Chlorinated Herbicides SW-846 Method 8151 Revision 0 (September 1994)


CHLORINATED HERBICIDES
SW-846 Method 8151,
Revision 0 (September 1994)
Table 1A. Summary of Holding Times and Preservation for Chlorinated
Herbicides
Analytical
Parameter a
Technical and Contract Holding
Times
Preservation
Chlorinated
Herbicides in
Water
Technical to Extraction: 7 davs
from collection;
Contract to Extraction: 5 davs
from receipt at laboratory
Technical and Contract to
Analvsis: 40 davs from
extraction
Cool to 4°C ±2°C;
Chlorinated
Herbicides in
Soil
Technical to Extraction: 14
days from collection;
Contract to Extraction: 10 davs
from receipt at laboratory
Technical and Contract to
Analvsis: 40 davs from
extraction
Cool to 4°C ±2°C;
a Target Compound List is provided in Table IB
Data Calculations and Reporting Units:
Calculate the sample results using calibration factors determined according to
Sections 7.4.2 and 7.8.1 of SW-846 Method 8000A.
Report water sample results in concentration units of micrograms per liter
(jUg/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 for Chlorinated Herbicides SW-846 Method 8151
Coitroound
CAS Number
Water (ua/L)
Soil (ua/Ka)
2 , 4-D
94-75-7
1 . 0
33
2,4-DB
94-82-6
1 . 0
33
2,4,5-T
93-76-5
1 . 0
33
2,4,5-TP (Silvex)
93-72-1
1 . 0
33
Dalapon
75-99-0
1 . 0
33
Dicamba
1918-00-9
1 . 0
33
Dichlorprop
120-36-5
1 . 0
33
Dinoseb
88-85-7
1 . 0
33
MCPP
93-65-2
500
17000
MCPA
94-74-6
500
17000
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Table 2. Summary of Calibration Procedures for Chlorinated Herbicides by SW-846 Method 8151
Calibration Element
Frequency
Acceptance Criteria
Corrective Action
Initial Calibration
(minimum blank + 5
points for each
analyte) (ICAL) b'c
Initially; whenever
required, due to
failure of CCV
RSD for CFs <20%;
or, if using a
linear calibration
curve, a correlation
coefficient (r) of
>0.99 for each
compound
1.	Terminate analysis
2.	Re-calibrate and verify before
sample analysis
Continuing Calibration
Verification (CCV) at
midpoint of ICAL
(Separate source from
ICAL standards)
Beginning of each
12-hour time period,
after every 10
samples and end of
run
%D between
calculated and
nominal amount for
each compound must
be between ±25.0%
1.	Re-calibrate and verify
2.	Re-analyze samples back to last
good CCV
Retention time
evaluation for CCV
standards
Each analysis of CCV
standards
±3 x the SD of the
avg ICAL RT for each
analyte
1.	Re-calibrate and verify
2.	Re-analyze samples back to last
good CCV
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 Report the retention time window for each analyte. Determine retention time windows as ±3 x the standard
deviation (SD) of the average initial calibration retention time for each analyte.
c ICAL and continuing CAL standards must contain all surrogate compounds and target analytes listed in Table
IB.
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Table 3. Summary of Internal Quality Control Procedures for Chlorinated Herbicides by SW-846 Method 8151
QC Element
Frequency
Acceptance Criteria
Corrective Action
Method Blank
(MB)
One per Batch or SDGa
(1 per 20 samples
minimum) per
analytical instrument
< CRQL for each compound
1.	Investigate source of
contamination and document
2.	All samples processed with a
method blank that is out of
control must be re-extracted and
re-analyzed
Surrogate Spike
Every standard, sample
and method blank at 10
times CRQL
Water:
75-125% of expected value
Soil:
65-135% of expected value
1.	Re-analyze all samples with
non-compliant surrogate recoveries
2.	If re-analysis does not solve
the problem, re-extract and re-
analyze
Matrix Spike
and Matrix
Spike Duplicate
(MS/MSD)
One MS/MSD set per
batch or SDG (1 MS/MSD
set per 20 samples
minimum) containing a
minimum of 5 of the
analytes chosen from
Table IB
40-160% of expected value
for dinoseb and 65-135% of
expected value for other
target analytes;
<30 RPD between MS and MSD
1. Report in Case Narrative
Laboratory
Control Sample
(LCS)
One LCS per batch or
SDG
40-160% for dinoseb;
80-120% for other target
analytes
1. Re-extract and re-analyze all
samples processed with an out-of-
control LCS
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.
Dilute and re-analyze samples with 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. Confirmation must be performed on a column
of a phase different from that used for quantitation. Confirmation analyses must meet all calibration
criteria specified in Table 2 and blank acceptance criteria specified in Table 3.
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