电感耦合等离子体发射光谱法测定粗二氧化碲中 铜、铅、锑、铋、砷和硒

粗二氧化碲作为碲精炼或碲化工产品生产的重要原料,其中共存元素铜、铅、砷、锑、铋、硒含量的准确测定对于生产过程质量控制和贸易结算具有重要意义,但目前没有粗二氧化碲中铜、铅、砷、锑、铋、硒含量检测的标准分析方法。采用王水和饱和氟化氢铵分解试样,在王水和酒石酸介质中,选用Cu 327.393 nm、Pb 220.353 nm、Sb 217.582 nm、Bi 223.061 nm、As 193.696 nm、Se 196.026 nm为分析谱线,采用电感耦合等离子体发射光谱(ICP-AES)法测定粗二氧化碲中铜、铅、锑、铋、砷和硒含量。各元素校准曲线的相关系数均大于0.999;铜、铅、锑、铋、砷和硒的检出限分别为0.0004%、0.0005%、0.0006%、0.0007%、0.0004%和0.0007%,定量检出限分别为0.0012%、0.0016%、0.0020%、0.0025%、0.0013%和0.0025%。按照实验方法测定5个粗二氧化碲样品中铜、铅、锑、铋、砷和硒,测定结果的相对标准偏差(RSD,n=7)为0.79%~4.8%,加标回收率为96.0%~103%。方法简单,精密度和准确度较高,可用于测定粗二氧化碲中铜、铅、砷、锑、铋、硒含量。

Determination of copper, lead, antimony, bismuth, arsenic and selenium in crude tellurium dioxide by inductively coupled plasma atomic emission spectrometry

Crude tellurium dioxide is an important raw material for tellurium refining or tellurium chemical production, in which the accurate determination of coexisting elements copper, lead, arsenic, antimony, bismuth and selenium is of great significance for production process quality control and trade settlement. However, there is no standard analytical method for the determination of copper, lead, arsenic, antimony, bismuth and selenium in crude tellurium dioxide. The samples were decomposed by aqua regia and saturated ammonium hydrogen fluoride. Cu 327.393nm, Pb 220.353nm, Sb 217.582nm, Bi 223.061nm, As 193.696nm and Se196.026nm were selected as analytical lines. The contents of copper, lead, antimony, bismuth, arsenic and selenium in crude tellurium dioxide were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) in the medium of aqua regia and tartaric acid. The correlation coefficients of the calibration curves of elements were all higher than 0.999. The limit of detection of copper, lead, antimony, bismuth, arsenic and selenium was 0.0004%, 0.0005%, 0.0006%, 0.0007%, 0.0004% and 0.0007%, respectively. The limit of quantification was 0.0012%, 0.0016%, 0.0020%, 0.0025%, 0.0013% and 0.0025%, respectively. The contents of copper, lead, antimony, bismuth, arsenic and selenium in five crude tellurium dioxide samples were determined according to the proposed method. The relative standard deviations (RSD, n=7) of the results were between 0.79% and 4.8%, and the recoveries were between 96% and 103%.