高稀释比熔融-X射线荧光光谱法分析硅酸盐岩石样品中18种组分

选取土壤、水系沉积物、岩石、超基性岩、黏土等标准物质，应用混合溶剂与样品质量比为14：1的高稀释比方法熔融制备测试样品，拟合校准曲线，建立X射线荧光光谱（XRF）同时测定硅酸盐岩石样品中18种组分（SiO₂、Al₂O₃、TFe₂O₃、MgO、CaO、K₂O、Na₂O、TiO₂、BaO、MnO、P₂O₅、Cr₂O₃、V₂O₅、Rb、Sr、Zr、Cu、Ni）的快速分析方法.应用帕纳科Eagon2全自动高频电感熔样机，称取7.0000 g（45Li₂B₄O₇+10LiBO₂+5LiF）混合溶剂与0.5000 g样品混合均匀，分别加入氧化剂饱和硝酸铵溶液2滴，脱模剂饱和溴化锂溶液4滴，于700℃先预氧化4 min，再1 120℃熔融9 min制备样片，自然冷却至室温.此熔样方法能保证样品中待测组分熔化完全，并制得表面光滑平整的样片.用国家标准物质验证，测试结果的准确度和精密度均符合《地质矿产实验室测试质量管理规范》（DZ/T 0130-2006）要求.

DETERMINATION OF EIGHTEEN COMPONENTS IN SILICATE ROCKS BY X-RAY FLUORESCENCE SPECTROMETRY WITH HIGH DILUTION RATIO FUSION SAMPLE PREPARATION

The paper introduces a rapid analysis method of X-ray fluorescence spectrometry (XRF) to determine 18 components (SiO₂, Al₂O₃, TFe₂O₃, MgO, CaO, K₂O, Na₂O, TiO₂, BaO, MnO, P₂O₅, Cr₂O₃, V₂O₅, Rb, Sr, Zr, Cu and Ni) in silicate samples. Selecting the reference materials such as soil, stream sediments, rocks of national first-class standard material, ultrabasic rocks and clay, the method applies high dilution ratio (14:1) of mixed solvent to sample mass for fusion sample preparation and fits the calibration curve. Through Eagon2 automatic high frequency inductance fusion machine, 7.0000 g of mixed solvent (45Li₂B₄O₇+10LiBO₂+5LiF) and 0.5000 g of sample are mixed uniformly, adding 2 drops of saturated ammonium nitrate solution as oxidant and then 4 drops of saturated lithium bromide solution as release agent, followed by preoxidation at 700℃ for 4 min and fusion at 1120℃ for 9 min, and finally cooling naturally to room temperature for sample preparation. The above fusion method can ensure that the components to be measured are completely melted and the sample surface is smooth and flat. Verified by national standard substances, the accuracy and precision of test results are in line with the requirements of Quality Management Code for Laboratory Testing of Geology and Mineral Resources (DZ/T 0130-2006).