EFFECT OF WATER-CONTENT IN PERCHLORIC-ACID ON THE NONAQUEOUS POTENTIOMETRIC TITRATION OF NITROGEN-CONTAINING COMPOUNDS

In the United States Pharmacopeia (USP), 0.1 N perchloric acid in acet ic acid volumetric solution (hereafter HClO4 VS) used for non-aqueous titration has specified a water content between 0.02 and 0.05%. Prepar ing this titrant with such a narrow range of water content is very tim e 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 HClO 4 VS containing more water were very close to those obtained using the USP specified titrants. A maximum assay difference of 0.7% in the tit rations of three selected nitrogen-containing compounds, clonidine hyd rochloride, 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 titr ation of nitrogen-containing compounds. (C) 1997 Elsevier Science B.V.