同位素稀释质谱法测定水和铀化合物中痕量硼
Determination of Trace Boron in Water and Uranium Compound by IDMS
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摘要: 通常测定痕量硼的主要困难是分离过程中硼的回收率不稳定。所以获得一个低而稳定的硼空白是非常重要然而又非常困难的课题。本文采用同位素稀释质谱法,用N-甲基葡萄糖络合树脂纯化试剂并简化了分离流程,合理选择发射剂用量,因而获得了低而稳定的硼空白和高的测定灵敏度。方法检出限为1.5×10~(-8)克。测定含硼23ppb的水样和含硼0.143ppm的铀化合物试样的精密度分别为±1.3%和±5.9%。本方法参加了国际原子能机构(IAEA)1984年组织的国际分析比对,在有25个国际上著名的实验室参加的比对中,我们的结果与最后的公认值相符。Abstract: Usually the main difficulty in determination of trace boron is its unsta-ble recovery in preliminary separation. It is very important to get a lowstable blank of boron. The conventional methods used for purifying boroninvolve distillatory method, extractive method and ion-exchange method etc.Distillatory method is of a good selectivity but too slow. The results fromextractive method are often unstable. In this paper, a low stable blank ofboron and a high sensitivity have been obtained owing to using N-methylglucose complex resin for purifying the reagents, simplifying the separationprocess and choosing the proper quantity of emitting agent. The determina-tion limit (three times standard deviation of blank) is 1.5×10~(-8)g of boron.The precision is ±1.3% for water sample containing 23 ppb boron and±5.9% for uranium compound sample containing 0.143 ppm boron, respecti-vely. At the intercomparison run organized by International Atomic EnergyAdministration (IAEA) in 1984 the results from this method were in agree-ment with the certified value.