HALOGENATED AND AROMATIC VOLATILE ORGANIC COMPOUNDS (VOCs) BY GAS CHROMATOGRAPHY SW-846 Methods 8010A and 8020A or Method 8021A Table 1A. Summary of Holding' Times and. Preservation for Halogenated and Aromatic Volatile Organic Compounds by Gas Chromatography Analytical Parameter a Technical and Contract Holding Times Preservation Volatile Organic Compounds (VOCs) in Water Technical: 7 davs from collection; Contract: 5 davs from receipt at laboratory Cool to 4°C ±2°C; VOCs in Water Technical: 14 davs from collection; Contract: 10 davs from receipt at laboratory HC1 to pH <2; Cool to 4 ° C ±2 ° C VOCs in Soil Technical: 48 hours Contract: 48 hours Cool to 4°C ±2°C; sealed zero headspace containers; freezing can extend the holding time b VOCs in Soil Technical: 14 davs from collection; Contract: 10 davs from receipt at laboratory Preserved samples: in methanol c or sodium bisulfate d a Individual target compounds are listed in Tables IB and 1C. b Freezing the sample can extend the holding time; however, 48 hours unfrozen holding time will be considered cumulative. c Use Method 5030 for purge and trap. d Use Method 5035 for purge and trap. pH of each sample must be recorded and reported with sample results. Data Calculations and Reporting Units: Calculate the calibration factors (CFs) and the concentration of individual analytes according to the equations specified in Sections 7.4.2 and 7.10.1, respectively, of Method 8000B. 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) . Report percent solid and percent moisture to the nearest whole percentage point. 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. 8021CRF 1 of 6 Revision 12/13/1999 ------- Table IB. Target Compound List, CAS Numbers, and Contract Required Quantitation Limits for Halogenated Volatile Organic Compounds by Gas Chromatography SW-846 Method 8010A or 8021A Coirroound CAS Number CRQL (,ug/L or jUg/kg) Benzyl chloride 100-44-7 1 Bromobenzene 108-86-1 1 Bromodi chloromethane 75-27-4 1 Bromoform 75-25-2 1 Bromomethane 74-83-9 1 Carbon tetrachloride 56-23-5 1 Chloroethane 75-00-3 1 2-Chloroethylvinylether 110-75-8 1 Chloroform 67-66-3 1 Chloromethane 74-87-3 1 Dibromochloromethane 124-48-1 1 Dibromomethane 74-95-3 1 Dichlorodi fluoromethane 75-71-8 1 1,1-Dichloroethane 75-34-3 1 1,2-Dichloroethane 107-06-2 1 1,1-Dichloroethene 75-35-4 1 trans-1,2-Dichloroethene 156-60-5 1 1,2-Dichloropropane 78-87-5 1 ci s-1,3-Dichloropropene 10061-01-5 1 trans-1,3-Dichloropropene 10061-02-6 1 Methylene chloride 75-09-2 5 1,1,2,2-Tetrachloroethane 79-34-5 1 1,1,1,2-Tetrachloroethane 630-20-6 1 Tetrachloroethene 127-18-4 1 1,1,1-Trichloroethane 71-55-6 1 1,1,2-Trichloroethane 79-00-5 1 Trichloroethene 79-01-6 1 8021CRF 2 of 6 Revision 12/13/1999 ------- Trichlorofluoromethane 75-69-4 1 1,2,3-Trichloropropane 96-18-4 1 Vinyl chloride 75-01-4 1 Additional Compounds: 1,2-Dibromo-3-chloropropane 96-12-8 1 1,2-Dibromoethane 106-93-4 1 1,3-Dichloropropane 142-28-9 1 Dichlorofluoromethane 75-43-4 1 Table 1C. Target Compound List, CAS Numbers, and Contract Required Quantitation Limits for Aromatic Volatile Organic Compounds by Gas Chromatography SW-846 Method 8020A or 8021A Compound CAS Number CRQL (jtfg/L or jUg/kg) Benzene 71-43-2 1 Chlorobenzene 108-90-7 1 1,2-Dichlorobenzene 95-50-1 1 1,3-Dichlorobenzene 541-73-1 1 1,4-Dichlorobenzene 106-46-7 1 Ethylbenzene 100-41-4 1 Toluene 108-88-3 1 Xylenes (Total) 1330-20-7 1 8021CRF 3 of 6 Revision 12/13/1999 ------- Table 2. Summary of Calibration Procedures for Halogenated and. Aromatic Volatile Organic Compounds by Gas Chromatography Calibration Element Frequency Acceptance Criteria Corrective Action Initial Calibration (minimum blank + 5 points for each analyte) (ICAL)3' b' c Initially; whenever required, due to failure of CCV RSD for CFs <30%; or, correlation coefficient (r) of linear regression >0.99 1. Terminate analysis 2. Recalibrate and verify before sample analysis Continuing Calibration Verification (CCV) Daily, every 12-hour, every ten samples, and end of run %D between CF of CCV and avg CFs from ICAL <±25% 1. Recalibrate and verify 2. Reanalyze samples back to last good CCV Retention time evaluation of CCV standards Each analysis of CCV standard ±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 ICAL and continuing CAL standards must contain all target analytes listed in Table IB. c 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. 8021CRF 4 of 6 Revision 12/13/1999 ------- Table 3. Summary of Internal Quality Control Procedures for Halogenated and. Aromatic Volatile Organic Compounds by Gas Chromatography QC Element Frequency Acceptance Criteria Corrective Action Method Blank (MB) Each 12-hour time period, minimum of one per SDG a < CRQL for each compound 1. Investigate the source of contamination and document. 2. Reanalyze all samples processed with a blank that is out of control. Instrument Blank After any sample which contains a target compound concentration >50 PPb < CRQL for each compound 1. Investigate the source of the problem and document. 2. Acceptance criterion must be met before proceeding with further analysis, in order to demonstrate that there is no analyte carryover. Surrogate Spikes b Every sample, standard and method blank Water Samole: 75-125% of expected value Soil Samole: 65-135% of expected value 1. Reanalyze 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) Water Samole: 75-125% of expected value; Soil Samole: 65-135% of expected value; <30% RPD between MS and MSD 1. Report 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. b Surrogates: Halogenated compounds - 50 ng of one of the following three compounds: bromochlormethane, 2- bromo-l-chloropropane, or 1,4-dichlorobutane. Aromatic compounds - 50 ng of one of the following two compounds: 1,1,1-trifluorotoluene and 4- bromofluorobenzene (BFB). 8021CRF 5 of 6 Revision 12/13/1999 ------- c Spike MS/MSD with 10 ppb of the following halogenated and aromatic VOCs: 1,1-dichloroethene, trichloroethene, chlorobenzene, toluene, and benzene. Dilute and reanalyze samples which contain one or more target analytes at concentrations above the initial calibration range. Results for such reanalyses 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. 8021CRF 6 of 6 Revision 12/13/1999 ------- |