USGS-NWQL: O-3120-90: 1,2-Dibromomethane (EDB) and 1,2-dibromo-3-chloropropane (DBCP) in Water by Gas Chromatography

Summary
Analytes
Revision
Data and Sites

Official Method Name

1,2-Dibromomethane (EDB) and 1,2-dibromo-3-chloropropane (DBCP), Gas Chromatography, Microextraction

Current Revision

1993

Media

WATER

Instrumentation

Gas Chromatography with Electron Capture Detection or Electrolytic Conductivity Detection

Method Subcategory

Organic

Method Source

USGS-NWQL

Citation

M.J. Fishman, 1993, Methods of analysis by the U.S. Geological Survey National Water Quality Laboratory--Determination of inorganic and organic constituents in water and fluvial sediments: U.S. Geological Survey Open-File Report 93-125

Brief Method Summary

The method is an adaptation of USEPA Method 504 (U.S Environmental Protection Agency, 1988). The aqueous sample is extracted with hexane and the extract is analyzed by capillary column gas chromatography using an electron capture detector. The analytes are identified by using two dissimilar capillary columns. Aqueous calibration standards are extracted and analyzed in the same manner as the samples to compensate for possible extraction losses.

Scope and Application

This method is suitable for the determination of 1,2-dibromoethane (EDB) and 1,2-dibromo-3-chloropropane (DBCP) in samples of water and water-suspended sediment containing at least 0.04 ug/L of EDB and 0.03 ug/L of DBCP but not more than 10 ug/L. This method was implemented in the National Water Quality Laboratory in August 1990.

Applicable Concentration Range

0.03 - 10 DBCP, 0.04 - 10 EDB

Interferences

Impurities in the extracting solvent, salt, or glassware might cause analytical problems. Analyze each new bottle of extracting solvent for contaminant interference before use. Analyze blanks daily to monitor the entire procedure. Whenever an interference is noted in the blank, identify and eliminate the source of interference. Hexane-extractable compounds with retention times similar to EDB and DBCP can cause interference, or misidentification, and improper quantitation. Dibromochloromethane interferes with the detection and quantitation of EDB on column B. Therefore, the quantitative results are reported only from column A.

Quality Control Requirements

Method blanks, reagent spikes, surrogate spikes, certified reference material samples, continuing calibration verification standards, field blanks, field replicates, matrix spikes and matrix spike duplicates, quarterly control samples and Branch of Quality Assurance samples are analyzed. Data from these are compiled to continually monitor the QA/QC of the analysis. Each analyst must undergo technical and ethics training, perform an initial demonstration of capability, and annually demonstrate continuing capability on an analysis. Additional QA/QC practices may be added.

Sample Handling

120mL GCV - This schedule consumes the entire container. Description: 40 mL Glass septum vial, amber. Treatment and Preservation: DO NOT RINSE VIAL. Completely fill vial with sample to exclude air bubbles. Preserve all volatiles samples except samples for Schedules 1306 and 4024 adjusting sample with 1:1 HCl/H2O solution to a pH of 2. If free chlorine is present, first add 25 mg of ascorbic acid to each vial before filling with sample, then fill with sample and adjust the sample to a pH of 2. Protect sample from sunlight, store sample at 4 deg C, ship immediately.

Maximum Holding Time

14 days from arrival at the National Water Quality Laboratory

Relative Cost

$51 to $200

Sample Preparation Methods

This method has 3 analytes associated with it.

Analyte	Detection Level	Bias	Precision	Spiking Level
1,2-Dibromoethane(106-93-4) 1,2-Dibromoethane Bromofume Dowfume EDB Ethane, 1,2-dibromo- Ethylene bromide Ethylene dibromide Glycol dibromide	0.050 ug/L	94% Rec (SL)	4.40 % RSD (SL)	1.70 ug/L
DBCP(96-12-8) 1,2-Dibromo-3-chloropropane Chloro-1,2-dibromopropane,3- DBCP Dibromochloropropane Fumagon, Fumazone Nemabrom, Nemafume, Nemagon, Nematocide Nemagon Nematocide Propane, 1,2-dibromo-3-chloro-	0.050 ug/L	100% Rec (SL)	2.00 % RSD (SL)	1.70 ug/L
Volatile organic compounds(E-12419) Organic compounds, volatile VOCs Volatile organic compounds	N/A	N/A	N/A

Precision Descriptor Notes:	For EDB in deionized water: 8, 8, 8 and 10 replicates were spiked at 0.040, 0.15, 0.30 and 1.7 ug/L. Mean recoveries were 0.030, 0.12, 0.24 and 1.8 ug/L with 4.1, 6.8, 1.5 and 2.1%-RSD, respectively. For EDB in Natural Water A: 9, 10 and 8 replicates were spiked with 0.030, 0.70 and 1.7 ug/L. Mean recoveries were 0.022, 0.60 and 1.8 ug/L with 5.2, 2.6 and 2.9 %-RSD, respectively. For EDB in Natural Water B: 7 replicates were spiked at 0.050 ug/L; mean recovery was 0.054 with 10%-RSD. For EDB in drinking water: 11 replicates were spiked with 0.030 ug/L. Mean recovery was 0.054 ug/L with < 0.04%-RSD. For DBCP in deionized water: 8, 8, 7 and 10 replicates were spiked at 0.040, 0.15, 0.30 and 1.7 ug/L. Mean recoveries were 0.04, 0.13, 0.26 and 1.8 ug/L with 4.0, 3.9, 1.9 and 2.5%-RSD, respectively. For DBCP in Natural Water A: 9, 10 and 8 replicates were spiked at 0.030, 0.70 and 1.7 ug/L. Mean recoveries were 0.055, 0.67 and 1.8 with 66, 6.0 and 3.6%-RSD, respectively. For DBCP in Natural Water B: 7 replicates were spiked at 0.050 ug/L. Mean recovery was 0.045 with 2.4%-RSD. For DBCP in drinking water: 11 replicates were spiked at 0.030 ug/L. Mean recovery was 0.034 ug/L with 5.6%-RSD.
Detection Level Note:	Method detection limits (MDL) for this method using U.S. Federal Register, 1984, Definition and Procedure for the Determination of the Method Detection Limit, Appendix B to Part 136, vol 49, no, 209, p. 198.

Precision Descriptor Notes:

For EDB in deionized water: 8, 8, 8 and 10 replicates were spiked at 0.040, 0.15, 0.30 and 1.7 ug/L. Mean recoveries were 0.030, 0.12, 0.24 and 1.8 ug/L with 4.1, 6.8, 1.5 and 2.1%-RSD, respectively.
For EDB in Natural Water A: 9, 10 and 8 replicates were spiked with 0.030, 0.70 and 1.7 ug/L. Mean recoveries were 0.022, 0.60 and 1.8 ug/L with 5.2, 2.6 and 2.9 %-RSD, respectively.
For EDB in Natural Water B: 7 replicates were spiked at 0.050 ug/L; mean recovery was 0.054 with 10%-RSD.
For EDB in drinking water: 11 replicates were spiked with 0.030 ug/L. Mean recovery was 0.054 ug/L with < 0.04%-RSD.
For DBCP in deionized water: 8, 8, 7 and 10 replicates were spiked at 0.040, 0.15, 0.30 and 1.7 ug/L. Mean recoveries were 0.04, 0.13, 0.26 and 1.8 ug/L with 4.0, 3.9, 1.9 and 2.5%-RSD, respectively.
For DBCP in Natural Water A: 9, 10 and 8 replicates were spiked at 0.030, 0.70 and 1.7 ug/L. Mean recoveries were 0.055, 0.67 and 1.8 with 66, 6.0 and 3.6%-RSD, respectively.
For DBCP in Natural Water B: 7 replicates were spiked at 0.050 ug/L. Mean recovery was 0.045 with 2.4%-RSD.
For DBCP in drinking water: 11 replicates were spiked at 0.030 ug/L. Mean recovery was 0.034 ug/L with 5.6%-RSD.

Detection Level Note:

Method detection limits (MDL) for this method using U.S. Federal Register, 1984, Definition and Procedure for the Determination of the Method Detection Limit, Appendix B to Part 136, vol 49, no, 209, p. 198.

Revision	PDF/Link
1993

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USGS-NWQL: O-3120-90: 1,2-Dibromomethane (EDB) and 1,2-dibromo-3-chloropropane (DBCP) in Water by Gas Chromatography

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