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Su A.-P.,Institute of Research and Designing of YTC | Chen L.,Institute of Research and Designing of YTC | Wang J.-F.,Institute of Research and Designing of YTC | Hai L.,Institute of Research and Designing of YTC | Shi R.-X.,Institute of Research and Designing of YTC
Yejin Fenxi/Metallurgical Analysis | Year: 2014

A quantitative analysis method for the determination of seventeen impurity elements(including aluminum, bismuth, cadmium, cobalt, chromium, copper, iron, gallium, indium, manganese, magnesium, nickel, lead, tellurium, vanadium, titanium and zinc) in crude selenium materials by inductively coupled plasma atomic emission spectrometry (ICP-AES) was established. The sample was dissolved with mixed acid of nitric acid and hydrochloric acid (V (HNO3):V (HCl)=5:10). Selenium was volatilized and removed using mixed hydrochloric acid-hydrobromic acid in presence of little sulfuric acid. After removing sulfuric acid fume by heating, the solution was determined in 15 %(V/V) hydrochloric acid-nitric acid mixed medium(V (HNO3):V (HCl)=3:1). Since the volatilization of selenium was not conducted in volatilizing furnace, the operation was simple and the volatilization efficiency was high. The testing elements had no volatilization loss. Moreover, the residual selenium and coexisting elements had no interference in the determination. The detection limit of method was 0.000 2-0.179 4 μg/mL, and the limit of quantitation was 0.1-15.0 μg/g. The correlation coefficient of calibration curve was higher than or equal to 0.999 9 when the mass concentration of elements was in range of 0-10 μg/mL. The proposed method was applied to the determination of seventeen impurity elements in crude selenium samples. The determination results were consistent with those obtained by nonferrous industrial standard analysis methods. The average recoveries were between 92% and 112%. The relative standard deviations (RSD, n=7) were less than 10% except for trace elements (Cd, Co, Cr, Ga, In and V) with low content. ©, 2014, Central Iron and Steel Research Institute. All right reserved.


Su A.-P.,Institute of research and designing of YTC | Hai L.,Institute of research and designing of YTC
Yejin Fenxi/Metallurgical Analysis | Year: 2012

A method for the determination of trace aluminum in tin ingot by graphite furnace atomic absorption spectrometry was established. The sample decomposition ways and the optimal conditions of determining aluminum by graphite furnace atomic absorption spectrometry was confirmed. Sample was dissolved in hydrochloric acid and hydrogen peroxide(V (hydrochloric acid):V (hydrogen peroxide) = 2.5:1.5). Aluminum was determined in 16 g/L citric acid and 0.12 mol/L hydrochloric acid medium with 4 g/L calcium nitrate as matrix modifier. The results showed that in the selected acidity medium, it was not necessary to volatilize tin that will not be hydrolyzed, and the sample solution was kept clear for a long time. Calcium nitrate improved the measurement sensitivity of aluminum and enhanced resistance to chloride interference. Tin and coexisting elements in sample did not interfere in the determination. The detection limit of this method was 2.96 μg/L. The linear range was between 0 μg/L and 100 μg/L. The correlation coefficient r was not less than 0.998 0. The relative standard deviation for the determination of aluminum in tin ingots was 6.6%, recovery rate was between 100 % to 119%, and the measured values of sample were consistent with that of the standard addition method and ICP-AES.


Su A.-P.,Institute of Research and Designing of YTC | Hai L.,Institute of Research and Designing of YTC | Shi R.-X.,Institute of Research and Designing of YTC
Yejin Fenxi/Metallurgical Analysis | Year: 2015

The sample was dissolved with nitric acid (1+2) and hydrochloric acid (1+1). Most lead and silver were precipitated by hydrochloric acid. Then, the supernatant liquid in medium of 16 g/L citric acid-0.12 mol/L hydrochloric acid was directly analyzed by graphite furnace atomic absorption spectrometry to determine the content of aluminum in tin-lead solder. The results showed that the tin was not hydrolyzed without volatilization in selected acidity medium. Most lead and silver were precipitated on the bottom in form of chlorides. The supernatant liquid could be directly analyzed without filtration to remove silver and lead precipitations by degreasing cotton-paper pulp which was treated by hydrochloric acid. The clarification of sample solution could last for long time. The tin and coexisting elements in sample did not interfere with the determination. The linear range of method was 3.00-100.00 μg/L, and the detection limit was 4.04 μg/L. The proposed method was applied to the determination of aluminum in certified reference materials of tin-lead solder. The found results were consistent with the certified values or those obtained by inductively coupled plasma atomic emission spectrometry (ICP-AES) in GB/T10574.13-2003. The relative standard deviations (RSD) were between 6.2% and 8.9%. ©, 2015, Central Iron and Steel Research Institute. All right reserved.

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