X射线荧光光谱法测定镁质耐火材料及其原料中10种成分  

Determination of ten components in magnesia refractory materials and raw materials by X-ray fluorescence spectrometry

作　　者：赵恩好[1] 岳明新[1] 周国兴[1] 肖刚[1] 张泉[1] 刘新 

机构地区：[1]沈阳地质矿产研究所,辽宁沈阳110032 [2]东煤地质局沈阳测试中心,辽宁沈阳110032

出　　处：《冶金分析》2013年第7期62-67,共6页Metallurgical Analysis

摘　　要：采用熔融制样,建立了镁质耐火材料(制品镁砖等)及其原料(水镁石,原料镁砂等)中MgO、Al2O3、SiO2、CaO、P2O5、TiO2、TFe2O3、Na2O、K2O、MnO的X射线荧光光谱分析方法。与以往方法相比,增加了Na2O、K2O的含量测试,为最终对于MgO的准确测试提供了依据。对高镁样品(MgO含量大于90%)的熔剂体系、样品与熔剂稀释比等方面进行了考察,同时对水镁石、菱镁矿等高烧失量样品的烧失量校正进行了探讨。采用国家标准样品GBW07105和高纯镁砂配制的系列校准样品来建立校准曲线,用经验系数法回归校正共存元素间的吸收增强效应。方法的检出限在0.031%～0.45%之间。对样品进行了精密度试验,各成分的相对标准偏差(RSD,n=10)在0.31%～3.4%之间。对人工合成样品及标准样品进行测试,结果与湿法测定结果吻合。The sample was prepared by fusion method.The analysis of MgO,Al2O3,SiO2,CaO,P2O5,TiO2,TFe2O3,Na2O,K2O and MnO in magnesia refractory materials（magnesium brick products）and raw materials（brucite and raw magnesite etc.）by X-ray fluorescence spectrometry was established.Compared with previous methods,the content test of Na2O and K2O was added.It provided basis for the final accurate test of MgO.The flux system for high magnesium sample（the content of MgO was higher than 90%）as well as the dilution ratio between sample and flux were discussed.Meanwhile,the correction of loss on ignition for samples with high ignition loss（such as brucite and magnesite） was also investigated.The calibration curves of the method were established with series calibration samples prepared by national standard sample GBW07105 and high-purity magnesia.The absorption enhancement effect among coexisting elements was regressed and corrected by empirical coefficient method.The detection limit of method was between 0.031%and 0.45%.The precision test of sample was conducted.The relative standard deviation（RSD,n=10） of each components was 0.31%-3.4%.Synthetic samples and CRM were tested,and the results were consistent with those obtained by wet method.

关 键 词：X射线荧光光谱法 熔融制样 镁质耐火材料及其原料 烧失量 

分 类 号：O657.34[理学—分析化学]