Determination of Major and Minor Components in Coal Ash by X-Ray Fluorescence Spectrometry Combined with Melting Method for Sample Preparation
摘 要
在铂金坩埚中依次加入4.000 0 g无水四硼酸锂,0.250 0 g试样,0.250 0 g钴内标试剂,搅拌均匀,再用3.000 0 g无水四硼酸锂覆盖在表面,加入1 000 g·L-1溴化锂溶液0.25 mL后,在电加热自动熔样机中于650℃预氧化10 min后,在1 080℃前置2 min,熔融17 min,后置3 min制得熔片,在所选仪器工作条件下测定煤灰中主次成分的含量。选用12份经国家标准方法定值的煤灰样品和两份铁矿石标准样品作为校准样品绘制标准曲线,采用经验系数法和理论α系数法对曲线进行基体校正和谱线重叠干扰校正。采用试验方法对煤灰样品中各组分进行测定,所得结果和标准方法测得值一致,测定值的相对标准偏差(n=11)在0.23%~5.3%之间。
Abstract
4.000 0 g of anhydrous lithium tetraborate, 0.250 0 g of the sample, and 0.250 0 g of Co internal standard were added into a platinum crucible successively. The mixture was stirred well, and then covered with 3.000 0 g of anhydrous lithium tetraborate on the surface. After 0.25 mL of 1 000 g·L-1 lithium bromide solution was added, the mixture was pre-oxidized at 650℃ for 10 min in an electric heating auto-melting sampler, and then placed at 1 080℃ for 2 min, melted for 17 min, and set for 3 min to obtain a fuse, for determination of major and minor components in the coal ash sample under selected working conditions. Twelve tandard coal ash samples determined by national stanard method and two iron ore standard samples were used as the calibration samples to draw the calibration curves. The matrix correction and spectral line overlap interference correction were performed by using the empirical coefficient method and theoretical α coefficient method. The components of the coal ash samples were determined by the proposed method, giving results were consistent with that obtained by the standard method, and RSDs (n=11) in the range of 0nent; coal ash
中图分类号 O657.34 DOI 10.11973/lhjy-hx201809012
所属栏目 工作简报
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收稿日期 2017/8/6
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备注邢文青,高级工程师,主要从事X射线荧光光谱分析应用工作,478547701@qq.com
引用该论文: XING Wenqing,YE Yufeng,WU Chaochao,WANG Yan,LIN Lifang. Determination of Major and Minor Components in Coal Ash by X-Ray Fluorescence Spectrometry Combined with Melting Method for Sample Preparation[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(9): 1049~1053
邢文青,叶玉锋,吴超超,王岩,林丽芳. 熔融法制样-X射线荧光光谱法测定煤灰中主次成分的含量[J]. 理化检验-化学分册, 2018, 54(9): 1049~1053
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参考文献
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【13】李小莉,安树清,徐铁民,等.熔片制样-X射线荧光光谱法测定煤灰样品中主次量组分[J].岩矿测试, 2009,28(4):385-387.
【2】傅永宁.40年来我国炼铁焦炭的研究概况[J].炼铁, 1989(5):32-34.
【3】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.
【4】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.
【5】GB/T 1574-2007煤灰成分分析方法[S].
【6】李国会,卜维,樊守忠,等.熔融法X射线荧光光谱法测定硅酸盐样品中的硫等20个元素[J].光谱学与光谱分析, 1994,14(1):105-110.
【7】李国会.X射线荧光光谱法测定橄榄岩主次痕量元素[J].光谱实验室, 1997,14(6):32-35.
【8】李国会.X射线荧光光谱法测定铬铁矿中主次量元素[J].岩矿测试, 1999,18(2):131-134.
【9】欧阳伦熬.X射线荧光光谱法测定多种铁矿和硅酸盐中主次量组分[J].岩矿测试, 2005,24(4):303-306.
【10】张勤.射线荧光光谱法测定化探样品中主、次和痕量组分[J].理化检验-化学分册, 2005,41(8):547-552.
【11】杨艳,李洁,张惠忠.X射线荧光光谱法测定煤灰成分[J].武钢技术, 2007,45(6):32-34.
【12】宋义,郭芬,谷松海.射线荧光光谱法同时测定煤灰中种成分[J].光谱学与光谱分析, 2008,28(6):1430-1434.
【13】李小莉,安树清,徐铁民,等.熔片制样-X射线荧光光谱法测定煤灰样品中主次量组分[J].岩矿测试, 2009,28(4):385-387.
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