粉末压片-波长色散X射线荧光光谱法测定地球化学样品中氯的方法研究

The Method Study on Determination of Chlorine in Geochemical Samples by Wavelength Dispersive X-ray Fluorescence Spectrometry with Pressed Powder

在对比已有相关分析方法的基础上,建立了粉末压片-波长色散X射线荧光光谱法测定地球化学样品中氯元素的分析方法。采用岩石、沉积物和土壤等78种国家一级地球化学标准物质作为校准系列建立校准曲线;利用经验系数法进行基体效应校正,利用含量校正法进行谱线重叠干扰校正;总结了地球化学样品中氯元素测定值随测定次数的变化规律及原因。结果表明:氯的检出限为7.95μg/g;分析3种国家一级地球化学标准物质12次,得到测定值的相对标准偏差均小于10%;采用国家一级地球化学标准物质验证方法准确度,测定值与标准物质认定值相吻合,测定平均值与标准物质认定值的对数差值的绝对值(∆lgω)均小于或等于0.02,满足多目标区域地球化学调查规范的要求。

Based on comparing the existing correlation analysis methods,a method for the determination of chlorine in geochemical samples by wavelength dispersion X-ray fluorescence spectrometry with pressed powder was established.Seventy eight types of national first-class geochemical standard substances including rock,sediment and soil were used as calibration series to establish calibration curves.The matrix effect was corrected by empirical coefficient method,and the spectra overlapping interference was corrected by content correction method.This paper summarizes the variation rule and reason of the measured values of chlorine with the determination times in geochemical samples.The results indicated that detection limit of chlorine was 7.95μg/g;three national first-class geochemical reference materials were analyzed twelve times,the relative standard deviations(RSD)were less than 10%;The accuracy of the method was verified by the national first-class geochemical reference materials,and the measured values were consistent with the certified values of the reference materials,the absolute values the logarithm difference between the measured average values and certified values of reference materials were all less than or equal to 0.02.The proposed method could meet the requirements of multi-objective regional geochemical survey specifications.