EPA-TSC/NERL: 508: Chlorinated Pesticides in Water Using GCECD
- Summary
- Analytes
- Revision
- Data and Sites
Official Method Name
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Determination of Chlorinated Pesticides in Water by Gas Chromatography with an Electron Capture Detector | ||||
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Current Revision
| Revision 3.1, 1995 | ||||
Media
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WATER | ||||
Instrumentation
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Gas Chromatography with Electron Capture Detection | ||||
Method Subcategory
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Organic | ||||
Method Source
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EPA-TSC/NERL
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Citation
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Methods for the Determination of Organic Compounds in Drinking Water - Supplement III (EPA/600/R-95-131)
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Brief Method Summary
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A 1-L sample is extracted with methylene chloride by shaking in a separatory funnel or mechanical tumbling in a bottle. The methylene chloride extract is isolated, dried and concentrated after solvent substitution with methyl tert-butyl ether (MTBE). The concentrations of pesticides in the extract are measured using a capillary column gas chromatography (GC) system equipped with an electron capture detector (ECD). NOTE: CAS Numbers in NEMI for cis- and trans- permethrin differ from those in the method. The CAS Numbers in NEMI are the correct ones. |
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Scope and Application
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This method determines certain chlorinated pesticides in groundwater and finished drinking water. | ||||
Applicable Concentration Range
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Ranges differ for each analyte. | ||||
Interferences
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(A) Glassware contamination: Thoroughly clean glassware, including baking or solvent rinse. (B) Reagent contamination: Use high purity reagents. (C) Phthalate ester interference: Avoid the use of plastics and use pure reagents to avoid contamination by these ubiquitous compounds. (D) Contamination from sample carryover: Rinsing apparatus with MTBE between analyses can minimize contamination. (E) Extracted interferences: Interference from extracted non-target compounds, with retention times similar to target compounds, can be reduced by using confirmation analysis. (F) Variable solvents: Use the same solvent for each analysis. |
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Quality Control Requirements
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Initial demonstration of laboratory capability, determination of surrogate compound recoveries in each sample and blank, monitoring internal standard peak area or height in each sample and blank (when internal standard calibration procedures are being employed), analysis of laboratory reagent blanks (LRBs), laboratory fortified samples, laboratory fortified blanks (LFBs), and QC samples. A MDL for each analyte must also be determined. | ||||
Sample Handling
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Grab samples must be collected in glass containers following conventional sampling practices without prerinsing the bottle before collection. Dechlorinate with the addition of 80 mg of sodium thiosulfate per L of sample prior to sample collection. Store samples at 4oC until analysis. NOTE: Samples analyzed for the following analytes must be extracted immediately after collection and preservation: chlorthalonil, alpha-HCH, delta-HCH, gamma-HCH, cis-permethrin, trans-permethrin, and trifluralin. |
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Maximum Holding Time
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7 days generally (see Sample Handling for exceptions). Extracts within 14 days. |
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Relative Cost
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$201 to $400 | ||||
Sample Preparation Methods
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Analyte | Detection Level |
Bias | Precision | Pct False Positive |
Pct False Negative |
Spiking Level |
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4,4'-DDD(72-54-8)
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0.004 ug/L | 115% Rec (SL) | 5.00 % RSD (SL) | 0.03 ug/L | ||
4,4'-DDE(72-55-9)
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0.003 ug/L | 127% Rec (SL) | 6.00 % RSD (SL) | 0.01 ug/L | ||
Aldrin(309-00-2)
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0.014 ug/L | 66% Rec (SL) | 9.00 % RSD (SL) | 0.08 ug/L | ||
Chlordane(57-74-9)
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N/A | N/A | N/A | |||
Chlorobenzilate(510-15-6)
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2.200 ug/L | 99% Rec (SL) | 5.00 % RSD (SL) | 5.00 ug/L | ||
Chloroneb(2675-77-6)
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0.500 ug/L | 47% Rec (SL) | 34.00 % RSD (SL) | 0.50 ug/L | ||
Chlorothalonil(1897-45-6)
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0.011 ug/L | 119% Rec (SL) | 12.00 % RSD (SL) | 0.03 ug/L | ||
DCPA(1861-32-1)
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0.003 ug/L | 112% Rec (SL) | 4.00 % RSD (SL) | 0.03 ug/L | ||
Dieldrin(60-57-1)
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0.011 ug/L | 77% Rec (SL) | 22.00 % RSD (SL) | 0.02 ug/L | ||
Endosulfan sulfate(1031-07-8)
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0.002 ug/L | 129% Rec (SL) | 4.00 % RSD (SL) | 0.02 ug/L | ||
Endosulfan-I(959-98-8)
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0.009 ug/L | 78% Rec (SL) | 25.00 % RSD (SL) | 0.02 ug/L | ||
Endosulfan-II(33213-65-9)
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0.024 ug/L | 148% Rec (SL) | 35.00 % RSD (SL) | 0.02 ug/L | ||
Endrin(72-20-8)
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0.006 ug/L | 72% Rec (SL) | 18.00 % RSD (SL) | 0.02 ug/L | ||
Endrin aldehyde(7421-93-4)
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0.011 ug/L | 95% Rec (SL) | 15.00 % RSD (SL) | 0.03 ug/L | ||
Etridiazole(2593-15-9)
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0.013 ug/L | 96% Rec (SL) | 17.00 % RSD (SL) | 0.03 ug/L | ||
Heptachlor(76-44-8)
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0.002 ug/L | 67% Rec (SL) | 7.00 % RSD (SL) | 0.01 ug/L | ||
Heptachlor epoxide(1024-57-3)
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0.006 ug/L | 71% Rec (SL) | 18.00 % RSD (SL) | 0.02 ug/L | ||
Herbicides(E-12839)
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N/A | N/A | N/A | |||
Hexachlorobenzene(118-74-1)
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0.008 ug/L | 115% Rec (SL) | 43.00 % RSD (SL) | 0.01 ug/L | ||
Hexachlorocyclopentadiene(77-47-4)
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N/A | N/A | N/A | |||
Lindane(58-89-9)
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0.006 ug/L | 80% Rec (SL) | 16.00 % RSD (SL) | 0.02 ug/L | ||
Methoxychlor(72-43-5)
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0.022 ug/L | 120% Rec (SL) | 11.00 % RSD (SL) | 0.05 ug/L | ||
Organics, semivolatile(E-12884)
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N/A | N/A | N/A | |||
Organochlorine pesticides(E-12851)
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N/A | N/A | N/A | |||
PCB-1016(12674-11-2)
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N/A | N/A | N/A | |||
PCB-1221(11104-28-2)
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N/A | N/A | N/A | |||
PCB-1232(11141-16-5)
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N/A | N/A | N/A | |||
PCB-1242(53469-21-9)
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N/A | N/A | N/A | |||
PCB-1248(12672-29-6)
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N/A | N/A | N/A | |||
PCB-1254(11097-69-1)
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N/A | N/A | N/A | |||
PCB-1260(11096-82-5)
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N/A | N/A | N/A | |||
PCBs(1336-36-3)
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N/A | N/A | N/A | |||
Propachlor(1918-16-7)
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0.250 ug/L | 90% Rec (SL) | 18.00 % RSD (SL) | 0.50 ug/L | ||
Toxaphene(8001-35-2)
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N/A | N/A | N/A | |||
Trifluralin(1582-09-8)
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0.003 ug/L | 108% Rec (SL) | 3.00 % RSD (SL) | 0.03 ug/L | ||
alpha-BHC(319-84-6)
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0.005 ug/L | 94% Rec (SL) | 8.00 % RSD (SL) | 0.03 ug/L | ||
alpha-Chlordane(5103-71-9)
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0.004 ug/L | 117% Rec (SL) | 8.00 % RSD (SL) | 0.02 ug/L | ||
beta-BHC(319-85-7)
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0.004 ug/L | 95% Rec (SL) | 12.00 % RSD (SL) | 0.01 ug/L | ||
cis-Permethrin(61949-76-6)
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0.250 ug/L | 64% Rec (SL) | 24.00 % RSD (SL) | 0.50 ug/L | ||
delta-BHC(319-86-8)
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0.002 ug/L | 84% Rec (SL) | 7.00 % RSD (SL) | 0.01 ug/L | ||
p,p'-DDT(50-29-3)
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0.039 ug/L | 87% Rec (SL) | 23.00 % RSD (SL) | 0.06 ug/L | ||
trans-Chlordane(5103-74-2)
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0.002 ug/L | 109% Rec (SL) | 3.00 % RSD (SL) | 0.02 ug/L | ||
trans-Permethrin(61949-77-7)
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0.180 ug/L | 122% Rec (SL) | 9.00 % RSD (SL) | 0.50 ug/L |
Precision Descriptor Notes: | Method precision and accuracy values were generated using 7 to 8 replicate analyses of fortified reagent water. The method contains additional data characterizing method performance. NOTES: (1) PCBs and chlordane are regulatory parameters representing the sum of specific compounds. See performance data for speicifc Arolclors and chlordanes, respectively. (2) This method is approved (as of 2002) for analysis of cyclohexapentadiene, though the analyte is not listed in the method. Check regulatory information for current status. NOTE: CAS Numbers in NEMI for cis- and trans- permethrin differ from those in the method. The CAS Numbers in NEMI are the correct ones. |
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Detection Level Note: | MDLs were determined using the standard deviation of 7 to 8 replicate analyses of an analyte-fortified reagent water sample multiplied by the t-value for (# of samples - 1) degrees of freedom at the 99% confidence level. Detailed instructions for how MDLs are determined are found at 40 CFR part 136, Appendix B. |
Revision | PDF/Link |
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Revision 3.1, 1995 |