Determination of trace arsenic in trichlorosilane by inductively coupled plasma mass spectrometry after trichlorosilane volatilization via low temperature heating
QIAN Jin-wang1,2, MAO Zhi-hui1,2, YANG Hong-yan1,2, ZHANG Yun-hui1,2, TAO Ming1,2
1. Yunnan Metallurgical Yunxin Silicon Material Co., Ltd., Qujing 655000, China; 2. Key Lab of Yunnan Province Optoelectronic Silicon Material Preparation Technology Enterprises, Qujing 655000, China
Abstract：During the determination of arsenic in trichlorosilane by inductively coupled plasma mass spectrometry (ICP-MS) in normal mode, the signal of 75As+ would be seriously interfered by 40Ar35Cl+. If the sample was determined directly, the presence of much silicon matrix not only had matrix effect, but also could cause the blocking of sampling cone, skimmer cone and sampling system. All these problems brought challenges for the determination of trace arsenic in trichlorosilane by ICP-MS. The liquid trichlorosilane sample was treated by nitrogen volatilization at 50-90℃ using graphite device. The sample residue after volatilization treatment was leached with hydrofluoric acid-nitric acid-hydrogen peroxide-water mixture with volume ratio of 1:1:1:8, solving the problem caused by the presence of much silicon matrix. Meanwhile, the hydrogen-helium mixing collision/reaction cell mode was used in experiments. The flow rate of mixing collision/reaction gas was controlled at 6.0mL/min to eliminate the interference of 40Ar35Cl+ to 75As+. The determination of trace arsenic in trichlorosilane by ICP-MS was finally realized. The standard series solution of arsenic was determined under the optimized instrumental conditions. The signal intensity and mass concentration of arsenic were treated by linear regression. The correlation coefficient was higher than 0.9990. The detection limit was 0.01ng/g. The experimental method was applied for the determination of arsenic in trichlorosilane sample. The relative standard deviations (RSD, n=11) of determination results were between 0.71% and 7.1%. The recoveries were between 87% and 105%. 1.00 and 15.00μL of standard stock solution of arsenic were accurately sampled and added into hyperpure trichlorosilane using micropipettor to prepare two simulated samples. The mass fraction of arsenic was 2.00ng/g and 30.00ng/g, respectively. The content of arsenic in these two simulated samples was determined according to the experimental method. The found results were basically consistent with the theoretical values. The absolute value of relative error was less than 1%.
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QIAN Jin-wang, MAO Zhi-hui, YANG Hong-yan, ZHANG Yun-hui, TAO Ming. Determination of trace arsenic in trichlorosilane by inductively coupled plasma mass spectrometry after trichlorosilane volatilization via low temperature heating. , 2018, 38(7): 44-50.
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