ICP-AES测定锑烟灰中铜、银、硒、碲、砷、铋方法研究

ICP-AES Determination of Cu,Ag,Se,Te,As and Bi in Antimony Soot

提出了电感耦合等离子体原子发射光谱法同时测定锑烟灰中有价金属及有害元素的方法。用硫酸完全溶解样品,试液中加入酒石酸络合大量锑(ⅴ),盐酸稀释至刻度定容。再移取一定量的试液于100 mL容量瓶中,稀释成20%的盐酸介质在电感耦合等离子体原子发射光谱测定。对光谱仪的工作条件及分析谱线的选择等分析条件作了试验优化。方法的检出限3S为1.2 ug/L(铜),0.08 ug/L(银),4.1 ug/L(硒),3.2 ug/L(碲),3.3 ug/L(砷),4.5 ug/L(铋)。对锑烟灰按所提出的方法分析并以此作基体加入两个不同浓度水平的铜、银、硒、碲、砷、铋标准,进行方法的准确度和精密度试验,测得回收率在95.5%～104.3%,相对标准偏差(n=6)在0.5%～2.0%。

Inductively coupled plasma atomic emission spectrometry was used for simultaneous determination of metals of valence and harmful elements in the antimony soot.The sample was completely dissolved with sulfuric acid,and tartaric acid complexing antimony（v） was added to the test solution that was diluted with hydrochloric acid to the mark with a constant volume.And then certain volume of the solution was shift into a 100mL volumetric flask,then diluted into 20% hydrochloric acid medium for determination by the inductively coupled plasma atomic emission spectrometry.Optimization for working conditions and the choice of the spectral lines of the spectrometer analysis of the conditions was made for the test.The detection limits of 3S were 1.2 ug.L-1（copper）,0.08 ug.L-1（silver）,4.1 ug.L-1（selenium）,3.2 ug.L-1（tellurium）,3.3 ug.L-1（arsenic） and 4.5 ug.L-1（bismuth）.Analysis was made for accuracy and precision test with the proposed method on antimony ash and mixture of antimony ash as matrix and two different density levels of copper,silver,selenium,Te,arsenic Bi standard.The measured recovery rate was 95.5% ~ 104.3%,and the relative standard deviation（n = 6） was in 0.5% to 2.0%.