The Method Study On The Multi-element In Antimony Oxide And Refined Antimony Slag By ICP-AES

Since70to80’s of the20th century,Inductively Coupled Plasma Atomic Emission Spectrometer has been widely used in metallurgy、 geology、chemical industry、food、environmental protection、biology and other fields, because of it’s high resolution、high sensitivity、wide linear range、less ionization and chemical interferences、high accuracy and precision. This method is an important technique in modern scientific research and production, also a trace element analysis method generally adopted at home and abroad. The determination method of impurity elements in antimony oxide and tellurium in refined antimony slag by Inductively Coupled Plasma Atomic Emission Spectrometer were established, according to the requirements of the high purity antimony oxide and the recycling of waste.The determination method of6elements in high purity antimony oxide by ICP-AES was established. Bi、Cd、Fe、Cu、Pb were determined by ICP-AES directly and HG-ICP-AES for As. Take aqua regia dissolved sample, adding sulfuric acid to control the temperature, and then through hydrochloric acid and hydrobromic acid reduce the interference of antimony. Discussed the analytical spectral line, dissolving methods and solution acidity, chose the best working conditions of instrument, including RF power, observation height, atomized gas velocity and other factors. The best solution is:handling the sample with HCl-HBr, volume by10%HC1, determined under the following condition:RF1300W, Atomized gas velocity:0.8L·min-1, observation height:15.0mm. The analysis results show that the method has low detection limit, recovery rate was95%～110%, the relative standard deviation<3%.In the method of HG-ICP-AES to determine As in antimony oxide, a lot of experiments were done, mainly including the acidity、reductant concentration、flow rate about the pre reduction reaction. Moreover, analytical spectral line and working conditions of the instrument were also discussed. Then the best determination method of As in antimony oxide by HG-ICP-AES was established. The detection limit of this method is0.0005mg/L, the recoveries were99.5%～101.7%, and the relative standard deviation was1.34%.The method was established on the determination of Te in refined antimony slag by ICP-AES. A lot of experimental studies were done from the dissolution of sample to analysis, mainly including the choice of spectral line、solvent and solution acidity, also the optimization of instrument working conditions. This method has certain guiding significance for the recycling of Te from the residue. After many experiments, the experiment scheme for the determination of tellurium in refined antimony slag by ICP-AES was established:the sample dissolved by aqua regia, volume by10%HC1, determined under the following condition:RF1300W, Atomized gas velocity:0.8L·min-1, observation height:15.0mm. The detection limit of this method is0.0072mg/L, the recoveries were97.2%～101.6%, and the relative standard deviation was0.16%.