Effect of sample preparation method on the determination of twenty-seven impurity elements in boron nitride by direct current glow discharge mass spectrometry
TAN Xiu-zhen1, LI Yao1, ZHU Liu1, DENG Yu-ning2
1. Guangdong First Rare Materials Co., Ltd., National Engineering and Technology Research Center of Scattered Metal, Qingyuan 511875, China; 2. Qingyuan First Materials Co., Ltd., Qingyuan 511517, China
Abstract：The influence of three sample preparation methods on the determination of twenty-seven impurity elements (including Na, Mg, Al, Si, etc) in boron nitride by direct current glow discharge mass spectrometry (dc-GDMS) was discussed. Three sample preparation methods were described as below. Method 1: the boron nitride was directly pressed on the thin sheet of indium; Method 2: after pressing boron nitride on the thin sheet of indium, a layer of indium cover was added; Method 3: the crushed boron nitride was placed on the needle-like tantalum spoon. The influence of three sample preparation methods on the signal intensity of matrix was compared under optimized glow discharge parameters. The results showed that: for Method 1, when the size of boron nitride was about 3mm×3mm with thickness less than 1mm, the signal intensity of matrix (11B) was up to 1.8×107 cps; for Method 2, if the hole size of indium cover was appropriate, the signal intensity of matrix (11B) reached 1.0×107 cps; for Method 3, the signal intensity of matrix was one order of magnitude higher than above two methods. The analytical results were good for most elements under moderate resolution mode. For the elements which were difficult to be separated at high resolution, the isotopes with low abundance could be selected for determined at moderate resolution mode, for example, 70Ge+ for Ge, 82Se+ for Se, 111Cd+ for Cd, 119Sn+ for Sn, 109Ag+ for Ag, and 104Pt+ for Pt. The content of impurity elements in boron nitride could be calculated by subtracting the results of impurities measured from the indium sheet or tantalum spoon. The sample was determined independently for five times, and the relative standard deviations (RSD) were all less than 20%. The analysis results of Al, Si and Ti were basically consistent for three sample preparation methods. In Method 1 and Method 2, the content of detected indium was relatively high, leading to high influence of Ni and Cu in indium on the determination of boron nitride. In Method 3, due to the contribution of Fe and Cu in tantalum, the detected values of Fe and Cu in boron nitride were relatively high. However, the signal intensity of matrix in Method 3 was high, which could reduce the detection limits of some elements such as Cr, Mn, Ga and Ge. Therefore, the Method 3 was the preferred method.
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TAN Xiu-zhen, LI Yao, ZHU Liu, DENG Yu-ning. Effect of sample preparation method on the determination of twenty-seven impurity elements in boron nitride by direct current glow discharge mass spectrometry. , 2019, 39(8): 23-29.
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