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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 color reaction of acetyl chlorophosphonazo (CPApA) with scandium (Ⅲ) was studied. The reaction of scandium (Ⅲ) with CPApA in the presence of TritonX-100 in HNO3 medium gave a stable molar ratio of 1: 1 The complex can be extracted and enriched with 717 anion exchange resin column, and then the scandium was determined by resin phase spectrophotometry. A new method was established for the determination of scandium. The maximum absorption wavelength of the adsorbed complex resin phase was 690 nm, and the apparent molar absorptivity was 9.56 × 10 5 L · mol -1 · cm -1. The scandium mass concentration conforms to the Beer’s law in the range of 0 ~ 480 μg / L. After the anion resin exchange column enrichment, scandium determination sensitivity can be increased several times, most common ions do not interfere with the determination. The method was applied to the determination of trace scandium in coal gangue with satisfactory results. The relative standard deviation (RSD) was less than 5% and the recoveries were 96.0% -102.5%.