摘要 |
<p>PURPOSE:To avoid the quantitative interfering action of nitric acid perfectly and simply, by dividing a specimen into two sections and respectively performing the quantitative analysis of monobutyl dihydrogenphosphate and that of dibutyl hydrogenphosphate in first and second sections. CONSTITUTION:In quantitatively analyzing monobutyl dihydrogenphosphate and dibutyl hydrogenphosphate in a nuclear fuel re-treatment solvent, wherein tributyl phosphate, 1wt% or less of monobutyl dihydrogenphosphate and 1wt% or less of dibutyl hydrogenphosphate coexist, existing in equilibrium with a 10N or less nitric acid aqueous solution, a specimen is divided into two sections. The methyl-esterification treatment of acidic phosphoric esters is directly performed in the first section by diazomethane to perform the quantitative analysis of monobutyl dihydrogenphosphate. One or more of an org. base selected from triethylamine, pyridine and picoline is preliminarily added to the second section in an amount (mol) twice or more than of coexisting dissolved nitric acid and the methyl-esterification of acidic phosphate esters is performed by diazomethane to perform the quantitative analysis of dibutyl hydrogenphosphate.</p> |