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Mercaptobenzothiazole, benzothiazolyl zinc and dibenzothiazolyl disulfide can be determined quantitatively by amperometric titration. The latter two are the products of the breakdown of mercaptobenzothiazole in the vulcanization reaction. It has been found that the mercaptobenzothiazole primitive form or the mercaptobenzothiazole formed from the appropriate reaction of the other two accelerators mentioned above can be quantitatively estimated by the amperometric method. In addition, it is possible to quantitatively estimate the total amount of mercaptobenzothiazole present in two or all three of these accelerator mixtures and the total amount of mercaptobenzothiazole released in two or three of these accelerator mixtures.