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本文推荐了一个对Purex流程样品中微量氟(1微克以上)的氟离子选择电极法的测定程序。样品中所含Zr~(4+),Al~(3+),Fe~(3+)等与F~-络合的阳离子,在有柠檬酸钠存在时,不影响F~-的电位测定。当铀量大于5.7毫克时影响较大,可用二-(2-乙基己基)磷酸酯-煤油溶液萃取除去。有机相样品中的F~-可用NaOH反萃后再按含铀水相样品分析。推荐方法的精密度以单值测定的相对标准偏差表示均不超过2%。与加入已知F~-量及萃取光度法比较,相对误差一般均小于3%。
This paper presents a procedure for the determination of trace fluoride (1 μg or more) by fluoride ion selective electrode method in a Purex process sample. The positive ions of F ~ - such as Zr ~ (4 +), Al ~ (3 +) and Fe ~ (3+) contained in the sample did not affect the potential of F ~ - in the presence of sodium citrate . When the amount of uranium is greater than 5.7 mg, it can be removed by extraction with di- (2-ethylhexyl) phosphate-kerosene solution. The F ~ in the organic phase sample can be back-extracted with NaOH and then analyzed according to the uranium-containing aqueous phase sample. The precision of the recommended method, expressed as a single standard relative standard deviation, does not exceed 2%. Compared with adding known F ~ - amount and extraction spectrophotometry, the relative errors are generally less than 3%.