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X-射线荧光光谱法快速测定半钢发热剂中Si,P,S
引用本文:段家华,赵征宇,马林泽,李 洁,杨文龙,严 海,何晓凤,孔翠芬,杨发文.X-射线荧光光谱法快速测定半钢发热剂中Si,P,S[J].中国无机分析化学,2014,4(2):54-57.
作者姓名:段家华  赵征宇  马林泽  李 洁  杨文龙  严 海  何晓凤  孔翠芬  杨发文
作者单位:昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302;昆明钢铁集团责任有限公司 质量计量检测中心,云南 安宁 650302
摘    要:目前,国内没有关于半钢发热剂的国家标准检测方法,只能根据组分范围分别检测各个组分,不仅耗时而且使用的大量化学试剂对环境造成污染。故研究了X-射线荧光光谱法快速测定半钢发热剂中Si,P,S的方法。采用粉末压片制样,研究其制样条件,包括磨样时间、压样时间和压力对测定结果的影响。采用其它方法定值提供的检测样品,作为X-射线荧光光谱法内控标准样品,采用经验系数法进行基体校正,通过解谱拟合建立校准曲线,校准曲线建立后仪器建立漂移校正程序。实验结果精密度好,各元素的相对标准偏差在0.15%~1.3%。准确度满足生产需求,实验方法可用于快速检测半钢发热剂化学组分。

关 键 词:X-射线荧光光谱法  快速测定  半钢发热剂  方法研究
收稿时间:1/2/2014 12:00:00 AM
修稿时间:2014/3/26 0:00:00

Determination of Si, P and S in the Semi-steel Heating Agents byX-ray Fluorescence Spectrometry
DUAN Jiahu,ZHAO Zhengyu,MA Linze,LI Jie,YANG Wenlong,YAN Hai,HE Xiaofeng,KONG Cuifen and YANG Fawen.Determination of Si, P and S in the Semi-steel Heating Agents byX-ray Fluorescence Spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2014,4(2):54-57.
Authors:DUAN Jiahu  ZHAO Zhengyu  MA Linze  LI Jie  YANG Wenlong  YAN Hai  HE Xiaofeng  KONG Cuifen and YANG Fawen
Institution:Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China;Quality and Calibration Testing Center, Kunming Iron and Steel Group Co., Ltd. , Anning, Yunnan 650302 ,China
Abstract:Currently, there is no national standard analysis method for semi-steel heating agents. The components have to be detected separately according to their composition range, which is not only time consuming but also generates a large number of chemical pollution to environment. Therefore, a rapid detection method for analyzing the component of semi-steel heating agents need to be investigated and in this paper, X-ray fluorescence spectrometry technique was used to established the method to analyze Si,P and S in semi-steel heating agents. Samples were made into pellets using pressed powder pellet technique. The effects of sample preparation conditions, including grinding time, pressing time and pressing pressure on the measurement results were investigated. The samples provided were valued by other methods and used as X-ray fluorescence spectrometry internal control standards. The empirical coefficient method was used to do matrix correction. A calibration curve was established by spectral fitting and used to build drift correction procedures. Experimental results have good precision and the relative standard deviation for each element is about 0.15%-1. 3%. The accuracy of the method can meet the production needs and the experimental method can be used by companies for rapid detection of chemical compositions of semi-steel heating agents.
Keywords:X-ray  determine  semi-steel heating agent  research methods
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