摘要
本文建立了测定湿法炼锌水解沉铟过程产生的副产石膏渣中铟的原子吸收光谱法,对仪器条件、测定介质、溶样方式及试样中干扰元素进行了考察。实验发现,仪器最佳状态为灯电流5 mA、乙炔流量1500 mL/min、燃烧器高度5 mm;在体积分数为5%~15%的硝酸介质中,铟的吸光度稳定而且远大于同体积分数的盐酸、王水介质;以20 mL盐酸分解试样至小体积后加20 mL硝酸可有效驱除残余的盐酸,保证了测定铟时吸光度稳定;试样中共存硫酸钙基体不干扰铟的测定。方法线性范围0.25~4μg/mL,相关系数为0.9997,方法检出限为0.053μg/mL,定量限为0.18μg/mL。方法用于实际样品分析,测定结果与萃取分离后原子吸收(AAS)测定结果基本一致,相对标准偏差(RSD,n=11)为1.3%~4.6%,加标回收率为95%~104%。
The by-product gypsum slag produced during the hydrolysis and precipitation of indium in wet zinc smelting contains a certain amount of indium.An experiment was conducted to establish a method for direct determination of indium in gypsum by flame atomic absorption spectroscopy(AAS)using an air acetylene flame in a nitric acid medium with a volume fraction of 5%.We investigated the instrument conditions,measuring medium,dissolution method,and interfering elements in the sample.The experiment found that the optimal state of the instrument is lamp current of 5 mA,acetylene flow rate of 1500 ml/min,and burner height of 5 mm;In nitric acid medium with a volume fraction of 5%-15%,the absorbance of indium is stable and much higher than that of hydrochloric acid and aqua regia medium with the same volume fraction;Decompose the sample with 20 ml hydrochloric acid to a small volume and add 20 ml nitric acid to effectively remove residual hydrochloric acid,ensuring stable absorbance during indium determination;The coexisting elements in the sample do not interfere with the determination of indium.The linear range of the method is 0.25-4μg/ml,with a correlation coefficient of 0.9997.The detection limit of the method is 0.053μg/ml,and the quantification limit is 0.18μg/ml.The method is used for actual sample analysis,and the measurement results are basically consistent with the atomic absorption spectroscopy(AAS)measurement results after extraction and separation.The relative standard deviation(RSD,n=11)is 1.3%-4.6%,and the spiked recovery rate is 95%-104%.
作者
韦元洲
刘传仕
魏巍
罗开良
Wei Yuan-zhou;Liu Chuan-shi;Wei Wei;Luo Kai-liang(Yunxi Wenshan zinc and indium smelting Co.,Ltd.,Maguan,Yunnan 663700,China)
出处
《福建分析测试》
2025年第3期36-40,共5页
Fujian Analysis & Testing
基金
云南省重大科技专项计划项目(NO.202302AB080014)。
关键词
石膏渣
铟
原子吸收(AAS)
gypsum slag
Indium
Atomic Absorption Spectroscopy(AAS)
