Code of Federal Regulations Title 40. Protection of Environment § 40.766.16 Developing the analytical test method

(a) Sample selection. The chemical product to be tested should be sampled so that the specimens collected for analysis are representative of the whole. Additional guidance for sample selection is provided under § 766.12.

(b) Sample preparation. The sample must be mechanically homogenized and subsampled as necessary. Subsamples must be spiked or reinforced with surrogate compounds or with standard stock solutions, and the surrogates or standards must be thoroughly incorporated by mechanical agitation. Additional guidance is provided under § 766.12.

(c) Sample extraction and cleanup. The spiked samples must be treated to separate the HDDs/HDFs from the sample matrix. Methods are reviewed in the Guidelines under § 766.12, but the final method or methods are left to the discretion of the analyst, provided the instrumental response of the surrogates meets the criteria listed in the Quality Assurance Plan for Measurement of Brominated or Chlorinated Dibenzofurans and Dibenzodioxins, Appendixes B and C of the Guidelines. Cleanup techniques are described in the Guidelines. These are chosen at the discretion of the analyst to meet the requirements of the chemical matrix.

(d) Analysis. The method of choice is High Resolution Gas Chromatographic/High Resolution Mass Spectrometric Determination, (HRGC/HRMS) but alternate methods may be used if the manufacturer can demonstrate that the method will reach the target LOQs as well as HRGC/HRMS. Specific operating requirements are found in the Guidelines.