高压制样X-射线荧光光谱法测定煤样品中17种元素和灰分  

Determination Multi-Elements and Ash in Coal Sample by X-Ray Fluorescence Spectrometer with High Pressure Pelletised Sample

作　　者：李小莉[1] 安树清[1] 于兆水[2] 白金峰[2] 张勤[2] 

机构地区：[1]天津地质调查中心,天津300171 [2]中国地质科学院地球物理地球化学研究所,廊坊065000

出　　处：《分析化学》2014年第2期283-287,共5页Chinese Journal of Analytical Chemistry

基　　金：国家重大科学仪器设备开发专项(No.2012YQ0076);中国地质大调查项目(No.1212011120277);物化探所基本科研业务费项目(No.AS2012J02)资助~~

摘　　要：采用自制的高压制样模具,在1400 kPa压力下直接压制煤样品,解决了由于煤样品粘结性差难以直接压制成型的难题。用电子显微镜对高压样片(1400 kPa)和常规压片(400 kPa)作了表面形态的比较,高压制备的样片表面致密、平整、光滑、不掉粉末。由于煤国家标准样品中定值的元素少,为了增加煤标样中可测定元素,以ICP-AES多次分析结果的平均值作为标准值,用高压制样建立了波长色散X射线荧光光谱测定煤样品中17个主次微量元素的分析方法,绝大部分组分的检出限较常规压力制备的样品有所改善,大部分组分的精密度都低于1%,制样的重现性好,X荧光的测定值与化学值基本相符。特别指出的是:使用SiKα测量强度和煤样品中的灰分含量建立的校准曲线,其RMS为0.9441,可直接用于测定煤样品中的灰分。The high pressure pelletizing technique for coal was researched with self-designed high-pressure pelletised mould. The coal sample can be directly briquetted without binder with the introduction of a high- pressure （1400 kPa） sample preparation technique. Under the high-pressure, the surface of the sample is more compacted, smooth and without falling of powder. The available value of the national coal CRM was limited, and in order to increase the assayed elements, the multitimes ICP measured value of CRM of coal was used as certified value to establish 17 major, minor and trace elements calibrations by WDXRF with high- pressure sample preparation. The detection limit of most component of coal sample prepared by high-pressure was much lower compared with routine sample preparation. The precision of the most component was lower than 1%, which indicated that the reproduction of the sample preparation was perfect. The determined value by WDXRF was basically coincided with chemical value. Particularly the calibration with intensity of silicon versus the content of the ash is created, the RMS is 0. 9441 and it can be used to measure the ash in the coal sample directly.

关 键 词：高压制样 煤 X-射线荧光光谱 

分 类 号：TQ533[化学工程—煤化学工程] O657.34[理学—分析化学]