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本文研究了对乙酰基偶氮羧-p与钙显色反应的条件,并建立了测定合金钢中微量钙的方法,在柠檬酸介质中,试剂与钙有灵敏的显色反应,其络合物最大吸收波长为705nm,摩尔吸光系数为1.50×10~5,在25ml溶液中,0～7μg钙符合比耳定律,用三乙醇胺-酒石酸钾钠作联合掩蔽剂,采用偶氮氧化偶氮BN-环已烷萃取分离钙,一次萃取和反萃取即可达到与大量基体元素定量分离的目的。该法用于测定合金钢中的钙,方法简便,结果与标准值一致,变异系数小于2.0%,回收率达97.0%以上。
In this paper, the conditions for the color reaction of acetyl-azocarboxy-p with calcium were studied. A method for the determination of trace calcium in alloy steel was established. In the citric acid medium, the reagent has a sensitive color reaction with calcium, The maximum absorption wavelength is 705nm, the molar absorptivity is 1.50 × 10 ~ 5. In 25ml solution, 0 ~ 7μg calcium conforms to Beer’s law. Using triethanolamine-potassium sodium tartrate as masking agent, azo oxyazo BN - Cyclohexane extraction and separation of calcium, one extraction and back extraction can be achieved with a large number of matrix elements quantitative separation purposes. The method is applied to the determination of calcium in alloy steel. The method is simple and has the same result with the standard value. The coefficient of variation is less than 2.0% and the recovery rate is over 97.0%.