过氧化钠碱熔-电感耦合等离子体原子发射光谱法测定富锡渣中锑  

Determination of antimony in tin-riched slag by inductively coupled plasma atomic emission spectrometry with sodium peroxide alkali fusion

作　　者：杨赟金 程婧娴 余波 余晓 YANG Yunjin;CHENG Jingxian;YU Bo;YU Xiao(Kunming Metallurgical Research Institute Co.,Ltd.,Kunming 650031,China)

机构地区：[1]昆明冶金研究院有限公司,云南昆明650031

出　　处：《冶金分析》2023年第1期49-53,共5页Metallurgical Analysis

基　　金：昆明市“春城计划”高层次人才培养工程“首席技师”专项。

摘　　要：富锡渣是锡一次还原熔炼后的含锡中间产品,一般含有难溶锡氧化物,普通酸溶法和微波消解法无法将样品完全分解,而采用酸溶-碱熔法虽能将样品完全分解,但其操作流程长且易造成待测元素的损失。采用过氧化钠为熔剂碱熔样品,再使用盐酸(1+1)提取,将溶液稀释后使用钠盐匹配的标准溶液系列绘制校准曲线,建立了电感耦合等离子体原子发射光谱法(ICP-AES)测定富锡渣中锑的方法。结果表明:锑的质量浓度为0.50~10.00μg/mL时,校准曲线的线性相关系数r为0.9998;方法检出限为0.002%。锡基体及样品中共存元素对锑的测定结果无影响。按照实验方法测定4个富锡渣中锑,测定结果的相对标准偏差(RSD,n=6)均小于2.0%;回收率为95%~101%。Tin-riched slag is a tin-containing intermediate product by one-time retailoring of tin.It generally contains insoluble tin oxides,which cannot be fully decomposed by ordinary acid dissolution and microwave digestion.Although the acid solution-alkali fusion method can completely decompose the sample,its operation process is long and easy to cause the loss of elements to be measured.Sodium peroxide was used as the flux for the alkali fusion of sample.After leaching with hydrochloric acid(1+1),the solution was diluted.The standard solution series after matching with sodium salt were used to prepare the calibration curve.Thus,a method for determination of antimony in tin-riched slag was established by inductively coupled plasma atomic emission spectrometry(ICP-AES).The results showed that the linear correlation coefficient(r)of calibration curve was 0.9998 when the mass concentration of antimony was in range of 0.50-10.00μg/mL.The limit of detection was 0.002%.The tin matrix and coexisting elements in sample had no influence on the determination results of antimony.The content of antimony in four tin-riched slag samples was determined according to the experimental method.The relative standard deviations(RSD,n=6)of determination results were all less than 2.0%.The recoveries were between 95%and 101%.

关 键 词：电感耦合等离子体原子发射光谱法(ICP-AES) 富锡渣 过氧化钠 碱熔 锑 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]