Add time:08/22/2019         Source:sciencedirect.com

A simple gas chromatographic method is described for the determination of dichloro-, trichloro-, and tetrachlorobenzene impurities in 1,3,5-trichlorobenzene samples. The sample is dissolved in carbon disulfide, and an aliquot is chromatographed on a 6-ft. long 10% Bentone 34 column. The peak heights and peak areas are measured and related to concentration by means of calibration curves. 1,3,5-Trichlorobenzene samples were found to contain small amounts of m-dichlorobenzene and 1,2,4-trichlorobenzene. From these data and thin-layer chromatographic analyses of crude 1,3,5-trichloro-2,4,6-trinitrobenzene, an explanation is proposed for the origin of the 1,3-dinitro-2,4,5,6-tetrachlorobenzene impurity found in 1,3,5-triamino-2,4,6- trinitrobenzene samples. It is concluded that 1,3-dinitro-2,4,5,6-tetrachlorobenzene is produced during the nitration of 1,3,5-trichlorobenzene.

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