OSWER9240.1-05A-P
PB99-963506
EPA540/R-99/008
October 1999
USEPA CONTRACT LABORATORY PROGRAM
NATIONAL FUNCTIONAL GUIDELINES
FOR
ORGANIC DATA REVIEW
Office of Emergency and Remedial Response
U.S. Environmental Protection Agency
Washington, DC 20460
-------
NOTICE
The polices and procedures set forth here are intended as guidance to the Agency and other governmental
employees. They do not constitute rule making by the agency, and may not be relied on 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.
Additional copies of this document can be obtained from:
National Technical Information Service (NTIS)
U.S. Department of Commerce
5285 Port Royal Road
Springfield, VA 22161
(703) 487-4650
Document Number PB 99-963506
This document can also be obtained from the EPA's Contract Laboratory Program Web site at:
http://www.epa.gov/superfund/programs/clp/guidance.htm
111
-------
TABLE OF CONTENTS
INTRODUCTION 1
PRELIMINARY REVIEW 2
DATA QUALIFIER DEFINITIONS 4
VOLATILE DATA REVIEW 5
I. Holding Times 6
II. GC/MS Instrument Performance Check 9
III. Initial Calibration 12
IV. Continuing Calibration 17
V. Blanks 20
VI. System Monitoring Compounds 24
VII. Matrix Spikes/Matrix Spike Duplicates 27
VIII. Laboratory Control Samples 29
IX. Regional Quality Assurance and Quality Control 31
X. Internal Standards 32
XI. Target Compound Identification 34
XII. Compound Quantitation and Reported CRQLs 36
XIII. Tentatively Identified Compounds 38
XIV. System Performance 42
XV. Overall Assessment of Data 44
-------
SEMIVOLATILE DATA REVIEW 45
I. Holding Times 46
II. GC/MS Instrument Performance Check 48
III. Initial Calibration 51
IV. Continuing Calibration 55
V. Blanks 58
VI. Surrogate Spikes 61
VII. Matrix Spikes/Matrix Spike Duplicates 64
VIII. Laboratory Control Samples 66
IX. Regional Quality Assurance and Quality Control 68
X. Internal Standards 69
XI. Target Compound Identification 71
XII. Compound Quantitation and Reported CRQLS 73
XIII. Tentatively Identified Compounds 75
XIV. System Performance 80
XV. Overall Assessment of Data 82
PESTICIDE/AROCLOR DATA REVIEW 83
I. Holding Times 84
II. GC/ECD Instrument Performance Check 86
III. Initial Calibration 92
IV. Calibration Verification 96
V. Blanks 99
VI. Surrogate Spikes 103
vi
-------
PESTICIDE/AROCLOR DATA REVIEW (cont.)
VII. Matrix Spikes/Matrix Spike Duplicates 106
VIII. Laboratory Control Samples 108
IX. Regional Quality Assurance and Quality Control 110
X. Pesticide Cleanup Checks Ill
XI. Target Compound Identification 113
XII. Compound Quantitation and Reported CRQLS 116
XIII. Overall Assessment of Data 118
vn
-------
INTRODUCTION
This document is designed to offer guidance on EPA Contract Laboratory Program (CLP) organic
analytical data evaluation and review. In some applications it may be used as a Standard Operating
Procedure (SOP). In other, more subjective areas, only general guidance is offered due to the
complexities and uniqueness of data relative to specific samples. For example, areas where the
application of specific SOPs are possible are primarily those in which definitive performance criteria are
established. These criteria are concerned with specifications that are not sample dependent; they specify
performance requirements that should fully be under a laboratory's control. These specific areas include
blanks, calibration standards, performance evaluation standard materials, and instrument performance
checks (tuning).
These guidelines include the requirements for the Organic Analysis Multi-Media, Multi-
Concentration method, and for the Low Concentration Water Organic Analysis method. To ensure that
the data review guidelines that are unique to the Low Concentration Water Samples are easily identified,
these requirements and procedures are presented in italics and contained within brackets ([ ]) throughout
the document.
This document is intended to assist in the technical review of analytical data generated through
the CLP. Determining contract compliance is not the intended objective of these guidelines. The data
review process provides information on analytical limitations of data based on specific quality control
(QC) criteria. In order to provide more specific usability statements, the reviewer must have a complete
understanding of the intended use of the data. For this reason, it is recommended that whenever possible
the reviewer obtain usability issues from the user prior to reviewing the data. When this is not possible,
the user should be encouraged to communicate any questions of the reviewer.
At times, there may be a need to use data which does not meet all contract requirements and
technical criteria. Use of these data does not constitute either a new requirement standard or full
acceptance of the data. Any decision to utilize data for which performance criteria have not been met is
strictly to facilitate the progress of projects requiring the availability of the data. A contract laboratory
submitting data which are out of specification may be required to rerun samples or resubmit data, even if
the previously submitted data have been utilized due to program needs. Data which do not meet specified
requirements are never fully acceptable. The only exception to this condition is in the area of the
requirements for individual sample analysis; if the nature of the sample itself inhibits the attainment of
specifications, appropriate allowances must be made.
-------
PRELIMINARY REVIEW
In order to use this document effectively, the reviewer should have a general overview of the
Sample Delivery Group (SDG) or sample Case at hand. The exact number of samples, their assigned
numbers, their matrix and the number of laboratories involved in their analysis are essential information.
Background information on the site is helpful but often this information may be difficult to locate. The
site manager is the best source for answers to questions or further direction.
Sample cases (SDGs) routinely have unique samples which require special attention by the
reviewer. These include field blanks, field duplicates, and performance audit samples which need to be
identified. The sampling records should identify:
1. The Project Officer for site.
2. The Complete list of samples with information on:
a. sample matrix,
b. field blanks,
c. field duplicates,
d. field spikes,
e. QC audit samples,
f shipping dates,
g. preservatives, and
h. laboratories involved.
The chain-of-custody record includes sample descriptions and date(s) of sampling. The reviewer
must take into account 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
matrices, insufficient sample volume for analysis or re-analysis, samples received in broken containers,
preservation, and unusual events should be found in the SDG Narrative.
The SDG Narrative for the sample data package must include a Laboratory Certification
Statement (exactly as written in the method), signed by the laboratory manager or his designee. This
statement authorizes the validation and release of the sample data results. In addition, the laboratory must
also provide comments in the SDG Narrative describing in detail any problems encountered in processing
the samples in the data package.
For every data package, the reviewer must verify that the laboratory certification statement is
present, exactly stated as in the method (i.e., verbatim to the statement in the method), and signed by the
laboratory manager or designee. The reviewer must further verify that the data package is consistent with
the laboratory's certified narrative. Also, the reviewer should check the comments provided in the
narrative to determine if they are sufficient to describe and explain any associated problem(s).
-------
The data review should include comments that clearly identify the problems associated with a
Case or Sample Delivery Group and to state the limitations of the data. Documentation should include
the sample number, analytical method, extent of the problem, and assigned qualifiers.
A data review narrative generally accompanies the laboratory data forwarded to the intended data
recipient (client) or user to promote communications. A copy of the data review narrative should be
submitted to the EPA Project Officer assigned oversight responsibility for the laboratory producing the
data.
It is a responsibility to notify the appropriate EPA Project Officer concerning problems and
deficiencies with regard to laboratory data. If there is an urgent requirement, the EPA Project Officer
may be contacted by telephone to expedite corrective action. It is recommended that all items for EPA
Project Officer action be presented at one time.
-------
DATA QUALIFIER DEFINITIONS
The following definitions provide brief explanations of the national qualifiers assigned to results
in the data review process. If the Regions choose to use additional qualifiers, a complete explanation of
those qualifiers should accompany the data review.
U - The analyte was analyzed for, but was not detected above the reported sample
quantitation limit.
J - The analyte was positively identified; the associated numerical value is the approximate
concentration of the analyte in the sample.
N - The analysis indicates the present of an analyte for which there is presumptive evidence
to make a "tentative identification".
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 not detected above the reported sample quantitation limit. However, the
reported quantitation limit is approximate and may or may not represent the actual limit
of quantitation necessary to accurately and precisely measure the analyte in the sample.
R - The sample results are rejected due to serious deficiencies in the ability to analyze the
sample and meet quality control criteria. The presence or absence of the analyte cannot
be verified.
-------
VGA
VOLATILE DATA REVIEW
* * *Data review guidelines that are unique to data generated through the Low Concentration Water
Method are contained within brackets ([]) and written in italics. * * *
The volatile data requirements to be checked are listed below:
I. Holding Times
II. GC/MS Instrument Performance Check
III. Initial Calibration
IV. Continuing Calibration
V. Blanks
VI. System Monitoring Compounds
VII. Matrix Spikes/Matrix Spike Duplicates
[VIII. Laboratory Control Samples]
IX. Regional Quality Assurance and Quality Control
X. Internal Standards
XI. Target Compound Identification
XII. Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)
XIII. Tentatively Identified Compounds
XIV. System Performance
XV. Overall Assessment of Data
-------
VGA
I. Holding Times
A. Review Items: Form I VOA-1 and Form I VOA-2 [Form ILCV], EPA Sample Traffic Report
and/or chain-of-custody, raw data, and SDG Narrative.
B. Objective:
The objective is to ascertain the validity of the analytical results based on the holding time of the
sample from the time of collection to the time of analysis.
C. Criteria:
Technical requirements for sample holding times have only been established for water matrices.
The technical holding time criteria for water samples are as follows:
For non-aromatic volatile compounds in cooled (@4°C) water samples, the maximum
holding time is 14 days from sample collection.
Maximum holding times for purgeable aromatic hydrocarbons in cooled (@4°C±2°C),
acid-preserved (with HC1 to pH 2 or below) water samples is 14 days from sample
collection.
Water samples that have not been maintained at 4°C (±2°C) and preserved to a pH of 2 or
below should be analyzed within 7 days from sample collection. If insufficient ice is
used to ship samples, the laboratory may receive samples with no ice left in the cooler.
Under these circumstances, the temperature of the samples may exceed 4°C.
NOTE: It is further recommended that volatile compounds in properly preserved
(4°C±2°C) nonaqueous samples be analyzed within 14 days of sample collection.
The method maximum holding times, which differ from the technical maximum holding times,
state that water and soil samples are to be analyzed within 10 days from the validated time of
sample receipt (VTSR) at the laboratory.
D. Evaluation:
Technical holding times are established by comparing the sampling dates on the EPA Sample
Traffic Report with dates of analysis on Form I VOA-1 and Form I VOA-2 [Form ILCV] and the
raw data. Information contained in the Complete SDG File should also be considered in the
determination of holding times. Verify that the analysis dates on the Form Is and the raw
data/SDG file are identical. Review the SDG Narrative to determine if samples were preserved.
If there is no indication in the SDG Narrative or the sample records that there was a problem with
the samples (e.g., samples not maintained @ 4°C or containing headspace in the samples), then
the integrity of samples can be assumed to be good. If it is indicated that there were problems
with the samples, then the integrity of the sample may have been compromised and professional
6
-------
VGA
judgement should be used to evaluate the effect of the problem on the sample results.
E. Action:
1. If technical holding times are exceeded, document in the data review narrative that
holding times were exceeded and qualify the sample results as follows (also see Table 1):
a. If there is no evidence that the samples were properly preserved and the technical
holding times exceeded 7 days, qualify positive results for aromatic compounds
with "J" and sample quantitation limits with "UJ". Use professional judgement
to determine if and how non-aromatic volatile compounds should also be
qualified.
b. If the samples were properly preserved but the technical holding times exceeded
14 days, qualify positive results with "J" and sample quantitation limits with
"UJ".
Table 1. Qualification of Volatile Analytes Based on Technical Holding Times
MATRIX
Water
Non-Aqueous
PRESERVED
No
Yes
No/Yes
> 7 DAYS
All Aromatics*
None
Professional
Judgement
> 14 DAYS
All Compounds
All Compounds
Professional
Judgement
* Reviewer should use professional judgement to determine if data for additional
compounds require qualification.
If technical holding times are grossly exceeded (e.g., by greater than two times the
required time for volatiles) either on the first analysis or upon re-analysis, the reviewer
must use professional judgement to determine the reliability of the data and the effects of
additional storage on the sample results. Should the reviewer determine that qualification
is necessary, non-detected volatile target compounds may be qualified unusable (R).
Positive results are considered approximates and are qualified with "J".
Due to limited information concerning holding times for non-aqueous samples, it is left to
the discretion of the data reviewer to apply water holding times or other
information that is available.
Whenever possible, the reviewer should comment on the effect of the holding time
exceedance on the resulting data in the data review narrative.
-------
VGA
5. When method and/or technical holding times are grossly exceeded, this should be noted
for EPA Project Officer action.
6. The reviewer should also be aware of the scenario in which the laboratory has exceeded
the technical holding times, but met method holding times. In this case, the data reviewer
should notify the EPA Project Officer (where samples were collected) and/or RSCC that
shipment delays have occurred so that the field problem can be corrected. The reviewer
may pass this information on to the laboratory's EPA Project Officer, but should explain
that the laboratory met the requirements in the method.
-------
VGA
II. GC/MS Instrument Performance Check
A. Review Items: Form V VOA [Form VLCV], BFB mass spectra and mass listing.
B. Objective:
Gas chromatograph/mass spectrometer (GC/MS) instrument performance checks are
performed to ensure mass resolution, identification, and to some degree, sensitivity.
These criteria are not sample specific. Conformance is determined using standard
materials, therefore, these criteria should be met in all circumstances.
C. Criteria:
The analysis of the instrument performance check solution must be performed at the
beginning of each 12-hour period during which samples or standards are analyzed. The
instrument performance check, bromofluorobenzene (BFB) for volatile analysis, must
meet the ion abundance criteria given below:
Bromofluorobenzene (BFB)
m/z ION ABUNDANCE CRITERIA
50 8.0-40.0% of m/z 95
75 30.0 - 66.0% of m/z 95
95 Base peak, 100% relative abundance
96 5.0-9.0% of m/z 95
173 Less than 2.0% of m/z 174
174 50.0-120.0% of m/z 95
175 4.0-9.0% of mass 174
176 93.0-101.0% of m/z 174
177 5.0-9.0% of m/z 176
NOTE: All ion abundances 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
percent that of m/z 95.
-------
VGA
D. Evaluation:
1. Compare the data presented for each Instrument Performance Check (Form V VOA
[Form VLCV]) with each mass listing submitted to ensure the following:
a. Form V VOA [Form VLCV] is present and completed for each 12-hour period
during which samples were analyzed.
b. The laboratory has not made transcription errors between the data and the form.
If there are major differences between the mass listing and the Form Vs, a more
in depth review of the data is required. This may include obtaining and
reviewing additional information from the laboratory.
c. The appropriate number of significant figures has been reported (number of
significant figures given for each ion in the ion abundance criteria column) and
that rounding is correct.
d. The laboratory has not made calculation errors.
2. Verify from the raw data (mass spectral listing) that the mass assignment is correct and
that the mass listing is normalized to m/z 95.
3. Verify that the ion abundance criteria was met. The criteria for m/z 173, 175, 176, and
177 are calculated by normalizing to the specified m/z.
4. If possible, verify that spectra were generated using appropriate background subtraction
techniques. Since the BFB spectrum is obtained from chromatographic peaks that should
be free from coelution problems, background subtraction should be done in accordance
with the following procedure. Three scans (the peak apex scan and the scans
immediately preceding and following the apex) are acquired and averaged. Background
subtraction is required, and must be accomplished using a single scan no more than 20
scans prior to the elution of BFB. Do not subtract as part of the background the BFB
peak.
NOTE: All 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 objectives and are therefore unacceptable.
E. Action:
1. 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.
10
-------
VGA
2. 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, then the
reviewer must use professional judgement to assess the data. The laboratory's EPA
Project Officer should be notified.
3. If mass assignment is in error (such as m/z 96 is indicated as the base peak rather than
m/z 95), classify all associated data as unusable (R).
4. If ion abundance criteria are not met, professional judgement may be applied to
determine to what extent the data may be utilized. Guidelines to aid in the application of
professional judgement to this topic are discussed as follows:
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,
74/176, and 176/177 ratios. The relative abundances of m/z 50 and 75 are of lower
importance.
5. Decisions to use analytical data associated with BFB instrument performance checks not
meeting contract requirements should be clearly noted on the data review narrative.
6. If the reviewer has reason to believe that instrument performance check criteria were
achieved using techniques other than those described in II.D.4, then additional
information on the instrument performance checks should be obtained. If the techniques
employed are found to be at variance with the contract requirements, the performance
and procedures of the laboratory may merit evaluation. Concerns or questions regarding
laboratory performance should be noted for EPA Project Officer action. For example, if
the reviewer has reason to believe that an inappropriate technique was used to obtain
background subtraction (such as background subtracting from the solvent front or from
another region of the chromatogram rather than the BFB peak), then this should be noted
for EPA Project Officer action.
11
-------
VGA
III. Initial Calibration
A. Review Items: Form VI VOA-1 and Form VI VOA-2 [Form VILCV], quantitation reports, and
chromatograms.
B. Objective:
Compliance requirements for satisfactory instrument calibration are established to ensure that the
instrument is capable of producing acceptable qualitative and quantitative data for compounds on
the volatile target compound list (TCL). Initial calibration demonstrates that the instrument is
capable of acceptable performance in the beginning of the analytical run and of producing a
linear calibration curve.
C. Criteria:
1. Initial calibration standards containing both volatile target compounds and system
monitoring compounds are analyzed at concentrations of 10, 20, 50, 100, and 200 ug/L
at the beginning of each analytical sequence or as necessary if the continuing calibration
acceptance criteria are not met. The initial calibration (and any associated samples and
blanks) must be analyzed within 12 hours of the associated instrument performance
check.
[For data generated through the Low Concentration Water Method: Initial calibration
standards containing both volatile target compounds and system monitoring compounds
are analyzed at concentrations of 1, 2, 5, 10, and25ug/Lfornon-ketonesand5, 10, 25,
50, and 125 ug/L for ketones at the beginning of each analytical sequence or as
necessary if the continuing calibration acceptance criteria are not met.]
2. Separate initial calibrations must be performed for water samples (or medium level soil
samples) and for low level soil samples. The calibration for water samples and medium
level soil samples is performed with an unheated purge and the calibration for low level
soil samples is performed with a heated purge.
3. Initial calibration standard Relative Response Factors (RRFs) for all volatile target
compounds and system monitoring compounds must be greater than or equal to 0.05.
(Contractual initial calibration RRF criteria are listed in the appropriate method.)
4. The Percent Relative Standard Deviation (%RSD) from the initial calibration must be
less than or equal to 30.0 percent for all compounds.
12
-------
VGA
D. Evaluation:
1. Verify that the correct concentration of standards were used for the initial calibration
(i.e., 10, 20, 50, 100, and 200 ug/L for water).
[Verify that the correct concentration of standards were used for the initial calibration
(i.e., 1, 2, 5, 10, and 25 ug/L for non-ketones and 5, 10, 25, 50, and 125 ug/L for
ke tones).]
2. Verify that the correct initial calibration was used for water and medium level soil
samples (i.e., unheated purge) and for low level soil samples (i.e., heated purge).
3. If any sample results were calculated using an initial calibration, verify that the correct
standard (i.e., the 50 ug/L standard) was used for calculating sample results and that the
samples were analyzed within 12 hours of the associated instrument performance check.
[If any sample results were calculated using an initial calibration, verify that the correct
standard (i.e., the 5 ug/L for non-ketones and 25 ug/L for ketones) was used for
calculating sample results and that the samples were analyzed within 12 hours of the
associated instrument performance check]
4. Evaluate the initial calibration RRFs and RRF for all volatile target compounds and
system monitoring compounds:
a. Check and recalculate the RRFs and RRF for at least one volatile target
compound associated with each internal standard; verify that the recalculated
value(s) agrees with the laboratory reported value(s).
b. Verify that for all volatile target compounds and system monitoring compounds,
the initial calibration RRFs are greater than or equal to 0.05.
NOTE: The criteria employed for technical data review purposes are different from those
used in the method. The laboratory must meet a minimum RRF criterion of 0.0
1, however, for data review purposes, the "greater than or equal to 0.05"
criterion is applied to all volatile compounds.
13
-------
VGA
Table 2. Volatile Target Compounds Exhibiting Poor Response
Acetone 1,2-Dichloropropane
2-Butanone 2-Hexanone
Carbon Bisulfide Methylene Chloride
Chloroethane 4-Methyl-2-pentanone
Chloromethane Toluene-d8 f
trans-1,2-Dichloroethene l,2-Dichloroethane-d4 f
cis-1,2-Dichloroethene 1,2-Dibromo-3 -chloropropane
f Multi-Media, Multi-Concentration only
5. Evaluate the %RSD for all volatile target compounds and system monitoring
compounds:
a. Check and recalculate the %RSD for one or more volatile target compound(s);
verify that the recalculated value(s) agrees with the laboratory reported value(s).
b. Verify that all volatile target compounds have a %RSD of less than or equal to
30.0 percent. The method criteria for an acceptable initial calibration specifies
that up to any 2 volatile target compounds may fail to meet minimum RRF or
maximum %RSD as long as they have RRFs that are greater than or equal to
0.010, and %RSD of less than or equal to 40.0 percent. For data review
purposes, however, all compounds must be considered for qualification when the
%RSD exceeds the ±30.0 percent criterion.
c. If the %RSD is greater than 30.0 percent, then the reviewer should use
professional judgement to determine the need to check the points on the curve
for the cause of the non-linearity. This is checked by eliminating either the high
point or the low point and recalculating the %RSD.
6. If errors are detected in the calculations of either the RRFs or the %RSD, perform a more
comprehensive recalculation.
14
-------
VGA
E. Action:
1. All volatile target compounds, including the 14 "poor performers" (See Table 2) will be
qualified using the following criteria:
a. If the %RSD is greater than 30.0 percent and all initial calibration RRFs greater
than or equal to 0.05, qualify positive results with "J", and non-detected volatile
target compounds using professional judgement.
b. If any initial calibration RRF is less than 0.05, qualify positive results that have
acceptable mass spectral identification with "J", using professional judgement,
and non-detected analytes as unusable (R).
2. At the reviewer's discretion, a more in-depth review to minimize the qualification of data
can be accomplished by considering the following:
a. If any of the required volatile compounds have a %RSD greater than 30.0
percent, and if eliminating either the high or the low point of the curve does not
restore the %RSD to less than or equal to 30.0 percent.
i. Qualify positive results for that compound(s) with "J".
ii. Qualify non-detected volatile target compounds based on professional
judgement.
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 positive results in the linear portion of the
curve.
ii. Qualify positive results outside of the linear portion of the curve with a
"J".
iii. No qualifiers are needed for volatile target compounds that were not
detected.
c. If the low end of the curve is outside of the linearity criteria:
i. No qualifiers are required for positive results in the linear portion of the
curve.
ii. Qualify low level positive results in the area of non-linearity with "J".
iii. Qualify non-detected volatile target compounds based on professional
judgement.
15
-------
VGA
3. 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
judgement to assess the data.
4. Whenever possible, the potential effects on the data due to calibration criteria
exceedance should be noted in the data review narrative.
5. If calibration criteria are grossly exceeded, this should be noted for EPA Project Officer
action.
16
-------
VGA
IV. Continuing Calibration
A. Review Items: Form VIIVOA-1 and Form VIIVOA-2 [Form VIILCV], quantitation reports,
and chromatograms.
B. Objective:
Compliance requirements for satisfactory instrument calibration are established to ensure that the
instrument is capable of producing acceptable qualitative and quantitative data. Continuing
calibration establishes the 12-hour relative response factors on which the quantitations are based
and checks satisfactory performance of the instrument on a day-to-day basis.
C. Criteria:
1. Continuing calibration standards containing both target compounds and system
monitoring compounds are analyzed at the beginning of each 12-hour analysis period
following the analysis of the instrument performance check and prior to the analysis of
the method blank and samples.
2. The continuing calibration RRF for volatile target compounds and system monitoring
compounds must be greater than or equal to 0.05.
3. The percent difference (%D) between the initial calibration RRF and the continuing
calibration RRF must be within ±25.0 percent.
[For data generated through the Low Concentration Water Method: The percent
difference (%D) between the initial calibration RRF and the continuing calibration RRF
must be within ±30.0 percent.]
D. Evaluation:
1. Verify that the continuing calibration was run at the required frequency and that the
continuing calibration was compared to the correct initial calibration.
2. Evaluate the continuing calibration RRF for all volatile target compounds and system
monitoring compounds:
a. Check and recalculate the continuing calibration RRF for at least one volatile
target compound associated with each internal standard; verify that the
recalculated value(s) agrees with the laboratory reported value(s).
b. Verify that all volatile target compounds and system monitoring compounds
meet the RRF specifications.
17
-------
VGA
NOTE: The criteria employed for data review purposes are different from those defined
in the method. The compounds listed in Table 2 (VOA Section III.D.4) have no
method maximum %D criteria. The laboratory must meet a minimum RRF
criterion of 0.01, however, for data review purposes, the "greater than or
equal to 0.05" criterion is applied to all volatile compounds.
3. Evaluate the %D between initial calibration RRF and continuing calibration RRF for one
or more compound(s).
a. Check and recalculate the %D for one or more volatile target compound(s)
associated with each internal standard; verify that the recalculated value(s)
agrees with the laboratory reported value(s).
b. Verify that the %D is within ±25.0 percent for all volatile target compounds and
system monitoring compounds. Note those compounds which have a %D
outside the ±25.0 percent criterion. The method criteria for an acceptable
continuing calibration specifies that up to any 2 volatile target compounds may
fail to meet minimum RRF or maximum %D as long as they have RRFs that are
greater than or equal to 0.010, and %D of less than or equal to 40.0 percent. For
data review purposes, however, all compounds must be considered for
qualification when the %D exceeds the ±25.0 percent criterion.
4. If errors are detected in the calculations of either the continuing calibration RRF or the
%D, perform a more comprehensive recalculation.
E. Action:
1. The reviewer should use professional judgement to determine if it is necessary to qualify
the data for any volatile target compound. If qualification of data is required, it should
be performed using the following guidelines:
a. If the %D is outside the ±25.0 percent criterion and the continuing calibration
RRF is greater than or equal to 0.05, qualify positive results with "J".
b. If the %D is outside the ±25.0 percent criterion and the continuing calibration
RRF is greater than or equal to 0.05, qualify non-detected volatile target
compounds with "UJ".
c. If the continuing calibration RRF is less than 0.05, qualify positive results that
have acceptable mass spectral identifications with "J" or use professional
judgement.
d. If the continuing calibration RRF is less than 0.05, qualify non-detected volatile
target compounds as unusable (R).
18
-------
VGA
2. 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
judgement to assess the data.
3. Whenever possible, the potential effects on the data due to calibration criteria
exceedance should be noted in the data review narrative.
4. If calibration criteria are grossly exceeded, this should be noted for EPA Project Officer
action.
19
-------
VGA
V. Blanks
A. Review Items: Form I VGA-1 and Form I VOA-2 [Form ILCV], Form IV VOA [Form IV
LCV], chromatograms, and quantitation reports.
B. Objective:
The purpose of laboratory (or field) blank analysis is to determine the existence and magnitude
of contamination resulting from laboratory (or field) activities. The criteria for evaluation of
blanks apply to any blank associated with the samples (e.g., method blanks, instrument blanks,
trip blanks, and equipment blanks). If problems with any blank exist, all associated data must be
carefully evaluated to determine whether or not there is an inherent variability in the data, or if
the problem is an isolated occurrence not affecting other data.
C. Criteria:
1. No contaminants should be found in the blanks.
2. A method blank analysis must be performed after the calibration standards and once for
every 12-hour time period beginning with the injection of BFB.
3. The method blank must be analyzed on each GC/MS system used to analyze samples for
each type of analysis (i.e., unheated purge (water and medium level soil) and heated
purge (low level soil)).
4. A storage blank must be prepared upon receipt of the first samples from an SDG, and
stored with samples until analysis. The storage blank must be analyzed once per SDG.
5. An instrument blank must be analyzed after any sample that has saturated ions from a
given compound to check that the blank is free of interference and the system is not
contaminated.
D. Evaluation:
1. Review the results of all associated blanks on the forms and raw data (chromatograms
and quantitation reports) to evaluate the presence of target and non-target compounds in
the blanks.
2. Verify that a method blank analysis has been reported per matrix, per concentration
level, for each 12-hour time period on each GC/MS system used to analyze volatile
samples. The reviewer can use the Method Blank Summary (Form IV VOA [Form IV
LCV]) to identify the samples associated with each method blank.
3. Verify that a storage blank has been analyzed and included with each SDG and that the
storage blanks are free of contamination.
20
-------
VGA
4. Verify that the instrument blank analysis has been performed following any sample
analysis where a target analyte(s) is/are reported at high concentration(s).
E. Action:
If the appropriate blanks were not analyzed with the frequency described in Criteria 2, 3, and 4,
and 5 then the data reviewer should use professional judgement to determine if the associated
sample data should be qualified. The reviewer may need to obtain additional information from
the laboratory. The situation should be noted for EPA Project Officer action.
Action regarding unsuitable blank results depends on the circumstances and origin of the blank.
Positive sample results should be reported unless the concentration of the compound in the
sample is less than or equal to 10 times (lOx) the amount in any blank for the common volatile
laboratory contaminants (methylene chloride, acetone, 2-butanone, and cyclohexane), or 5
times (5x) the amount for other volatile target compounds. In instances where more than one
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. The results must not be
corrected by subtracting any blank value.
Specific actions are as follows:
1. If a volatile compound is found in a blank but not found in the sample, no action is
taken. If the contaminants found are volatile target compounds (or interfering non-target
compounds) at significant concentrations above the CRQL, then this should be noted for
EPA Project Officer action.
2. Any volatile compound detected in the sample (other than the common volatile
laboratory contaminants), that was also detected in any associated blank, is qualified if
the sample concentration is less than five times (5x) the blank concentration. The
quantitation limit may also be elevated. Typically, the sample CRQL is elevated to the
concentration found in the sample. The reviewer should use professional judgement to
determine if further elevation of the CRQL is required. For the common volatile
laboratory contaminants, the results are qualified by elevating the quantitation limit to
the concentration found in the sample when the sample concentration is less than 10
times (lOx) the blank concentration.
The reviewer should note that blanks may not involve the same weights, volumes, or
dilution factors as the associated samples. These factors must be taken into
consideration when applying the "5x" and "lOx" criteria, such that a comparison of the
total amount of contamination is actually made.
Additionally, 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, he/she 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
21
-------
VGA
detected when contaminants are found in the diluted sample result, but are absent in the
undiluted sample result. Since both results are not routinely reported, it may be
impossible to verify this source of contamination. In this case, the "5x" or "lOx" rules
may not apply; the target compound should be reported as not detected, and an
explanation of the data qualification should be provided in the data review narrative.
3. If gross contamination exists (i.e., saturated peaks by GC/MS), all affected compounds in
the associated samples should be qualified as unusable (R) due to interference. This
should be noted for EPA Project Officer action if the contamination is suspected of
having an effect on the sample results.
4. If inordinate numbers of other target compounds are found at low levels in the blank(s),
it may be indicative of a problem and should be noted for EPA Project Officer action.
5. The same consideration given to the target compounds should also be given to
Tentatively Identified Compounds (TICs), which are found in both the sample and
associated blank(s). (See VOA Section XII for TIC guidance.)
6. If contaminants are found in the storage blanks, the following action is recommended:
a. The associated method blank data should be reviewed to determine if the
contaminant(s) was also present in the method blank. If the analyte was present
at a comparable level in the method blank, then the source of the contamination
may be in the analytical system and the action recommended for the method
blank would apply.
If the analyte was not present in the method blank, then the source of
contamination may be in the storage and all associated samples should be
considered for possible cross-contamination.
b. If the storage blank contains a volatile TCL compound(s) at a concentration
greater than the CRQL, then all positive results for that compounds(s) should be
qualified with "J". If the concentration level in the blank is significantly high,
then positive sample results may require rejection and be qualified with "R".
Non-detected volatile target compounds should not require qualification unless
the contamination is so high that it interferes with the analysis of the non-detect
compounds.
7. If an instrument blank was not analyzed following a sample analysis which contained an
analyte(s) at high concentration(s), sample analysis results after the high concentration
sample must be evaluated for carryover. Professional judgement should be used to
determine if instrument cross-contamination has affected any positive compound
identification(s). If instrument cross-contamination is suggested, then this should be
noted for EPA Project Officer action if the cross-contamination is suspected of having an
effect on the sample results.
22
-------
VGA
The following are examples of applying the blank qualification guidelines. Certain
circumstances may warrant deviations from these guidelines.
Example 1:
Example 2:
Example 3:
Sample result is greater than the Contract Required Quantitation Limit
(CRQL), but is less than the 5x or lOx multiple of the blank result.
Rule
Blank Result
CRQL
Sample Result
Final Sample Result
lOx
7
5
60
60U
5x
7
5
30
30U
In the example for the "lOx" rule, sample results less than 70 (or 10x7)
would be qualified as not detected. In the case of the "5x" rule, sample
results less than 35 (or 5x7) would be qualified as not detected.
Sample result is less than the CRQL, and is also less than the 5x or lOx
multiple of the blank result.
Rule
Blank Result
CRQL
Sample Result
Final Sample Result
lOx
6
5
4J
5U
5x
6
5
4J
5U
Note that data are not reported as 4U, as this would be reported as a
detection limit below the CRQL.
Sample result is greater than the 5x or lOx multiple of the blank result.
Rule
Blank Result
CRQL
Sample Result
Final Sample Result
lOx
10
5
120
120
5x
10
5
60
60
For both the "lOx" and "5x" rules, sample results exceeded the adjusted
blank results of 100 (or 10x10) and 50 (or 5x10), respectively, and
therefore are not qualified.
23
-------
VGA
VI. System Monitoring Compounds
A. Review Items: Form IIVOA-1 and Form IIVOA-2 [Form IILCV], quantitation reports, and
chromatograms.
B. Objective:
Laboratory performance on individual samples is established by means of spiking activities. All
samples are spiked with system monitoring compounds, SMC, (formerly referred to as
surrogates) just prior to sample purging. The evaluation of the results of these system monitoring
compounds is not necessarily straightforward. The sample itself may produce effects due to such
factors as interferences and high concentrations of analytes. Since the effects of the sample
matrix are frequently outside the control of the laboratory and may present relatively unique
problems, the evaluation and review of data based on specific sample results is frequently
subjective and demands analytical experience and professional judgement. Accordingly, this
section consists primarily of guidelines, in some cases with several optional approaches
suggested.
C. Criteria:
1. Three system monitoring compounds (l,2-Dichloroethane-d4, bromofluorobenzene, and
toluene-d8) are added to all samples and blanks to measure their recovery in
environmental samples in sample and blank matrices.
[For data generated through the Low Concentration Water Method: A single system
monitoring compound, bromofluorobenzene, is added to all samples and blanks to
measure the recovery in sample and blank matrices.]
2. Recoveries for system monitoring compounds in volatile samples and blanks must be
within the limits specified in the method.
D. Evaluation:
1. Check raw data (e.g., chromatograms and quantitation reports) to verify the recoveries on
the System Monitoring Compound Recovery Form - Form II VOA-1 and Form IIVOA-
2 [Form IILCV]. Check for any calculation or transcription errors.
2. Check that the system monitoring compound recoveries were calculated correctly. The
equation can be found in the method.
24
-------
VGA
3. The following should be determined from the System Monitoring Compound Recovery
form(s):
a. If any system monitoring compound(s) in the volatile fraction is out of
specification, there should be a re-analysis to confirm that the non-compliance is
due to sample matrix effects rather than laboratory deficiencies.
NOTE: When there are unacceptable system monitoring compound recoveries followed
by acceptable re-analyses, the laboratories are required to report only the
successful run.
b. The laboratory failed to perform acceptably if system monitoring compounds are
outside criteria with no evidence of re-analysis. Medium soils must first be re-
extracted prior to re-analysis when this occurs.
c. Verify that no blanks have system monitoring compounds outside the criteria.
4. Any time there are two or more analyses for a particular sample, the reviewer must
determine which are the best data to report. Considerations should include but are not
limited to:
a. System monitoring compound recovery (marginal versus gross deviation).
b. Technical holding times.
c. Comparison of the values of the target compounds reported in each sample
analysis.
d. Other QC information, such as performance of internal standards.
E. Action:
Data are qualified based on system monitoring compounds results if the recovery of any volatile
system monitoring compound is out of specification. For system monitoring compound
recoveries out of specification, the following approaches are suggested based on a review of all
data from the package, especially considering the apparent complexity of the sample matrix.
1. If a system monitoring compound in the volatile sample has a recovery greater than the
upper acceptance limit (UL):
a. Detected volatile target compounds are qualified "J".
b. Results for non-detected volatile target compounds should not be qualified.
25
-------
VGA
If a system monitoring compound in the volatile sample has a recovery greater than or
equal to 10 percent but less than the lower acceptance limit (LL):
a. Detected volatile target compounds are qualified "J".
b. For non-detected volatile target compounds, the sample quantitation limit is
qualified as approximated (UJ).
If a system monitoring compound in a volatile sample shows less than 10 percent
recovery:
a. Detected volatile target compounds are qualified "J".
b. Non-detected volatile target compounds may be qualified as unusable (R).
Table 3. Qualification of Volatile Analytes Based on
System Monitoring Compound Recoveries
Detected analytes
Non-detected analytes
SMC Recovery
>UL 10%toLL <10%
J
No
Qualification
J
UJ
J
R
In the special case of a blank analysis with system monitoring compounds 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
system monitoring compound recoveries, the reviewer may choose to consider the blank
problem to be an isolated occurrence. However, even if this judgment allows some use
of the affected data, analytical problems should be noted for EPA Project Officer action.
Also note if there are potential contractual problems associated with the lack of re-
analysis of samples that were out of specification.
Whenever possible, potential effects of the data resulting from system monitoring
recoveries not meeting the advisory limits should be noted in the data review narrative.
26
-------
VGA
VII. Matrix Spikes/Matrix Spike Duplicates
(Not Required for Low Concentration Water Data)
A. Review Items: Form III VOA- 1, Form III VOA-2, chromatograms, and quantitation reports.
B. Objective:
Data for matrix spike/matrix spike duplicates (MS/MSD) are generated to determine long-term
precision and accuracy of the analytical method on various matrices and to demonstrate
acceptable compound recovery by the laboratory at the time of sample analysis. These data
alone cannot be used to evaluate the precision and accuracy of individual samples. However,
when exercising professional judgement, this data should be used in conjunction with other
available QC information.
C. Criteria:
1. Matrix spikes (MS) and matrix spike duplicate (MSD) samples are analyzed at a
frequency of one MS and MSD per 20 samples of similar matrix, unless MS/MSD
analyses are not required.
2. Spike recoveries should be within the advisory limits provided on Form III VOA-1 and
Form III VOA-2.
3. Relative percent difference (RPD) between MS and MSD recoveries must be within the
advisory limits provided on Form III VOA- 1 and Form III VOA-2.
D. Evaluation:
1. Verify that MS and MSD samples were analyzed at the required frequency and that
results are provided for each sample matrix.
2. Inspect results for the MS/MSD Recovery on Form III VOA- 1 and Form III VOA-2 and
verify that the results for recovery and RPD are within the advisory limits.
3. Verify transcriptions from raw data and verify calculations.
4. Check that the matrix spike recoveries and RPD were calculated correctly.
5. Compare %RSD results of non-spiked compounds between the original result, MS, and
MSD.
E. Action:
1. No action is taken on MS/MSD data alone. However, using informed professional
judgment the data reviewer may use the MS and MSD results in conjunction with other
QC criteria and determine the need for some qualification of the data.
27
-------
VGA
2. The data reviewer should first try to determine to what extent the results of the MS/MSD
affect the associated data. This determination should be made with regard to the
MS/MSD sample itself as well as specific analytes for all samples associated with the
MS/MSD.
3. In those instances where it can be determined that the results of the MS/MSD affect only
the sample spiked, then qualification should be limited to this sample alone. However, it
may be determined through the MS/MSD results that a laboratory is having a systematic
problem in the analysis of one or more analytes, which affects all associated samples.
4. The reviewer must use professional judgement to determine the need for qualification of
positive results of non-spiked compounds.
NOTE: If a field blank was used for the MS/MSD, the EPA Project Officer must be
notified.
28
-------
VGA
VIII. Laboratory Control Samples
(Low Concentration Water)
[A. Review Items: Form III LCV- 1, LCS chromatograms, and quantitation reports.
B. Objective:
Data for laboratory control samples (LCS) are generated to provide information on the accuracy
of the analytical method and on the laboratory performance.
C. Criteria:
1. A laboratory control sample (LCS) must be analyzed once per SDG and concurrently
with the samples in the SDG.
2. The LCS contains the following volatile compounds, in addition to the required SMC
(Bromofluorobenzene):
Vinyl chloride Benzene
1,2-Dichloroethane cis-1,3-Dichloropropene
Carbon tetrachloride Bromoform
1,2-Dichloropropane Tetrachloroethene
Trichloroethene 1,2-Dibromoethane
1, 1, 2-Trichloroethane 1,4-Dichlorobenzene
3. The percent recoveries for the LCS compounds must be within the QC limits. The LCS
must meet this recovery criteria for the sample data to be accepted.
4. The criteria for system monitoring compound recovery and internal standard
performance also apply.
D. Evaluation:
1. Verify that LCS samples were analyzed at the required frequency and that results are
provided for each SDG.
2. Inspect results for the LCS Recovery on Form III LCV-1 and verify that the results for
recovery are within the QC limits.
3. Verify transcriptions from raw data and verify calculations.
4. Check that the LCS recovery was calculated correctly by using the correct equation.
29
-------
VGA
E. Action:
If the LCS criteria are not met, then the laboratory performance and method accuracy are in
question. Professional judgement should be used 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. Action on the LCS recovery should be based on both the number of compounds that are
outside of the recovery criteria and the magnitude of the exceedance of the criteria.
2. If the LCS recovery criteria are not met, then the LCS results should be used to qualify
sample data for the specific compounds that are included in the LCS solution.
Professional judgement should be used to qualify data for compounds other than those
compounds that are included in the LCS. Professional judgement to qualify non-LCS
compounds should take into account the compound class, compound recovery efficiency,
analytical problems associated with each compound, and comparability in performance
of the LCS compound to the non-LCS compound.
3. If the LCS recovery is greater than the upper control limit, then positive sample results
for the affected compound(s) should be qualified with a "J\
4. If the mass spectral criteria are met but the LCS recovery is less than the lower control
limit, then the associated detected target compounds should be qualified "J" and the
associated non-detected target compounds should be qualified "K\
5. If more than half of the compounds in the LCS are not within the required recovery
criteria, then all of the associated detected target compounds should be qualified "J"
and all associated nondetected target compounds should be qualified "R ".
6. Action on non-compliant system monitoring compound recovery and internal standard
performance should follow the procedures provided in VI.EandX.E, respectively.
Professional judgement should be used to evaluate the impact that non-compliance for
system monitoring compound recovery and internal standard performance in the LCS
has on the associated sample data.
7. It should be noted for EPA Project Officer action if a laboratory fails to analyze an LCS
with each SDG, or if a laboratory consistently fails to generate acceptable LCS
recoveries.]
30
-------
VGA
IX. Regional Quality Assurance and Quality Control
A. Review items: Form I VOA-1 and Form I VOA-2 [Form ILCV], chromatograms, and
quantitation reports.
B. Objective:
Regional Quality Assurance and Quality Control (QA/QC) refer to any QA and/or QC samples
initiated by the Region, including field duplicates, Performance Evaluation (PE) samples, blind
spikes, and blind blanks. (It is highly recommended that Regions adopt the use of these QA/QC
samples.)
C. Criteria:
Criteria are determined by each Region.
1. Performance Evaluation sample frequency may vary.
[For data generated through the Low Concentration Water Method: A PE sample can be
included as frequently as once per SDG].
2. The analytes present in the PE sample must be correctly identified and quantified.
D. Evaluation:
Evaluation procedures must follow the Region's SOP for data review. Each Region will handle
the evaluation of PE samples on an individual basis. Results for PE samples should be compared
to the acceptance criteria for the specific PE samples, if available.
E. Action:
Any action must be in accordance with Regional specifications and the criteria for acceptable PE
sample results. Unacceptable results for PE samples should be noted for EPA Project Officer
action.
31
-------
VGA
X. Internal Standards
A. Review Items: Form VIII VOA [Form VIIILCV], quantitation reports, and chromatograms.
B. Objective:
Internal Standards (IS) performance criteria ensures that GC/MS sensitivity and response are
stable during each analysis.
C. Criteria:
1. Internal standard area counts must not vary by more than a factor of two (-50 percent to
+100 percent) from the associated 12hr calibration standard.
[For data generated through the Low Concentration Water Method: Internal standard
area counts must not vary by more than a factor of ±40.0 percent from the associated
calibration standard.]
2. The retention time of the internal standard must not vary more than ±30 seconds from the
retention time of the associated 12hr calibration standard.
[For data generated through the Low Concentration Water Method: The retention time
of the internal standard must not vary more than ±20.0 seconds from the retention time
of the associated I2hr calibration standard.]
D. Evaluation:
1. Check raw data (e.g., chromatograms and quantitation lists) to verify the internal
standard retention times and areas reported on the Internal Standard Area Summary
(Form VIII VOA [Form VIIILCV]).
2. Verify that all retention times and IS areas are within criteria.
3. If there are two analyses for a particular fraction, the reviewer must determine which are
the best data to report. Considerations should include:
a. Magnitude and direction of the IS area shift.
b. Magnitude and direction of the IS retention time shift.
c. Technical holding times.
d. Comparison of the values of the target compounds reported in each fraction.
e. Other QC.
32
-------
VGA
E. Action:
1. If an IS area count for a sample or blank is outside -50 percent or +100 percent of the
area for associated standard:
a. Positive results for compounds quantitated using that IS should be qualified with
"J".
b. Non-detected compounds quantitated using an IS area count greater than 100
percent should not be qualified.
c. Non-detected compounds quantitated using an IS area count less than 50 percent
are reported as the associated sample quantitation limit and qualified with "UJ".
d. If extremely low area counts are reported, or if performance exhibits a major
abrupt drop-off, then a severe loss of sensitivity is indicated. Non-detected
target compounds should then be qualified as unusable (R).
[If an IS area count for a sample or blank is outside ± 40.0 percent of the area for
associated standard:
a. Positive results for compounds quantitated using that IS should be qualified with
"J".
b. Non-detected compounds quantitated using an IS area count greater than 40
percent should not be qualified.
c. Non-detected compounds quantitated using an IS area count less than 40
percent are reported as the associated sample quantitation limit and qualified
with "UJ".
d. If extremely low area counts are reported, or if performance exhibits a major
abrupt drop-off, then a severe loss of sensitivity is indicated. Non-detected
target compounds should then be qualified as unusable (R).]
2. If an IS retention time varies by more than 30 seconds:
[If an IS retention time varies by more than 20.0 seconds:]
The chromatographic profile for that sample must be examined to determine if any false
positives or negatives exist. For shifts of a large magnitude, the reviewer may consider
partial or total rejection of the data for that sample fraction. Positive results should not
need to be qualified as "R" if the mass spectral criteria are met.
3. If the internal standards performance criteria are grossly exceeded, then this should be
noted for EPA Project Officer action. Potential effects on the data resulting from
unacceptable internal standard performance should be noted in the data review narrative.
33
-------
VGA
XL Target Compound Identification
A. Review Items: Form I VOA-1 and Form I VOA-2 [Form ILCV], quantitation reports, mass
spectra, and chromatograms.
B. Objective:
The objective of the criteria for GC/MS qualitative analysis is to minimize the number of
erroneous identifications of compounds. An erroneous identification can either be a false
positive (reporting a compound present when it is not) or a false negative (not reporting a
compound that is present).
The identification criteria can be applied more easily in detecting false positives than false
negatives. More information is available for false positives due to the requirement for submittal
of data supporting positive identifications. Negatives, or non-detected compounds, on the other
hand represent an absence of data and are, therefore, more difficult to assess. One example of
detecting false negatives is the not reporting of a target compound that is reported as a TIC.
C. Criteria:
1. The relative retention times (RRTs) must be within ±0.06 RRT units of the standard
RRT.
2. Mass spectra of the sample compound and a current laboratory-generated standard (i.e.,
the mass spectrum from the associated calibration standard) must match according to the
following criteria:
a. All ions present in the standard mass spectrum at a relative intensity greater than
10 percent must be present in the sample spectrum.
[For data generated through the Low Concentration Water Method: All ions
present in the standard mass spectrum at a relative intensity greater than 25
percent must be present in the sample spectrum.]
b. The relative intensities of these ions must agree within ±20 percent between the
standard and sample spectra. (Example: For an ion with an abundance of 50
percent in the standard spectrum, the corresponding sample ion abundance must
be between 30 percent and 70 percent.)
c. Ions present at greater than 10 percent in the sample mass spectrum but not
present in the standard spectrum must be considered and accounted for.
[For data generated through the Low Concentration Water Method: Ions
present at greater than 25 percent in the sample mass spectrum but not present
in the standard spectrum must be considered and accounted for.]
34
-------
VGA
D. Evaluation:
1. Check that the RRT of reported compounds is within ±0.06 RRT units of the standard
RRT.
2. Check the sample compound spectra against the laboratory standard spectra to see that it
meets the specified criteria.
3. The reviewer should be aware of situations (e.g., high concentration samples preceding
low concentration samples) when sample carryover is a possibility and should use
judgment to determine if instrument cross-contamination has affected any positive
compound identification. The method specifies that an instrument blank must be run
after samples in which a target analyte ion(s) saturates the detector.
[The reviewer should be aware of situations when sample carryover is a possibility and
should use judgment to determine if instrument cross-contamination has affected any
positive compound identification. The method specifies that an instrument blank must be
run after samples which contain target compounds at levels exceeding the initial
calibration range (25 ug/Lfor non-ketones, 125 ug/Lfor ketones) or non-target
compounds at concentrations greater than 100 ug/L or saturated ions from a compound
(excluding the compound peaks in the solvent front).]
4. Check the chromatogram to verify that peaks are accounted for (i.e., major peaks are
either identified as target compounds, TICs, system monitoring compounds, or internal
standards).
E. Action:
1. The application of qualitative criteria for GC/MS analysis of target compounds requires
professional judgement. It is up to the reviewer's discretion to obtain additional
information from the laboratory. If it is determined that incorrect identifications were
made, all such data should be qualified as not detected (U) or unusable (R).
2. Professional judgement must be used to qualify the data if it is determined that cross-
contamination has occurred.
3. Any changes made to the reported compounds or concerns regarding target compound
identifications should be clearly indicated in the data review narrative. The necessity for
numerous or significant changes should be noted for EPA Project Officer action.
35
-------
VGA
XII. Compound Ouantitation and Reported CRQLs
A. Review Items: Forms IVOA-1 and Form IVOA-2 [Form ILCV], sample preparation sheets,
SDG Narrative, quantitation reports, and chromatograms.
B. Objective:
The objective is to ensure that the reported quantitation results and Contract Required
Quantitation Limits (CRQLs) are accurate.
C. Criteria:
1. Compound quantitation, as well as the adjustment of the CRQLs, must be calculated
according to the correct equation.
2. Compound RRFs must be calculated based on the internal standard (IS) associated with
that compound, as listed in the method. Quantitation must be based on the quantitation
ion (m/z) specified in the method for both the IS and target analytes. The compound
quantitation must be based on the RRF from the appropriate daily standard.
D. Evaluation:
1. For all fractions, raw data should be examined to verify the correct calculation of all
sample results reported by the laboratory. Quantitation lists and chromatograms should
be compared to the reported positive sample results and quantitation limits. Check the
reported values.
2. Verify that the correct internal standard, quantitation ion, and RRF were used to
quantitate the compound. Verify that the same internal standard, quantitation ion, and
RRF are used consistently throughout, in both the calibration as well as the quantitation
process.
3. Verify that the CRQLs have been adjusted to reflect all sample dilutions and dry weight
factors that are not accounted for by the method.
E. Action:
If any discrepancies are found, the laboratory may be contacted by the Region's
designated representative to obtain additional information that could resolve any
differences. If a discrepancy remains unresolved, the reviewer must use professional
judgement to decide which value is the best value. Under these circumstances, the
reviewer may determine qualification of data is warranted. A description of the reasons
for data qualification and the qualification that is applied to the data should be
documented in the data review narrative.
36
-------
VGA
2. Numerous or significant failures to accurately quantify the target compound or to
properly evaluate and adjust CRQLs should be noted for EPA Project Officer action.
37
-------
VGA
XIII. Tentatively Identified Compounds
A. Review Items: Form I VOA-TIC [Form ILCV- TIC], chromatograms, and library search
printouts and spectra for the TIC candidates.
B. Objective:
Chromatographic peaks in volatile fraction analyses that are not target analytes, system
monitoring compounds, or internal standards are potential tentatively identified compounds
(TICs). TICs must be qualitatively identified via a forward search of the NIST/EPA/NIH and/or
Wiley Mass Spectral Library, and the identifications assessed by the data reviewer.
C. Criteria:
For each sample, the laboratory must conduct a mass spectral search of the NIST library and
report the possible identity for the appropriate number of the largest volatile fraction peaks which
are not system monitoring compounds, internal standards, or target compounds, but which have
area or height greater than 10 percent of the area or height of the nearest internal standard. TIC
results are reported for each sample on the Organic Analyses Data Sheet (Form I VOA-TIC).
[For data generated through the Low Concentration Water Method: For each sample, the
laboratory must conduct a mass spectral search of the NIST/EPA/NIH and/or Wiley mass
spectral library and report the possible identity for the appropriate number of the largest volatile
fraction peaks which are not system monitoring compounds, internal standards, or TCL
compounds, but which have area greater than or equal to 40 percent of the area of the nearest
internal standard. Estimated concentrations for TICs are calculated similarly to the TCL
compounds, using total ion areas for the TIC and the internal standard, and assuming a relative
response factor of 1.0. TIC results are reported for each sample on the Organic Analyses Data
Sheet (Form ILCV-TIC).]
NOTE: Since the method revision of October 1986, the CLP does not allow the laboratory
to report as tentatively identified compounds any target compound which is
properly reported in another fraction. For example, late eluting volatile target
compounds should not be reported as semivolatile TICs.
D. Evaluation:
1. Guidelines for tentative identification are as follows:
a. Major ions (greater than 10 percent relative intensity) in the reference spectrum
should be present in the sample spectrum.
[Major ions (greater than 25 percent relative intensity) in the reference
spectrum should be present in the sample spectrum.]
b. The relative intensities of the major ions should agree within ±20 percent
38
-------
VGA
between the sample and the reference spectra.
c. Molecular ions present in the reference spectrum should be present in the sample
spectrum.
d. Ions present in the sample spectrum but not in the reference spectrum should be
reviewed for possible background contamination, interference, or coelution of
additional TIC or target compounds.
e. When the above criteria are not met, but in the technical judgement of the data
reviewer or mass spectral interpretation specialist the identification is correct, the
data reviewer may report the identification.
f If, after careful review and in the technical judgement of the mass spectral
interpretation specialist, no valid identification can be made, the compound
should be reported as follows:
If the library search produces a match at or above 85%, report that
compound.
If the library search produces more than one compound at or above 85%,
report the first compound (highest).
If the library search produces no matches at or above 85%, the
compound should be reported as unknown. The mass spectral specialist
should give additional classification of the unknown compound, if
possible (i.e., unknown hydrocarbon, unknown acid type, unknown
chlorinated coumpound). If probable molecular weights can be
distinguished, include them.
2. Check the raw data to verify that the laboratory has generated a library search for all
required peaks in the chromatograms for samples and blanks.
3. Blank chromatograms should be examined to verify that TIC peaks present in samples
are not found in blanks. When a low-level non-target compound that is a common
artifact or laboratory contaminant is detected in a sample, a thorough check of blank
chromatograms may require looking for peaks which are less than 10 percent of the
internal standard height, but present in the blank chromatogram at similar relative
retention time.
[Blank chromatograms should be examined to verify that TIC peaks present in samples
are not found in blanks. When a low-level non-TCL compound that is a common artifact
or laboratory contaminant is detected in a sample, a thorough check of blank
39
-------
VGA
chromatograms may require looking for peaks which are less than 40 percent of the
internal standard area but present in the blank chromatogram at similar relative
retention time.]
4. All mass spectra for every sample and blank must be examined.
5. Since TIC library searches often yield several candidate compounds having a close
matching score, all reasonable choices must be considered.
6. The reviewer should be aware of common laboratory artifacts/contaminants and their
sources (e.g., aldol condensation products, solvent preservatives, and reagent
contaminants). These may be present in blanks and not reported as sample TICs.
Examples:
a. Common laboratory contaminants: C02 (m/z 44), siloxanes (m/z 73),
diethyl ether, hexane, certain freons, and phthalates at levels less than
100ug/Lor4000ug/Kg.
b. Solvent preservatives such as cyclohexene which is a methylene chloride
preservative. Related by-products include cyclohexanone,
cyclohexenone, cyclohexanol, cyclohexenol, chlorocyclohexene, and
chlorocyclohexanol.
c. Aldol condensation reaction products of acetone include: 4-hydroxy-4-
methyl-2-pentanone, 4-methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-
furanone.
7. Occasionally, a target compound may be identified in the proper analytical fraction by
non-target library search procedures, even though it was not found on the quantitation
list. If the total area quantitation method was used, the reviewer should request that the
laboratory recalculate the result using the proper quantitation ion. In addition, the
reviewer should evaluate other sample chromatograms and check library reference
retention times on quantitation lists to determine whether the false negative result is an
isolated occurrence or whether additional data may be affected.
8. Target compounds could be identified in more than one fraction. Verify that quantitation
is made from the proper fraction.
9. Library searches should not be performed on internal standards or system monitoring
compounds.
10. TIC concentration should be estimated assuming a RRF of 1.0.
40
-------
VGA
E. Action:
1. All TIC results should be qualified "NJ", tentatively identified, 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 not
acceptable, the tentative identification should be changed to "unknown" or an
appropriate identification.
b. If all contractually required peaks were not library searched and quantitated, the
Region's designated representative could request these data from the laboratory.
3. TIC results which are not sufficiently above lOx the level in the blank should not be
reported. (Dilutions and sample size must be taken into account when comparing the
amounts present in blanks and samples.)
4. When a compound is not found in any blanks, but is a suspected artifact of common
laboratory contaminant, the result may be qualified as unusable (R).
5. In deciding whether a library search result for a TIC represents a reasonable
identification, professional judgment must be exercised. If there is more than one
possible match, the result may be reported as "either compound X or compound Y". If
there is a lack of isomer specificity, the TIC result may be changed to a non-specific
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 substituted aromatic compound).
6. The reviewer may elect to report all similar compounds as a total, (e.g., All alkanes may
be summarized and reported as total hydrocarbons.)
7. Other case factors may influence TIC judgements. If a sample TIC match is poor but
other samples have a TIC with a good library match, similar relative retention time, and
the same ions, identification information may be inferred from the other sample TIC
results.
8. Physical constants, such as boiling point, may be factored into professional judgement of
TIC results.
9. Any changes made to the reported data or any concerns regarding TIC identifications
should be indicated in the data review narrative.
10. Failure to properly evaluate and report TICs should be noted for EPA Project Officer
action.
41
-------
VGA
XIV. System Performance
A. Review Items: Form VIII VGA [Form VIIILCV], Form III VOA-1 and Form III VOA-2 [Form
IIILCV-1], and chromatograms.
B. Objective:
During the period following Instrument Performance QC checks (e.g., blanks, tuning,
calibration), changes may occur in the system that degrade the quality of the data. While this
degradation would not be directly shown by QC checks until the next required series of
analytical QC runs, a thorough review of the ongoing data acquisition can yield indicators of
instrument performance.
C. Criteria:
There are no specific criteria for system performance. Professional judgement should be applied
to assess the system performance.
D. Evaluation:
1. Abrupt discrete shifts in the reconstructed ion chromatogram (RIC) baseline may
indicate a change in the instrument's sensitivity or the zero setting. A baseline "shift"
could indicate a decrease in sensitivity in the instrument or an increase in the instrument
zero, possibly causing target compounds, at or near the detection limit, to miss detection.
A baseline "rise" could indicate problems such as a change in the instrument zero, a leak,
or degradation of the column.
2. Poor chromatographic performance affects both qualitative and quantitative results.
Indications of substandard performance include:
a. High RIC background levels or shifts in absolute retention times of internal
standards.
b. Excessive baseline rise at elevated temperature.
c. Extraneous peaks.
d. Loss of resolution.
e. Peak tailing or peak splitting that may result in inaccurate quantitation.
[3. A drift in instrument sensitivity may occur during the 12-hour time period. This could be
discerned by examination of the IS area on Form VIII LCV for trends such as a
continuous or near continuous increase or decrease in the IS area over time.
42
-------
VGA
4. The results of the LCS analysis (Form III LCV) may also be used to assess instrument
performance.]
E. Action:
Professional judgement must be used to qualify the data if it is determined that system
performance has degraded during sample analyses. Any degradation of system performance
which significantly affected the data should be documented for EPA Project Officer action.
43
-------
VGA
XV. Overall Assessment of Data
A. Review Items: Entire data package, data review results, and (if available) Quality Assurance
Project Plan (QAPjP), and Sampling and Analysis Plan (SAP).
B. Objective:
The overall assessment of a data package is a brief narrative in which the data reviewer expresses
concerns and comments on the quality and, if possible, the useability of the data.
C. Criteria:
Assess the overall quality of the data.
Review all available materials to assess the overall quality of the data, keeping in mind the
additive nature of analytical problems.
D. Evaluation:
1. Evaluate any technical problems which have not been previously addressed.
2. If appropriate information is available, the reviewer may assess the useability of the data
to assist the data user in avoiding inappropriate use of the data. Review all available
information, including the QAPjP (specifically the Data Quality Objectives), SAP, and
communication with data user that concerns the intended use and desired quality of these
data.
E. Action:
1. Use professional judgement to determine if there is any need to qualify data which were
not qualified based on the QC criteria previously discussed.
2. Write a brief narrative to give the user an indication of the analytical limitations of the
data. Any inconsistency of the data with the SDG Narrative should be noted for EPA
Project Officer action. If sufficient information on the intended use and required quality
of the data are available, the reviewer should include his/her assessment of the useability
of the data within the given context.
44
-------
sv
SEMIVOLATILE DATA REVIEW
***Data review guidelines that are unique to data generated through the Low Concentration Water
Method are contained within brackets ([]) and written in italics. ***
The semivolatile data requirements to be checked are listed below:
I. Holding Times
II. GC/MS Instrument Performance Check
III. Initial Calibration
IV. Continuing Calibration
V. Blanks
VI. Surrogate Spikes
VII. Matrix Spikes/Matrix Spike Duplicates
[VIII. Laboratory Control Samples]
IX. Regional Quality Assurance and Quality Control
X. Internal Standards
XI. Target Compound Identification
XII. Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)
XIII. Tentatively Identified Compounds
XIV. System Performance
XV. Overall Assessment of Data
45
-------
sv
I. Holding Times
A. Review Items: Form I SV-l[Form I LCSV-1], Form I SV-2 [Form ILCSV-2], EPA Sample
Traffic Report and/or chain of-custody, raw data, and sample extraction sheets.
B. Objective:
The objective is to ascertain the validity of results based on the holding time of the sample from
time of collection to time of sample extraction and analysis.
C. Criteria:
Technical requirements for sample holding times have only been established for water matrices.
The technical holding time criteria for water samples, are as follows:
For semivolatile compounds in cooled (@ 4°C) water samples, the maximum holding
time is 7 days from sample collection to extraction and 40 days from sample extraction
to analysis.
It is recommended that semivolatile compounds in soil samples be extracted within 14 days of
sample collection.
The method holding times, which differ from the technical holding times, state that water
samples are to be extracted within 5 days from the validated time of sample receipt (VTSR) at
the laboratory, and soil samples are to be extracted within 10 days from the VTSR. Also,
contractually both water and soil sample extracts must be analyzed within 40 days of sample
extraction.
[For data generated through the Low Concentration Method: The method holding times
requirements are that the extraction of all samples must be started within 5 days of the VTSR,
and the extracts must be analyzed within 40 days of VTSR.]
D. Evaluation:
Technical holding times for sample extraction are established by comparing the sampling date on
the EPA Sample Traffic Report with the dates of extraction on Form I SV-1 [Form ILCSV-1]
and Form I SV-2 [Form ILCSV-2] and the sample extraction sheets. To determine if the
samples were analyzed within the holding time after extraction, compare the dates of extraction
on the sample extraction sheets with the dates of analysis on Form I SV-1 [Form I LCSV-1] and
Form I SV-2 [Form ILCSV-2].
Verify that the Traffic Report indicates that the samples were received intact and iced. If the
samples were not iced or there were any problems with the samples upon receipt, then
discrepancies in the sample condition could affect the data.
46
-------
sv
E. Action:
1. If technical holding times are exceeded, flag all positive results as estimated "J", and
sample quantitation limits as estimated "UJ" and document that holding times were
exceeded.
2. If technical holding times are grossly exceeded, either on the first analysis or upon re-
analysis, the reviewer must use professional judgement to determine the reliability of the
data and the effect of additional storage on the sample results. The reviewer may
determine that positive results or the associated quantitation limits are approximates and
should be qualified with "J" or "UJ", respectively. The reviewer may determine that
non-detect data are unusable (R).
3. Due to limited information concerning holding times for soil samples, it is left to the
discretion of the data reviewer to apply water holding time criteria to soil samples.
Professional judgement is required to evaluate holding times for soil samples.
4. Whenever possible, the reviewer should comment on the effect of the holding time
exceedance on the resulting data in the data review narrative.
5. When method and/or technical holding times are exceeded, this should be noted as an
action item for the EPA Project Officer.
6. The reviewer should also be aware of the scenario in which the laboratory has exceeded
the technical holding times, but met method holding times. In this case, the data
reviewer should notify the EPA Project Officer (where samples were collected) and/or
RSCC that shipment delays have occurred so that the field problem can be corrected.
The reviewer may pass this information on to the laboratory's EPA Project Officer, but
should explain that the laboratory met the requirements in the method.
47
-------
sv
A.
B.
C.
II. GC/MS Instrument Performance Check
Review Items: Form V SV [Form VLCSV], and DFTPP mass spectra and mass listing.
Objective:
Gas chromatograph/mass spectrometer (GC/MS) instrument performance checks (formerly
referred to as tuning) are performed to ensure mass resolution, identification and, to some degree,
sensitivity. These criteria are not sample specific. Conformance is determined using standard
materials, therefore, these criteria should be met in all circumstances.
Criteria:
The analysis of the instrument performance check solution must be performed at the beginning of
each 12-hour period during which samples or standards are analyzed. The instrument
performance check, decafluorotriphenylphosphine (DFTPP) for semivolatile analysis, must meet
the ion abundance criteria given below.
Decafluorotriphenylphosphine (DFTPP)
m/z
51
68
69
70
127
197
198
199
275
365
441
442
443
ION ABUNDANCE CRITERIA
30.0-80.0% of m/z 198
Less than 2.0% of m/z 69
Present
Less than 2.0% of m/z 69
25.0-75.0% of m/z 198
Less than 1.0% of m/z 198
Base peak, 100% relative abundance
5.0-9.0% of m/z 198
10.0-30.0% of m/z 198
Greater than 0.75% of m/z 198 Present,
but less than m/z 443
40.0- 110.0% of m/z 198
15.0-24.0% of m/z 442
NOTE: All ion abundances must be normalized to m/z 198, the nominal base peak, even
though the ion abundances of m/z 442 may be up to 110 percent that of m/z 198.
D.
Evaluation:
1. Compare the data presented on each GC/MS Instrument Performance Check (Form V SV
[Form VLCSV]) with each mass listing submitted and ensure the following:
48
-------
sv
a. Form V SV [Form VLCSV] is present and completed for each 12-hour period
during which samples were analyzed.
b. The laboratory has not made any transcription errors between the data and the
form. If there are major differences between the mass listing and the Form Vs, a
more in-depth review of the data is required. This may include obtaining and
reviewing additional information from the laboratory.
c. The appropriate number of significant figures has been reported (number of
significant figures given for each ion in the ion abundance criteria column) and
that rounding is correct.
d. The laboratory has not made any calculation errors.
2. Verify from the raw data (mass spectral listing) that the mass assignment is correct and
that the mass is normalized to m/z 198.
3. Verify that the ion abundance criteria was met. The criteria for m/z 68, 70, 441, and 443
are calculated by normalizing to the specified m/z.
4. If possible, verify that spectra were generated using appropriate background subtraction
techniques. Since the DFTPP spectrum is obtained from chromatographic peaks that
should be free from coelution problems, background subtraction should be done in
accordance with the following procedure. Three scans (the peak apex scan and the scans
immediately preceding and following the apex) are acquired and averaged. Background
subtraction is required, and must be accomplished using a single scan acquired no more
than 20 scans prior to the elution of DFTPP. Do not subtract as part of the background
the DFTPP peak.
NOTE: All 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 contract specifications are contrary to the quality
assurance objectives and are therefore unacceptable.
E. Action:
1. 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.
2. 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, then the
reviewer must use professional judgement to assess the data. The laboratory's EPA
Project Officer should be notified.
49
-------
sv
3. If mass assignment is in error (such as m/z 199 is indicated as the base peak rather than
m/z 198), classify all associated data as unusable (R).
4. If ion abundance criteria are not met, professional judgement may be applied to
determine to what extent the data may be utilized. Guidelines to aid in the application of
professional judgement in evaluating ion abundance criteria are discussed as follows:
a. Some of the most critical factors in the DFTPP criteria are the non-instrument
specific requirements that are also not unduly affected by the location of the
spectrum on the chromatographic profile. The m/z ratios for 198/199 and
442/443 are critical. These ratios are based on the natural abundances of carbon
12 and carbon 13 and should always be met. Similarly, the relative abundances
for m/z 68, 70, 197, and 441 indicate the condition of the instrument and the
suitability of the resolution adjustment and are very important. Note that all of
the foregoing abundances relate to adjacent ions; they are relatively insensitive
to differences in instrument design and position of the spectrum on the
chromatographic profile.
b. For the ions at m/z 51, 127, and 275, the actual relative abundance is not as
critical. For instance, if m/z 275 has 40 percent relative abundance (criteria:
10.0-30.0 percent) and other criteria are met, then the deficiency is minor.
c. The relative abundance of m/z 365 is an indicator of suitable instrument zero
adjustment. If relative abundance for m/z 365 is zero, minimum detection limits
may be affected. On the other hand, if m/z 365 is present, but less than the 0.75
percent minimum abundance criteria, the deficiency is not as serious.
5. Decisions to use analytical data associated with DFTPP instrument performance checks
not meeting method requirements should be clearly noted in the data review narrative.
6. If the reviewer has reason to believe that instrument performance check criteria were
achieved using techniques other than those specified in the method and Section II.D.4
above, additional information on the DFTPP instrument performance checks should be
obtained. If the techniques employed are found to be at variance with contract
requirements, the procedures of the laboratory may merit evaluation. Concerns or
questions regarding laboratory performance should be noted for EPA Project Officer
action. For example, if the reviewer has reason to believe that an inappropriate
technique was used to obtain background subtraction (such as background subtracting
from the solvent front or from another region of the chromatogram rather than the
DFTPP peak), then this should be noted for EPA Project Officer action.
50
-------
sv
III. Initial Calibration
A. Review Items: Form VI SV-1 [Form VILCSV-I], Form VI SV-2 [Form VILCSV-2],
quantitation reports, and chromatograms.
B. Objective:
Compliance requirements for satisfactory instrument calibration are established to ensure that the
instrument is capable of producing acceptable qualitative and quantitative data for compounds on
the semivolatile Target Compound List (TCL). Initial calibration demonstrates that the
instrument is capable of acceptable performance in the beginning of the analytical run and of
producing a linear calibration curve.
C. Criteria:
1. Initial calibration standards containing both semivolatile target compounds and
surrogates are analyzed at concentrations of 20, 50, 80, 120, and 160 ng/2uL at the
beginning of each analytical sequence or as necessary if the continuing calibration
acceptance criteria are not met. The initial calibration (and any associated samples and
blanks) must be analyzed within 12 hours of the associated instrument performance
check.
[For data generated through the Low Concentration Method: Initial calibration
standards containing both semivolatile TCL compounds and surrogates are analyzed at
concentrations of 5, 10, 20, 50, and 80 ng/2uL at the beginning of each analytical
sequence or as necessary if the continuing calibration acceptance criteria are not met.
The initial calibration (and any associated samples and blanks) must be analyzed within
12 hours of the associated instrument performance check. The following nine
compounds require initial calibration at 20, 50, 80, 100, and 120 ng/2uL: 2,4-
dinitrophenol, 2,4,5-trichlorophenol, 2-nitroaniline, 3-nitroaniline, 4-nitroaniline, 4-
nitrophenol, 4,6-dinitro-2-methylphenol, pentachlorophenol, and 2,4,6-tribromophenol
(surrogate).]
2. Minimum Relative Response Factor (RRF) criteria must be greater than or equal to 0.05.
(Initial RRF criteria are listed in the appropriate method.)
3. The Percent Relative Standard Deviations (%RSD) for the RRFs in the initial calibration
must be less than or equal to 30 percent.
D. Evaluation:
1. Verify that the correct concentration of standards were used for the initial calibration
(i.e., 20, 50, 80, 120, and 160 ng/2uL). For the eight compounds with higher CRQLs,
only a four-point initial calibration is required (i.e., 50, 80, 120, and 160 ng/2uL).
51
-------
sv
[Verify that the correct concentration of standards were used for the initial calibration
(i.e., 5, 10, 20, 50, and 80 ng). For the nine compounds listed in SV Section III.C.I. with
higher CRQLs, verify that a five point initial calibration at 20, 50, 80, 100, and 120 ng
was performed.]
2. If any sample results were calculated using an initial calibration, verify that the correct
standard (i.e., the 50 ng standard) was used for calculating sample results and that the
samples were analyzed within 12 hours of the associated instrument performance check.
[If any sample results were calculated using an initial calibration, verify that the correct
standard (i. e., the 20 ng standard or 80 ngfor the compounds listed in III.C.I) was used
for calculating sample results and that the samples were analyzed within 12 hours of the
associated DFTPP tuning/instrument performance check]
3. Evaluate the RRFs for all semivolatile target compounds and surrogates:
a. Check and recalculate the RRF and RRF for at least one semivolatile target
compound associated with each internal standard. Verify that the recalculated
value(s) agrees with the laboratory reported value(s).
b. Verify that all semivolatile target compounds and surrogates have RRFs that are
greater than or equal to 0.05.
NOTE: The criteria used for data review purposes are different from those used for
contractual purposes. The laboratory must meet a minimum RRF criteria of
0.01, however, for data review purposes, the "greater than or equal to 0.05"
criterion is applied to all semivolatile compounds.
Table 4. Semivolatile Target Compounds Exhibiting Poor Response
2,2'-oxybis( 1 -Chloropropane) Diethylphthalate
4-Chloroaniline 4-Nitroaniline
Hexachlorobutadiene 4,6-Dinitro-2-methylphenol
Hexachlorocyclopentadiene N-Nitrosodiphenylamine
2-Nitroaniline Di-n-butylphthalate
Dimethylphthalate Butylbenzylphthalate
3 -Nitroaniline 3 -3 '-Dichlorobenzidine
2,4-Dinitrophenol bis(2-Ethylhexyl)phthalate
4-Nitrophenol Di-n-octylphthalate
Carbazolef 2,4,6-Tribromophenol (surr)
Nitrobenzene-d5 (surr)
f Multi-Media, Multi-Concentration only
52
-------
sv
4. Evaluate the %RSD for all semivolatile target compounds and surrogates:
a. Check and recalculate the %RSD for one or more semivolatile target
compound(s); verify that the recalculated value(s) agrees with the laboratory
reported value(s).
b. Verify that all semivolatile target compounds have a %RSD of less than 30
percent. The method criteria for an acceptable initial calibration specifies that up
to any 4 semivolatile target compounds may fail to meet minimum RRF or
maximum %RSD as long as they have RRFs that are greater than or equal to
0.010, and %RSD of less than or equal to 40.0 percent. For data review
purposes, however, all compounds must be considered for qualification when the
%RSD exceeds the <30.0 percent criterion.
c. If the %RSD is greater than 30.0 percent, then the reviewer should use
professional judgement to determine the need to check the points on the curve
for the cause of the non-linearity. This is checked by eliminating either the high
point or the low point and recalculating the %RSD.
5. If errors are detected in the calculations of either the RRF or the %RSD, perform a more
comprehensive recalculation.
E. Action:
1. All semivolatile target compounds, including the 19 "poor performers" will be qualified
using the following criteria:
a. If the %RSD is greater than 30.0 percent and the RRF is greater than 0.05,
qualify positive results with "J", and non-detected semivolatile target
compounds using professional judgement.
b. If the RRF is less than 0.05, qualify positive results that have acceptable mass
spectral identification with "J" using professional judgement, and non-detects as
unusable (R).
2. At the reviewer's discretion, a more in-depth review to minimize the qualification of data
can be accomplished by considering the following:
a. If any of the required semivolatile compounds have a %RSD greater than 30.0
percent, and if eliminating either the high or the low point of the curve does not
restore the %RSD to less than or equal to 30.0 percent:
i. Qualify positive results for that compound(s) with "J".
ii. Qualify non-detected semivolatile target compounds based on
professional judgement.
53
-------
sv
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 positive results in the linear portion of the
curve.
ii. Qualify positive results outside of the linear portion of the curve with
"J".
iii. No qualifiers are needed for non-detected target compounds.
c. If the low end of the curve is outside of the linearity criteria:
i. No qualifiers are required for positive results in the linear portion of the
curve.
ii. Qualify low level positive results in the area of non-linearity with "J".
iii. Qualify non-detected semivolatile target compounds using professional
judgement.
3. 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
judgement to assess the data.
4. Whenever possible, the potential effects on the data due to calibration criteria
exceedance should be noted in the data review narrative.
5. If calibration criteria are exceeded, this should be noted for EPA Project Officer action.
54
-------
sv
IV. Continuing Calibration
A. Review Items: Form VII SV-1 [Form VIILCSV-1], Form VII SV-2 [Form VIILCSV-2],
quantitation reports, and chromatograms.
B. Objective:
Compliance requirements for satisfactory instrument calibration are established to ensure that the
instrument is capable of producing acceptable qualitative and quantitative data for semivolatile
target compounds. Continuing calibration establishes the 12-hour relative response factors on
which the quantitations are based and checks satisfactory performance of the instrument on a
day-to-day basis.
C. Criteria:
1. Continuing calibration standards containing both target compounds and surrogates are
analyzed at the beginning of each 12-hour analysis period following the analysis of the
instrument performance check and prior to the analysis of blanks and samples.
2. The minimum Relative Response Factors (RRF) for semivolatile target compounds and
surrogates must be greater than or equal to 0.05.
1. 3. The percent difference (%D) between the initial calibration RRF and the
continuing calibration RRF must be within ± 25.0 percent for all target
compounds.
D. Evaluation:
1. Verify that the continuing calibration was run at the required frequency and that the
continuing calibration was compared to the correct initial calibration.
2. Evaluate the continuing calibration RRF for all semivolatile target compounds and
surrogates.
a. Check and recalculate the continuing calibration RRF for at least one
semivolatile target compound for each internal standard; verify that the
recalculated value(s) agrees with the laboratory reported value(s).
b. Verify that all semivolatile target compounds and surrogates have RRFs within
specifications.
NOTE: The criteria employed for the data review purposes are different from those used
for contractual purposes. The laboratory must meet a minimum RRF criterion of
0.01, however, for data review purposes, the "greater than or equal to 0.05"
criterion is applied to all semivolatile compounds.
55
-------
sv
3. Evaluate the %D between initial calibration RRF and continuing calibration RRF for one
or more semivolatile compounds.
a. Check and recalculate the %D for at least one semivolatile target compound for
each internal standard; verify that the recalculated value(s) agrees with the
laboratory reported value (s).
b. Verify that the %D is within the ±25.0 percent criterion, for all semivolatile
target compounds and surrogates. Note those compounds which have a %D
outside the ±25.0 percent criterion. The method criteria for an acceptable
continuing calibration specifies that up to any 4 semivolatile target compounds
may fail to meet minimum RRF or maximum %D as long as they have RRFs that
are greater than or equal to 0.010, and %D of less than or equal to 40.0 percent.
For data review purposes, however, all compounds must be considered for
qualification when the %D exceeds the ±25.0 percent criterion.
4. If errors are detected in the calculations of either the continuing calibration RRF or the
%D, perform a more comprehensive recalculation.
E. Action:
1. The reviewer should use professional judgement to determine if it is necessary to qualify
the data for any semivolatile target compound. If qualification of data is required, it
should be performed using the following guidelines:
a. If the %D is outside the ±25.0 percent criterion and the continuing calibration
RRF is greater than or equal to 0.05, qualify positive results "J".
b. If the %D is outside the ±25.0 percent criterion and the continuing calibration
RRF is greater than or equal to 0.05, qualify non-detected semivolatile target
compounds "UJ".
c. If the continuing calibration RRF is less than 0.05, qualify positive results that
have acceptable mass spectral identification with "J" or use professional
judgement.
d. If the continuing calibration RRF is less than 0.05, qualify non-detected
semivolatile target compounds as unusable (R).
2. 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
judgement to assess the data.
3. Whenever possible, the potential effects on the data due to calibration criteria
exceedance should be noted in the data review narrative.
56
-------
sv
4. If calibration criteria are grossly exceeded, this should be noted for EPA Project Officer
action.
57
-------
sv
V. Blanks
A. Review Items: Form I SV-1 [Form ILCSV-1], Form I SV-2 [Form ILCSV-2], Form IV SV
[Form IVLCSV], chromatograms, and quantitation reports.
B. Objective:
The purpose of laboratory (or field) blank analyses is to determine the existence and magnitude
of contamination problems resulting from laboratory (or field) activities. The criteria for
evaluation of blanks apply to any blank associated with the samples (e.g., method blanks,
instrument blanks, trip blanks, and equipment blanks). If problems with any blank exist, all
associated data must be carefully evaluated to determine whether or not there is an inherent
variability in the data, or if the problem is an isolated occurrence not affecting other data.
C. Criteria:
1. No contaminants should be found in the blanks.
2. The method blank must be analyzed on each GC/MS system used to analyze that specific
group or set of samples.
D. Evaluation:
1. Review the results of all associated blank, Form I SV-1, Form I SV-2, and raw data
(chromatograms and quantitation reports) to evaluate the presence of target and non-
target compounds in the blanks.
2. Verify that a method blank analysis has been reported per matrix, per concentration
level, for each extraction batch and for each GC/MS system used to analyze semivolatile
samples. The reviewer can use the method blank summary (Form IV SV) to assist in
identifying samples associated with each method blank.
E. Action:
If the appropriate blanks were not analyzed with the frequency described above, then the data
reviewer should use professional judgement to determine if the associated sample data should be
qualified. The reviewer may need to obtain additional information from the laboratory. The
situation should be noted for EPA Project Officer action.
Action in the case of unsuitable blank results depends on the circumstances and origin of the
blank. Positive sample results should be reported unless the concentration of the compound in
the sample is less than or equal to 10 times (lOx) the amount in any blank for the common
phthalate contaminants, or 5 times the amount for other compounds. In instances where more
than one 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. The
results must not be corrected by subtracting any blank value.
58
-------
sv
Specific actions are as follows:
If a semivolatile compound is found in a blank but not found in the sample, no action is taken. If
the contaminants found are volatile target compounds (or interfering non-target compounds) at
significant concentrations above the CRQL, then this should be noted for EPA Project Officer
action.
2. Any semivolatile compound detected in the sample (other than the common phthalate
contaminants), that was also detected in any associated blank, is qualified if the sample
concentration is less than five times (5x) the blank concentration. The quantitation limit
may also be elevated. Typically, the sample CRQL is elevated to the concentration
found in the sample. The reviewer should use professional judgement to determine if
further elevation of the CRQL is required. For phthalate contaminants, the results are
qualified "U" by elevating the sample quantitation limit to the sample concentration
when the sample result is less than lOx the blank concentration.
The reviewer should note that blanks may not involve the same weights, volumes, or
dilution factors as the associated samples. These factors must be taken into
consideration when applying the "5x" and "lOx" criteria, such that a comparison of the
total amount of contamination is actually made.
Additionally, there may be instances where little or no contamination was present in the
associated blanks, but qualification of the sample was deemed necessary. Contamination
introduced through dilution 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. Since both results
are not routinely reported, it may be impossible to verify this source of contamination.
However, if the reviewer determines that the contamination is from a source other than
the sample, he/she should qualify the data. In this case, the "5x" or "lOx" rules may not
apply; the sample value should be reported as a non-detect. An explanation of the
rationale used for this determination should be provided in the narrative accompanying
the Regional Data Assessment Summary.
3. If gross contamination exists (i.e., saturated peaks by GC/MS), all affected compounds in
the associated samples should be qualified as unusable (R), due to interference. This
should be noted for EPA Project Officer action if the contamination is suspected of
having an effect on the sample results.
4. If inordinate amounts of other target compounds are found at low levels in the blank(s),
it may be indicative of a problem and should be noted for EPA Project Officer action.
5. The same consideration given to the target compounds should also be given to
Tentatively Identified Compounds (TICs) which are found in both the sample and
associated blank(s). (See SV Section XIII for TIC guidance.)
59
-------
sv
The following are examples of applying the blank qualification guidelines. Certain
circumstances may warrant deviations from these guidelines.
Example 1:
Example 2:
Example 3:
Sample result is greater than the Contract Required Quantitation Limit
(CRQL), but is less than the 5x or lOx multiple of the blank result.
Rule
Blank Result
CRQL
Sample Result
Qualified Sample Result
lOx
12
10
50
SOU
5x
12
10
40
40U
In the example for the "lOx" rule, sample results less than 120 (or 10 x
12) would be qualified as non-detects. In the case of the "5x" rule,
sample results less than 60 (or 5 x 12) would be qualified as non-detects.
Sample result is less than CRQL, and is also less than the 5x or lOx
multiple of the blank result.
Rule
Blank Result
CRQL
Sample Result
Qualified Sample Result
lOx
12
10
8J
10U
5x
12
10
8J
10U
Note that data are not reported as 8U, as this would be reported as a
detection limit below the CRQL.
Sample result is greater than the 5x or lOx multiple of the blank result.
Rule
Blank Result
CRQL
Sample Result
Qualified Sample Result
lOx
15
10
160
160
5x
15
10
80
80
For both the "lOx" and "5x" rules, sample results exceeded the adjusted
blank results of 150 (or 10x15) and 75 (or 5x15), respectively, and
therefore are not qualified.
60
-------
sv
VI. Surrogate Spikes
A. Review Items: Form II SV-1 and Form II SV-2 [Form IILCSV], chromatograms, and
quantitation reports.
B. Objective:
Laboratory performance on individual samples is established by means of spiking activities. All
samples are spiked with surrogate compounds prior to sample preparation. The evaluation of the
results of these surrogate spikes is not necessarily straightforward. The sample itself may
produce effects due to such factors as interferences and high concentrations of analytes. Since
the effects of the sample matrix are frequently outside the control of the laboratory and may
present relatively unique problems, the evaluation and review of data based on specific sample
results is frequently subjective and demands analytical experience and professional judgment.
Accordingly, this section consists primarily of guidelines, in some cases with several optional
approaches suggested.
C. Criteria:
1. Surrogate spikes, 4 acid compounds (3 required and 1 advisory) and 4 base/neutral
compounds (3 required and 1 advisory) are added to all samples and blanks to measure
their recovery in sample and blank matrices.
[For data generated through the Low Concentration Method: Surrogate spikes, 3 acid
compounds and 3 base/neutral compounds, are added to all samples and blanks to
measure their recovery in sample and blank matrices.]
2. Surrogate spike recoveries for semivolatile samples and blanks must be within the limits
specified on in the method and on Form II SV- 1 and Form II SV-2.
[For data generated through the Low Concentration Method: Surrogate spike recoveries
for semivolatile samples and blanks must be within the limits specified in the method and
on Form II LCSV.]
D. Evaluation:
1. Check raw data (e.g., chromatograms and quantitation reports) to verify the surrogate
spike recoveries on the Surrogate Recovery Form II SV-1 and Form II SV-2 [Form II
LCSV]. Check for any transcription or calculation errors.
2. Check that the surrogate spike recoveries were calculated correctly. The equation can be
found in the method.
61
-------
sv
3. The following should be determined from the Surrogate Recovery form(s):
a. If any two base/neutral or acid surrogates are out of specification, or if any one
base/neutral or acid extractable surrogate has a recovery of less than 10 percent,
then there should be a re-analysis to confirm that the non-compliance is due to
sample matrix effects rather than laboratory deficiencies.
NOTE: When there are unacceptable surrogate recoveries followed by successful re-
analyses, the laboratories are required to report only the acceptable run.
b. The laboratory has failed to perform satisfactorily if surrogate recoveries are out
of specification and there is no evidence of reinjection of the extract, or
reextraction and re-analysis (if reinjection fails to resolve the problem).
c. Verify that no blanks have surrogate recoveries outside the criteria.
4. Any time there are two or more analyses for a particular fraction the reviewer must
determine which are the best data to report. Considerations should include but are not
limited to:
a. Surrogate recovery (marginal versus gross deviation).
b. Technical holding times.
c. Comparison of the values of the target compounds reported in each fraction.
d. Other QC information, such as performance of internal standards.
E. Action:
Data are not qualified with respect to surrogate recovery unless two or more semivolatile
surrogates, within the same fraction (base/neutral or acid fraction), are out of specification. For
surrogate spike recoveries out of specification, the following approaches are suggested based on
a review of all data from the Case, especially considering the apparent complexity of the sample
matrix.
1. If two or more surrogates in either semivolatile fraction (base/neutral or acid fraction)
have a recovery greater than the upper acceptance limit (UL):
a. Specify the fraction that is being qualified (i.e. acid, base/neutral, or both).
b. Detected semivolatile target compounds are qualified "J."
c. Results for non-detected semivolatile target compounds should not be qualified.
62
-------
sv
2. If two or more surrogates in either semivolatile fraction have a recovery greater than or
equal to 10 percent but less than the lower acceptance limit (LL):
a. Specify the fraction that is being qualified (i.e. acid, base/neutral, or both).
b. Detected semivolatile target compounds are qualified "J".
c. For non-detected semivolatile target compounds, the sample quantitation limit is
qualified as approximated (UJ).
3. In the case where two or more surrogates are out in either semivolatile fraction; one with
a recovery greater than the upper acceptance limit and one with a recovery greater than
or equal to 10 percent but less than the lower acceptance limit, qualify as described in SV
Section VI.E.2 a, b, and c above.
4. If any surrogate in either semivolatile fraction show less than 10 percent recovery:
a. Specify the fraction that is being qualified (i.e. acid, base/neutral, or both).
b. Detected semivolatile target compounds are qualified "J".
c. Non-detected semivolatile target compounds may be qualified 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.
6. Whenever possible, the potential effects of the data resulting from surrogate recoveries
not meeting the advisory limits should be noted in the data review narrative.
Additionally, the lack of re-analysis of samples that were out of specification should be
noted for EPA Project Officer action.
63
-------
sv
VII. Matrix Spikes/Matrix Spike Duplicates
(Not Required for Low Concentration Water Data)
A. Review Items: Form III SV-1, Form III SV-2, chromatograms, and quantitation reports.
B. Objective:
Data for matrix spikes/matrix spike duplicates (MS/MSD) are generated to determine long-term
precision and accuracy of the analytical method on various matrices and to demonstrate
acceptable compound recovery by the laboratory at the time of sample analysis. These data
alone cannot be used to evaluate the precision and accuracy of individual samples. However,
when exercising professional judgement, this data should be used in conjunction with other
available QC information.
C. Criteria:
1. A matrix spike and matrix spike duplicate are extracted and analyzed for every 20 field
samples of similar matrix in an SDG, whenever samples are extracted by the same
procedure, unless MS/MSD analyses are not required.
2. Matrix spike and matrix spike duplicate recoveries should be within the advisory limits
established on Form III SV- 1 and Form III SV-2.
3. The Relative Percent Differences (RPDs) between matrix spike and matrix spike
duplicate recoveries should be within the advisory limits listed on Form III SV-1 and
Form III SV-2.
D. Evaluation:
1. Verify that MS and MSD samples were analyzed at the required frequency and that
results are provided for each sample matrix.
2. Inspect results for the MS/MSD Recovery on Form III SV-1 and Form III SV-2 and
verify that the results for recovery and RPD are within the advisory limits.
3. Verify transcriptions from raw data and verify calculations.
4. Check that the recoveries and RPD were calculated correctly.
5. Compare results (%RSD) of non-spiked compounds between the original result, MS, and
MSD.
64
-------
sv
E. Action:
1. No action is taken on MS/MSD data alone. However, using informed professional
judgment the data reviewer may use the matrix spike and matrix spike duplicate results
in conjunction with other QC criteria and determine the need for some qualification of
the data.
2. The data reviewer should first try to determine to what extent the results of the MS/MSD
effect the associated data. This determination should be made with regard to the
MS/MSD sample itself as well as specific analytes for all samples associated with the
MS/MSD.
3. In those instances where it can be determined that the results of the MS/MSD effect only
the sample spiked, then qualification should be limited to this sample alone. However, it
may be determined through the MS/MSD results that a laboratory is having a systematic
problem in the analysis of one or more analytes, which affects all associated samples.
4. The reviewer must use professional judgement to determine the need for qualification of
positive results of non-spiked compounds.
NOTE: If a field blank was used for the MS/MSD, the EPA Project Officer must be
notified.
65
-------
sv
VIII. Laboratory Control Samples
(Low Concentration Water)
[A. Review Items: Form III LCSV, LCS chromatograms, and quantitation reports.
B. Objective:
Data for Laboratory Control Samples (LCS) are generated to provide information on the
accuracy of the analytical method and the laboratory performance.
C. Criteria:
1. Laboratory control samples are prepared, extracted, analyzed, and reported once per
SDG. The LCS must be extracted and analyzed concurrently with the samples in the
SDG, using the same instrumentation as the samples in the SDG.
2. LCS percent recoveries must he within the QC limits provided on Form III LCSV. The
LCS must meet the recovery criteria for the sample data to be accepted.
3. The LCS contains the following semivolatile target compounds, in addition to the
required surrogates:
Phenol Naphthalene
2-Chlorophenol 2,4-Dinitrotoluene
4-Chloroaniline Diethylphthalate
2,4,6-Trichlorophenol N-Nitrosodiphenylamine
bis(2-Chloroethyl)ether Hexachlorobenzene
N-Nitroso-di-n-propylamine Benzo (a)pyrene
Hexachloroethane
Isophorone
4. The criteria for surrogate recovery and internal standard performance also apply.
D. Evaluation:
1. Verify that LCS samples were analyzed at the required frequency.
2. Inspect the results for LCS Recovery on Form III LCSV and verify that the results for
recovery are within the QC limits.
3. Verify transcriptions from raw data and verify calculations.
4. Check that the recoveries were calculated correctly.
66
-------
sv
E. Action:
If the LCS criteria are not met, then the laboratory performance and method accuracy are in
question. Professional judgement should be used 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. Action on the LCS recovery should be based on both the number of compounds that are
outside of the recovery criteria and the magnitude of the exceedance of the criteria.
2. If the LCS recovery criteria are not met, then the LCS results should be used to qualify
sample data for the specific compounds that are included in the LCS solution.
Professional judgement should be used to qualify data for compounds other than those
compounds that are included in the LCS. Professional judgement to qualify non-LCS
compounds should take into account the compound class, compound recovery efficiency,
analytical problems associated with each compound, and comparability in performance
of the LCS compound to the non-LCS compound.
3. If the LCS recovery is greater than the upper acceptance limit, then positive sample
results for the affected compound(s) should be qualified with a "J\
4. If the mass spectral criteria are met but the LCS recovery is less than the lower
acceptance limit, then the associated detected target compounds should be qualified "J"
and the associated non-detected target compounds should be qualified "K\
5. If more than half of the compounds in the LCS are not within the recovery criteria, then
all of the associated detected target compounds should be qualified "J" and all
associated non-detected target compounds should be qualified "K\
6. Action on non-compliant surrogate recovery and internal standard performance should
follow the procedures provided in SV Section VI.EandX.E, respectively. Professional
judgement should be used to evaluate the impact that non-compliance for surrogate
recovery and internal standard performance in the LCS has on the associated sample
data.
7. It should be noted for EPA Project Officer action if a laboratory fails to analyze an LCS
with each SDG, or if a laboratory consistently fails to generate acceptable LCS
recoveries.]
67
-------
sv
IX. Regional Quality Assurance and Quality Control
A. Review Items: Form I SV-1 [Form ILCSV-1], Form I SV-2 [Form ILCSV-2], chromatograms,
quantitation report, Traffic Report, and raw data for Regional QC samples.
B. Objective:
Regional Quality Assurance and Quality Control (QA/QC) refer to any QA and/or QC initiated
by the Region, including field duplicates, Regional Performance Evaluation (PE) samples, blind
spikes, and blind blanks. (It is highly recommended that Regions adopt the use of these QA/QC
samples.)
C. Criteria:
Criteria are determined by each Region.
1. Performance Evaluation sample frequency may vary.
[For data generated through the Low Concentration Method: A PE sample can be
included as frequently as once per SDG.J
2. The analytes present in the PE sample must be correctly identified and quantified.
D. Evaluation:
Evaluation procedures must follow the Region's SOP for data review. Each Region will handle
the evaluation of PE samples on an individual basis. Results for PE samples should be compared
to the acceptance criteria for the specific PE samples, if available.
E. Action:
Any action must be in accordance with Regional specifications and the criteria for acceptable PE
sample results. Unacceptable results for PE samples should be noted for EPA Project Officer
action.
68
-------
sv
X. Internal Standards
A. Review Items: Form VIII SV-1 [Form VIIILCSV-1], Form VIII SV-2 [Form VIIILCSV-2],
quantitation reports, and chromatograms.
B. Objective:
Internal Standards (IS) performance criteria ensure that GC/MS sensitivity and response are
stable during every analytical run.
C. Criteria:
1. Internal standard area counts for samples and blanks must not vary by more than a factor
of two (-50 percent to + 100 percent) from the associated 12hr calibration standard.
2. The retention time of the internal standards in samples and blanks must not vary by more
than ±30 seconds from the retention time of the associated 12hr calibration standard.
[For data generated through the Low Concentration Method: The retention time of the
internal standards in samples and blanks must not vary by more than ±20.0 seconds
from the retention time of the associated calibration standard.]
D. Evaluation:
1. Check raw data (e.g., chromatograms and quantitation lists) for samples and blanks to
verify the internal standard retention times and areas reported on the Internal Standard
Area Summary (Form VIII SV-1 [Form VIIILCSV-1] and Form VIII SV-2 [Form VIII
LCSV-2]).
2. Verify that all retention times and IS areas are within the required criteria.
3. If there are two analyses for a particular fraction, the reviewer must determine which are
the best data to report. Considerations should include:
a. Magnitude and direction of the IS area shift.
b. Magnitude and direction of the IS retention time shift.
c. Technical holding times.
d. Comparison of the values of the target compounds reported in each fraction.
69
-------
sv
E. Action:
1. If an IS area count for a sample or blank is outside -50 percent or +100 percent of the
area for the associated standard:
a. Positive results for compounds quantitated using that IS should be qualified with
"J".
b. Non-detected compounds quantitated using an IS area count greater than 100
percent should not be qualified.
c. Non-detected compounds quantitated using an IS area count less than 50 percent
are reported as the associated sample quantitation limit and qualified with "UJ".
d. If extremely low area counts are reported, or if performance exhibits a major
abrupt drop-off, then a severe loss of sensitivity is indicated. Non-detected
target compounds should then be qualified as unusable (R).
2. If an IS retention time varies by more than 30 seconds:
[If an IS retention time varies by more than 20.0 seconds:]
The chromatographic profile for that sample must be examined to determine if any false
positives or negatives exist. For shifts of a large magnitude, the reviewer may consider
partial or total rejection (R) of the data for that sample fraction. Positive results should
not need to be qualified with "R" if the mass spectral criteria are met.
3. If the internal standards performance criteria are grossly exceeded, then this should be
noted for EPA Project Officer action. Potential effects on the data resulting from
unacceptable internal standard performance should be noted in the data review narrative.
70
-------
sv
XL Target Compound Identification
A. Review Items: Form I SV-1 [Form ILCSV-1], Form I SV-2 [Form ILCSV-2], quantitation
reports, mass spectra, and chromatograms.
B. Objective:
Qualitative criteria for compound identification have been established to minimize the number of
erroneous identifications of compounds. An erroneous identification can either be a false
positive (reporting a compound present when it is not) or a false negative (not reporting a
compound that is present).
The identification criteria can be applied much more easily in detecting false positives than false
negatives. More information is available due to the requirement for submittal of data supporting
positive identifications. Negatives, or non-detected compounds, on the other hand represent an
absence of data and are, therefore, much more difficult to assess. One example of detecting false
negatives is the reporting of a Target Compound as a TIC.
C. Criteria:
1. Compound must be within ±0.06 relative retention time (RRT) units of the standard
RRT.
2. Mass spectra of the sample compound and a current laboratory-generated standard must
match according to the following criteria:
a. All ions present in the standard mass spectrum at a relative intensity greater than
10 percent must be present in the sample spectrum.
[For data generated through the Low Concentration Method: All ions present in
the standard mass spectrum at a relative intensity greater than 25 percent must
be present in the sample spectrum.]
b. The relative intensities of these ions must agree within ±20 percent between the
standard and sample spectra. (Example: For an ion with an abundance of 50
percent in the standard spectrum, the corresponding sample ion abundance must
be between 30 percent and 70 percent.)
c. Ions present at greater than 10 percent in the sample mass spectrum but not
present in the standard spectrum must be considered and accounted for.
[For data generated through the Low Concentration Method: Ions present at
greater than 25 percent in the sample mass spectrum but not present in the
standard mass spectrum must be considered and accounted for.]
71
-------
sv
D. Evaluation:
1. Check that the RRT of reported compounds is within ±0.06 RRT units of the standard
relative retention time.
2. Check the sample compound spectra against the laboratory standard spectra to verify that
it meets the specified criteria.
3. The reviewer should be aware of situations (e.g., high concentration samples preceding
low concentration samples) when sample carryover is a possibility and should use
judgment to determine if instrument cross-contamination has affected any positive
compound identification.
4. Check the chromatogram to verify that peaks are accounted for (i.e., major peaks are
either identified as target compounds, TICs, surrogates, or internal standards).
E. Action:
1. The application of qualitative criteria for GC/MS analysis of target compounds requires
professional judgement. It is up to the reviewer's discretion to obtain additional
information from the laboratory. If it is determined that incorrect identifications were
made, all such data should be qualified as not detected (U) or unusable (R).
2. Professional judgement must be used to qualify the data if it is determined that cross-
contamination has occurred.
3. Any changes made to the reported compounds or concerns regarding target compound
identifications should be clearly indicated in the data review narrative. The necessity for
numerous or significant changes should be noted for EPA Project Officer action.
72
-------
sv
XII. Compound Ouantitation and Reported CRQLS
A. Review Items: Form I SV-1 [Form ILCSV-1], Form I SV-2 [Form ILCSV-2], sample
preparation sheets, SDG Narrative, sample clean-up sheets, quantitation reports, and
chromatograms.
B. Objective:
The objective is to ensure that the reported quantitation results and Contract Required
Quantitation Limits (CRQLs) for semivolatile target compounds are accurate.
C. Criteria:
1. Compound quantitation, as well as the adjustment of the CRQL, must be calculated
according to the correct equation.
2. Compound area responses must be calculated based on the internal standard (IS)
associated with that compound, as listed in the method. Quantitation must be based on
the quantitation ion (m/z) specified in the method for both the IS and target analytes.
The compound quantitation must be based on the RRF from the appropriate daily
calibration standard.
D. Evaluation:
1. For all fractions, raw data should be examined to verify the correct calculation of all
sample results reported by the laboratory. Quantitation lists, chromatograms, and sample
preparation log sheets should be compared to the reported positive sample results and
quantitation limits. Check the reported values.
2. Verify that the correct internal standard, quantitation ion, and RRF were used to
quantitate the compound. Verify that the same internal standard, quantitation ion, and
RRF are used consistently throughout the calibration and quantitation processes.
3. Verify that the CRQLs have been adjusted to reflect all sample dilutions, concentrations,
splits, clean-up activities, and dry weight factors that are not accounted for by the
method.
E. Action:
If there are any discrepancies found, the laboratory may be contacted by the Region's
designated representative to obtain additional information that could resolve any
differences. If a discrepancy remains unresolved, the reviewer must use professional
judgement to decide which value is the best value. Under these circumstances, the
reviewer may determine qualification of data is warranted. Decisions made on data
73
-------
sv
quality should be included in the data review narrative. A description of the reasons for
data qualification and the qualification that is applied to the data should be documented
in the data review narrative.
2. Numerous or significant failures to accurately quantify the target compound or to
properly evaluate and adjust CRQLs should be noted for EPA Project Officer action.
74
-------
sv
XIII. Tentatively Identified Compounds
A. Review Items: Form I SV-TIC [Form ILCSV-TIC], chromatograms, and library search
printouts with spectra for the TIC candidates.
B. Objective:
Chromatographic peaks in semivolatile fraction analyses that are not target analytes, surrogates,
or internal standards are potential tentatively identified compounds (TICs). TICs must be
qualitatively identified by a National Institute of Standards and Technology (NIST) mass spectral
library search and the identifications assessed by the data reviewer.
C. Criteria:
For each sample, the laboratory must conduct a mass spectral search of the NIST library and
report the possible identity for the appropriate number of the largest semivolatile fraction peaks
which are not surrogate, internal standard, or target compounds, but which have area or height
greater than 10 percent of the area or height of the nearest internal standard. Peaks that are
suspected to be part of an alkane series shall be library searched and reported, as the alkane series
(e.g., C5-C9), as a single entry along with the estimate for the total concentration of the series.
TIC results are reported for each sample on the Organic Analyses Data Sheet (Form I SV-TIC).
[For data generated through the Low Concentration Method: For each sample, the laboratory
must conduct a mass spectral search of the NIST library and report the possible identity for the
appropriate number of the largest semivolatile fraction peaks which are not surrogates, internal
standards, or target compounds, but which have an area greater than 50 percent of the area of
the nearest internal standard. Estimated concentrations for TICs are calculated similarly to the
target compounds, using total ion areas for the TIC and the internal standard, and assuming a
relative response factor of 1.0. Peaks that are suspected to be part of an alkane series shall be
library searched and reported, as the alkane series (e.g., C5-C9), as a single entry along with the
estimate for the total concentration of the series. TIC results are reported for each sample on the
Organic Analyses Data Sheet (Form ILCSV- TIC).]
NOTE: Since the method revision of October 1986, the CLP does not allow the
laboratory to report as tentatively identified compounds any target compound
which is properly reported in another fraction. For example, late eluting volatile
target compounds should not be reported as semivolatile TICs.
75
-------
sv
D. Evaluation:
1. Guidelines for tentative identification are as follows:
a. Major ions (greater than 10 percent relative intensity) in the reference spectrum
should be present in the sample spectrum.
[Major ions (greater than 25 percent relative intensity) in the reference
spectrum should be present in the sample spectrum.]
b. The relative intensities of the major ions should agree within ±20 percent
between the sample and the reference spectra.
c. Molecular ions present in the reference spectrum should be present in the sample
spectrum.
d. Ions present in the sample spectrum but not in the reference spectrum should be
reviewed for possible background contamination, interference, or coelution of
additional TIC or target compounds.
e. When the above criteria are not met, but in the technical judgment of the data
reviewer or mass spectral interpretation specialist the identification is correct, the
data reviewer may report the identification.
f If, after careful review and in the technical judgement of the mass spectral
interpretation specialist, no valid identification can be made, the compound
should be reported as follows:
If the library search produces a match at or above 85%, report that
compound.
If the library search produces more than one compound at or above 85%,
report the first compound (highest).
If the library search produces no matches at or above 85%, the
compound should be reported as unknown. The mass spectral specialist
should give additional classification of the unknown compound, if
possible (i.e., unknown hydrocarbon, unknown acid type, unknown
chlorinated coumpound). If probable molecular weights can be
distinguished, include them.
76
-------
sv
2. Check the raw data to verify that the laboratory has generated a library search for all
required peaks in the chromatograms for samples and blanks.
[Check the raw data to verify that the laboratory has generated a library search for all
required peaks in the chromatograms for samples and blanks with areas greater than or
equal to 50 percent of the area of the nearest internal standard.]
3. Blank chromatograms should be examined to verify that TIC peaks present in samples
are not found in blanks. When a low-level non-target compound that is a common
artifact or laboratory contaminant is detected in a sample, a thorough check of blank
chromatograms may require looking for peaks which are less than 10 percent of the
internal standard height, but present in the blank chromatogram at a similar relative
retention time.
[Blank chromatograms should be examined to verify that TIC peaks present in samples
are not found in blanks. When a low-level non-TCL compound that is a common artifact
or laboratory contaminant is detected in a sample, a thorough check of blank
chromatograms may require looking for peaks which have areas less than 50 percent of
the internal standard area, but present in the blank chromatogram at a similar relative
retention time.]
4. All mass spectra for each sample and blank must be examined.
5. Since TIC library searches often yield several candidate compounds having a close
matching score, all reasonable choices should be considered.
6. Check the raw data to verify that the laboratory has properly identified and assigned
peaks to the alkane series.
7. The reviewer should be aware of common laboratory artifacts/contaminants and their
sources (e.g., aldol condensation products, solvent preservatives, and reagent
contaminants). These may be present in blanks and not reported as sample TICs.
Examples:
a. Common laboratory contaminants: CO2 (m/z 44), siloxanes (m/z 73), diethyl
ether, hexane, certain freons, and phthalates at levels less than 100 ug/L or 4000
ug/Kg.
b. Solvent preservatives, such as cyclohexene which is a methylene chloride
preservative. Related by-products include cyclohexanone, cyclohexenone,
cyclohexanol, cyclohexenol, chlorocyclohexene, and chlorocyclohexanol.
c. Aldol reaction products of acetone include: 4-hydroxy-4-methyl-2-pentanon, 4-
methyl-2-penten-2-one, and 5,5-dimethyl-2(5H)-furanone.
77
-------
sv
8. Occasionally, a target compound may be identified as a TIC in the proper analytical
fraction by non-target library search procedures, even though it was not found on the
quantitation list. If the total area quantitation method was used, the reviewer should
request that the laboratory recalculate the result using the proper quantitation ion. In
addition, the reviewer should evaluate other sample chromatograms and check library
reference retention time quantitation lists to determine whether the false negative result is
an isolated occurrence whether additional data may be affected.
9. Target compounds may be identified in more than one fraction. Verify that quantitation
is made from the proper fraction.
10. Library searches should not be performed on internal standards or surrogates.
11. TIC concentration should be estimated assuming a RRF of 1.0.
E. Action:
1. All TIC results should be qualified "NJ", tentatively identified, 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 not
acceptable, the tentative identification should be changed to "unknown" or an
appropriate identification.
b. If all contractually required peaks were not library searched and quantitated, the
Region's designated representative could request these data from the laboratory.
3. TIC results which are not sufficiently above the level in the blank should not be reported.
(Dilutions and sample size must be taken into account when comparing the amounts
present in blanks and samples.)
4. When a compound is not found in any blanks, but is a suspected artifact of common
laboratory contamination, the result may be qualified as unusable (R).
5. In deciding whether a library search result for a TIC represents a reasonable
identification, professional judgment must be exercised. If there is more than one
possible match, the result may be reported as "either compound X or compound Y". If
there is a lack of isomer specificity, the TIC result may be changed to a non-specific
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 substituted aromatic compound).
78
-------
sv
6. The reviewer may elect to report all similar isomers as a total. All alkanes may be
summarized and reported as total hydrocarbons (e.g., alkane series C5-C9). Reporting an
alkane series counts only as one of the 30 most intense non-target semi-volatile
compounds.
7. Other case factors may influence TIC judgments. If a sample TIC match is poor but
other samples have a TIC with a good library match, similar relative retention time, and
the same ions, identification information may be inferred from the other sample TIC
results.
8. Physical constants, such as boiling point, may be factored into professional judgment of
TIC results.
9. Any changes made to the reported data or any concerns regarding TIC identifications
should be indicated in the data review narrative.
10. Failure to properly evaluate and report TICs should be noted for EPA Project Officer
action.
79
-------
sv
XIV. System Performance
A. Review Items: Form III SV-1 and Form III SV-2 [Form IIILCSV], Form VIII SV-1 [Form VIII
LCSV-1], Form VIII SV-2 [Form VIIILCSV-2], and chromatograms.
B. Objective:
During the period following Instrument Performance QC checks (e.g., blanks, tuning,
calibration), changes may occur in the system that degrade the quality of the data. While this
degradation would not be directly shown by QC checks until the next required series of
analytical QC runs, a through review of the ongoing data acquisition can yield indicators of
instrument performance.
C. Criteria:
There are no specific criteria for system performance. Professional judgement should be used to
assess the system performance.
D. Evaluation:
1. Abrupt, discrete shifts in the reconstructed ion chromatogram (RIC) baseline may
indicate a change in the instrument's sensitivity or the zero setting. A baseline shift
could indicate a decrease in sensitivity in the instrument or an increase in the instrument
zero, possibly causing target compounds at or near the detection limit to be non-detects.
A baseline "rise" could indicate problems such as a change in the instrument zero, a leak,
or degradation of the column.
2. Poor chromatographic performance affects both qualitative and quantitative results.
Indications of substandard performance include:
a. High RIC background levels or shifts in absolute retention times of internal
standards.
b. Excessive baseline rise at elevated temperature.
c. Extraneous peaks.
d. Loss of resolution as suggested between by factors such as non-resolution of 2,4-
and 2,5- dinitrotoluene.
e. Peak tailing or peak splitting that may result in inaccurate quantitation.
[3. A drift in instrument sensitivity may occur during the 12-hour time period. This could be
discerned by examination of the IS area on Form VIII LCSV-1 and Form VIIILCSV-2
for trends such as a continuous or near-continuous increase or decrease in the IS area
over time.
80
-------
sv
4. The results of the LCS analysis (Form III LCSV) may also be used to assess instrument
performance.]
E. Action:
Professional judgement must be used to qualify the data if it is determined that system
performance has degraded during sample analyses. Any degradation of system performance
which significantly affected the data should be documented for EPA Project Officer action.
81
-------
sv
XV. Overall Assessment of Data
A. Review Items: Entire data package, data review results, and (if available) Quality Assurance
Project Plan (QAPjP), and Sampling and Analysis Plan (SAP).
B. Objective:
The overall assessment of a data package is a brief narrative in which the data reviewer expresses
concerns and comments on the quality and, if possible, the useability of the data.
C. Criteria:
Assess the overall quality of the data.
D. Evaluation:
1. Evaluate any technical problems which have not been previously addressed.
2. Review all available materials to assess the overall quality of the data, keeping in mind
the additive nature of analytical problems.
3. If appropriate information is available, the reviewer may assess the useability of the data
to assist the data user in avoiding inappropriate use of the data. Review all available
information, including the QAPjP (specifically the Data Quality Objectives), SAP, and
communication with data user that concerns the intended use and desired quality of the
data.
E. Action:
1. Use professional judgement to determine if there is any need to qualify data which were
not qualified based on the QC criteria previously discussed.
2. Write a brief narrative to give the user an indication of the analytical limitations of the
data. Any inconsistency of that data with the SDG Narrative should be noted for EPA
Project Officer action. If sufficient information on the intended use and required quality
of the data are available, the reviewer should include his/her assessment of the useability
of the data within the given context.
82
-------
PEST
PESTICIDE/AROCLOR DATA REVIEW
***Data review guidelines that are unique to data generated through the Low Concentration Water
Method are contained within brackets ([]) and written in italics. ***
The pesticide/Aroclor data requirements to be checked are listed below.
I. Holding Times
II. GC/ECD Instrument Performance Check
III. Initial Calibration
IV. Calibration Verification
V. Blanks
VI. Surrogate Spikes
VII. Matrix Spikes/Matrix Spike Duplicates
[VIII. Laboratory Control Samples]
IX. Regional Quality Assurance and Quality Control
X. Pesticide Cleanup Checks
XI. Target Compound Identification
XII. Compound Quantitation and Reported Contract Required Quantitation Limits (CRQLs)
XIII. Overall Assessment of Data
83
-------
PEST
I. Holding Times
A. Review Items: Form I PEST [Form ILCP], EPA Sample Traffic Report and/or chain-of-
custody, raw data, sample extraction sheets, and SDG Narrative.
B. Objective:
The objective is to ascertain the validity of results based on the holding time of the sample from
time of collection to time of sample extraction and analysis.
C. Criteria:
Technical requirements for sample holding times have only been established for water matrices.
The technical holding time criteria for water samples are as follows:
For pesticides and Aroclors in cooled (@ 4°C) water samples, 7 days from sample
collection to time of extraction and then 40 days from sample extraction to analysis.
It is recommended that pesticides and Aroclors in soil samples be extracted within 14 days of
sample collection.
The method holding times, which differ from the technical holding times, state that extraction of
water samples by separatory funnel must be completed within 5 days of validated time of sample
receipt (VTSR), extraction of water samples by continuous liquid-liquid extraction procedures
must be started within 5 days of VTSR, and soil/sediment samples are to be extracted within 10
days of VTSR. Also, contractually both water and soil sample extracts must be analyzed within
40 days of sample extraction.
[For data generated through the Low Concentration Method: The holding times requirements
are that the extraction of all samples must be started within 5 days of the VTSR, and the extracts
must be analyzed within 40 days of VTSR.]
D. Evaluation:
Technical holding times for sample extraction are established by comparing the sample
collection date on the EPA Sample Traffic Report with the dates of extraction on Form I PEST
[Form I LCP] and the sample extraction sheets. To determine if the samples were analyzed
within the holding time after extraction, compare the dates of extraction on the sample extraction
sheets with the dates of analysis on Form I PEST [Form I LCP].
Verify that the Traffic Report indicates that the samples were received intact and iced. If the
samples were not iced or there were any problems with the samples upon receipt, then
discrepancies in the sample condition could effect the data.
84
-------
PEST
E. Action:
1. If technical holding times are exceeded, qualify all detected compound results as
estimated "J" and sample quantitation limits as estimated "UJ", and document in the data
review narrative that holding times were exceeded.
2. If technical holding times are grossly exceeded, either on the first analysis or upon re-
analysis, the reviewer must use professional judgement to determine the reliability of the
data and the effect of additional storage on the sample results. The reviewer may
determine that detected compound results or the associated quantitation limits are
approximates and should be qualified with "J" or "UJ", respectively. The reviewer may
determine that non-detected target compound data are unusable (R).
3. Due to limited information concerning holding times for soil samples, it is left to the
discretion of the data reviewer to apply water holding time criteria to soil samples.
Professional judgement is required to evaluate holding times for soil samples.
4. Whenever possible, the reviewer should comment on the effect of exceeding the holding
time on the resulting data in the data review narrative.
5. When method and/or technical holding times are exceeded, this should be noted as an
action item for the EPA Project Officer.
6. The reviewer should also be aware of the scenario in which the laboratory has exceeded
the technical holding times, but met contractual holding times. In this case, the data
reviewer should notify the EPA Project Officer (where samples were collected) and/or
RSCC that shipment delays have occurred so that the field problem can be corrected.
The reviewer may pass this information on to the laboratory's EPA Project Officer, but
should explain that contractually the laboratory met the method requirements.
85
-------
PEST
II. GC/ECD Instrument Performance Check
A. Review Items: Forms VI PEST-4 [Form VILCP-4], Form VI PEST-5/Forra VILCP-5], Form
VII PEST-1 [Form VULCP-l], FormVIII PEST [Form VIIILCP], chromatograms, and data
system printouts.
B. Objective:
Performance checks on the gas chromatograph with electron capture detector (GC/ECD) system
are performed to ensure adequate resolution and instrument sensitivity. These criteria are not
sample specific. Conformance is determined using standard materials, therefore, these criteria
should be met in all circumstances.
C. Criteria:
1 . Resolution Check Mixture
a. The Resolution Check Mixture must be analyzed at the beginning of every initial
calibration sequence, on each GC column and instrument used for analysis. The
Resolution Check Mixture contains the following pesticides and surrogates:
gamma-Chlordane Endrin ketone
Endosulfan I Methoxychlor
4,4'-DDE Tetrachloro-m-xylene
Dieldrin Decachlorobiphenyl
Endosulfan sulfate
b. The depth of the valley between two adjacent peaks in the Resolution Check
Mixture must be greater than or equal to 60.0 percent of the height of the shorter
peak.
2. Performance Evaluation Mixture
a. The Performance Evaluation Mixture (PEM) must be analyzed at the beginning
(following the resolution check mixture) and at the end of the initial calibration
sequence. The PEM must also be analyzed at the beginning of every other 12-
hour analytical period. The PEM contains the following pesticides and
surrogates:
86
-------
PEST
gamma-BHC Endrin
alpha-BHC Methoxychlor
4,4'-DDT Tetrachloro-m-xylene
beta-BHC Decachlorobiphenyl
b. All peaks in the Performance Evaluation Mixture injections must be greater than
or equal to 90 percent resolved on each GC column. This applies to both initial
and continuing calibrations.
c. The absolute retention times of each of the single component pesticides and
surrogates in all PEM analyses must be within the specific retention time
windows centered around the mean retention times determined from the three-
point initial calibration using the Individual Standard Mixtures.
For example, for a given pesticide the mean retention time is first determined
from the initial calibration and found to be 12.69 minutes. The retention time
window for this pesticide is ±0.05 minutes. Therefore, the calculated retention
time window would range from 12.64 to 12.74 minutes.
d. The percent difference between the calculated amount (amount found) and the
nominal amount (amount added) for each of the single component pesticides and
surrogates in both of the PEM analyses on each GC column must be greater than
or equal to -25.0 percent, AND less than or equal to 25.0 percent using the
equation as specified in the method.
e. The percent breakdown is the amount of decomposition that 4,4'-DDT and
Endrin undergo when analyzed on the GC column. For Endrin, the percent
breakdown is determined by the presence of Endrin aldehyde and/or Endrin
ketone in the GC chromatogram. For 4,4-DDT, the percent breakdown is
determined from the presence of 4,4'-DDD and/or 4,4'-DDE in the GC
chromatogram.
i. The percent breakdown for both 4,4'-DDT and Endrin in each PEM must
be less than or equal to 20.0 percent for both GC columns.
ii. The combined percent breakdown for 4,4'-DDT and Endrin in each PEM
must be less than or equal to 30.0 percent for both GC columns.
87
-------
PEST
D. Evaluation:
1 . Resolution Check Mixture
a. Verify from the Form VIII PEST [Form VIIILCP] that the resolution check
mixture was analyzed at the beginning of the initial calibration sequence on each
GC column and instrument used for analysis.
b. Check the resolution check mixture data and Form VI PEST-4 [Form VILCP-4]
to verify that the resolution criterion between two adjacent peaks for the required
compounds is greater than or equal to 60 percent.
2. Performance Evaluation Mixture
a. Verify from the Form VIII PEST [Form VIII LCP] that the Performance
Evaluation Mixture (PEM) was analyzed at the proper frequency and position
sequence.
b. Check the PEM data from Form VI PEST-5, and the initial and continuing
calibrations to verify that the resolution between adjacent peaks is greater than or
equal to 90 percent on both GC columns.
c. Check the PEM data from the initial and continuing calibrations and Form VII
PEST-1 to verify that the absolute retention times for the pesticides in each
analysis are within the calculated retention time windows based on the mean
retention time from the three-point initial calibration.
d. Verify that the percent difference between the calculated amount (amount found)
and the nominal amount (amount added) for each of the single component
pesticides and surrogates in both of the PEM analyses on each GC column must
be greater than or equal to -25.0 percent, AND less than or equal to 25.0 percent.
e. Verify that the individual breakdowns for 4,4'-DDT and Endrin are less than or
equal to 20.0 percent, and that the combined breakdown is less than or equal to
30.0 percent.
E. Action:
1. Resolution Check Mixture
a. If the Resolution Check Mixture was not analyzed with the frequency described
in PEST Section II.C. 1, then the data reviewer should use professional
judgement to determine if the associated sample data should be qualified. The
reviewer may need to obtain additional information from the laboratory. This
situation should be brought to the attention of the EPA Project Officer.
88
-------
PEST
b. If resolution criteria are not met, the quantitative results may not be accurate due
to inadequate resolution. Detected target compounds that were not adequately
resolved should be qualified with "J". Qualitative identifications may also be
questionable if coelution exists. Non-detects with retention times in the region
of coelution may not be valid, depending on the extent of the problem.
Professional judgement should be used to determine the need to qualify data as
unusable (R).
2. Performance Evaluation Mixture Frequency
If the Performance Evaluation Mixture was not analyzed with the frequency described in
PEST Section II.C.2, then the data reviewer should use professional judgement to
determine if the associated sample data should be qualified. The reviewer may need to
obtain additional information from the laboratory. This situation should be brought to
the attention of the EPA Project Officer.
3. Performance Evaluation Mixture Resolution
If PEM resolution criteria are not met, then the quantitative results may not be accurate
due to inadequate resolution. Positive sample results for compounds that were not
adequately resolved should be qualified with "J". Qualitative identifications may be
questionable if coelution exists. Non-detected target compounds that elute in the region
of coelution may not be valid depending on the extent of the coelution problem.
Professional judgement should be used to qualify data as unusable (R).
4. Performance Evaluation Mixture Retention Times
Retention time windows are used in qualitative identification. If the retention times of
the pesticides in the PEM do not fall within the retention time windows, the associated
sample results should be carefully evaluated. All samples injected after the last in-
control standard are potentially affected. It should be noted for EPA Project Officer
action if the PEM retention time criteria are grossly exceeded.
a. For the affected samples, check to see if the sample chromatograms contain any
peaks that are close to the expected retention time window of the pesticide of
interest. If no peaks are present either within or close to the retention time
window of the deviant target pesticide compound, then there is usually no effect
on the data (i.e., non-detected values can be considered valid). Sample data that
are potentially affected by standards not meeting the retention time windows
should be noted in the data review narrative.
89
-------
PEST
b. If the affected sample chromatograms contain peaks which may be of concern
(i.e., above the CRQL and either close to or within the expected retention time
window of the analyte of interest), then the reviewer should determine the extent
of the effect on the data and may choose to qualify detected target compounds
"NJ" and non-detected target compounds "UJ". In some cases, additional effort
by the reviewer may be necessary to determine if sample peaks represent the
compounds of interest, for example:
i. The reviewer can examine the data package for the presence of three or
more standards containing the pesticide of interest that were run within a
72-hour period during which the sample was analyzed.
ii. If three or more such standards are present, the mean and standard
deviation of the retention time window can be re-evaluated by using the
mean retention times of the standards.
iii. If all standards and matrix spikes fall within the revised window, the
valid positive or negative sample results can be determined using this
window.
iv. The data review narrative should identify the additional efforts taken by
the reviewer and the resultant impact on data usability. In addition, the
support documentation should contain all calculations and comparisons
generated by the reviewer.
c. If the reviewer cannot do anything with the data to resolve the problem of
concern, all positive results and quantitation limits should be qualified "R".
5. If percent difference criteria are not met, qualify all associated positive results generated
during the analytical sequence with "J" and the sample quantitation limits for non-
detected target compounds with "UJ".
6. 4,4'-DDT/Endrin Breakdown:
a. If 4,4'-DDT breakdown is greater than 20.0 percent:
i. Qualify all positive results for DDT with "J". If DDT was not detected,
but ODD and DDE are detected, then qualify the quantitation limit for
DDT as unusable (R).
ii. Qualify positive results for ODD and/or DDE as presumptively present
at an approximated quantity (NJ).
90
-------
PEST
b. If Endrin breakdown is greater than 20.0 percent:
i. Qualify all positive results for Endrin with "J". If Endrin was not
detected, but Endrin aldehyde and Endrin ketone are detected, then
qualify the quantitation limit for Endrin as unusable (R).
ii. Qualify positive results for Endrin Aldehyde and Endrin ketone as
presumptively present at an approximated quantity (NJ).
c. If the combined 4,4'-DDT and Endrin breakdown is greater than 30.0 percent:
i. The reviewer should consider the degree of individual breakdown of
DDT and Endrin and apply qualifiers as described above.
7. Potential effects on the sample data resulting from the instrument performance check
criteria should be noted in the data review narrative. If the data reviewer has knowledge
that the laboratory has repeatedly failed to comply with the requirements for frequency,
linearity, retention time, resolution, or DDT/Endrin breakdown, the data reviewer should
notify the EPA Project Officer.
91
-------
PEST
III. Initial Calibration
A. Review Items: Forms VI PEST-1 [Form VILCP-1], Form VI PEST-2 [Form VILCP-2], Form
VI PEST-3 [Form VILCP-3J, Form VI PEST-4 [Form VILCP-4], Form VII PEST-1 [Form VII
LCP-1], Form VIII PEST [Form VIIILCP], chromatograms, and data system printouts.
B. Objective:
Compliance requirements for satisfactory initial calibration are established to ensure that the
instrument is capable of producing acceptable qualitative and quantitative data for pesticide and
Aroclor compounds on the Target Compound List (TCL). Initial calibration demonstrates that
the instrument is capable of acceptable performance at the beginning of the analytical sequence
and of producing a linear calibration curve.
C. Criteria:
1 . Individual Standard Mixtures
a. Individual Standard Mixtures A and B (containing all of the single component
pesticides and surrogates) must be analyzed at low, midpoint, and high levels
during the initial calibration, on each GC column and instrument used for
analysis.
b. The resolution between any two adjacent peaks in the midpoint concentration of
Individual Standard Mixtures A and B in the initial calibration must be greater
than or equal to 90.0 percent on each column.
c. The absolute retention times of each of the single component pesticides and
surrogates are determined from three-point initial calibration using the Individual
Standard Mixtures. The retention time window for each single component
compound can be found in the appropriate method. An example for determining
retention time windows is given in PEST Section II.C.2.C above.
d. At least one chromatogram from each of the Individual Standard Mixtures A and
B must yield peaks that give recorder deflections between 50 to 100 percent of
full scale.
e. The concentrations of the low, medium, and high level standards containing all
of the single component pesticides and surrogates (Individual Standard Mixtures
A and B) are as follows:
The low point corresponds to the CRQL for each analyte. The midpoint
concentration must be 4 times the low point. The high point must be at least 16
times the low point, but a higher concentration may be chosen.
92
-------
PEST
f. The Percent Relative Standard Deviation (%RSD) of the calibration factors for
each of the single component pesticides and surrogates in the initial calibration
on both columns for Individual Standard Mixtures A and B must be less than or
equal to 20.0 percent, except as stated below. For the two surrogates, the %RSD
must be less than or equal to 30.0 percent. Up to two single component target
pesticides (other than the surrogates) per column may exceed the 20.0 percent
limit but the %RSD must be less than or equal to 30.0 percent.
Note: Either peak area or peak height may be used to calculate the calibration factors
that are, in turn, used to calculate %RSD. However, the type of peak
measurement used to calculate each calibration factor for a given compound
must be consistent. For example, if peak area is used to calculate the low point
calibration factor for endrin, then the mid and high point calibration factors for
endrin must also be calculated using peak area.
2. Multi-component Target Compounds
a. The multi-component target compounds (the 7 Aroclors and Toxaphene) must
each be analyzed separately at a single concentration level during the initial
calibration sequence. The analysis of the multi-component target compounds
must also contain the pesticide surrogates.
b. For each multi-component analyte, the retention times are determined for three
to five peaks. A retention time window of ±0.07 minutes is used to determine
retention time windows for all multi-component analyte peaks, as stated in the
appropriate method.
c. Calibration factor data must be determined for each peak selected from the
multi-component analytes.
D. Evaluation:
1. Individual Standard Mixtures
a. Verify from the Form VIII PEST [Form VIIILCP] that the Individual Standard
Mixtures A and B were analyzed at the proper frequency on each GC column
and instrument used for analysis. Check the raw data (chromatograms and data
system printouts) for each standard to verify that each of the standards was
analyzed at the required concentration levels.
b. Check Form VII PEST-2 with the raw data, and determine that the midpoint
standard concentration is 4 times the concentration of the low point standard
concentration and verify that resolution is greater than 90 percent.
93
-------
PEST
c. Check the Individual Standard Mixtures A and B data and Form VI PEST-1
[Form VILCP-1] and review the calculated retention time windows for
calculation and transcription errors.
d. Check the chromatograms and verify that at least one chromatogram from each
of the Individual Standard Mixtures A and B yields peaks registering
recorder/printer deflections between 50 and 100 percent of full scale.
e. Verify that the concentrations of the low, medium and high level standards of
Individual Standard Mixtures A and B meet the criteria in PEST Section III. C.I.
above.
f Check the Individual Standard Mixtures A and B data and Form VI PEST-2
[Form VILCP-2] to verify that the %RSD for the calibration factors in each of
the single component pesticides and surrogates in the initial calibration analyses
on both columns are in compliance with the criteria in PEST Section III.C above.
Check and recalculate the calibration factors and %RSD for one or more
pesticides; verify that the recalculated values agree with the reported values. If
errors are detected, more comprehensive recalculation and review should be
performed.
2. Multi-component Target Compounds
a. Verify from the Form VIII PEST [Form VIIILCP] that each of the multi-
component target compounds were analyzed at the required frequency. Check
the raw data for the standards to verify that the multi-component analytes were
analyzed at the required concentration.
b. Check the data for the multi-component target compounds and Form PEST VI-3
[Form VILCP-3] to verify that at least three peaks were used for calibration and
that retention time windows were calculated as required.
c. Check the data to verify that calibration factors have been determined for each
selected peak.
E. Action:
1. If the initial calibration sequence was not followed as required, then professional
judgement must be used to evaluate the effect of the non-compliance on the sample data.
If the requirements for the initial calibration sequence were not met, then this should be
noted for EPA Project Officer action. If the non-compliance has a potential effect on the
data, then the data should be qualified according to the professional judgement of the
reviewer and this should be noted in the data review narrative.
2. If resolution criteria are not met, then the quantitative results may not be accurate due to
peak overlap and lack of adequate resolution. Positive sample results for compounds
94
-------
PEST
that were not adequately resolved should be qualified with "J". Qualitative
identifications may be questionable if coelution exists. Non-detected target compounds
that elute in the region of coelution may not be valid, depending on the extent of the
coelution problem. Professional judgement should be used to qualify data as unusable
(R).
3. If retention time windows are not calculated correctly, recalculate the windows and use
the corrected values for all evaluations.
4. If the chromatogram display (recorder deflection) criteria are not met, use professional
judgement to evaluate the effect on the data. If the data reviewer has knowledge that the
laboratory has repeatedly failed to comply with this requirement, the data reviewer
should notify the EPA Project Officer.
5. If the sample concentration exceeds the linearity of the calibration curve, and the sample
is not properly diluted and re-analyzed, flag the positive results "J".
6. If the standard concentration criteria are not met, use professional judgement to evaluate
the affect on the data and notify the EPA Project Officer. This is especially critical for
the low level standards and non-detects.
7. If the %RSD linearity criteria are not met for the compound(s) being quantified, qualify
all associated positive quantitative results with "J" and the sample quantitation limits for
non-detected target compounds with "UJ".
8. Potential effects on the sample data due to problems with calibration should be noted in
the data review narrative. If the data reviewer has knowledge that the laboratory has
repeatedly failed to comply with the requirements for frequency, linearity, retention time,
or resolution, the data reviewer should notify the EPA Project Officer.
95
-------
PEST
IV. Calibration Verification
A Review Items: Form VI PEST-6 [Form VILCP-6], Form VI PEST-7 [Form VILCP-7J, Form
VII PEST-1 [Form VIILCP-1], Form VII PEST-2 [Form VIILCP-2], Form VIII PEST [Form
VIIILCP], chromatograms, and data system printouts.
B. Objective:
Compliance requirements for satisfactory instrument calibration are established to ensure that the
instrument is capable of producing acceptable qualitative and quantitative data. Calibration
verification checks and documents satisfactory performance of the instrument over specific time
periods during sample analysis. To confirm the calibration and evaluate instrument performance,
calibration verification is performed, consisting of the analyses of instrument blanks, the PEM,
and the midpoint concentration of Individual Standard Mixtures A and B.
C. Criteria:
1. An instrument blank and the PEM must bracket one end of a 12-hour period during
which samples are analyzed, and a second instrument blank and the midpoint
concentration of Individual Standard Mixtures A and B must bracket the other end of the
12-hour period.
2. The resolution between any two adjacent peaks in the midpoint concentration of
Individual Standard Mixtures A and B must be greater than or equal to 90.0 percent.
3. The absolute retention time for each single component pesticide and surrogate in the
midpoint concentration of Individual Standard Mixtures A and B must be within the
retention time windows determined from the initial calibration.
4. The percent difference between the calculated amount and the true amount for each of
the pesticides and surrogates in the midpoint concentration of the Individual Standard
Mixtures A and B must not exceed ±25.0 percent.
D. Evaluation:
1. Check the Form VIII PEST [Form VIIILCPJ to verify that the instrument blanks, PEMs,
and Individual Standard Mixtures were analyzed at the proper frequency and that no
more than 12 hours was elapsed between continuing calibration brackets in an ongoing
analytical sequence.
2. Check Form VI PEST-6 [Form VILCP-6] and Form VI PEST-7 [Form VILCP-7], and
the data for the midpoint concentration of Individual Standard Mixtures A and B to
verify that the resolution between any two adjacent peaks is greater than or equal to 90.0
percent.
96
-------
PEST
Check the data for each of the single component pesticides and surrogates in the
midpoint concentration of Individual Standard Mixtures A and B and Form VII PEST-2
[Form VIILCP-2] to verify that the absolute retention times are within the appropriate
retention time windows.
Check the data from the midpoint concentration of Individual Standard Mixtures A and
B and Form VII PEST-2 [Form VII LCP-2] to verify that the percent difference between
the calculated amount and the true amount for each of the pesticides and surrogates
(must be within ±25).
E. Action:
1. If the continuing calibration sequence was not followed as required, then professional
judgement must be used to evaluate the effect of the non-compliance on the sample data.
If the requirements for the continuing calibration sequence were not met, then this should
be noted for EPA Project Officer action. If the non-compliance has a potential effect on
the data, then the data should be qualified according to the professional judgement of the
reviewer and this should be noted in the data review narrative.
2. If resolution criteria are not met, then the quantitative results may not be accurate due to
inadequate resolution. Positive sample results for compounds that were not adequately
resolved should be qualified with "J". Qualitative identifications may be questionable if
coelution exists. Non-detected target compounds that elute in the region of coelution
may not be valid depending on the extent of the coelution problem. Professional
judgement should be used to qualify data as unusable (R).
3. Retention time windows are used in qualitative identification. If the standards do not fall
within the retention time windows, the associated sample results should be carefully
evaluated. All samples injected after the last in-control standard are potentially affected.
a. For the affected samples, check to see if the sample chromatograms contain any
peaks that are close to the expected retention time window of the pesticide of
interest. If no peaks are present either within or close to the retention time
window of the deviant target pesticide compound, then non-detected values can
be considered valid. Sample data that is potentially affected by the standards not
meeting the retention time windows should be noted in the data review narrative.
If the retention time window criteria are grossly exceeded, then this should be
noted for EPA Project Officer action.
b. If the affected sample chromatograms contain peaks which may be of concern
(i.e., above the CRQL and either close to or within the expected retention time
window of the pesticide of interest), then the reviewer should follow the
guidelines provided in Pesticide Section III.E.3 to determine the extent of the
effect on the data.
97
-------
PEST
4. If the percent difference is greater than 25 percent for the compound(s) being quantified,
qualify all associated positive quantitative results with "J" and the sample quantitation
limits for non-detects with "UJ".
5. Potential effects on the sample data due to problems with calibration should be noted in
the data review narrative.
98
-------
PEST
V. Blanks
A. Review Items: Form I PEST [Form ILCP], Form IV PEST [Form IVLCP], chromatograms,
and data system printouts.
B. Objective:
The purpose of laboratory (or field) blank analyses is to determine the existence and magnitude
of contamination problems resulting from laboratory (or field) activities. The criteria for
evaluation of laboratory blanks apply to any blank associated with the samples (e.g., method
blanks, instrument blanks, and sulfur cleanup blanks). If problems with any blank exist, all
associated data must be carefully evaluated to determine whether or not there is an inherent
variability in the data, or if the problem is an isolated occurrence not affecting other data.
C. Criteria:
1 . No contaminants should be present in the blanks.
2. Method Blanks
a. A method blank analysis must be performed for each 20 samples of similar
matrix in each Sample Delivery Group (SDG) or whenever a sample extraction
procedure is performed. The method blank should be analyzed on each GC
system used to analyze that set of associated samples.
3. Instrument Blanks
a. An acceptable instrument blank must be run at least once every 12 hours and
immediately prior to the analysis of either the performance evaluation mixture or
Individual Standard Mixtures A and B, depending on the position in the
analytical sequence.
4. Sulfur Cleanup Blanks
a. A sulfur cleanup blank must be analyzed whenever part of a set of samples
extracted together requires sulfur cleanup. If the entire set of samples associated
with a method blank requires sulfur cleanup, then the method blank also serves
the purpose of a sulfur blank and no separate sulfur blank is required. The sulfur
cleanup blank should be analyzed on each GC system used to analyze the
associated samples.
D. Evaluation:
1. Review the results of all associated blanks, Form I PEST [Form I LCP] and Form IV
PEST [Form IVLCP], and raw data (chromatograms and data system printouts) to
evaluate presence of target or non-target analytes in the blanks.
99
-------
PEST
2. Verify that method blank analysis has been reported per SDG, per matrix, per
concentration level, for each GC system used to analyze samples, and for each extraction
batch. The reviewer can use Form IV PEST [Form IVLCP] to assist in identifying
samples associated with each blank.
3. Verify that the method blank analysis(es) contains less than the Contract Required
Quantitation Limit (CRQL) of any target pesticide or Aroclor/Toxaphene or any
interfering peak.
4. Verify that the instrument blank analysis has been performed every 12 hours as the first
analysis of the continuing calibration sequence. All acceptable sample analyses are to be
bracketed by acceptable instrument blanks. Additionally, the instrument blank must
follow sample analyses which contain an analyte at high concentration. Evaluate the
results from the various instrument blanks to verify that they do not contain any target
analytes above one-half the CRQL values for water samples (assuming a 1-L extraction
of a water sample).
5. Verify that the sulfur cleanup blanks were analyzed at the required frequency and that
(assuming a 1-L extraction of a water sample) the sulfur blanks do not contain any target
compounds above the CRQL. If a separate sulfur cleanup blank was prepared, one
version of Form IV PEST [Form IVLCP] should be completed associating all the
samples with the method blank, and a second version of Form IV PEST [Form IVLCP]
should be completed listing only those samples associated with the separate sulfur
cleanup blank.
E. Action:
If the appropriate blanks were not analyzed with the frequency described in the previous PEST
Section V.C., then the data reviewer should use professional judgement to determine if the
associated sample data should be qualified. The reviewer may need to obtain additional
information from the laboratory. The situation should be brought to the attention of the EPA
Project Officer.
Action in the case of unsuitable blank results depends on the circumstances and the origin of the
blank. Detected compounds should be reported unless the concentration of the compound in the
sample is less than or equal to 5 times (5x) the amount in any blank. In instances where more
than one 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. The
results must not be corrected by subtracting the blank value.
Specific actions are as follows:
1. If a target pesticide or Aroclor/Toxaphene is found in the blank but not found in the
sample(s), no qualification is required. If the contaminants found are at levels
significantly greater than the CRQL, then this should be noted for EPA Project Officer
action.
100
-------
PEST
2. Any pesticide or Aroclor/Toxaphene detected in the sample, that was also detected in
any associated blank, is qualified if the sample concentration is less than five times (5x)
the blank concentration. The quantitation limit may also be elevated. Typically, the
sample CRQL is elevated to the concentration found in the sample. The reviewer should
use professional judgement to determine if further elevation of the CRQL is required.
The reviewer should note that analyte concentrations calculated for method, sulfur, or
instrument blanks may not involve the same weights, volumes, or dilution factors as the
associated samples. These factors must be taken into consideration when applying the
"5x" criteria, such that a comparison of the total amount of contamination is actually
made.
Additionally, there may be instances when little or no contamination was present in the
associated blanks, but qualification of the sample was deemed necessary. Contamination
introduced through dilution 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 absent in the undiluted sample result. Since both results are
not routinely reported, it may be impossible to verify this source of contamination.
However, if the reviewer determines that the contamination is from a source other than
the sample, he/she should qualify the data. In this case, the "5x" rule does not apply; the
sample value should be reported as a non-detected target compound ("U"). An
explanation of the rationale for this determination should be provided in the data review
narrative.
3. If gross contamination exists (e.g., saturated peaks, "hump-o-grams", "junk" peaks), all
affected compounds in the associated samples should be qualified as unusable (R), due to
interference. This should be noted in the data review narrative and as a EPA Project
Officer action item if the contamination is suspected of having an effect on the sample
results.
4. If inordinate amounts of target pesticides, Aroclors/Toxaphene, or other interfering non-
target compounds are found at low levels in the blank(s), it may be indicative of a
problem at the laboratory and should be noted for EPA Project Officer action.
5. If an instrument blank was not analyzed following a sample analysis which contained an
analyte(s) at high concentration(s), sample analysis results after the high concentration
sample must be evaluated for carryover. Professional judgement should be used to
determine if instrument cross-contamination has affected any positive compound
identification(s), and if so, detected compound results should be qualified. If instrument
cross-contamination is suggested, then this should be noted in the data review narrative,
and for EPA Project Officer action, if the cross-contamination is suspected of having an
affect on the sample results.
101
-------
PEST
The following are examples of applying the blank qualification guidelines.
Example 1: Sample result is greater than the CRQL, but is less than the 5x multiple
of the blank result.
Blank Result
CRQL
Sample Result
Qualified Sample Result
5x
1.0
0.5
4.0
4.0U
Example 2: Sample result is less than the CRQL, and is also less than the 5x multiple
of the blank result.
Blank Result
CRQL
Sample Result
Qualified Sample Result
5x
1.0
0.5
0.4J
0.5U
Example 3: Sample result is greater than the 5x multiple of the blank result.
Blank Result
CRQL
Sample Result
Qualified Sample Result
5x
1.0
0.5
10.0
10.0
In this case, the sample result exceeded the adjusted blank result (5 x
1.0) and the sample result is not qualified.
102
-------
PEST
VI. Surrogate Spikes
A. Review Items: Form II PEST-1 and Form II PEST-2 [Form IILCP], Form VIII PEST [Form
VIII LCP], chromatograms, and data system printouts.
B. Objective:
Laboratory performance on individual samples is established by means of spiking samples prior
to extraction and analysis to determine surrogate spike recoveries. All samples are spiked with
surrogate compounds prior to sample extraction. The evaluation of the recovery results of these
surrogate spikes is not necessarily straightforward. The sample itself may produce effects due to
such factors as interferences and high concentrations of target and/or non-target analytes. Since
the effects of the sample matrix are frequently outside the control of the laboratory and may
present relatively unique problems, the evaluation and review of data based on specific sample
results is frequently subjective and demands analytical experience and professional judgement.
Accordingly, this section consists primarily of guidelines, in some cases with several optional
approaches suggested.
C. Criteria:
1. Two surrogate spikes, tetrachloro-m-xylene and decachlorobiphenyl, are added to all
samples, Individual Standard Mixtures, PEMs, blanks, and matrix spikes to measure their
recovery in sample and blank matrices.
2. The limits for recovery of the surrogates tetrachloro-m-xylene (TCX) and
decachlorobiphenyl (DCB) are 30-150 percent for both water and soil samples.
3. The retention times of both of the surrogates in the PEM, Individual Standard Mixtures,
and samples must be within the calculated retention time windows. TCX must be within
±0.05 minutes, and DCB must be within ±0.10 minutes of the mean retention time
determined from the initial calibration.
D. Evaluation:
1. Check the raw data (e.g., chromatograms and data system printouts) to verify that the
recoveries on the Surrogate Recovery Form II PEST-1 and Form II PEST-2 [Form II
LCP] are calculated and transcribed correctly.
2. If recoveries are not within limits, check the raw data for possible interferences which
may have affected surrogate recoveries. If low surrogate recoveries are observed, the
reviewer should investigate whether the low recoveries were a result of sample dilution.
3. Check the raw data (e.g., chromatograms and data system printouts) to verify that the
retention times on Form VIII PEST [Form VIIILCP] are accurate and within retention
time windows.
103
-------
PEST
4. If retention times were not met, check the raw data for possible mis-identification of GC
peaks. Non-recovery of surrogates may also be due to shifts in retention times.
E. Action:
1. If either surrogate spike recovery is outside of advisory limits, the following guidance is
suggested. Professional judgement must be used in applying these criteria, as
surrogate recovery problems may not directly apply to target analytes.
a. If low recoveries (i.e., between 10 and 30 percent) are obtained, associated
detected compounds should be qualified "J" and quantitation limits "UJ".
b. If high recoveries (i.e., greater than 150 percent) are obtained, this may be an
indication of a high bias due to co-eluting interferences. Using professional
judgement, qualify associated detected compound data with "J". Non-detected
analytes do not require qualification.
c. If either pesticide surrogate recovery is reported as between 0 percent and 10
percent, the reviewer should examine the sample chromatogram to assess the
qualitative validity of the analysis. If low surrogate recoveries are found to be
due to sample dilution, then professional judgement should be used to determine
if the resulting data should be qualified. If sample dilution is not a factor, then
detected target compounds may be qualified "J" and non-detected target
compound results should be qualified unusable (R).
d. If zero pesticide surrogate recovery is reported, the reviewer should examine the
sample chromatogram to determine if the surrogate may be present, but slightly
outside its retention time window. If this is the case, in addition to assessing
surrogate recovery for quantitative bias, the overriding consideration is to
investigate the qualitative validity of the analysis. If the surrogate is not present,
qualify all nondetected target compounds as unusable (R).
2. If surrogate retention times in PEMs, Individual Standard Mixtures, samples, and blanks
are outside of the retention time limits, qualification of the data is left up to the
professional judgement of the reviewer. Refer to Pesticide Section II.E.2 for more
guidance.
3. 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. Data is
qualified on the professional judgement of the reviewer.
104
-------
PEST
4. Extreme or repeated analytical problems with surrogate recoveries should be noted for
EPA Project Officer action.
5. If possible, the impact on the data resulting from surrogate recoveries not meeting the
advisory limits, should be noted in the data review narrative.
105
-------
PEST
VII. Matrix Spikes/Matrix Spike Duplicates
(Not Required for Low Concentration Water Data)
A. Review Items: Form III PEST-1, Form III PEST-2, chromatograms, and data system printouts.
B. Objective:
Data for matrix spikes (MS) and matrix spike duplicates (MSD) are generated to determine long-
term precision and accuracy of the analytical method on various matrices. These data alone
cannot be used to evaluate the precision and accuracy of individual samples. However, when
exercising professional judgement, MS/MSD data should be used in conjunction with
information on other deficiencies.
C. Criteria:
1. Matrix spikes (MS) and matrix spike duplicate (MSD) samples are analyzed at a
frequency of at least one MS and MSD per 20 samples of each matrix, unless MS/MSD
analyses are not required.
2. Matrix spike recoveries should be within the advisory limits provided on Form III PEST-
1 and Form III PEST-2.
3. Relative percent difference (RPD) between MS and MSD recoveries should be within
the advisory limits provided on Form III PEST-1 and Form III PEST-2.
D. Evaluation:
1. Verify that MS and MSD samples were analyzed at the required frequency and that
results are provided for each sample matrix.
2. Check the raw data and Form III PEST-1 and Form III PEST-2 to verify that the results
for matrix spike recoveries were calculated and transcribed correctly.
3. Check the raw data and Form III PEST-1 and Form III PEST-2 to verify that the matrix
spike Relative Percent Difference (RPD) was calculated and transcribed correctly.
4. Compare %RSD results of non-spiked compounds between the original result, MS, and
MSD.
E . Action:
1. No action is taken on MS/MSD data alone. However, using informed professional
judgment, the data reviewer may use the MS and MSD results in conjunction with other
QC criteria and determine the need for some qualification of the data.
106
-------
PEST
2. The data reviewer should first try to determine to what extent the results of the MS/MSD
affect the associated sample data. This determination should be made with regard to the
MS/MSD sample itself, as well as specific analytes for all samples associated with the
MS/MSD.
3. In those instances where it can be determined that the results of the MS/MSD affect only
the sample spiked, then qualification should be limited to this sample alone. However, it
may be determined through the MS/MSD results that a laboratory is having a systematic
problem in the analysis of one or more analytes, which affects all associated samples.
For example, if the recoveries for MS and MSD are consistently low for both water and
soil samples, this could be indicative of a systematic problem in the laboratory and
recoveries should be examined in all associated samples.
4 The reviewer must use professional judgement to determine the need for qualification of
positive results of non-spiked compounds.
NOTE: If a field blank was used for the MS/MSD, unless designated as such by the
Region, the EPA Project Officer must be notified.
107
-------
PEST
VIII. Laboratory Control Samples
(Low Concentration Water)
[A. Review Items: Form ILCP, Form III LCP, LCS chromatograms, and data system printouts.
B. Objective:
Data for laboratory control samples (LCSs) are generated to provide information on the
accuracy of the analytical method and laboratory performance.
C. Criteria:
1. Laboratory control samples are analyzed at a frequency of once per SDG.
2. The LCS contains the following pesticides: gamma-BHC, heptachlor epoxide, dieldrin,
4,4-DDE, endrin, endosulfan sulfate, and gamma-chlordane, in addition to the two
required surrogates.
3. The percent recoveries for the LCS compounds must be within the QC limits provided on
Form III LCP. The LCS must meet the recovery criteria for the sample data to be
accepted.
4. The criteria for surrogate recovery and target compound identification also apply.
D. Evaluation:
1. Verify that LCS samples were analyzed at the required frequency.
2. Verify that the LCS recoveries reported on Form III LCP are within the QC limits.
3. Check that the LCS recoveries were calculated correctly.
4. Verify transcriptions from raw data to Forms I and III LCP.
E. Action:
If the LCS criteria are not met, then laboratory performance and method accuracy are in
question. Professional judgement should be used 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. Action on the LCS recovery should be based on both the number of compounds that are
outside of the recovery criteria and the magnitude of the noncompliance.
108
-------
PEST
2. If the LCS recovery criteria are not met, then the LCS results should be used to qualify
sample data for the specific compounds that are included in the LCS solution. If the LCS
recovery exceeds the upper acceptance limit, detected target compounds may be
qualified "J\ If the LCS recovery exceeds the lower acceptance limit, detected target
compounds may be qualified "J" and non-detects may be qualified unusable (R).
Professional judgement should be used to qualify data for compounds other than those
compounds that are included in the LCS. Professional judgement to qualify non-LCS
compounds should 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.
3. If more than half of the compounds in the LCS are not within the recovery criteria, then
all of the associated detected target compounds may be qualified "J" and all associated
non-detected target compounds may be qualified unusable (R).
4. It should be noted for EPA Project Officer action if a laboratory fails to analyze an LCS
with each SDG, or if the reviewer has knowledge that a laboratory consistently fails to
generate acceptable LCS recoveries.]
109
-------
PEST
IX. Regional Quality Assurance and Quality Control
A. Review Items: Form I PEST [Form ILCP], chromatograms, data system printouts, Traffic
Reports and raw data for Regional QC samples.
B. Objective:
Regional Quality Assurance and Quality Control (QA/QC) refers to any QA and/or QC initiated
by the Region, including field duplicates, Regional Performance Evaluation (PE) samples, blind
spikes, and blind blanks. (It is highly recommended that Regions adopt the use of these QA/QC
samples.)
C. Criteria:
Criteria are determined by each Region.
1. Performance Evaluation sample frequency may vary.
[For data generated through the Low Concentration Method: A PE sample can be
included as frequently as once per SDG.J
2. The analytes present in the PE sample must be correctly identified and quantified.
D. Evaluation:
Evaluation procedures must follow the Region's SOP for data review. Each Region will handle
the evaluation of PE samples on an individual basis. Results for PE samples should be compared
to the acceptance criteria for the specific PE samples, if available.
E. Action:
Any action must be in accordance with Regional specifications and the criteria for acceptable PE
sample results. Unacceptable results for PE samples should be noted for EPA Project Officer
action.
110
-------
PEST
X. Pesticide Cleanup Checks
A. Review Items: Forms IX PEST-1 [Form IXLCP], Form IX PEST-2, GPC/Florisil raw data,
chromatograms, and data system printouts.
B. Objective:
Pesticide cleanup procedures are utilized to remove matrix interferences from sample extracts
prior to analysis. The use of the Florisil cartridge cleanup procedure significantly reduces matrix
interferences caused by polar compounds. Gel permeation chromatography (GPC) is used to
remove high molecular weight contaminants that can interfere with the analysis of target
analytes. Pesticide cleanup procedures are checked by spiking the cleanup columns and
cartridges, and verifying the recovery of pesticides through the cleanup procedure.
C. Criteria:
1. Florisil Cartridge Cleanup
a. Florisil cartridges must be used for the cleanup of all sample extracts.
b. Every lot number of Florisil cartridges used for sample cleanup must be checked
by spiking with 2,4,5-trichlorophenol and the midpoint concentration of
Individual Standard Mixture A at least once, or every six months, whichever is
most frequent.
c. The lot of Florisil cartridges is acceptable if the recoveries for all of the
pesticides and surrogates in Individual Standard Mixture A are within 80 to 120
percent, the recovery of 2,4,5-trichlorophenol is less than 5 percent, and no
peaks interfering with the target analytes are detected.
2. Gel Permeation Chromatography (GPC)
a. GPC is used for the cleanup of all soil sample extracts and for water sample
extracts that contain high molecular weight components that interfere with the
analysis of the target analytes.
b. At least once every 7 days, the calibration of the GPC unit must be checked by
spiking with two check mixtures: the matrix spiking solution and a mixture of
Aroclors 1016 and 1260.
c. The GPC calibration is acceptable if the recovery of the pesticides in the matrix
spiking solution are within 80 to 110 percent, and the Aroclor patterns should
match those generated for previously run standards.
d. A GPC blank must be analyzed after each GPC calibration and is acceptable if
the blank does not exceed one-half the CRQL for any target analytes.
Ill
-------
PEST
D. Evaluation:
1. Florisil Cartridge Check
Check the data from the Florisil cartridge solution analyses and the Form IX PEST-1
[Form IXLCP]. Recalculate some of the percent recoveries to verify that the percent
recoveries of the pesticides and surrogates in Individual Standard Mixture A are within
80 to 120 percent, the recovery of 2,4,5-trichlorophenol is less than 5 percent, and no
interfering peaks are present. Compare the raw data to the reported results and verify
that no calculation or transcription errors have occurred.
2. Gel Permeation Chromatography (GPC)
Check the data from the GPC calibration check analyses and the Form IX PEST-2, and
recalculate some of the percent recoveries to verify that the percent recoveries of the
pesticides in the matrix spike solution are within 80 to 110 percent and that the Aroclor
patterns are similar to those of previous standards. Aroclor pattern comparison within a
laboratory can be checked if more than one GPC calibration was performed for that
SDG. The Region may devise other means to compare this information. Check to make
sure that no transcription errors have occurred.
E. Action:
1. If Florisil Cartridge Check criteria are not met, the raw data should be examined for the
presence of polar interferences and professional judgement should be used in qualifying
the data. If a laboratory analyzes samples under an unacceptable Florisil Cartridge
Check, then the EPA Project Officer should be notified.
2. If Gel Permeation Criteria are not met, the raw data should be examined for the presence
of high molecular weight contaminants, subsequent sample data should be examined for
unusual peaks, and professional judgement should be used in qualifying the data. If a
laboratory chooses to analyze samples under unacceptable Gel Permeation Criteria, then
the EPA Project Officer should be notified.
3. If zero recovery was obtained for the pesticide compounds and surrogates during either
check, then the non-detected target compounds may be suspect and the data may be
qualified unusable (R).
4. If high recoveries (i.e., greater than 120 percent) were obtained for the pesticides and
surrogates during either check, use professional judgement to qualify detected target
compounds. Non detected target compounds do not require qualification.
5. Potential effects on the sample data resulting from the pesticide cleanup analyses not
yielding acceptable results should be noted in the data review narrative.
112
-------
PEST
XI. Target Compound Identification
A. Review Items: Form I PEST [Form ILCPJ, Form X PEST-1 [Form XLCP-1J, Form X PEST-2
[Form XLCP-2J, chromatograms, and data system printouts.
B. Objective:
Qualitative criteria for compound identification have been established to minimize the number of
false positives (reporting a compound present when it is not) and false negatives (not reporting a
compound that is present).
C. Criteria:
1. The retention times of both of the surrogates, matrix spikes, and reported compounds in
each sample must be within the calculated retention time windows on both columns.
TCX must be within ±0.05 minutes of the mean retention time determined from the
initial calibration and DCB must be within ±0.10 minutes of the mean retention time
determined from the initial calibration.
2. GC/MS confirmation is required if the concentration of a compound exceeds 10 ng/uL in
the final sample extract. Pesticides that are confirmed by GC/MS should be identified
with a "C" in the Q column on Form I PEST [Form ILCPJ.
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 detected in the sample and the
largest peak of any multicomponent analyte detected in the sample at less than full scale.
5. If an extract must be diluted, chromatograms must display single component pesticides
between 10 and 100 percent of full scale, and multicomponent analytes between 25 and
100 percent of full scale.
6. For any sample, the baseline of the chromatogram must return to below 50 percent of full
scale before the elution time of alpha-BHC, and also return to below 25 percent of full
scale after the elution time of alpha-BHC and before the elution time of decachloro-
biphenyl.
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.
113
-------
PEST
D. Evaluation:
1. Review Form I PEST [Form ILCP], the associated raw data (chromatograms and data
system printouts) and Form X PEST- 1 [FormXLCP-1} and Form X PEST-2 [FormX
LCP-2J. Confirm reported detected analytes by comparing the sample chromatograms to
the tabulated results and verifying peak measurements and retention times. Confirm
reported non-detected analytes by a review of the sample chromatograms. Check the
associated blank data for potential interferences (to evaluate sample data for false
positives) and check the calibration data for adequate retention time windows (to
evaluate sample data for false positives and false negatives).
2. For multi-component target compounds (Toxaphene and Aroclors), the retention times
and relative peak height ratios of major component peaks should be compared against the
appropriate standard chromatograms.
3. Verify that GC/MS confirmation was performed for pesticide concentrations in the final
sample extract which exceeded 10 ng/uL.
E. Action:
1. If the qualitative criteria for both columns were not met, all target compounds that are
reported detected should be considered non-detected. The reviewer may need to use the
qualifiers that are specific to pesticides. The reviewer should use professional judgement
to assign an appropriate quantitation limit using the following guidance:
a. If the misidentified peak was sufficiently outside the target pesticide retention
time window, then the reported values may be a false positive and should be
replaced with the sample CRQL value.
b. If the misidentified peak poses an interference with potential detection of a target
peak, then 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 retention time windows, but was reported as a non-detect, then the
compound may be a false negative. Professional judgement should be used to decide if
the compound should be included. All conclusions made regarding target compound
identification should be included in the data review narrative.
3. If multi-component target compounds exhibit marginal pattern-matching quality,
professional judgement should be used 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 a multi-component pesticide is strongly
suggested, results should be reported as presumptively present (N).
114
-------
PEST
If an observed pattern closely matches more than one Aroclor, professional judgement
should be used to decide whether the neighboring Aroclor is a better match, or if
multiple Aroclors are present.
4. If GC/MS confirmation was required but not performed, the reviewer should report this
for EPA Project Officer action.
115
-------
PEST
XII. Compound Ouantitation and Reported CRQLS
A. Review Items: Form I PEST [Form ILCPJ, Form X PEST-1 [Form XLCP-1J, Form X PEST-2
[Form XLCP-2J, sample preparation log sheets, chromatograms, SDG Narrative, and data
system printouts.
B. Objective:
The objective is to ensure that the reported quantitative results and contract required quantitation
limits (CRQLs) are accurate.
C. Criteria:
Compound quantitation, as well as the adjustment of the CRQL, must be calculated according to
the equations provided in the method.
D. Evaluation:
1. Raw data should be examined to verify the correct calculation of all sample results
reported by the laboratory. Data system printouts, chromatograms, and sample
preparation log sheets should be compared to the reported positive sample results and
quantitation limits. Verify that the sample values are reported correctly.
2. Verify that the CRQLs have been adjusted to reflect all sample dilutions, concentrations,
splits, clean-up activities, and dry weight factors that are not accounted for by the
method.
E. Action:
1. Quantitation limits affected by large, off-scale peaks should be qualified as unusable (R).
If the interference is on-scale, the reviewer can provide an approximated quantitation
limit (UJ) for each affected compound.
NOTE: Single-peak pesticide results are checked for rough agreement between
quantitative results obtained on the two GC columns. The potential for coelution
should be considered and the reviewer should use professional judgment to
decide whether a much larger concentration obtained on one column versus the
other indicates the presence of an interfering compound. If an interfering
compound is indicated, professional judgement must be used to determine how
best to report, and if necessary, qualify the data. Contractually the lower of the
two values is reported.
116
-------
PEST
If there are any discrepancies found, the laboratory may be contacted by the Region's
designated representative to obtain additional information that could resolve any
differences. If a discrepancy remains unresolved, the reviewer must decide which value
is the best value. Under these circumstances, the reviewer may determine if qualification
of the data is warranted. A description of the reasons for data qualification and the
qualification that is applied to the data should be documented in the data review
narrative.
117
-------
PEST
XIII. Overall Assessment of Data
A. Review Items: Entire data package, data review results, and (if available) Quality Assurance
Project Plan (QAPjP), and Sampling and Analysis Plan (SAP).
B. Objective:
The overall assessment of a data package is a brief narrative in which the data reviewer expresses
concerns and comments on the quality and, if possible, the useability of the data.
C. Criteria:
Assess the overall quality of the data.
Review all available materials to assess the overall quality of the data, keeping in mind the
additive nature of analytical problems.
D. Evaluation:
1 . Evaluate any technical problems which have not been previously addressed.
2. If appropriate information is available, the reviewer may assess the useability of the data
to assist the data user in avoiding inappropriate use of the data. Review all available
information, including the QAPjP (specifically the Data Quality Objectives), SAP, and
communication with data user that concerns the intended use and desired quality of the
data.
E. Action:
1. Use professional judgement to determine if there is any need to qualify data which were
not qualified based on the QC criteria previously discussed.
2. Write a brief narrative to give the user an indication of the analytical limitations of the
data. Any inconsistency of that data with the SDG Narrative should be noted for EPA
Project Officer action. If sufficient information on the intended use and required quality
of the data are available, the reviewer should include his/her assessment of the useability
of the data within the given context.
118
------- |