Modification of the Method of Componental Analysis of Coal Ash by XRFS
摘 要
样品以四硼酸锂和偏硼酸锂为熔剂,硝酸铵为氧化剂,溴化锂为脱模剂,采用玻璃状熔片法制样。选用标准样品及其标准样品间相混合配制的混合样品制作工作曲线,并以α系数和经验系数法校正元素谱线干扰和基体效应,用X射线荧光光谱法对煤灰中的二氧化硅、氧化铝、氧化铁、氧化钙、氧化镁、五氧化二磷、氧化钾、氧化钠、氧化钛、五氧化二钒、氧化锰和三氧化硫等12种主次组分进行测定。方法分析结果与化学法和电感耦合等离子体原子发射光谱法测定值相符;对同一样品按所建方法分别熔融制备10个熔片进行测定,各组分测定值的相对标准偏差(n=10)在0.06%~2.4%之间。
Abstract
Twelve components (i.e., SiO2, Al2O3, Fe2O3, CaO, MgO, P2O5, K2O, Na2O, TiO2, V2O5, MnO and SO3) in coal ash were determined by XRFS. The glassy melt of sample of coal ash was obtained by fusion with Li2B4O7 and LiBO2 as flax, NH4NO3 as oxidant and LiBr as demoulding agent. Standard working curves were prepared by using standard samples and mixtures of standard samples. Interferences due to matrix effects and overlapping of spectral lines were overcomed by the methods of α-coefficient and empirical coefficient. Results of 12 components obtained by the present method were found to check quite well with those obtained by chemical method and ICP-AES. Ten glassy melts were prepared from the same sample of coal ash and the 12 components were determined by the present method, values of RSD′s (n=10) found were in the range of 0.06%-2.4%.
中图分类号 O657.34
所属栏目 工作简报
基金项目
收稿日期 2012/3/6
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备注朱春要(1982-),男,安徽淮南人,工程师,主要从事冶金分析工作。
引用该论文: ZHU Chun-yao,NIAN Ji-qiang,LU Na-ping,ZHOU Qiang,GU Feng. Modification of the Method of Componental Analysis of Coal Ash by XRFS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(4): 439~441
朱春要,年季强,陆娜萍,周强,顾锋. X射线荧光光谱法测定煤灰成分的改进[J]. 理化检验-化学分册, 2013, 49(4): 439~441
被引情况:
【1】韩蔚,丁建军,梅一飞,马振珠, "X射线荧光光谱法测定石膏中11种元素的含量",理化检验-化学分册 51, 188-191(2015)
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参考文献
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【2】韩晓玉,李建军,于杰华.工业分析在煤炭炼焦中的作用[J].山西煤炭, 2008,28(2):52-53.
【3】边丽君.浅谈焦炭质量对高炉冶炼的影响[J].本钢技术, 2008(6):36-37.
【4】GB/T 212-2008煤的工业分析方法[S].
【5】GB/T 1574-2007煤灰成分分析方法[S].
【6】ASTM D4236-04Standard test method for major and minor elements in coal and coal ash by X-ray fluorescence[S].
【7】李国会.X射线荧光光谱测定硅酸盐中20个主次,痕量元素[J].光谱学与光谱分析, 1994,14(1):105-110.
【8】吴静,王富仲,许增平.熔融制样-X射线荧光光谱法测定铁矿石中主次成分[J].冶金分析, 2009,29(9):40-43.
【9】CSM 05119501-2006冶金用煤-硅、铝、铁、钙、镁、钠、钾磷、钛、锰等氧化物含量的测定 X射线荧光光谱法[S].
【10】李咏霞.X射线荧光经验系数法测定神东煤灰成分[J].煤质技术, 2006(3):36-38.
【11】SN/T 1599-2005煤灰中主要成分的测定 电感耦合等离子体原子发射光谱法[S].
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