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《Rock and Mineral Analysis》 2002-01
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Determination of Trace Br, Cl and S in Rock, Soil and Sediment Samples by X-Ray Fluorescence Spectrometry

ZHAN Xiu chun 1,CHEN Yong jun 1,ZHENG Miao zi 1, WANG Jian 1,LI Ying chun 1,LI Bing 1,ZHANG Qin 2 (1.National Research Center of Geoanalysis, Beijing 100037, China; 2.Institute of Geophysical and Geochemical Exploration,Chinese Academy of  
An X ray fluorescence spectrometric method has been developed for the determination of trace Br, Cl and S in rock, soil and sediment samples. Pressed powder pellets were used for measurements. Calibration was carried out using Chinese National Standard Materials with similar matrix elemental compositions to the samples. For Br, two matrix correction techniques, namely the scattering background internal standard method (in which raw peak intensity instead of net peak intensity is used) and the commonly used target Compton scattering internal standard method, were tested. And the former was found out more effective when the analyte concentration levels are near the detection limits. The precision is generally better than 10% RSD and the relative deviation of the average (6 measurements) is better than 24%. The fact that the measured concentration of S and Cl became higher and higher when the same sample pellet was repeatedly measured, brought about some analytical problems. Thus only newly prepared sample pellets can be used for S and Cl analysis. For Cl analysis, direct correlation generally exists between its concentration and XRF intensity. Matrix correction is needed only when the sample contains extremely high concentration of Ca. The precision is generally better than 5% RSD and the relative deviation of the average (6 measurements) is better than 25%. S is the most problematic element to analyze. The precision is really good with 0.87%~5.6% RSD( n =6).But the poor relative deviation (36%, some even worse) excludes its use in precise analysis. Extensive experiments were conducted in finding out the factors affecting the S accuracy. And it was concluded that the mineral effect plays the most important role. The detection limits of this method are 0.43, 2.2 and 5.8 μg/g for Br, S and Cl respectively.
【Fund】: 国土资源部地质大调查项目 (DKD 990 40 17)
【CateGory Index】: O657.3
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