Organochlorine Pesticides and Polychlorinated Biphenyls (PCBs)SW-846 Method 8081 or 8080


ORGANOCHLORINE PESTICIDES AND POLY CHLORINATED BIPHENYLS (PCBs)
SW-846 Method 8081 or 8080
Table 1A. Summary of Holding' Times and. Preservation for Organochlorine
Pesticides and Poly chlorinated Biphenyls (PCBs)
Analytical
Parameter a
Technical and Contract
Holding Times
Preservation
Organochlorine
Pesticides and
Polychlorinated
Biphenyls (PCBs)
in Water Samples
Technical for Extraction:
Cool to 4 ° C ±2 ° C
7 days from collection;
Contract for Extraction:
5 days from receipt at
laboratory
Technical and Contract for
Analvsis: 40 davs from
extraction
Organochlorine
Pesticides and
Polychlorinated
Biphenyls (PCBs)
in Soil Samples
Technical for Extraction:
Cool to 4 ° C ±2 ° C
14 days from collection;
Contract for Extraction:
10 days from receipt at
laboratory
Technical and Contract for
Analvsis: 40 davs from
extraction
a Individual target compounds are listed in Table IB.
Data Calculations and Reporting Units:
Calculate the calibration factors (CF) of single component pesticides
according to Section 7.4.2 of SW-846 Method 8000A. Calculate sample results
using the analyte CFs from the midpoint standard of the associated initial
calibration curve. Perform sample quantitation for multiple components
pesticides according to Section 7.6 of SW-846 Method 8080A or 8081.
Report water sample results in concentration units of micrograms per liter
(/ig/L) . Report soil sample results on a dry-weight basis in micrograms per
kilogram (/ig/kg) .
For rounding results, adhere to the following rules:
a)If	the number following those to be retained is less than 5, round down;
b)If	the number following those to be retained is greater than 5, round up; or
c)If	the number following the last digit to be retained is equal to 5, round
down if the digit is even, or round up if the digit is odd.
All records of analysis and calculations must be legible and sufficient to
recalculate all sample concentrations and QC results. Include an example
calculation in the data package.
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TABLE IB. Target Compound. List, CAS Numbers, and Contract Required
Quantitation Limits (CRQL) for SW-846 Method 8081 or Method 8080
COMPOUND
CAS No.
CRQL Water
pg/L
CRQL Soil
pg/kg
alpha-BHC
319-84-6
0 . 05
2
beta-BHC
319-85-7
0 . 05
2
delta-BHC
319-86-8
0 . 05
2
gairana-BHC (Lindane)
58-89-9
0 . 05
2
Heptachlor
76-44-8
0 . 05
2
Aldrin
309-00-2
0 . 05
2
Heptachlor epoxide
1024-57-3
0 . 05
2
Endosulfan I
959-98-8
0 . 05
2
Dieldrin
60-57-1
0 .1
3
4,4'-DDE
72-55-9
0 .1
3
Endrin
72-20-8
0 .1
3
Endosulfan II
33213-65-9
0 .1
3
4,4'-DDD
72-54-8
0 .1
3
Endosulfan sulfate
1031-07-8
0 .1
3
4,4'-DDT
50-29-3
0 .1
3
Methoxychlor
72-43-5
0 . 5
17
Endrin ketone
53494-70-5
0 .1
3
Endrin aldehyde
7421-93-4
0 .1
3
alpha-Chiordane
5103-71-9
0 . 05
2
gamma-Chiordane
5103-74-2
0 . 05
2
Toxaphene
8001-35-2
5
170
Aroclor-1016
12674-11-2
1
33
Aroclor-1221
11104-28-2
2
67
Aroclor-1232
11141-16-5
1
33
Aroclor-1242
53469-21-9
1
33
Aroclor-12 48
12672-29-6
1
33
Aroclor-12 54
11097-69-1
1
33
Aroclor-12 60
11096-82-5
1
3
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Table 2. Summary of Calibration Procedures for Organochlorine Pesticides and Polychlorinated Biphenyls
(PCBs) by SW-846 Method 8081 or 8080
Calibration Element
Frequency
Acceptance
Criteria
Corrective Action
Initial Calibration
(minimum blank + 3
points for each
analyte) (ICAL) a' b,c
Initially; whenever
required, due to
failure of CCV
RSD for CFs <20%
(<30% for
Surrogate
compounds)
1.	Terminate analysis
2.	Re-calibrate and verify before
sample analysis
Continuing Calibration
Verification (CCV) at
midpoint of ICAL
Beginning of each
day, after every 10
samples, and end of
run
%D between CF of
CCV and avg CFs
from ICAL <2 5%
1.	Re-calibrate and verify
2.	Re-analyze samples back to last good
CCV
Endrin and 4,4'-DDT
Breakdown
Beginning and end of
analytical sequence
<20% each or
<30% combined
1.	Investigate source of the problem
and document
2.	If either Endrin, 4,4'-DDT, or their
breakdown products were detected, re-
analyze the samples
a The ICAL low standard must be above but near the CRQL. The low ICAL standard must have a signal to noise
ratio >5:1. If this requirement cannot be met, the laboratory must submit a MDL study as part of the data
package.
b ICAL Prepare initial calibration individual standard mixtures A and B (IND A and IND B) containing the
single component pesticides specified in Table 9 of SW-846 Method 8081 at three concentration levels. For
multiple response pesticides, including toxaphene and Aroclors (except 1016 and 1260), prepare separate
initial calibration standards at the following concentration levels: Aroclors (except 1221)at 100 ng/mL;
Aroclor-1221 at 200 ng/mL; and toxaphene at 500 ng/mL. Aroclor-1016 and Aroclor-1260 may be combined into a
single standard solution. Spike all calibration standards with the surrogate compounds discussed in Table 3
at a concentration of 20 ng/mL.
c Report the retention time window for each analyte. For multiple component pesticides, calculate the
retention time window for 5 major peaks from the initial calibration standard analysis.
Determine retention time windows for both single and multiple component pesticides using the following
guidelines:
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Column Type
Packed Column
Mega bore or wide
bore capillary column
Retention Time Window
in Minutes
<± 2=8
±0.05 for tetrachloro-m-xylene through Aldrin
±0.07 for compounds which elute after Aldrin
±0.1 for decachlorobiphenyl
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Table 3. Summary of Internal Quality Control Procedures for Organochlorine Pesticides and Polychlorinated
Biphenyls (PCBs) by SW-846 Method 8081 or 8080
QC Element
Frequency
Acceptance
Criteria
Corrective Action
Method Blank
(MB)
One per Batch or SDGa
(1 per 20 samples
minimum)
< CRQL for
each compound
1. Investigate source of contamination and
document
2. Re-extract and re-analyze all samples
processed with a non-compliant method blank
Surrogate b
Every standard,
sample, method blank
and QC sample at 10
times CRQL
60-150% of
expected
value
1. Re-analyze all samples with non-compliant
surrogate recoveries
Matrix Spike
and Matrix
Spike Duplicate
(MS/MSD)c
One MS/MSD set per
batch or SDG (1
MS/MSD set per 20
samples minimum)
50-135% of
expected
value; <30
RPD between
MS and MSD
1. Address in narrative
a SDG - Sample Delivery Group - each case of field samples received; or each 20 field samples within a case;
or each 14 calendar day period during which field samples in a case are received.
b Spike each standard, sample, and blank with lmL of a solution containing 0.2 /ig/mL each of tetrachloro-m-
xylene and decachlorobiphenyl
c Spike MS/MSD samples with lmL of a solution containing the following compounds and levels:
Target compound Concentration tua/mLl Target Compound Concentration tua/mLl
?-BHC 0.5 Heptachlor 0.5
4, 4'-DDT 1.0 Aldrin 0.5
Endrin 1.0 Dieldrin 1.0
Dilute and re-analyze samples with one or more analytes at concentrations exceeding the range of the
calibration curve. Results for such re-analyses should fall within the mid-range of the calibration curve.
Report results and submit documentation for both analyses.
Second column confirmation is required for all positive results. Perform confirmation analyses on a column
of a phase different from that used for quantitation. Confirmation analyses must meet all instrument
calibration criteria and blank acceptance criteria specified in Table 2, above.
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