[Code of Federal Regulations]
[Title 40, Volume 28]
[Revised as of July 1, 2003]
From the U.S. Government Printing Office via GPO Access
[CITE: 40CFR766.16]

[Page 807]
 
                   TITLE 40--PROTECTION OF ENVIRONMENT
 
         CHAPTER I--ENVIRONMENTAL PROTECTION AGENCY (CONTINUED)
 
PART 766--DIBENZO-PARA-DIOXINS/DIBENZOFURANS--Table of Contents
 
                      Subpart A--General Provisions
 
Sec. 766.16  Developing the analytical test method.

    Because of the matrix differences of the chemicals listed for 
testing, no one method for sample selection, preparation, extraction and 
clean up is prescribed. For analysis, High Resolution Gas Chromatography 
(HRGC) with High Resolution Mass Spectrometry (HRMS) is the method of 
choice, but other methods may be used if they can be demonstrated to 
reach the target LOQs as well as HRGC/HRMS.
    (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 
Sec. 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 Sec. 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 Sec. 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.