Determination of organic halogen in hexane solution

NISHI Sueo, HORIMOTO Yoshiyuki

doi:10.2116/bunsekikagaku.26.11_757

The photochemical dehalogenation reaction of organohalogen compounds was developed to the determination of organic halogen dissolved in hexane. The hexane solution of organohalogen compound was added with 2-propanol solution of sodium hydroxide and was irradiated by a high pressure mercury lamp. In the case of the organohalogen compound which had the absorption band within the wavelength range of the emission from the irradiation source {(220600)nm}, the photochemically initiated free radical reaction proceeded and resulted in the quantitative release of halogen ion. If, however, the organohalogen compound had no or extremely weak absorption band in the above range, extremely slow rate of the reaction was observed and the quantitative halogen recovery was not achieved. Halogen ion thus formed was extracted with water and determined spectrometrically using mercuric thiocyanate method for chlorine, bromide and iodine, and alizarin-lanthanum complex method for fluorine. Some of coexistent organic sulfur or nitrogen compounds gave positive errors to the results due to the formation of interference compounds during the irradiation such as thiol compounds, cyanate, or others which were sensitive to the analytical method. The ion exchange technique for the clean up of halogen ion was successfully used for the elimination of such interferences.

Determination of organic halogen in hexane solution

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