Non aqueous titration

Why 0.02 to 0.5% water is necessary in perchloric acid?

In the United States Pharmacopeia (USP), 0.1 N perchloric acid in acetic acid volumetric solution (hereafter HClO4 VS) used for non-aqueous titration has specified a water content between 0.02 and 0.05%. Preparing this titrant with such a narrow range of water content is very time consuming, precludes the use of commercially available titrants, and, consequently, prompted an investigation to try and expand the range up to 0.5%. In this study, the titrimetric results obtained using HClO4 VS containing more water were very close to those obtained using the USP specified titrants. A maximum assay difference of 0.7% in the titrations of three selected nitrogen-containing compounds, clonidine hydrochloride, dipyridamole, and adenosine were observed. The titrimetric results obtained using these titrants were also precise with RSDs of not more than 0.4%. Therefore, a wider range of water content in HClO4 VS between 0.02 and 0.5% is suggested for the USP potentiometric titration of nitrogen-containing compounds.


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