ORGANOPHOSPHORUS PESTICIDES SW-8 4 6 Method 8141A Table 1A. Summary of Holding Times and Preservation for Organophosphorus Pesticides Analytical Parameter a Technical and Contract Holding Times Preservation Organophosphorus Technical for Cool to 4°C ±2°C; Pesticides in Extraction: 7 davs Water from collection; Contract for Extraction: 5 davs from receipt at laboratory Technical and Contract for Analysis: 40 davs from extraction Organophosphorus Pesticides in Soil Technical for Extraction: 14 davs from collection; Contract for Extraction: 10 davs from receipt at laboratory Technical and Contract for 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 (/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. 8141CRF 1 of 4 Revision 12/03/1999 ------- TABLE IB. Target Compound. List, CAS Numbers, and Contract Required Quantitation Limits for Organophosphorus Pesticides SW-846 Method 8141 Compound CAS Number CRQL Water (jig/L) CRQL Soil (jig/Kg) Azinphos methyl 86-50-0 1. 0 50 . 0 Bolstar (Sulprofos) 35400-43-2 0 . 7 35 . 0 Chlorpyrifos 2921-88-2 0 . 7 50 . 0 Coumaphos 56-72-4 2 . 0 100 . 0 Demeton, 0,S 8065-48-3 1. 2 60 . 0 Diazinon 333-41-5 2 . 0 100 . 0 Dichlorvos 62-73-7 8 . 0 400 . 0 Dimethoate 60-51-5 2 . 6 130 . 0 Disulfoton 298-04-4 0 . 7 35 . 0 EPN 2104-64-5 0 . 4 20.0 Ethoprop 13194-48-4 2 . 0 100 . 0 Fensulfothion 115-90-2 0 . 8 40 . 0 Fenthion 55-38-9 0 . 8 50 . 0 Malathion 121-75-5 1. 1 55 . 0 Merphos 150-50-5 2 . 0 100 . 0 Mevinphos 7786-34-7 5 . 0 250 . 0 Monocrotophos 6923-22-4 ND ND Naled 300-76-5 5 . 0 250 . 0 Parathion-ethyl 56-38-2 0 . 6 30 . 0 Parathion-methyl 298-00-0 1. 2 60 . 0 Phorate 298-02-2 0 . 4 20.0 Ronnel 299-84-3 0 . 7 35 . 0 Sulfotep 3689-24-5 0 . 7 35 . 0 TEPP 21646-99-1 8 . 0 400 . 0 Stirophos (Tetrachlorovinsphos) 22248-79-9 8 . 0 400 . 0 Tokuthion (Protothiofos) 34643-46-4 0 . 7 55 . 0 Trichloronate 327-98-0 8 . 0 400 . 0 ND - Not Determined 8141CRF 2 of 4 Revision 12/03/1999 ------- Table 2. Summary of Calibration Procedures for Organophosphorus Pesticides by SW-846 Method 8141 Calibration Element Frequency Acceptance Criteria Corrective Action Initial Calibration (minimum blank + 5 points for each analyte) (ICAL) a' b,c Initially; whenever required, due to failure of CCV RSD for CFs <20%; 1. Terminate analysis 2. Re-calibrate and verify before sample analysis Continuing Calibration Verification (CCV) at midpoint of ICAL (Separate source from ICAL standards) Following ICV and before sample analysis; after every 10 samples and end of run %D between CF of CCV and avg CFs from ICAL <15% 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 of the average initial calibration retention time for each analyte. c ICAL and continuing CAL standards must contain all target analytes listed in Table IB. 8141CRF 3 of 4 Revision 12/03/1999 ------- Table 3. Summary of Internal Quality Control Procedures for Organophosphorus Pesticides by SW-846 Method 8141 QC Element Frequency Acceptance Criteria Corrective Action Method Blank (MB) One per Batch or SDGa (1 per 2 0 samples minimum) < 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 Matrix Spike and Matrix Spike Duplicate (MS/MSD) One MS/MSD set per batch or SDG (1 MS/MSD set per 2 0 samples minimum) containing a minimum of 5 of the analytes chosen from Table IB 65-135% of expected value; <30 RPD between MS and MSD 1. Address in Case 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. 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. 8141CRF 4 of 4 Revision 12/03/1999 ------- |