A methodology for quantitative chemical analysis of the complex “borohydride-borate-hydroxide-carbonate-water” mixtures used as fuel in the borohydride fuel cell was developed and optimized. The methodology includes the combined usage of the acid-base and iodometric titration methods. The acid-base titration method, which simultaneously uses the technique of differentiation and computer simulation of titration curves, allows one to determine the contents of hydroxide (alkali), carbonate, and total “borate + borohydride” content. The iodometric titration method allows one to selectively determine borohydride, so the content of each ofOH-,BH4-,BO2-, andCO32-anions in the fuel becomes estimated. The average determination error depends on the number and ratio of compounds in a mixture. Specific details of the analysis of various fuel mixtures are discussed.