粉末压片-X射线荧光光谱法测定煤矸石中主量元素  

Determination of Major Elements in Coal Gangue by Powder Compaction-X-ray Fluorescence Spectrometry

作　　者：马彦斌 杨凡燕 董爱俊 刘颖 王鸿 马程 唐文涛 MA Yanbin;YANG Fanyan;DONG Aijun;LIU Ying;WANG Hong;MA Cheng;TANG Wentao(Ningxia Hui Autonomous Region Basic Geological Survey Institute(Ningxia Geology and Mineral Resources Center Laboratory),Yinchuan 750021,China)

机构地区：[1]宁夏回族自治区基础地质调查院(宁夏回族自治区地质矿产中心实验室),宁夏银川750021

出　　处：《宁夏工程技术》2023年第4期366-370,共5页Ningxia Engineering Technology

基　　金：宁夏回族自治区基础地质调查院(宁夏回族自治区地质矿产中心实验室)自筹资金项目。

摘　　要：煤矸石中的化学成分决定着煤矸石的利用方向及综合利用率,而传统的煤矸石检测方法过程繁琐、人工误差较大。为了快速准确地测定煤矸石中的主量元素,采用粉末压片法制样,选取与待测样品同一粒度、基体类似、各组分质量分数有梯度的高岭土及黏土标准样品作为校准样品系列,利用X射线荧光光谱法(XRF)测定校准样品系列中SiO_(2),Al_(2)O_(3),Fe_(2)O_(3),CaO,MgO,TiO_(2),K_(2)O,Na_(2)O,P_(2)O_(5),MnO的质量分数,以各组分的质量分数与其相对应的X射线荧光强度绘制校准曲线,并以此计算待测样品中各组分的质量分数。通过试验优化了粉末压片制样的粒度及压力,采用经验系数法对谱线重叠干扰和基体效应进行了校正。利用该检测方法对煤矸石样品进行精密度和准确度试验,结果表明,测定结果的精密度、准确度均满足行业标准《地质矿产实验室测试质量管理规范》(DZ/T 0130—2006)的要求。The chemical composition of coal gangue determines the direction of its utilization and the rate of comprehensive utilization.However,traditional methods for testing coal gangue are cumbersome and prone to significant human error.In order to rapidly and accurately determine the major elements in coal gangue,the powder pellet pressing method was used for sample preparation.Calibration sample series were selected from kaolin and clay standard samples with the same granularity,similar matrix,and gradient of mass fractions of each component as the samples to be tested.The mass fractions of SiO_(2),Al_(2)O_(3),Fe_(2)O_(3),CaO,MgO,TiO_(2),K_(2)O,Na_(2)O,P_(2)O_(5),and MnO in the calibration sample series were determined using X-ray fluorescence spectroscopy(XRF).Calibration curves were drawn based on the mass fractions and the corresponding X-ray fluorescence intensity,and these curves were used to calculate the mass fractions of each component in the samples to be tested.The granularity and pressure of powder pellet pressing were optimized through experimentation,and the empirical coefficient method was used to correct for spectral line overlap interference and matrix effects.The precision and accuracy of the coal gangue samples were tested using this detection method,and the results showed that both the precision and accuracy meet the requirements of the industry standard The Specification of Testing Quality Management for Geological Laboratories(DZ/T 0130—2006).

关 键 词：煤矸石 粉末压片 X射线荧光光谱法 主量元素 

分 类 号：O657.34[理学—分析化学] P575[理学—化学]