粉末压片-X射线荧光光谱法测定高钛型高炉渣中化学成分
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摘要
应用粉末压片制样-X射线荧光光谱法测定了高钛高炉渣中SiO2、CaO、TiO2等8项化学组成。取过0.125mm筛孔的网筛样品,在25MPa压力下保持30s的条件下制成样片,供X射线荧光光谱分析。分析中选择工作电压为50kV,工作电流为40mA,解决了高含量组分(Si、Ca、Ti)所造成的信号与噪声不易有效分离的问题。按所提出方法分析了高、中、低不同含量的炉渣样品,所测得结果表明方法具有较好的精密度和准确性。与熔融制样-X射线荧光光谱法所测得结果相比,相对误差均在允许范围内。
X-ray fluorescence spectrometry(XRFS)with sample preparation by pressure powder molding was applied to the determination of 8 chemical components(including SiO2,CaO,TiO2 etc.)in high-titanium blast furnace slag.Powdered slag sample with granular size<0.125 mm was taken and pressed under 25 MPa for 30 sto give sample tablet for use in XRFS analysis.A higher working voltage of 50 kV and lower current of 40 mA were chosen for the X-ray tube,to solve the problem of dificulty in separation of analytical signals from interfering noise caused by the high-bearing elements of Si,Ca and Ti.Good precision and accuracy were shown by the results obtained in analysis of slag samples of high,medium and low contents of the analytes by the proposed method.As compared with the results found by XRFS with the fusion sample preparation,values of relative errors obtained were within the allowable limits.
X-ray fluorescence spectrometry(XRFS)with sample preparation by pressure powder molding was applied to the determination of 8 chemical components(including SiO2,CaO,TiO2 etc.)in high-titanium blast furnace slag.Powdered slag sample with granular size<0.125 mm was taken and pressed under 25 MPa for 30 sto give sample tablet for use in XRFS analysis.A higher working voltage of 50 kV and lower current of 40 mA were chosen for the X-ray tube,to solve the problem of dificulty in separation of analytical signals from interfering noise caused by the high-bearing elements of Si,Ca and Ti.Good precision and accuracy were shown by the results obtained in analysis of slag samples of high,medium and low contents of the analytes by the proposed method.As compared with the results found by XRFS with the fusion sample preparation,values of relative errors obtained were within the allowable limits.
引文
[1] YB/T 505.2-2007钒钛炉渣二氧化钛含量的测定滴定法[S].
[2] YB/T 505.3-2007钒钛炉渣三氧化二铝含量的测定滴定法[S].
[3] YB/T 505.4-2007钒钛炉渣氧化钙、氧化镁含量的测定滴定法[S].
[4] YB/T 505.7-2007钒钛炉渣五氧化二钒含量的测定滴定法[S].
[5]丁美英,乔宇,张桂梅.电感耦合等离子体原子发射光谱法测定炉渣中10种化学成分[J].冶金分析,2011,31(9):38-41.
[6] YB/T 4177-2008炉渣X射线荧光光谱分析方法[S].
[7]张德贵.熔融法在高炉渣X射线荧光光谱分析中的应用[J].冶金标准化与质量,2013(2):35-37.
[8]杨新能,冯宗平.熔融制样-X射线荧光光谱法测定钒钛渣中10种组分[J].冶金分析,2018,38(7):57-62.
[9]冯钦忠,陈改明.粉末压片法-能量色散X荧光光谱法快速测定高炉渣[J].冶金分析,1999,19(3):1-9.
[10]吴子良,李树金.X射线荧光光谱法同时测定高炉渣中9元素[J].冶金标准化与质量,2013,51(4):25-26.
[11]孙丽,李德才.X荧光光谱分析法测定高炉炉渣[J].冶金动力,2006,118(6):79-80.
[12]杨宗强,梁文.岛津多道X射线荧光光谱仪测定高炉渣中硅钙镁铝钛[J].冶金标准化与质量,2006,44(4):15-16.
[13]武映梅,罗惠君,林丽芳,等.X射线荧光光谱法测定冶金炉渣中9种成分[J].冶金分析,2010,30(8):7-11.
[14]罗立强,詹秀春,李国会.X射线荧光光谱仪[M].北京:化学工业出版社,2008.
[2] YB/T 505.3-2007钒钛炉渣三氧化二铝含量的测定滴定法[S].
[3] YB/T 505.4-2007钒钛炉渣氧化钙、氧化镁含量的测定滴定法[S].
[4] YB/T 505.7-2007钒钛炉渣五氧化二钒含量的测定滴定法[S].
[5]丁美英,乔宇,张桂梅.电感耦合等离子体原子发射光谱法测定炉渣中10种化学成分[J].冶金分析,2011,31(9):38-41.
[6] YB/T 4177-2008炉渣X射线荧光光谱分析方法[S].
[7]张德贵.熔融法在高炉渣X射线荧光光谱分析中的应用[J].冶金标准化与质量,2013(2):35-37.
[8]杨新能,冯宗平.熔融制样-X射线荧光光谱法测定钒钛渣中10种组分[J].冶金分析,2018,38(7):57-62.
[9]冯钦忠,陈改明.粉末压片法-能量色散X荧光光谱法快速测定高炉渣[J].冶金分析,1999,19(3):1-9.
[10]吴子良,李树金.X射线荧光光谱法同时测定高炉渣中9元素[J].冶金标准化与质量,2013,51(4):25-26.
[11]孙丽,李德才.X荧光光谱分析法测定高炉炉渣[J].冶金动力,2006,118(6):79-80.
[12]杨宗强,梁文.岛津多道X射线荧光光谱仪测定高炉渣中硅钙镁铝钛[J].冶金标准化与质量,2006,44(4):15-16.
[13]武映梅,罗惠君,林丽芳,等.X射线荧光光谱法测定冶金炉渣中9种成分[J].冶金分析,2010,30(8):7-11.
[14]罗立强,詹秀春,李国会.X射线荧光光谱仪[M].北京:化学工业出版社,2008.