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本文介绍了用偶氮胂-K测定大量铀中微量镎的分光光度法。首先用铁(Ⅱ)将镎还原为镎(Ⅳ),在2N HNO_3的条件下吸附于三月桂胺(TLA)色层柱上,而与样品中大量铀(铀:镎高达10~6:1)、微量钚和钍以及不诱钢腐蚀产物分离,然后用0.15N HNO_3洗脱镎(Ⅳ),并在665毫微米处测量镎(Ⅳ)同偶氮胂-K生成的蓝绿色络合物的消光值。此络合物的克分子消光系数为77000。在0.2—1.0微克镎(Ⅳ)/2毫升的范围内服从比尔定律。方法的精密度为±7%。在3小时内,一人操作可以完成6个样品的测定。
This paper presents a spectrophotometric method for the determination of trace amounts of uranium in arsenite with arsenazo-K. At first, iron (Ⅱ) was used to reduce 镎 to 镎 (Ⅳ), adsorbed onto trillamine (TLA) chromatographic column under 2N HNO_3, and compared with a large amount of uranium (uranium: 镎 up to 10 ~ 6: 1 ), Trace amounts of plutonium and thorium, and non-induced corrosion products were separated, and then eluted with 0.15 N HNO 3 (IV), and a blue-green complex of arsenazo-K was measured at 665 nm Extinction. The molar extinction coefficient of this complex was 77,000. Beer’s law is obeyed in the range of 0.2-1.0 microgram Ⅳ (IV) / 2 ml. The precision of the method is ± 7%. Within 3 hours, one person can complete the determination of 6 samples.