance Team
GC
Gas Chromatograph
GC/MS
Gas Chromatograph/Mass Spectrometer
HWSS
Hazardous Waste Support Section
LCS
Laboratory Control Sample
MA
Modified analysis
OSRTI
Office of Superfund Remediation and Technology Innovation
PO
Project Officer (responsible for the Regional Contract Laboratory)
QA
Quality Assurance
QAC
Quality Assurance Coordinator
QAPP
Quality Assurance Project Plan
QC
Quality Control
RAS
Routine Analytical Services
RIC
Reconstructed Ion Chromatogram
RPD
Relative Percent Difference
RRF
Relative Response Factor
RRF
Mean Relative Response Factor
RRT
Relative Retention Time
RSCC
Regional Sample Control Center Coordinator
RSD
Relative Standard Deviation
RT
Retention Time
SAP
Sampling and Analysis Plan
SDG
Sample Delivery Group
SIM
Selected Ion Monitoring
SMO
Sample Management Office
SOP
Standard Operating Procedure
SOW
Statement of Work
TCL
Target Compound List
TIC
Tentatively Identified Compound
TOPO
Task Order Project Officer
TR/COC
Traffic Report/Chain of Custody Record
USEPA
United States Environmental Protection Agency
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INTRODUCTION
This document is designed to offer the data reviewer guidance in determining the validity of
analytical data from the analysis of Volatile Organic Compounds in air samples taken in
canisters and analyzed by method TO-15. 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 method and/or addenda to it (e.g. modified analysis request), and
(b) the usability /validity and extent of bias of any data not meeting the specific technical and QC
criteria established in the method. 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/ feasibility 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 of guidance and information, as well as professional judgment,
should also be used to determine the ultimate validity of data, especially in those cases where all
data does not meet specific technical criteria.
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DATA QUALIFIER DEFINITIONS
The following definitions provide brief explanations of the 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.
UJ
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.
DATA PACKAGE INSPECTION
Validation should include inspection of the data package to identify any missing and/or incorrect
information or need for reanalysis. The laboratory may submit a reconciliation package for any
missing items or to correct data.
If there are any concerns regarding the data package, Regional Laboratory Contract Project
Officer (PO) should be contacted. Initial Review of data package should include any need for
reanalysis on priority basis because of holding time and preservation reasons.
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HWSS DATA VALIDATION PROCESS
The data validator will use the recommendations in this SOP as well as their own professional
judgment to validate the data.
The data will be saved in the following location, under the appropriate case number folder:
G:\DESADIV\HWSS\DATA VALIDATION
The file naming conventions will consist of
A. case number i.e., 12345
B. SDG name i.e., BXY12
C. level of validation performed i.e., VM
Examples: 12345_BXY12_VM.xls
12345 BXY12 VM.pdf
When data validation is completed, the data package is uploaded for the client to download from
the HWSS data delivery website:
https://epaqpx.rtp.epa.gov/hwssclpdeliverables
The completed data package includes the Executive Narrative (see Appendix B for template), the
Sample Summary Report, when applicable (see Appendix C for example), and the Electronic
Data Deliverable (EDD) (see Appendix D for a list of the column headers included in this
document).
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PRELIMINARY REVIEW
This document is for the review of analytical data generated through the Compendium Method
TO-15 (Determination of Volatile Organic Compounds (VOCs) In Air Collected In Specially-
Prepared Canisters and Analyzed by Gas Chromatography Mass Spectrometry (GC/MS), and
any supplements, additions and future editorial revisions of this method as appropriate. To use
this document effectively, the reviewer should have an understanding of the analytical method
and a general overview of the Case, Sample Delivery Group (SDG) at hand. The exact number of
samples, their assigned numbers, their matrix, their location, 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., Modified 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 Program Project Officer (PO) to obtain copies of the QAPP and
relevant site information. This information is necessary in determining the final data usability.
The SDGs or Cases routinely have unique samples that require special attention from the
reviewer. These include field blanks and trip blanks, field duplicates, and Performance
Evaluation (PE) samples which must be identified in the sampling records. The sampling records
(e.g., TR/COC records, field logs, and/or contractor tables) should identify:
1. The Region where the samples were taken,
2. The Case number,
3. The complete list of samples with information on:
a. Sample locations
b. Sample matrix;
c. Field blanks and trip blanks;
d. Field duplicates;
e. QC audit samples;
f. Shipping dates;
g. Laboratories involved.
h. Initial/final canister pressure
i. Initial/final canister temperature
The TR/COC documentation includes sample descriptions, date(s) of sampling, starting canister
pressure, temperature and time, and ending canister pressure, temperature and time. The reviewer
must consider lag times between sampling and start of analysis when assessing technical sample
holding times.
The laboratory's SDG Narrative is another source of general information. Notable problems with
matrix, canister pressure, insufficient sample volume for analysis or reanalysis, samples received
in abused containers/clogged flow controllers with high negative, zero or positive pressure and
unusual events should be documented in the SDG Narrative. The reviewer should also inspect
any e-mail or telephone/communication logs detailing any discussion of sample or analysis
issues between the laboratory and the Project Manager, USEPA Region 2. If the laboratory SDG
narrative is inadequate and fails to mention important issues, validator should note it in the report
and bring it to the attention of the Project Officer.
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Sample Integrity and Preservation
1. Presampling Criteria:
Canister Suitability:
Canister used for the sampling of the ambient air must be demonstrated clean, and leak
free prior to sample collection. This cleanliness is demonstrated by analysis of an
individual canister or analysis of a representative canister, if only batch cleaning was
required. Leak proof testing is performed on individual canisters. Canisters are used in
conjunction with gauges, valves and flow controllers. Therefore, canister should be
demonstrated clean and leak free inclusive of these components as appropriate.
a. Leak Proof Test:
Canisters are tested by their ability to hold vacuum/pressure within +/- 2 psi for a
period of 24 hours preceding sampling. Any nonconformance issues must be reported
to the laboratory, regional PO and sampler immediately and their explanation
considered. Actions for use of canisters with failing leak test criteria are indicated in
the Table 1 below.
Table 1. Canister Leak test Actions for TO-15 Analysis*
Difference in
Action
Matrix
initial and 24
Detected
Non-Detected
hour pressure
Associated
Associated
(psi) Criteria
Compounds
Compounds
Air
<5
No qualification
Air
> 5
J
UJorR
*Excessive time period (> 3months) elapsed between leak test and actual use should be
considered in evaluation of canister integrity.
b. Cleanliness:
Integrity of the canister used for sampling of air for analysis should be maintained at
all times including the time of shipment to the field, sampling, shipment back to the
laboratory and time of analysis. Analytical results of canister cleaning verification
must be taken into account in the validation of sample results. Canister contamination
actions are stated in Table 2 below.
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Table 2. Canister Contamination Actions for TO-15 Analyses
Contamination
Type/level
Canister
Cleaning
Result
Sample Result
Action for Samples
Detects
Analytes found in
clean canister
analysis are non-
detects
No qualification required
< CRQL
Report CRQL value with a U
CRQL and < 2x
the CRQL
Report concentration of sample
with a U
Clean Canister
analysis
> 2x the CRQL
No qualification required
< CRQL
Report CRQL value with a U
> CRQL and <
clean canister
Report clean canister value with
aU
> CRQL
value
> CRQL and >
clean canister
value
No qualification required
= CRQL
< CRQL
Report CRQL value with a U
> CRQL
No qualification required
2. Post Sampling Criteria
Holding Times and Sample Integrity:
Specially prepared SUMMA canisters are designed to minimize sample changes or
loss for majority of the analytes. Method TO-15 states, "Fortunately, under
conditions of normal usage for sampling ambient air, most VOCs may be recovered
from canisters near their original concentrations after storage times of up to thirty
days". This assumes that sample integrity is maintained by ensuring the system is
closed tight and canister pressure from the time of sampling to the time of analysis is
maintained within a difference allowable due to temperature change.
Qualify sample results using technical holding time information as stated in Table 3:
a. If there is no evidence that the samples were properly preserved (pressure
inside the canister maintained within +/- 5 psi from sampling to check in the
laboratory or analysis) and samples were analyzed within technical holding
time [30 days from sample collection], qualify detects as estimated (J) and
non-detects as "UJ".
b. If there is no evidence that the samples were properly preserved (pressure
inside the canister maintained within +/- 5 psi from sampling to check in the
laboratory or analysis) and the samples were analyzed outside of the
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technical holding time [30 days from sample collection], qualify detects for
all volatile compounds as estimated (J) and non-detects as unusable (R).
c. If the samples were properly preserved (pressure inside the canister
maintained within +/- 5 psi from sampling to analysis), and the samples were
analyzed within the technical holding time [30 days from sample collection],
no qualification of the data is necessary.
d. If the samples were properly preserved (pressure inside the canister
maintained within +/- 5 psi from sampling to analysis), but were analyzed
outside of the technical holding time [30 days from sample collection],
qualify detects as estimated (J) and non-detects as "UJ".
2. Whenever possible, the reviewer should comment on the effect of the holding time
exceedance on the resulting data in the Data Review Narrative.
Table 3. Holding Time Actions for TO-15 Volatile Analyses
Matrix
Preserved
(Pressure difference
between sampling
and analysis < 5psi)
Criteria
Action
Detected
Associated
Compounds
Non-Detected Associated
Compounds
Air
Yes
<30
days
No qualification
Yes
>30
days
J
UJ
Air
No
<30
days
J
UJ
No
>30
days
J
R
3. QC for canister cleaning verification:
It is expected that for canister cleaning analysis laboratory will use identical method and QC
criteria as for the analysis of samples contained in the canister. Any QC defects and omissions in
clean canister GCMS analysis should be evaluated by the validator and any deficiencies noted
and rectified as necessary in collaboration with PO. These findings and defects should be noted
in the data assessment narrative and reported to the PO. Professional judgment should be used in
this evaluation to qualify the data. Gross multiple exceedances in the QC of canister cleaning
analysis can be used to invalidate canister cleaning verification and reject data with professional
judgment and justification.
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Gas Chromatograph/Mass Spectrometer (GC/MS) Instrument Performance
Check
Action:
NOTES: This requirement does not apply when samples are analyzed by the Selected Ion
Monitoring (SIM) technique.
All mass spectrometer instrument conditions must be identical to those used
during the sample analysis. Background subtraction actions resulting in spectral
distortions for the sole purpose of meeting the method specifications are contrary
to the Quality Assurance (QA) objectives, and are therefore unacceptable.
NOTES: No data should be qualified based on BFB or DFTTP failure. Instances of this
should be noted in the narrative.
All ion abundance ratios must be normalized to m/z 95, the nominal base peak,
even though the ion abundance of m/z 174 may be up to 120% that of m/z 95.
1. If samples are analyzed without a preceding valid instrument performance check, qualify
all data in those samples as unusable (R).
2. If the laboratory has made minor transcription errors which do not significantly affect the
data, the data reviewer should make the necessary corrections on a copy of the form.
3. If the laboratory has failed to provide the correct forms or has made significant
transcription or calculation errors, the Region's designated representative should contact
the laboratory and request corrected data. If the information is not available, the reviewer
must use professional judgment to assess the data and notify the Project Officer (PO).
4. If ion abundance criteria are not met, professional judgment may be applied to determine
to what extent the data may be utilized. When applying professional judgment to this
topic, the most important factors to consider are the empirical results that are relatively
insensitive to location on the chromatographic profile and the type of instrumentation.
Therefore, the critical ion abundance criteria for BFB are the m/z 95/96, 174/175,
174/176, and 176/177 ratios. The relative abundances of m/z 50 and 75 are of lower
importance. This issue is more critical for Tentatively Identified Compounds (TICs) than
for target analytes.
5. Note, in the Data Review Narrative, decisions to use analytical data associated with BFB
instrument performance check failures (not meeting contract requirements).
6. If the reviewer has reason to believe that instrument performance check criteria were
achieved using techniques other than those described in the Compendium method TO-15
entitled "Determination Of Volatile Organic Compounds(VOCs) In Air Collected In
Specially-Prepared Canisters And Analyzed By Gas Chromatography/Mass
Spectrometry(GC/MS)", section 10.4, obtain additional information on the instrument
performance checks. If the techniques employed are found to be at variance with the
contract requirements, the performance and procedures of the laboratory may merit
evaluation.
7. Use professional judgment to determine whether associated data should be qualified
based on the spectrum of the mass calibration compound.
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METHOD DETECTION LIMITS (MDL)
Data validator should be familiar with the MDL requirements in the QAPP and the method used.
MDLs should be lower than reporting limits and satisfy data quality requirements for samples as
well as and clean canister analysis. Method TO-15 (Determination Of Volatile Organic
Compounds (VOCs) In Air Collected In Specially-Prepared Canisters And Analyzed By Gas
Chromatography Mass Spectrometry (GC/MS) states that to qualify under Compendium Method
TO-15 the method detection limit should be < 0.5 ppbv (section 11.1.1). The method also states
that "any canister that has not tested clean (compared to direct analysis of humidified zero air of
less than 0.2 ppbv of targeted VOCs) should not be used." Table 4 of the compendium method
TO-15 lists method detection limits for certain analytes. Much lower detection limits are
generally achievable. Document, "Supplement to Compendium Method TO-15-Reduction of
Method Detection Limits to Meet Vapor Intrusion Monitoring Needs" suggests that requirements
for monitoring at 10"6 risk levels are possible with TO-15 method. In addition, reporting limits
should be < reporting limits (RL). Any observations in this regard must be reported to the PO,
noted in the data assessment report and considered during validation.
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Initial Calibration
Instalment calibration compliance requirements are established to ensure that the instrument is
capable of generating acceptable data for qualitative as well as quantitative use. Initial calibration
demonstrates that the instrument is capable of acceptable performance in the beginning of the
analytical run and of producing linear calibration curve and provides Mean Relative Response
Factors (RRFs) suitable for quantitation.
Table 4. TO 15 Volatile Compounds List*
Compound
CAS
Number
Synonyms
Acetone
67-64-1
Dimethyl ketone; Dimethylformaldehyde; 2-Propanone
Allyl chloride
107-05-1
3-Chloropropene; 3-Chloroprene
Benzene
71-43-2
Benzol; Benzine
Benzyl chloride
100-44-7
Chloromethylbenzene; alpha-Chlorotoluene
Bromodichloro methane
75-27-4
Monobromodichloromethane; Methane-bromodichloro
Bromoethene
593-60-2
Vinyl bromide; Monobromoethene
Bromoform
75-25-2
Tribromoethane
Bromomethane
74-83-9
Methyl bromide; Monobromomethane
1,3-Butadiene
106-99-0
Biethylene; Erythrene; Pyrrolyene
Carbon disulfide
75-15-0
Carbon bisulfide; Carbon sulfide
Carbon tetrachloride
56-23-5
Carbon tet; Tetrachloromethane
Chlorobenzene
108-90-7
Monochlorobenzene; Chlorobenzol; Benzene chloride
Chloroethane
75-00-3
Ethyl chloride; Chlorene; Chloryl
Chloroethene
75-01-4
Vinyl chloride; Ethylene monochloride
Chloroform
67-66-3
Triehloromethane; Methyltrichloride; Methane trichloride
Chloromethane
74-87-3
R40; Methyl chloride; Monochloromethane
Cyclohexane
110-82-7
Hexamethylene; Hexahydrobenzene; Hexanaphthene
Dibromochloromethane
124-48-1
Chlorodibromomethane
1,2-Dibromoethane
106-93-4
EDB; Ethylene dibromide
1,2-Dichlorobenzene
95-50-1
ODB; Chloroben
1,3 -Dichlorobenzene
541-73-1
meta-Dichlorobenzene; m-Phenylenedichloride
1,4-Dichlorobenzene
106-46-7
para-Dichlorobenzene; Parazene; Santochlor
1,1 -Dichloroethane
75-34-3
Ethylidene chloride; Ethylidene dichloride
1,2 -Dichloroethane
107-06-2
Ethylene dichloride; Glycol dichloride; 1,2-DCA
1,1 -Dichloroethene
75-35-4
1,1-DCE; Vinylidene chloride
cis-l,2-Dichloroethylene
156-59-2
cis-l,2-DCE; cis-Acetylene dichloride
trans-l,2-Dichloroethylene
156-60-5
trans-1,2-DCE; trans-Acetylene dichloride
1,2-Dichloropropane
78-87-5
Propylene dichloride; Propylene chloride
cis-1,3 -Dichloropropene
10061-01-5
l-Propene,l,3-dichloro-,(z)-; cis-l,3-Dichloro-l-Propene
trans-1,3 -Dichloropropene
10061-02-6
trans-1,3 -Dichloro-1 -Propene; trans-1,3 -Dichloropropylene
1,4-Dioxane
123-91-1
Diethylene dioxide; Diethylene ether
Ethyl acetate
141-78-6
Acetic acid ethyl ester; Acetic ether
Ethylbenzene
100-41-4
Ethylbenzol; Phenylethane
4-Ethyltoluene
622-96-8
l-Ethyl-4-methyl benzene; p-Methylethylbenzene
Freon 11 (CC13F)
75-69-4
Trichlorofluoromethane; Fluorotrichloromethane;
Fluorocarbon 11
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Freon 12 (CC12F2)
75-71-8
Dichlorodifluoromethane; Fluorocarbon 12
Freon 113 (C2C13F3)
76-13-1
l,l,2-Trichloro-l,2,2-trifluoroethane; Fluorocarbon 113; 1,1,2-
T richlorotrifluoroethane
Freon 114 (C2C12F4)
76-14-2
1,2-Dichlorotetrafluoroethane; Halocarbon 114; 1,2-Dichloro-
1,1,2,2-tetrafluoroethane
Heptane
142-82-5
Dipropylmethane; Heptyl hydride
Hexachlorobutadiene
87-68-3
1,3 -Hexachlorobutadiene; Perchlorobutadiene
Hexane
110-54-3
n-Hexane; Hexyl hydride
2-Hexanone
591-78-6
Methyl butyl ketone; Butyl methyl ketone; Hexan-2-one
Isopropyl alcohol
67-63-0
2-Propanol; Isopropanol
Methylene chloride
75-09-2
Dichloromethane; Methylene dichloride
Methyl ethyl ketone
78-93-3
MEK; 2-Butanone; Ethyl methyl ketone
Methyl isobutyl ketone
108-10-1
MIBK; 2-Pentanone; Hexone; Isopropylacetone
Methyl tert-butyl ether
1634-04-4
MTBE; 2-Methoxy-2-methylpropane; tert-Butyl methyl ether
Propylene
115-07-1
Propene; Methylethylene
Styrene
100-42-5
Vinylbenzene; Phenylethylene
1,1,2,2-Tetrachloroethane
79-34-5
Tetrachloroethane; Acetylene tetrachloride; Bonoform
T etrachloroethene
127-18-4
PCE; PERC; Perchloroethylene; Ethylene tetrachloride; Carbon
bichloride; Carbon dichloride
Tetrahydrofuran
109-99-9
Diethylene oxide; Butylene oxide
Toluene
108-88-3
Toluol; Methylbenzene
1,2,4-Trichlorobenzene
120-82-1
1,2,4-Trichlorobenzol
1,1,1 -T richloroethane
71-55-6
Methyl chloroform; Trichloroethane
1,1,2-Trichloroethane
79-00-5
beta-Trichloroethane; Ethane trichloride; Vinyl trichloride
Trichloroethene
79-01-6
TCE; Acetylene trichloride; Ethinyl trichloride
1,2,4-Trimethylbenzene
95-63-6
Pseudocumene; Pseudocumol
1,3,5 -T rimethylbenzene
108-67-8
Mesitylene; Trimethylbenzol
2,2,4-Trimethylpentane
540-84-1
Iso-octane; Isobutyltrimethylmethane
Vinyl acetate
108-05-4
Acetic acid ethenyl ether; Ethenyl acetate
p-Xylene
106-42-3
p-Methyltoluene; 1,4-dimethylbenzene
m-Xylene
108-38-3
m-Methyltoluene; 1,3 -dimethy lbenzene
o-Xylene
95-47-6
o-Methyltoluene; 1,2-Dimethy lbenzene
* Laboratories use different sets and subsets of analytes on as needed basis.
NOTES:
Compounds in bold italicized letters may have poor GCMS response. These poor response
compounds are evaluated using more relaxed relative response factor criteria as stated below.
Action:
Qualify all volatile target compounds, using the following criteria (see Table 5):
a. If any volatile target compound has an RRF value less than the minimum
criterion of 0.01 for poor response compounds and 0.05 for all other
compounds listed in the table 4 above, use professional judgment for detects,
based on mass spectral identification to qualify the data as estimated (J).
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b. If any volatile target compound has an RRF value less than the minimum
criterion of 0.01 for poor response compounds and 0.05 for other compounds
listed in Table 4, qualify non-detected compounds as unusable (R).
c. If any of the poor response target compounds listed in Table 4 has %RSD
greater than 40.0%, qualify detects as estimated (J), and non-detected
compounds using professional judgment.
d. For all other volatile target compounds, if %RSD is greater than 30.0%,
qualify detects as estimated (J), and non-detected compounds using
professional judgment.
At the reviewer's discretion, and based on the project-specific Data Quality
Objectives (DQOs), a more in-depth review may be considered using the following
guidelines:
a. If any volatile target compound has a %RSD greater than the maximum
criterion of 30.0%, and if eliminating either the high or the low-point of the
curve does not restore the %RSD to less than or equal to the required
maximum:
i. Qualify detects for that compound(s) as estimated (J).
ii. Qualify non-detected volatile 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. Qualify detects outside of the linear portion of the curve as estimated
(J).
ii. No qualifiers are required for detects in the linear portion of the curve.
iii. No qualifiers are required for volatile target compounds that were not
detected.
c. If the low-point of the curve is outside of the linearity criteria:
i. Qualify low-level detects in the area of non-linearity as estimated (J).
ii. No qualifiers are required for detects in the linear portion of the curve.
iii. For non-detected volatile compounds, use the lowest point of the
linear portion of the curve to determine the new quantitation limit.
If the laboratory has failed to provide adequate calibration information, the Region's
designated representative should contact the laboratory and request the necessary
information. If the information is not available, the reviewer must use professional
judgment to assess the data.
Note in the Data Review Narrative, whenever possible, the potential effects on the
data due to calibration criteria exceedance.
Note, for Project Officer (PO) action, if calibration criteria are grossly exceeded.
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Table 5. Initial Calibration Actions for TO-15 Analyses
Criteria for TO-15 Analysis
Action
Detected
Associated
Compounds
Non-Detected
Associated
Compounds
RRF < 0.010 (poor response volatile target
compounds, Table 4)
RRF < 0.050 (all other volatile target compounds)
J (based on mass
spectral
identification)
R
RRF > 0.010 (poor response volatile target
compounds, Table 4)
RRF > 0.050 (all other volatile target compounds)
No qualification
% RSD > 40.0 or < -40.0 (poor response volatile
target compounds, Table 4)
% RSD > 30.0 or < -30.0 (all other
Volatile target compounds)
No qualification
% RSD < 40.0 and > -40.0 (poor response volatile
target compounds, Table 4)
% RSD < 30.0 and > -30.0 (all other
volatile target compounds)
J
Use professional
judgment
Continuing Calibration Verification (CCV)
Action:
1. If a CCV/daily calibration was not run at the appropriate frequency (< 20 field samples or
24 hours), qualify data using professional judgment.
2. Qualify all volatile target compounds using the following criteria:
a. For a CCV, if any volatile target compound has an RRF value less than the
minimum criterion (0.01), use professional judgment for detects, based on mass
spectral identification, to qualify the data as estimated (J).
b. For a CCV, if any volatile target compound has an RRF value less than the
minimum criterion (0.010), qualify non-detected compounds as unusable (R).
c. For a CCV, if the Percent Difference value for poor performance volatile target
compound is outside the ±40.0% criterion, qualify detects as estimated (J) and
non-detected compounds as estimated (UJ).
d. For a CCV, if the Percent Difference value for any other volatile target compound
is outside the ±30.0% criterion, qualify detects as estimated (J) and non-detected
compounds as estimated (UJ).
e. If the volatile target compounds meet the acceptable criteria for RRF and the
Percent Difference, no qualification of the data is necessary.
3. If the laboratory has failed to provide adequate calibration information, the Region's
designated representative should contact the laboratory and request the necessary
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information. If the information is not available, the reviewer must use professional
judgment to assess the data.
4. Note in the Data Review Narrative, whenever possible, the potential effects on the data
due to calibration criteria exceedance.
5. Note, for Laboratory Project Officer (PO) action, if calibration criteria are grossly
exceeded.
Table 6. Continuing Calibration Verification (CCV) Actions for TO-15 Analyses
Criteria for CCV
Action
Detected
Associated
Compounds
Non-Detected
Associated
Compounds
RRF < 0.010 (poor response volatile target
compounds, Table 4)
RRF < 0.050 (all other volatile target
compounds)
J (based on mass
spectral
identification)
R
RRF > 0.010 (poor response volatile target
compounds, Table 4)
RRF > 0.050 (all other volatile target
compounds)
No qualification
%D > 40.0 or < -40.0 (poor response volatile
target compounds, Table 4)
%D > 30.0 or < -30.0 (all other
Volatile target compounds)
J
UJ
%D <40.0 and > -40.0 (poor response
volatile target compounds, Table 4)
%D < 30.0 and > -30.0 (all other
volatile target compounds)
No qualification
If the % D for daily calibration exceeds -90, use professional judgment to see if non-detects need
to be qualified as unusable "R"
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Blanks
Action:
If trip blanks are present, the data reviewer should evaluate this data to ensure that
it can be used for qualification of samples.
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 volatile compound is found in a method blank or trip blank, but not found in the
sample, no qualification of the data is necessary.
2. If the method or trip blanks contain a volatile Target Compound List (TCL) compound(s)
at a concentration less than the CRQL and:
a. The sample concentration is less than the CRQL, report the CRQL value with a
"U".
b. The sample concentration is greater than or equal to the CRQL, and less than 2x
the CRQL, report the concentration of the compound in the sample and qualify
with a "U".
c. The sample concentration is greater than or equal to 2x the CRQL, no
qualification of the data is necessary.
3. If the method, or trip blanks contain a volatile TCL compound(s) at a concentration
greater than the CRQL and:
a. The sample concentration is less than the CRQL, report the CRQL value with a
"U".
b. The sample concentration is greater than or equal to the CRQL, and less than the
blank concentration, report the concentration of the compound in the sample at
the same concentration found in the blank and qualify with a "U".
c. The sample concentration is greater than or equal to the CRQL and greater than
the blank concentration, no qualification is required.
4. If the method , storage, field, or trip blanks contain a volatile TCL compound(s) at a
concentration equal to the CRQL and:
a. The sample concentration is less than or equal to the CRQL, report the CRQL
value with a "U".
b. The sample concentration is greater than the CRQL, no qualification is required.
5. If gross contamination exists (i.e., blank contamination > 2x the CRQL) in the method, or
trip blanks, raise the CRQL to the level of the blank contamination and report the
associated sample data below this level as CRQL-U.
6. If contaminants are found in the trip blank, the following is recommended:
a. Review the associated method blank data to determine if the contaminant(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.
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ii. If the analyte was not present in the method blank, the source of
contamination may be in the storage area or during sample transport.
Consider all associated samples for possible cross-contamination.
7. Tentatively Identified Compounds (TICs) should only be considered if requested.
For TICs, if the concentration in the sample is less than two times the concentration in the
most contaminated associated blank (TIC concentration < 2xblank concentration), qualify
the sample data as unusable (R).
8. If an instrument blank was not analyzed following a sample analysis which contained an
analyte(s) at high concentration(s) (i.e., exceeding the calibration range), evaluate the
sample analysis results immediately after the high concentration sample for carryover.
The system is considered uncontaminated if the target analyte is below the CRQL. Use
professional judgment to determine if instrument cross-contamination has affected any
positive compound identification(s). Note, for PO action, if instrument cross-
contamination is suggested and suspected of having an effect on the sample results.
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 qualify 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.
Table 7. Blank Actions for TO-15 Analyses
Blank Type
Blank Result
Sample Result
Action for Samples
Method, Storage,
Field, Trip,
Instrument***
Detects
Not detected
No qualification required
< CRQL *
< CRQL*
Report CRQL value with a U
> CRQL* and < 2x
the CRQL**
Report concentration of sample
with a "U"
> 2x the CRQL**
No qualification required
> CRQL *
< CRQL*
Report CRQL value with a U
> CRQL* and <
blank concentration
Report blank value for sample
concentration with a U
> CRQL* and >
blank concentration
No qualification required
= CRQL*
< CRQL*
Report CRQL value with a U
> CRQL*
No qualification required
Gross
contamination **
Detects
Report blank value for sample
concentration with a U
* 2x the CRQL for methylene ch
oride, 2-butanone anc
acetone.
4x the CRQL for methylene chloride, 2-butanone, and acetone.
Qualifications based on instrument blank results affect only the sample analyzed
immediately after the sample that has target compounds that exceed the calibration range
or non-target compounds that exceed 100 (J,g/L.
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Field or Trip blank when available should be assessed for possible contaminants in the canister
used for trip blank. This canister and its analytical results are specific to the trip blank sample
only. If contaminants are present in the canister used for trip blank, its suitability for use as trip
blank can be assessed using the following criteria.
Table 8. Field/Trip Blank suitability based on Canister contamination
Clean canister
Result
Field/Trip Blank Result
Action for Field/Trip Blank
Detects
Not detected
No qualification, no action for
samples is required
Detects
< clean canister result or >
clean canister result but <
2X the clean canister result
Report as non-detect "U",
invalid as trip blank, no action
for samples is required.
> 2x the clean canister
result
No qualification, valid trip
blank for sample actions.
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Laboratory Control Sample/Laboratory Control Sample Duplicate
Data for Laboratory control sample (LCS) and Laboratory Control Sample Duplicate (LCSD) is
generated to ensure accuracy and reproducibility of the method and the laboratory. LCS and
LCSD samples are analyzed using concentration in the middle of the calibration range and under
the same conditions as samples to be analyzed. LCS/LCSD analysis should be performed once
per 24 hour analytical sequence and concurrently with the samples in a given SDG. Actions for
LCS/LCSD criteria are summarized below.
Action:
Table 9. LCS/LCSD Actions for TO-15 Analyses
Action
Criteria
Detected
Non-detected
Associated
Associated
Compounds
Compounds
Percent recovery Criteria
%R > Upper Acceptance Limit (>130%)
J
No qualification
%R in the acceptable range, 70-130%
No qualification
%R < Lower Acceptance Limit (<70 %)
J
UJ
%R < 50%
J
R
Lower Acceptance Limit < %R < Upper Acceptance
Limit
No qualification
Relative Percent Difference Criteria
% RPD < 25%
No qualification
% RPD > 25 %
J
UJ
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Internal Standards
Action:
1. If an internal standard area count for a sample or blank is greater than 140.0% of the
area for the associated standard (CCV or mid-point standard from initial calibration)
(see Table 10):
a. Qualify detects for compounds quantitated using that internal standard as
estimated low (J-).
b. Do not qualify non-detected associated compounds.
2. If an internal standard area count for a sample or blank is less than 60.0% of the area
for the associated standard (CCV or mid-point standard from initial calibration):
a. Qualify detects for compounds quantitated using that internal standard as
estimated high (J+).
b. Qualify non-detected associated compounds as unusable (R).
3. If an internal standard area count for a sample or blank is greater than or equal to
60.0%), and less than or equal tol40%> of the area for the associates standard opening
CCV or mid-point standard from initial calibration, no qualification of the data is
necessary.
4. If an internal standard RT varies by more than 20.0 seconds: Examine the
chromatographic profile for that sample 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 fraction. Detects should not need to be
qualified as unusable (R) if the mass spectral criteria are met.
5. If an internal standard RT varies by less than or equal to 20.0 seconds, no
qualification of the data is necessary.
6. Note, for Laboratory Project Officer (PO) action, if the internal standard
performance criteria are grossly exceeded. Note in the Data Review Narrative
potential effects on the data resulting from unacceptable internal standard
performance.
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Table 10. Internal Standard Actions for TO-15 Analyses
Criteria
Act
ion
Detected
Associated
Compounds*
Non-detected
Associated
Compounds*
Area counts > 140% of CCV or mid-point standard from
initial calibration)
J-
No
qualification
Area counts < 60% of CCV or mid-point standard from initial
calibration)
J+
R
Area counts > 60% but < 140%) of CCV or mid-point
standard from initial calibration)
No qualification
RT difference > 20.0 seconds between samples CCV or mid-
point standard from initial calibration)
R*
RT difference < 20.0 seconds between samples and CCV or
mid-point standard from initial calibration)
No qualification
* Examine the chromatographic profile for that sample 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 fraction. Detects should not need to be qualified as
unusable (R) if the mass spectral criteria are met.
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Standards Data
Action:
If any calibration standards data are missing, contact the Laboratory Project Officer to obtain an
explanation/resubmittal from the lab. If missing deliverables are unavailable, document the effect
in the Data Assessment.
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Target Compound Identification
Action:
1. The application of qualitative criteria for GC/MS analysis of target compounds requires
professional judgment. It is up to the reviewer's discretion to obtain additional
information from the laboratory. If it is determined that incorrect identifications were
made, qualify all such data as unusable (R).
2. Use professional judgment to qualify the data if it is determined that cross-contamination
has occurred.
3. Note in the Data Review Narrative any changes made to the reported compounds or
concerns regarding target compound identifications. Note, for Laboratory Project Officer
(PO) action, the necessity for numerous or significant changes.
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Tentatively Identified Compounds (TICs)
Action:
NOTE: Tentatively identified compounds should only be evaluated when requested by a
party from outside of the Hazardous Waste Support Section (HWSS).
1. Qualify all TIC results for which there is presumptive evidence of a match (e.g. greater
than or equal to 85% match) as tentatively identified (NJ), with approximated
concentrations.
2. General actions related to the review of TIC results are as follows:
a. If it is determined that a tentative identification of a non-target compound is
unacceptable, change the tentative identification to "unknown" or another
appropriate identification, and qualify the result as estimated (J).
b. If all contractually-required peaks were not library searched and quantitated, the
Region's designated representative may request these data from the laboratory.
3. In deciding whether a library search result for a TIC represents a reasonable
identification, use professional judgment. If there is more than one possible match, report
the result as "either compound X or compound Y". If there is a lack of isomer specificity,
change the TIC result to a nonspecific isomer result (e.g., 1, 3, 5-trimethyl benzene to
trimethyl benzene isomer) or to a compound class (e.g., 2-methyl, 3-ethyl benzene to a
substituted aromatic compound).
4. The reviewer may elect to report all similar compounds as a total (e.g., all alkanes may be
summarized and reported as total hydrocarbons).
5. Target compounds from other fractions and suspected laboratory contaminants should be
marked as "non-reportable".
6. Other Case factors may influence TIC judgments. If a sample TIC match is poor, but
other samples have a TIC with a valid library match, similar RRT, and the same ions,
infer identification information from the other sample TIC results.
7. Note in the Data Review Narrative any changes made to the reported data or any
concerns regarding TIC identifications.
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Compounds Quantitation and Reported Contract Required Quantitation Limits (CRQLs)
Action:
1. When a sample is analyzed 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 "E" and its corresponding value on the original Form I and substituting the data from
the diluted sample. This result value consolidation is also reflected in the EDDs and
documented in the data assessment report.
2. 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.
3. Note, for Laboratory Project Officer (PO) action, numerous or significant failures to
accurately quantify the target compounds or to properly evaluate and adjust CRQLs.
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Field Duplicates
Action:
NOTE: Criteria provided in the QAPP should be applied. In the absence of QAPP
guidance for validating data from field duplicates, the following action will be
taken.
Identify which samples within the data package are field duplicates. Estimate the relative percent
difference (RPD) between the values for each compound. Note large RPDs (> 50%) in the
narrative. Use professional judgment to qualify data when RPD is > 50%.
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System Performance
Action:
Use professional judgment to qualify the data if it is determined that system performance has
degraded during sample analyses. Note, for Laboratory Project Officer (PO) action, any
degradation of system performance which significantly affected the data.
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Regional Quality Assurance (OA) and Quality Control (OC)
Action:
Any action must be in accordance with Regional specifications and the criteria for acceptable PE
sample results. Note, for Laboratory Project Officer (PO) action, unacceptable results for PE
samples.
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Overall Assessment of Data
Action:
1. Use professional judgment to determine if there is any need to qualify 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 of the analytical limitations of the
data. Note, for Laboratory Project Officer (PO) action, any inconsistency of the data with
the Sample Delivery Group (SDG) Narrative. If sufficient information on the intended
use and required quality of the data is available, the reviewer should include their
assessment of the usability of the 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
Analyte The element of interest, ion, or parameter an analysis seeks to determine.
Analytical Sample Any solution or media introduced into an instrument on which an analysis
is performed excluding instrument calibration, Initial Calibration Verification (ICV), Continuing
Calibration Verification (CCV), and daily calibration. Note that the following are all defined as
analytical samples: undiluted and diluted samples (USEPA and non-USEPA); duplicate samples;
serial dilution samples; Laboratory Control Samples (LCSs).
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.
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 finite, usually predetermined number of samples collected over a given time 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.
Continuing Calibration Verification (CCV) A single parameter or multi-parameter standard
solution prepared by the analyst and used to verify the stability of the instrument calibration with
time, and the instrument performance during the analysis of samples. The CCV can be one of the
calibration standards. However, 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.
Laboratory Project Officer (PO) The Regional USEPA official responsible for monitoring
laboratory performance and/or requesting analytical data or services from a 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 of the method.
Field Blank Any sample that is submitted from the field and identified as a blank. A field
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 field, not in the laboratory.
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Holding Time The maximum amount of time samples may be held before they are processed.
Contractual The maximum amount of time that the Contract Laboratory Program (CLP)
laboratory may hold the samples from the sample receipt date until analysis and still be in
compliance with the terms of the contract, as specified in the CLP Analytical Services Statement
of Work (SOW). These 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 specified
concentrations to define the quantitative response, linearity, and dynamic range of the instrument
to target analytes.
CCV or daily calibrationPrior to sample analysis but after tuning criteria have been met, the
initial calibration of each GC/MS must be routinely checked by analyzing a daily calibration
standard to ensure initial calibration still holds and the instrument continues to remain under
control. Typically this standard is the mid-level calibration standard that contains all the target
compounds.
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 of assessing overall instrument performance.
Matrix The predominant material of which the sample to be analyzed is composed. For the
purposes of this document, the matrix is air.
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 of the sample, the mean value must be 3.14s above the
blank, where "s" is the standard deviation of the 7 replicates.
Narrative (SDG 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 USEPA office that provides
policy, guidance, and direction for the USEPA's solid waste and emergency response programs,
including Superfund.
Percent Difference (%D) As used in this document and the Statement of Work (SOW), is
used to compare two values. The difference between the two values divided by one of the values.
Performance Evaluation (PE) Sample A sample of known composition provided by USEPA
for contractor analysis. Used by USEPA to evaluate Contractor performance.
Method Blank An analytical control that contains humid air-and internal standards, which is
analyzed under the same conditions as standards and sample.
Relative Percent Difference (RPD) As used in this document and the Statement of Work 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).
Relative Standard Deviation (RSD) As used in this document and the Statement of Work,
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 a canister
and identified by a unique Sample Number.
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Sample Delivery Group (SDG) A unit within a sample Case that is used to identify a group
of samples for delivery. An SDG is defined by the following, whichever is most frequent:
a. Each 20 field samples [excluding Performance Evaluation (PE) 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 SDG).
c. Scheduled at the same level of deliverable.
In addition, all samples and/or sample fractions assigned to an SDG must be scheduled under the
same contractual turnaround time. Preliminary Results have no impact on defining the SDG.
Samples may be assigned to SDGs by matrix (i.e., all soil/sediment samples in one SDG, all
aqueous/water samples in another) at the discretion of the laboratory.
Statement of Work (SOW) A document which specifies how laboratories analyze samples
under a particular Contract Laboratory Program (CLP) analytical program.
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APPENDIX B: ORGANIC DATA EXECUTIVE NARRATIVE TEMPLATE
UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
REGION 2
DESAj'HWSB.'KWSS
2 BSC, Wood bridge- Avenue, Edison, NJ 08837
EXECUTIVE NARRATIVE
Case No.:
Site:|
Number of Samples:
Analysis:
SDG No.:
Laboratory:
Sampling dates:
QAPP
HWSS #:
Contractor Document #:
SUMMARY:
Critical: Results have an unacceptable level of uncertainty and should not 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:
COMMENT:
Reviewer Name(s|:
Approver's Signature:
Name:
Affiliation: USEPA'R2/HWSBj'HWSS
Page 1 of 3
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APPENDIX C: ELECTRONIC DATA DELIVERABLE TEMPLATE
DATA PROVIDER
LAB MATRIX CODE
RESULT UNIT
SYS SAMPLE CODE
ANAL LOCATION
DETECTION LIMIT UNIT
SAMPLE NAME
BASIS
TIC RETENTION TIME
SAMPLE MATRIX CODE
CONTAINER ID
RESULT COMMENT
SAMPLE TYPE CODE
DILUTION FACTOR
QC ORIGINAL CONC
SAMPLE SOURCE
PREP METHOD
QC SPIKE ADDED
PARENT SAMPLE CODE
PREP DATE
QC SPIKE MEASURED
SAMPLE DEL GROUP
LEACHATE METHOD
QC SPIKE RECOVERY
SAMPLE DATE
LEACHATE DATE
QC DUP ORIGINAL CONC
SYS LOC CODE
LAB NAME CODE
QC DUP SPIKE ADDED
START DEPTH
QC LEVEL
QC DUP SPIKE MEASURED
END DEPTH
LAB SAMPLE ID
QC DUP SPIKE RECOVERY
DEPTH UNIT
PERCENT MOISTURE
QC RPD
CHAIN OF CUSTODY
SUB SAMPLE AMOUNT
QC SPIKE LCL
SENT TO LAB DATE
SUB SAMPLE AMOUNT UNIT
QC SPIKE UCL
SAMPLE RECEIPT DATE
ANALYST NAME
QC RPD CL
SAMPLER
INSTRUMENT ID
QC SPIKE STATUS
SAMPLING COMPANY CODE
COMMENT
QC DUP SPIKE STATUS
SAMPLING REASON
PRESERVATIVE
QC RPD STATUS
SAMPLING TECHNIQUE
FINAL VOLUME
BREAK 2
TASK CODE
FINAL VOLUME UNIT
SYS SAMPLE CODE
COLLECTION QUARTER
CAS RN
LAB ANL METHOD NAME
COMPOSITE YN
CHEMICAL NAME
ANALYSIS DATE
COMPOSITE DESC
RESULT VALUE
TOTAL OR DISSOLVED
SAMPLE CLASS
RESULT ERROR DELTA
COLUMN NUMBER
CUSTOM FIELD 1
RESULT TYPE CODE
TEST TYPE
CUSTOM FIELD 2
REPORTABLE RESULT
TEST BATCH TYPE
CUSTOM FIELD 3
DETECT FLAG
TEST BATCH ID
COMMENT
LAB QUALIFIERS
CASE
BREAK 1
VALIDATOR QUALIFIERS
CONTRACT NUM
SYS SAMPLE CODE
INTERPRETED QUALIFIERS
SCRIBE SAMPLE ID
LAB ANL METHOD NAME
ORGANIC YN
SAMPLE TIME
ANALYSIS DATE
METHOD DETECTION LIMIT
FRACTION
TOTAL OR DISSOLVED
REPORTING DETECTION LIMIT
PH
COLUMN NUMBER
QUANTITATION LIMIT
DATA VAL LABEL
TEST TYPE
38
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REQUEST FOR SOP CHANGE
Requestor
Name:
Narendra Kumar
Date of
Initiation:
July 20, 2023
Dept.:
LSASD-HWSB-
HWSS
SOP #: HW-31
Revision #: 6
Date: Sept. 2016
SOP Title:
Analysis of Volatile Organic Compounds in Air Contained in Canisters by
Method TO-I5
Please Check One
MINOR REVISION
MAJOR REVISION X
CHANGE(S) (Use attachment if necessary):
CHANGE FROM:
1)
Difference in
Action
Matrix
initial and 24
Detected
Non-Detected
hour pressure
Associated
Associated
(psi) Criteria
Compounds
Compounds
Air
<5
No qualification
Air
> 5
UJorR
2)
Field Duplicates
Action:
NOTE: Criteria provided in the QAPP should be applied. In the absence of QAPP
guidance for validating data from field duplicates, the following action will be taken.
Identify which samples within the data package are field duplicates. Estimate the relative percent
difference (RPD) between the values for each compound. Note large RPDs (> 50%) in the
narrative. Use professional judgment to qualify data when RPD is > 50%.
3)
Target Compound Identification
Action:
1. The application of qualitative criteria for GC/MS analysis of target compounds requires
professional judgment. It is up to the reviewer's discretion to obtain additional
information from the laboratory. If it is determined that incorrect identifications were
Page 1 of 3
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REQUEST FOR SOP CHANGE
made, qualify all such data as unusable (R).
2. Use professional judgment to qualify the data if it is determined that cross-contamination
has occurred.
3. Note in the Data Review Narrative any changes made to the reported compounds or
concerns regarding target compound identifications. Note, for Laboratory Project Officer
(PO) action, the necessity for numerous or significant changes.
CHANGE TO:
1)
Difference in
Action
Matrix
initial and 24-
Detected
Non-Detected
hour pressure
Associated
Associated
(psi) Criteria
Compounds
Compounds
Air
<2
No qualification
Air
>2
UJorR
Field Duplicates
Action:
Identify which samples within the data package are field duplicates.
Calculate the relative percent difference (RPD) of the results of these samples for each
target analyte if both are detects.
Note/highlight large RPDs (> QAPP criteria) in the narrative.
Criteria and guidance provided in the QAPP should then be applied.
In the absence of QAPP guidance for validating data for field duplicates, if both the
results are detects, > CRQL and RPD is > 50% note the difference in the Field
Duplicates section of the narrative.
Target Compound Identification
Action:
The Relative Retention Time (RRT) for a positively identified target analyte should be
within ±0.06 RRT units of the RRT for the same analyte in the associated opening CCV
or mid-point standard from the associated ICAL.
All ions present in the calibration standard mass spectrum should be present in the
sample spectrum.
If mass spectrum does not match or the RRT is outside the specified RRT windows, qualify
detects as unusable (R), or report the result at QL and qualify as non-detect (U).
Page 2 of 3
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REQUEST FOR SOP CHANGE
REASON(S) FOR CHANGE(S): To clarify and add details for Data validation actions.
APPROVAL
NAME:
Signature/Date
EPA Branch Chief /
Section Chief/Team
Leader
Donna Ringel
Z^ts-ruuz- 07/20/2023
EPA TOCOR
Narendra Kumar
/^ukyUiSL- 07/20/2023
REQUESTOR
Narendra Kumar
/^uhuzsi- 07/20/2023
Effective Date
July 25, 2023
Page 3 of 3
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