Study on High Pressure Sample Preparation Method for Pressed Powder Pellet and Its Application in X-Ray Fluorescence Spectrum Analysis
ZHANG Qin1, YU Zhao-shui1*, LI Xiao-li2, LI Guo-hui1
1. Institute of Geophysical and Geochemical Exploration, Chinese Academy of Geological Sciences, Langfang 065000, China 2. Tianjin Institute of Geology and Mineral Resources, Tianjin 300170, China
Abstract：Using the independently designed high pressure sample preparation mold and high pressure sample preparation technology (patent number: 201310125772.5), studies on the high pressure pressed various geological samples such as rocks, soils and stream sediments were first described in the present paper. It is the first experiment conducted in this field with significant achievements obtained. Without any binder, various types of geological powder samples can be pelleted well using 1600KN high pressure method. Such pellet has the characteristics of dense, flat, smooth and shiny surface, no cracks, no delamination, and no powder dropping. The study provides a new and contamination-free approach to sample preparation of X-ray fluorescence spectrum analysis. The comparison study conducted between the same samples pelleted under the low pressure (400 kN) and high pressure (1 600 kN) showed that using the high pressure the element peak to background ratios, and sensitivities are significantly improved, the detection limits are lowed, and the accuracies, the precisions and sample preparation repeatability are greatly improved. The Si FWHM became wider for the high pressure (1 600 kN) pellet than the same sample pelleted under the lower pressure (400 kN). The further SEM observation revealed that variation of Si spectrum shape may be caused by that the silica crystal lattices are destroyed and the particle size becomes smaller by using the high pressure pelleting techniques. So the particle size and mineral effects are also effectively reduced and the precisions and accuracies of the analytical method are improved.
Key words：Method and technique for high pressure pressed;Geological sample;X-ray fluorescence spectrometry
张 勤1，于兆水1*，李小莉2，李国会1 . X射线荧光光谱高压制样方法和技术研究 [J]. 光谱学与光谱分析, 2013, 33(12): 3402-3407.
ZHANG Qin1, YU Zhao-shui1*, LI Xiao-li2, LI Guo-hui1 . Study on High Pressure Sample Preparation Method for Pressed Powder Pellet and Its Application in X-Ray Fluorescence Spectrum Analysis . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2013, 33(12): 3402-3407.
[1] ZHANG Qin, FAN Shou-zhong, PAN Yan-shan, et al(张 勤 , 樊守忠，潘宴山，等). Rock and Mineral Analysis(岩矿测试)，2004, 23(1): 19. [2] LI Guo-hui, XU Li, ZHANG Yun-guo(李国会，许 力，张运国). Rock and Mineral Analysis(岩矿测试)，1987, 6(1): 15. [3] LI Guo-hui(李国会). Geological Laboratory(地质实验室), 1997, 13(4): 225. [4] Kikkert J. Spectrochimica Acta. 1983, 33B(56): 809. [5] LUO Li-qiang, ZHAN Xiu-chun, LI Guo-hui(罗立强，詹秀春，李国会). X-Ray Fluorescence Spectrometer(X射线荧光光谱仪). Beijing: Chemical Industry Press(北京：化学工业出版社), 2008, 107. [6] Mortimire D M, Romans P A, Tews J L. Norelco Reporter, 1954, 1: 107. [7] Gunn E L. Anal. Chem., 1957, 29: 184. [8] Zyl C V. X-Ray Spectrom., 1982, 11(1): 29. [9] CAI Shu-lin, LI Jie, LU Yi, et al(才树林，李 杰，陆 义，等). Chinese Journal of Analysis Laboratory(分析试验室), 1986, 5(12): 5. [10] CHEN Yong-jun, LIU Yu-jian(陈永君，刘玉建). Chinese J. Anl. Chem.(分析化学), 1991, 19(5): 560. [11] Potts P J, Webb P C, Waston J S. X-Ray Spectrom., 1984, 13: 2. [12] Bower N W, Valentine G. X-Ray Spectrom., 1986, 15(1): 73. [13] LU Shao-lan, LI Shi-zhen, HAO Gong-zhang，et al(陆少兰，李世珍，郝贡章，等). Chinese Journal of Analysis Laboratory(分析试验室), 1995, 14(1): 66. [14] Pearce Bill C, Hill John W F, Kerry Lan. Analyst, 1990, 115(11): 1397. [15] LUO Chong-qing, XIA Hong-wei, FAN Jian(罗重庆，夏红卫，范 键). Chinese Journal of Analysis Laboratory(分析试验室), 1995, 14(5): 75. [16] Demir F, Budak G, Baydas E,Sahin Y. Nuclear Instruments and Methods in Physics Research., 2006, 243: 423. [17] CHEN Yue, LUO Wu-qian, MU Qing, et al(陈 岳，罗武千，穆 青，等). Rock and Mineral Analysis(岩矿测试)，2013，32(1): 66.
