高氯酸脱水重量法测定锰硅合金中硅
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摘要
锰硅合金中硅含量对炼钢过程用料配比具有重要指导作用,也是交易计价的重要指标之一,因此,快速准确地测定锰硅合金中硅显得尤为重要。采用盐酸、硝酸分开加入的模式分解样品,通过冒两次高氯酸烟使样品中碳炭化,再加入过氧化氢可得到清澈溶液利于过滤及灼烧。试验结果表明,滤液中二氧化硅含量与二氧化硅沉淀中杂质含量相当,由此引入的系统误差可相互抵消,实际工作中可不予校正。按照实验方法测定4个锰硅合金标准物质中硅,结果的相对标准偏差(RSD)为0.47%~0.69%,测定值与认定值相符。
The content of silicon in manganese silicon alloy has important guiding significance to the ratio of the materials in steel-making process.Moreover,it is also one of important indexes for the valuation in trade.Therefore,it is critical to rapidly and accurately determine the silicon content in manganese-silicon alloy.The sample was decomposed by adding hydrochloric acid and nitric acid separately.The carbon in samples was carbonized through perchloric acid fuming for twice.Then hydrogen peroxide was added to obtain clear solution,which was advantageous to filtration and calcinations.The experimental results showed that the content of silicon dioxide in filtrate was equivalent to the impurity content in silicon dioxide precipitation.Therefore,the introduced system error could be cancelled out,and the correction was not necessary in practical test.The content of silicon in four certified reference materials of manganese-silicon alloy was determined according to the experimental method.The relative standard deviations(RSD)ranged from 0.47% to 0.69%.The found results were consistent with the certified values.
The content of silicon in manganese silicon alloy has important guiding significance to the ratio of the materials in steel-making process.Moreover,it is also one of important indexes for the valuation in trade.Therefore,it is critical to rapidly and accurately determine the silicon content in manganese-silicon alloy.The sample was decomposed by adding hydrochloric acid and nitric acid separately.The carbon in samples was carbonized through perchloric acid fuming for twice.Then hydrogen peroxide was added to obtain clear solution,which was advantageous to filtration and calcinations.The experimental results showed that the content of silicon dioxide in filtrate was equivalent to the impurity content in silicon dioxide precipitation.Therefore,the introduced system error could be cancelled out,and the correction was not necessary in practical test.The content of silicon in four certified reference materials of manganese-silicon alloy was determined according to the experimental method.The relative standard deviations(RSD)ranged from 0.47% to 0.69%.The found results were consistent with the certified values.
引文
[1]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 5686.2-2008锰铁、锰硅合金、氮化锰铁和金属锰硅含量的测定钼蓝光度法、氟硅酸钾滴定法和高氯酸重量法[S].北京:中国标准出版社,2008.
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[3]王爱国.碱熔-氟硅酸钾滴定法测定锰硅洗渣中的硅含量[J].铁合金,2015(8):46-48.WANG Ai-guo.Alkali fusion-potassium fluorosilicate titration determination of Si content of washery slag from ferromanganese-silicon[J].Ferro-Alloys,2015(8):46-48.
[4]贺红侠,王洁源,许鸿英,等.氟硅酸钾容量法测定硅锰合金中硅含量的影响因素[J].河北冶金,2015(2):71-72.HE Hong-xia,WANG Jie-yuan,XU Hong-ying,et al.Factors affecting measurement of silicon content in silicon-manganese alloy with potassium fluosilicate volumetric method[J].Hebei Metallurgy,2015(2):71-72.
[5]张爱华.锰硅合金中硅的测定[J].理化检验:化学分册,2000,36(2):93-94.ZHANG Ai-hua.Determination of silicon in manganesesilicon alloy[J].Physiscal Testing and Chemical Analysis Part B:Chemical Analysis,2000,36(2):93-94.
[6]李建民.熔融制样-X射线荧光光谱法测定硅锰合金中的硅、锰和磷[J].理化检验:化学分册,2016,52(4):484-486.LI Jian-min.Determination of silicon,manganese and phosphorus in silicon-manganese alloy with fusion sampling X-ray fluorescence spectrometry[J].Physiscal Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(4):484-486.
[7]邢文青,吴超超,王岩,等.X射线荧光熔融法测定锰系合金中硅、锰和磷含量[J].南方金属,2016(3):8-10.XING Wen-qing,WU Chao-chao,WANG Yan,et al.Determination of contents of Mn,Si and P in manganese ferroalloys by X-ray fluorescence spectrometer[J].Southern Metals,2016(3):8-10.
[8]游华,刘梅山,徐文荣.X射线荧光光谱法测定硅锰合金[J].福建分析测试,2001,10(1):1363-1365.YOU Hua,LIU Mei-shan,XU Wen-rong.XRF spectrometry of silicomanganese ferroalloy using pressed disc sampling of the sample powder[J].Fujian Analysis&Testing,2001,10(1):1363-1365.
[9]王剑云.X-荧光光谱法分析硅锰中的化学元素[J].浙江冶金,2013(3):44-45.WANG Jian-yun.Analysis of chemical elements in silicon-manganese with X-ray fluorescence spectrometry[J].Zhejiang Metallurgy,2013(3):44-45.
[10]刘伟,曹吉祥,郭云涛,等.熔融制样-X射线荧光光谱法测定硅锰合金中硅锰磷[J].冶金分析,2015,35(8):51-54.LIU Wei,CAO Ji-xiang,GUO Yun-tao,et al.Determination of silicon,manganese,phosphorus in silicon-manganese alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(8):51-54.