SOP HW-17
Revision #3.1
December 2010
Page 1 of 13
Validating Chlorinated Herbicides
GC, SW-846, Method 8151A
%
PREPARED BY:
Russell Arnone, Chemist
Hazardous Waste Support Section
Peer Reviewed by:
Concurred by:
Approved by:
Date:
Date:
Muhammad Sheikh, Chemist
Hazardous Waste Support Section
Michael Mercado, Acting Chief
Hazardous Waste Support Section
Robert Runyon, Chief
Hazardous Waste Support Branch
Annual Review
Date:
Date:
Reviewed by:
Date:
Reviewed by:
Date:

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GC, SW-846, Method 8151 A/Herbicides SOP HW-17 EPA/Region II
TABLE OF CONTENTS
1.	Traffic Reports and Laboratory Narratives	3
2.	Holding Times	3
3.	Surrogate Recovery ( Form I I/Equivalent)	4
4.	Matrix Spikes (Form Ill/Equivalent)	5
5.	Blanks (Form IV/Equivalent)	6
6.	Contamination	7
7.	Calibration and GC Performance	8
8.	Laboratory Control Samples	8
9.	Equivalent-Herbicides-1 (Form VI)	9
10.	Continuing Calibration (Form VII)	10
11.	Analytical Sequence Check (Form VIII)	11
12.	Herbicides Identification	11
13.	Compound Quantitation and Reported Detection Limits	13
14.	Chromatogram Quality	14
15.	Field Duplicates	16

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USEPA Region II
SW846 Method 8151 A/Chlorinated Herbicides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
1.0	Traffic Reports and Laboratory Narrative
1.1	Are Traffic Report Forms present for all samples?	jj _ _
ACTION: If no, contact lab for replacement of
missing or illegible copies.
1.2	Do the Traffic Reports or SDG Narrative indicate
any problems with sample receipt, condition of
the samples, analytical problems or special
circumstances affecting the quality of the data?	_ jj _
ACTION: If any sample analyzed as a soil, other
than TCLP, contains 50%-90% water, all
data should be qualified as estimated
(J). If a soil sample, other than TCLP,
contains more than 90% water, all data
should be qualified as unusable (R).
ACTION: If samples were not iced (4°C) upon receipt
at the laboratory, flag all positive results
"J" and all non-detects "UJ".
2.0 Holding Times
2.1 Has the technical holding times, determined from
date of sample receipt to date of extraction,
been exceeded?	_ jj _
Note: Samples may be analyzed for herbicide ester
and acid. Check Laboratory SDG Narrative.
Note: Aqueous samples must be extracted within 7
days. Extracts must be analyzed within 40
days following extraction.
Soil/Concentrated Waste samples must be
extracted within 14 days and extracts analyzed
within 40 days following extraction.
ACTION: If technical holding times are exceeded,
flag all positive results and non-detects(U)as
estimated ("J") and document in the narrative
that holding times were exceeded.
Samples extracted more than 28 days from
sample receipt, either on the first analysis or
Herbicides- 3 -

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USEPA Region II	Date:December 2010
SW846 Method 8151 A/Chlorinated Herbicides	SOP: HW-17, Rev 3.1
YES NO N/A
upon re-analysis, flag all positive results as
Estimate ("J") and non-detects as unusable (R).
3.0 Surrogate Recovery (Form I I/Equivalent)
3.1	Are the Herbicide Surrogate Recovery Summaries
(Form I I/Equivalent) present for each of the
following matrices?
a.	Aqueous	JJ _
b.	Soil	U _
3.2	Are all the samples listed on the appropriate
Surrogate Recovery Summary for each of the
following matrices?
a.	Aqueous	JJ _
b.	Soil/Concentrated Waste	JJ _
ACTION: Contact lab for explanation/resubmittals.
If missing deliverables are unavailable,
document effect in data assessments.
3.3	Were outliers marked correctly with an asterisk?	JJ
ACTION: Circle all outliers with red pencil.
Note: recommend surrogate is 2,4-Dichlorophenylacetic acid (DCAA)
3.4	Did the laboratory provide their developed in-house QC
limits/recoveries?	U
ACTION: If no, use 70 -130% recovery to qualify data
ACTION: No qualification is done if the surrogate
is diluted out. If recovery for the
surrogate is below the QC limit, but above
10%, flag all results for that sample "J".
If recovery is < 10%, qualify postive
results "J" and flag non-detects "R".
If recovery is above the QC limits limit,
qualify positive values "J".
Herbicides- 4 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Herbicides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
Note: In-house QC limits must be examined for
reasonableness, e.g. 10-170% may be appropriate
for analytes not present in the sample.
Note: Matrix effect is indicated if the LCS data are
within limits but surrogate data exceeds QC limits.
3.5	Were surrogate retention times (RT) within the
windows established during the initial 5-point
calibration analysis?	jj _ _
ACTION: If the RT limits are not met, the
analysis may be qualified unusable (R)
for that sample on the basis of
professional judgement.
3.6	Are there any transcription/calculation errors
between raw data and Form I I/Equivalent?	_ jj _
ACTION: If large errors exist, call lab for
explanation/resubmittal. Make any
necessary corrections and document
effect in data assessments.
4.0 Matrix Spikes (Form Ill/Equivalent)
4.1	Is the Matrix Spike/Matrix Spike Duplicate
Recovery Form (Form Ill/Equivalent) present?	jj _ _
4.2	Were matrix spikes analyzed at the required
frequency for each of the following matrices?
Note: At a minimum, analysis of at least one matrix
spike and one duplicate unspiked sample or one matrix
spike/matrix spike duplicate pair with each batch of
up to 20 samples.
a.	Aqueous	jj _ _
b.	Soil/Concentrated Waste	jj _ _
ACTION: If any matrix spike data are missing,
take the action specified in 3.2 above.
Herbicides- 5 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Herbicides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
4.3 Did the laboratory provide their developed in-house
QC limits/recoveries?	U 	 	
ACTION: If no, use 70 -130% recovery to qualify data
ACTION: No action is taken on MS/MSD data alone.
However, using informed professional
judgement, the data reviewer may use the
matrix spike results in conjunction with
other QC criteria (e.g. LCS) to determine
the need for qualification of the data.
5.0 Blanks (Form IV/Equivalent)
5.1	Is the Method Blank Summary (Form IV) present?	jj _ _
5.2	Frequency of Analysis: has a reagent/method
blank been analyzed for each SDG or every 20
samples of similar matrix or concentration
or each extraction batch, whichever is more
frequent?	jj _ _
ACTION: If any blank data are missing, take
the action specified above in 3.2. If
blank data is not available, reject
(R) all associated positive data.
However, using professional judgement,
the data reviewer may substitute field
blank data for missing method blank data.
5.3	Has a Herbicide instrument blank been analyzed
at the beginning of every analytical sequence of
10 samples?	jj _ _
ACTION: If any blank data are missing, call lab for
explanation/resubmittals. If missing
deliverables are unavailable, document the
effect in data assessments.
5.4	Chromatography: review the blank raw data -
chromatograms, quant reports or data system
printouts.
Is the chromatographic performance (baseline
stability) for each instrument acceptable for
Herbicides- 6 -

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USEPA Region II	Date:December 2010
SW846 Method 8151 A/Chlorinated Herbicides	SOP: HW-17, Rev 3.1
YES NO N/A
Herbicides?	JJ _
ACTION: Use professional judgement to determine
the effect on the data.
Contamination
NOTE: "Water blanks", "distilled water blanks" and
"drilling water blanks" are validated like any
other sample and are not used to qualify the
data. Do not confuse them with the other QC
blanks discussed below.
Herbicides- 7 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
6.1
6.2
Do any method/instrument/reagent/cleanup blanks
have positive results for Herbicides? When applied
as described in table below, the contaminant concentration
in the method blank is multiplied by the sample
dilution factor and corrected for % moisture when
necessary.
Do any field/rinse blanks have positive
Herbicides results?
ACTION: Prepare a list of the samples associated
with each of the contaminated blanks.
(Attach a separate sheet)
NOTE: All field blank results associated to a particular
group of samples (may exceed one per case or one per
day) may be used to qualify data. Blanks may not be
qualified because of contamination in another blank.
Field blanks must be qualified for surrogate,
calibration, or any QC problems.
ACTION: Follow the directions in the table below
to qualify TCL results due to contamination.
Use the largest value from all the associated blanks.
Li
U
Sample cone > CRQL
Sample cone < CRQL & Sample cone > CRQL
but < 5x blank
is < 5x blank value
& > 5x blank value
Flag sample result
Report CRQL &
with a "U":
No qualification
qualify "U"	is needed
NOTE: If gross blank contamination exists, all data
in the associated samples should be qualified
as unusable (R).
6.3 Are there field/rinse/equipment blanks associated
with every sample?	jj _ _
ACTION: For low level samples, note in data assessment
that there is no associated field/rinse/equipment blank.
Herbicides- 8 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
Exception: samples taken from a drinking water tap
do not have associated field blanks.
7.0 Calibration and GC Performance
7.1	Are the Gas Chromatograms and Data Systems
printouts for both columns present for all samples,
blanks, QC Check references, and matrix spikes?	LJ _ _
ACTION: If no, take action specified in 3.2 above.
7.2	Are Form Vl/Equivalent present and complete
for each column and each analytical sequence?	LJ _ _
ACTION: If no, take action specified in 3.2
above.
7.3	Are there any transcription/calculation errors
between raw data and Forms VI?	_ LJ _
ACTION: If large errors exist, call lab for
explanation/resubmittal, make
necessary corrections and document
effect in data assessments.
7.4	Were the retention time windows calculated using the
average absolute retention time (at least three
measurements) + three times the standard deviation
of the absolute retention time, for each standard?
(Refer to Method 8000A, section 7.5).	LJ _ _
7.5. Was a LCS check standard analyzed prior to
environmental samples?	LJ _ _
7.5.1	If yes, was the surrogate recovery >50%?	LJ _ _
7.5.2	Was the LCS check standard re-extracted/re-analyzed,
if surrogate recovery was <50%, or any one analyte
was < 40%, or two analytes < 70% ?	LJ _ _
Action: If No/' to any of the above, then qualify
positive hits as estimated "J" and non-detects
as rejected "R" in the original analysis of all
samples in the associated analytical sequence.
Herbicides- 9 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
7.6 Do all standard retention times, including each
Herbicides in each level of Initial Calibration
fall within the windows established
during the initial calibration analytical
sequence? (For Initial Calibration Standards,
Form Vl/Equivalent - Herbicides -1).	jj _ _
ACTION: If no, all samples in the entire
analytical sequence are potentially
affected. Check to see if the
chromatograms contain peaks within an
expanded window surrounding the expected
retention times. If no peaks are found
and the surrogate is visible, non-
detects are valid. If peaks are present
and cannot be identified through pattern
recognition or using a revised RT window,
qualify all positive results and non-detects
as unusable (R).
7.7 Are the linearity criteria for the Initial
Calibration analyses within limits for both
columns? (% RSD must be < 20.0% for all
analytes).	jj
ACTION: If no, qualify all associated positive
results generated during the entire
analytical sequence "J" and all non-
detects "UJ". When RSD >90%, flag all
non-detect results for that analyte R (unusable).
7.8 Are there any transcription/calculation errors
between raw data and Form VII - Herbicides-2?	_ jj
ACTION: If large errors exists, call lab for
explanation/resubmittal, make any
necessary corrections and document
effect in data assessments.
7.9 Is the resolution between any two adjacent
peaks in the QC Reference Check Mixture > 60.0%
for both columns? (Form Vl-Herbicides- 4)	JJ
Herbicides- 10 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
ACTION: If no, positive results for compounds
that were not adequately resolved should
be qualified "J". Use professional
judgement to determine if non-detects
which elute in areas affected by co-eluting
peaks should be qualified "N" as presumptive
evidence of presence or unusable (R).
10 Is Form VII -Continuing Calibration present and
complete for each analytical sequence for both
ACTION: If no, take action as specified in
3.2 above.
11 Have all samples been injected within a 24 hr.
period beginning with the injection of the first
ACTION: If no, use professional judgement to
determine the severity of the effect
on the data and qualify accordingly.
12 Do all analyte retention times for
the Mid-concentration Check standard (Form VII Herb-2)
fall within the windows established by the initial
calibration sequence?	JJ
ACTION: If no, beginning with the samples which
followed the last in-control standard,
check to see if the chromatograms contain
peaks within an expanded window surrounding
the expected retention times. If no peaks
are found and the surrogates are visible,
non-detects are valid. If peaks are present
and cannot be identified through pattern
recognition or using a revised RT window,
qualify all positive results and non-detects
as unusable (R).
columns?
U
standard?
U
Herbicides- 11-

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
7.13 Are RPD values for all verification calibration
standard compounds < 25.0%	jj _ _
ACTION:	The "associated samples" are those which
followed the last in-control standard up
to the next passing standard containing
the analyte which failed the criteria.
If %D is 25 -50% qualify as "J"
If %D is 51-100% qualify as "NJ"
If %D is >100% qualify as "R"
If %D is >100% with visible interferences/qualify as "JN"
8.0 Analytical Sequence Check (Form VIM)
8.1	Is Form VIII present and complete for each column
and each period of analyses?	JJ
ACTION: If no, take action specified in 3.2 above.
8.2	Was the proper analytical sequence followed for
each initial calibration and subsequent analyses?
(see SAS Client Request/section 8/paragraph 6)	JJ
ACTION: If no, use professional judgement to
determine the severity of the effect
on the data and qualify it accordingly.
Generally, the effect is negligible
unless the sequence was grossly altered
or the calibration was also out of limits.
9.0 Herbicides Identification
9.1	Is Form X complete for every sample in
which a Herbicide was detected?	£J _
ACTION: If no, take action specified in 3.2 above.
9.2	Are there any transcription/calculation errors
between raw data and Form X.	_ JJ
Herbicides- 12 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
ACTION: If large errors exist, call lab for
explanation/resubmittal, make necessary
corrections and note errors in data assessment.
9.3 Are retention times (RT) of sample compounds
within the established RT windows for both
columns?
Was GC/MS confirmation provided instead of
confirmation by a second dissimilar column?
Action: Qualify as unusable (R) all
positive results which were not confirmed
by second GC column analysis or by GC/MS.
Also qualify as unusable (R) all positive
results not meeting RT window unless
associated standard compounds show a similar
RT shift. The reviewer should use professional
judgement to assign an appropriate
quantitation limit.
9.4 Is the percent difference (% D) calculated for the
positive sample results on the two GC columns
< 25.0%?
ACTION: If the reviewer finds neither column
shows interference for the positive
hits, the data should be flagged
as follows:
% Difference Qualifier
25-50 %	J
50-90 %	JN
> 90 %	R
NOTE: The lower of the two values is reported
on Form I. If using professional judgement,
the reviewer determines that the higher
result was more acceptable, the reviewer
should replace the value and indicate the
reason for the change in the data assessment.
YES NO N/A
u _ _
u _ _
Herbicides- 13 -

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USEPA Region II	Date:December 2010
SW846 Method 8151 A/Chlorinated Hericides	SOP: HW-17, Rev 3.1
YES NO N/A
9.5 Check chromatograms for false negatives.
Were there any false negatives?	_ jj _
ACTION: Use professional judgement to decide
if the compound should be reported.
10.0 Compound Quantitation and Reported Detection Limits
10.1 Are there any transcription/calculation errors in
Form I results? Check at least two positive values.
Were any errors found?	_ jj _
NOTE: The reviewer should use professional judgement 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, the lower of the two values should be
reported and qualified as presumptively present at an approximated quantity (NJ). This
necessitates a determination of an estimated concentration on the confirmation column. The
narrative should indicate the presence of interferences during the evaluation of the second
column confirmation.
10.2 Are the CRQLs adjusted to reflect sample dilutions
and, for soils, % moisture?	JJ
ACTION: If errors are large, call lab for
explanation/resubmittal, make any
necessary corrections and document
effect in data assessments.
ACTION: When a sample is analyzed at more than
one dilution, the lowest CRQLs are used
(unless a QC exceedance dictates the use
of the higher CRQL data from the diluted
sample analysis). Replace concentrations
that exceed the calibration range in the
original analysis by crossing out the "E"
value on the original Form I and substituting
it with data from the analysis of diluted
sample. Specify which Form I is to be used,
then draw a red "X" across the entire page
of all Form I's that should not be used,
including any in the summary package.
Herbicides- 14 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
ACTION: 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.
10.3 Have all data (Forms and associated chromatograms and
quantitation reports) been submitted for original,
diluted or re-extraction/re-analysis samples?	JJ
11.0 Chromatogram Quality
11.1	Were baselines stable?	jj _
11.2	Were any electropositive displacement
(negative peaks) or unusual peaks seen?	_ JJ
ACTION: Address comments under System
Performance of data assessment.
Explain use of professional judgement
where used to qualify data.
Herbicides- 15 -

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USEPA Region II
SW846 Method 8151 A/Chlorinated Hericides
Date: December 2010
SOP: HW-17, Rev 3.1
YES NO N/A
12.0
Field Duplicates
12.1 Were any field duplicates submitted for
Herbicides analysis?
U _ _
Note: Check whether SAS Client Request required
field duplicates.
ACTION: Compare the reported results for
field duplicates and calculate the
relative percent difference.
ACTION: Any gross variation between field
duplicate results must be addressed
in the reviewer narrative. However, if
large differences exist, identification
of field duplicates should be confirmed
by contacting the sampler.
Herbicides- 16 -

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SOP HW-17
Revision #3.1
December 2010
Page 1 of 13
Validating Chlorinated Herbicides
GC, SW-846, Method 8151A
PREPARED BY:
uk

Russell Arnone, Che
Iter
Hazardou
Peer Reviewed by:
Concurred by:
Approved by:
s Waste Support Section
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Muhammad Shaikh, Chemist
Hazardous Waste Support Section
fichael Wercado-,-Acting Chief
Hazardous Waste StyppqftSection
Robert Runyo?CChief y
Hazardous Waste Support Branch
Date: '2
/
Date:
|W zff/tr,
Date:
Date: /

Annual Review
Reviewed by:
Date:
Reviewed by:
Date:

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