US EPA

2074614 

Journal Article 

Perchlorination reaction applied to the rapid determination of PCBs 

Takamiya, K 

1983 

Yes 

Bulletin of Environmental Contamination and Toxicology
ISSN: 0007-4861
EISSN: 1432-0800 

30 

5 

600-605 

English 

6407552 

WOS:A1983QM12400015 

An analytical method for the determination of polychlorinated biphenyl (PCB) by perchlorination was tested. One milliliter (ml) of a hexane solution of PCB was evaporated to dryness in a specially designed apparatus. One ml of thionyl-chloride containing 1 percent sulfuryl-chloride and 40 to 100 milligrams of aluminum-chloride were added. The mixture was heated with reflux for 45 minutes at 64 to 67 degrees-C or 1 hour at 59 to 62 degrees. The reaction product decachlorobiphenyl (2051243) (DCB) was treated with 5ml distilled water and then extracted with 5 to 10ml hexane. The hexane layer was separated and washed with 5ml of sodium-hydroxide. The hexane layer was then dried with 1 gram anhydrous sodium-sulfate. An unspecified amount of the dried hexane solution was injected into a gas chromatograph equipped with an electron capture detector. The concentration of DCB was determined. The concentration of PCB in the sample could be calculated from the DCB concentration and the reaction stoichiometry. The method was evaluated against commercial PCB mixtures. The concentrations were determined with errors of less than 10 percent.