自动粉末压片-能量色散X射线荧光光谱法快速测定水泥生料组分  

Rapid Determination of Cement Raw Material Components by Energy Dispersive X-ray Fluorescence Spectroscopy with Automated Powder Pressing

作　　者：孙圣君 喻国安 向征宇 黄先旺 SUN Shengjun;YU Guoan;XIANG Zhengyu;HUANG Xianwang(School of Automotive and Mechanical Engineering,Changsha University of Science and Technology,Changsha,Hunan 410114,China;Hunan Sundy Science and Technology Co.,Ltd.,Changsha,Hunan 410205,China)

机构地区：[1]长沙理工大学汽车与机械工程学院,长沙410114 [2]湖南三德科技股份有限公司,长沙410205

出　　处：《中国无机分析化学》2023年第9期999-1006,共8页Chinese Journal of Inorganic Analytical Chemistry

基　　金：国家自然科学基金资助项目(61871060)。

摘　　要：为了解决荧光分析测定水泥生料组分时前处理时间过长、重复性和准确度差、多元素分析效率低以及粉尘污染等问题,通过升级自动制样流程,优化助剂添加方式,设计原料清洗功能,调整荧光分析仪器及测试条件,建立了自动粉末压片制样,并用能量色散X射线荧光光谱仪(EDXRF)快速测定各组分含量的方法。自动进样方法的应用确保了磨制物料中样品和助剂比例的稳定性,提高了样片的一致性。使用自动研磨压片机进行连续压片可得到表面光滑均匀且未出现开裂的样片,并且仅需进行一次原料清洗即可消除不同样品间的交叉污染。相较于传统的粉末压片-波长色散X射线荧光光谱法(WDXRF),自动压片法将样品制备时间缩短至360 s,荧光分析计数时间缩短至90 s,并消除了粉尘污染和人为因素对荧光分析结果的影响。针对四个含量不同水平的生料样品进行的准确度实验表明,测试结果与化学分析法的测定值基本一致,且各组分含量的最大误差均符合国家标准要求。对同一生料进行精密度实验(RSD,n=10)的结果表明,生料中主要组分CaO、SiO_(2)、Al_(2)O_(3)、Fe_(2)O_(3)的相对标准偏差分别为0.054%、0.14%、0.60%、0.31%,最大偏差为Na_(2)O的4.4%,方法表现出良好的稳定性。因此,进一步明确了生料快速制样与能量色散荧光分析的最佳条件,方法准确度及重复性满足日常分析检测要求,对水泥生料组分快速检测具有指导意义。In order to address the issues of long preprocessing time,poor repeatability and accuracy,low efficiency of multi-element analysis,and dust pollution in the fluorescence analysis of cement raw material components,an automatic powder tabletting sample preparation method was established.The automatic sample preparation process was upgraded,the additive addition method was optimized,the raw material cleaning function was designed,the fluorescence analysis instrument and testing conditions were adjusted.Then the rapid determination of each component content was achieved by energy-dispersive X-ray fluorescence spectroscopy(EDXRF).The application of the automatic sample injection method ensured the stability of the sample and aid ratio in the ground material,and improved the consistency of the sample pieces.The use of automatic grinding and pressing machine for continuous pressing produced smooth and uniform samples without cracking,and cross-contamination between different samples was eliminated with only one raw material cleaning.Compared with the traditional powder pressing-wavelength dispersive X-ray fluorescence spectroscopy(WDXRF)method,the preparation time of automatic compression method for the samples was reduced to 360 s,and the fluorescence analysis counting time was reduced to 90 s.Moreover,dust pollution and human factors on the fluorescence analysis results were eliminated.Accuracy experiments on four raw material samples with different content levels showed that the test results were basically consistent with the determination values by the chemical analysis method,and the maximum error of each component content met the national standard requirements.Precision experiments(RSD,n=10)on the same raw material showed that the relative standard deviations of the main components CaO,SiO_(2),Al_(2)O_(3)and Fe_(2)O_(3)were 0.054%,0.14%,0.60%and 0.31%,respectively,with a maximum deviation of Na_(2)O being 4.4%.This method showed good stability.Therefore,the optimal conditions for rapid sample preparation of raw ma

关 键 词：粉末压片制样 能量色散X射线荧光光谱法 水泥 生料 

分 类 号：O657.34[理学—分析化学] TH744.15[理学—化学]