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采用低压聚乙烯镶边垫底的粉末压饼法制样,X射线荧光光谱法直接测定了地质样品中痕量元素As、Ga、Sc、La、Y、Ce、W、Mo、Sn、Co和Pb。讨论了背景校正、谱线重叠校正、基体效应校正和仪器漂移校正等问题。利用理论α系数代替经验系数,使方法具有较高的准确度和较低的检出限。所测11个元素的检出限在(0.30~2.02)×10-6水平,精度(RSD,n=11)在0.95%~13.0%。方法经国家一级标准物质分析验证,结果与标准值相符。
The method of XRD was used to directly determine the trace elements As, Ga, Sc, La, Y, Ce, W, Mo, Sn, Co and Pb in geological samples by the method of powder compacting with low pressure polyethylene trimmed bottom. The issues of background correction, line overlap correction, matrix effect correction and instrument drift correction are discussed. Using the theoretical α coefficient instead of the empirical coefficient, the method has higher accuracy and lower detection limit. The detection limits of the 11 elements ranged from (0.30 ~ 2.02) × 10-6, and the accuracy (RSD, n = 11) ranged from 0.95% to 13.0%. The method is verified by the national first-level reference material and the result is consistent with the standard value.