EPA-OW/OST: 1614:  Brominated Diphenyl Ethers in Water, Soil, Sediment, and Tissue by HRGC/HRMS

  • Summary
  • Analytes
  • Revision
  • Data and Sites
Official Method Name
Brominated Diphenyl Ethers in Water, Soil, Sediment, and Tissue by HRGC/HRMS
Current Revision
August 2007
Media
VARIOUS
Instrumentation
Gas Chromatography with Mass Spectrometry Detection
Method Subcategory
Organic
Method Source
  EPA-OW/OST
Citation
USEPA, 2007, Method 1614: Brominated diphenyl ethers in water, soil, sediment, and tissue by HRGC/HRMS, EPA-821-R-07-005.
Brief Method Summary
EPA Method 1614 was developed by the Office of Water's Office of Science and Technology (OST) to determine polybrominated diphenyl ether (PBDE) congeners in aqueous, solid, tissue, and multi-phase matrices. These ethers are used in brominated flame retardants. The method uses isotope dilution and internal standard high resolution gas chromatography/high resolution mass spectrometry (HRGC/HRMS).

This version revises the August 2003 version to include use of a temperature programmed injector/vaporizer and a short column to improve recoveries of the octa-, nona- and decabrominated diphenyl ethers.

Disclaimer

This PBDE-congener method is patterned after the EPA PCB-congener Method 1668A. The method specifications are based on data from Axys Analytical. Method 1614 has been reviewed by the Engineering and Analytical Support Branch in the Engineering and Analysis Division (EAD) of OST. The method is available for general use, but has not been published in 40 CFR Part 136. Mention of trade names or commercial products does not constitute endorsement or recommendation for use.
Scope and Application
EPA Method 1614 is for determination of brominated diphenyl ether (BDE) congeners in water, soil, sediment, biosolids, tissue, and other sample matrices by high resolution gas chromatography combined with high resolution mass spectrometry (HRGC/HRMS).

This method can also be used to test for other brominated flame retardants (BFR) and brominated organic compounds in the event that new products come on the market.
Applicable Concentration Range
N/A
Interferences
Solvents, reagents, glassware, and other sample processing hardware may yield artifacts, elevated baselines, and/or lock-mass suppression causing misinterpretation of chromatograms. Proper cleaning of glassware is extremely important, because glassware may not only contaminate the samples but may also remove the analytes of interest by adsorption on the glass surface. Contamination of calibration solutions can be overcome by preparing solution in an area free from BDE contamination using glassware free from contamination. The natural lipid content of tissue can interfere in the analysis of tissue samples for the BDEs. Lipids must be removed by the anthropogenic isolation column procedure followed by the gel permeation chromatography procedure.
Quality Control Requirements
The minimum requirements of this program consist of an initial demonstration of laboratory capability, analysis of samples spiked with labeled compounds to evaluate and document data quality, and analysis of standards and blanks as tests of continued performance.
Sample Handling
Maintain aqueous, solid, mixed phase, and semi-solid samples in the dark at <6 °C from the time of collection until receipt at the laboratory. Ideally, tissue samples should be frozen upon collection and shipped to the laboratory under dry ice.
Maximum Holding Time
There are no demonstrated maximum holding times associated with the BDEs in aqueous, solid, semi-solid, tissue, or other sample matrices. If stored in the dark at <6 °C, aqueous samples may be stored for up to one year. Similarly, if stored in the dark at
Relative Cost
$201 to $400
Sample Preparation Methods
See EPA method 1614 section 11.0