Abstract
A method for addition of electrolytically generated bromine was applied for determination of 10-100 g m−3 of 2-butyne-1,4-diol in a nickel-plating solution. Distinct from existing methods, this method generates bromine electrolytically from a KBr solution before each analysis. Amounts of bromine generated using electrolysis agreed with the theoretical value using 1.5 M HCl in a KBr solution. Bromine addition to 2-butyne-1,4-diol was completed with more than 30 min reaction time. Additionally, blank correlation was necessary because small amounts of bromine disappeared during the reaction. It was possible to determine 2-butyne-1,4-diol in nickel plating solutions based on the findings described above. The lower limit of around 5 g m−3 was achieved. This method was not influenced by main components of the nickel-plating solution. However, the presence of allylsulfonic acid as a brightening agent elevated the quantitative values of 2-butyne-1,4-diol. Further investigation revealed that allylsulfonic acid reacts with bromine quantitatively and too rapidly. Results show that the selective determination of 2-butyne-1,4-diol and allylsulfonic acid in a nickel-plating solution became possible using different reaction times for brightening agents and bromine.
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