阴离子树脂萃取富集-分光光度法测定煤矸石中痕量钪

Spectrophotometric determination of trace scandium in coal gangue after extraction and enrichment with anion resin

研究了对乙酰基偶氮氯膦(CPApA)与钪(Ⅲ)的显色反应,在HNO3介质中,在TritonX-100存在下,CPApA与钪(Ⅲ)反应生成摩尔比为1:1的稳定配合物,该配合物可用717型阴离子树脂交换柱萃取富集,再通过树脂相光度法测定钪,由此建立了测定钪的新方法。吸附配合物树脂相的最大吸收波长为690nm,表观摩尔吸光系数为9.56×105L.mol-1.cm-1。钪的质量浓度在0～480μg/L范围内符合比耳定律。经阴离子树脂交换柱萃取富集后,钪的测定灵敏度可提高数倍,大多数常见离子不干扰测定。方法应用于煤矸石痕量钪的测定,结果满意。样品分析结果的相对标准偏差小于5%,加标回收率为96.0%～102.5%。

The chromogenic reaction of p-acetylchlorophosphonazo (CPApA) with scandium(Ⅲ) was studied.It was found that CPApA with scandium(Ⅲ) could form a stable complex with the mole ratio of 1:1 in the presence of Triton X-100 and nitric acid medium and this complex could be enriched on the column of 717# anion resin.The resulted resin could be used to determine scandium by spectrophotometry at a maximum absorption wavelength of 690 nm.A new spectrophotometric determination method of trace scandium was developed.It...