ICP-AES法测定高钛渣中氧化钙、氧化镁、三氧化二铝等元素
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摘要
高钛渣中各元素分析一般采用行业标准方法,流程长、步骤繁琐、效率低。本方法采用ICP-AES测定高钛渣中三氧化二铝、氧化镁、氧化钙、钠、锰、五氧化二钒和三氧化二铁的含量,方法简单快速、准确有效,能满足冶金分析要求。以盐酸、硝酸、氢氟酸、高氯酸、硫酸溶解样品。试验了样品基体及共存元素之间的干扰影响,选择元素较佳分析谱线和仪器工作参数。运用基体匹配和同步背景校正相结合的方式消除基体影响。方法的检测限(3s)在0.001～0.030 mg/L范围内,回收率在97.4%～108.2%之间,相对标准偏差(n=12)小于2.5%。
The analysis of elements in high titanium slag generally adopts the industry standard method, but it is long process, cumbersome steps, low efficiency. This method uses ICP-AES to determine the content of aluminum trioxide, magnesium oxide, calcium oxide, sodium, manganese, vanadium pentoxide and ferric oxide in high titanium slag. The method is simple, rapid, accurate and effective, and can meet the requirements of metallurgical analysis.The samples were dissolved by mixed acid of HCl+HNO_3+HF+HClO_4+H_2SO_4, and test conditions for the sample interfering effects of the titanium matrix and coexisted elements, Elements were determined by selecting the optimum analysis spectrum line and suitable working parameters of instrument, by the use of the substrate matching and the synchronized background correction spectral interference and matrix effect were eliminated.The detection limits,0.001 mg/L-0.030 mg/L, RSD(n+12) < 2.5,and the recovery rates were97.4% ～ 108.2%.
The analysis of elements in high titanium slag generally adopts the industry standard method, but it is long process, cumbersome steps, low efficiency. This method uses ICP-AES to determine the content of aluminum trioxide, magnesium oxide, calcium oxide, sodium, manganese, vanadium pentoxide and ferric oxide in high titanium slag. The method is simple, rapid, accurate and effective, and can meet the requirements of metallurgical analysis.The samples were dissolved by mixed acid of HCl+HNO_3+HF+HClO_4+H_2SO_4, and test conditions for the sample interfering effects of the titanium matrix and coexisted elements, Elements were determined by selecting the optimum analysis spectrum line and suitable working parameters of instrument, by the use of the substrate matching and the synchronized background correction spectral interference and matrix effect were eliminated.The detection limits,0.001 mg/L-0.030 mg/L, RSD(n+12) < 2.5,and the recovery rates were97.4% ～ 108.2%.
引文
[1]GB/T4102.1-1983中国人民共和国国家标准.高钛渣,金红石化学分析方法[S].
[2]YS/T 514-2009中国人民共和国有色金属行业标准.高钛渣、金红石化学分析方法[S].
[3]仵利萍,刘卫.熔融制样-X射线荧光光谱法测定钒钛磁铁矿中主次组分含量[J].理化检验-化学分册,2013,49(9):1107-1113.
[4]张争京,王凯,张永文.X射线荧光光谱法测定钒钛磁铁矿中的主次量元素[J].理化检验-化学分册,2014,50(10):1274-1277.
[5]成勇.微波消解样品-电感耦合等离子体质谱法测定钒钛磁铁矿中杂质元素[J].理化检验-化学分册,2011,47(44):1329-1332.
[6]魏轶,谈建安,余志峰,等.ICP-AES测定钛铁矿、钒钛磁铁矿中钛[J].光谱试验室,2013,30(3):1492-1495.
[7]肖军,宁燕平.ICP-AES法测定矿石及原料中痕量钒钛[J].钢铁钒钛,1998,19(1):62-65.
[8]关雄俊,李德芳,张兰,等.ICP-AES测定钢铁样中硅、磷、锰、铬、镍、铜和铝[J].分析测试学报,1998,17(2):69-71.
[9]成勇.微波消解-电感耦合等李字体原子发射光谱法测定富钛料中14种杂质元素[J].冶金分析,2012,32(3):59-63.
[10]成勇,袁金红,胡金荣,等.微波消解-ICP-OES测定钛渣中常量或微量杂质[J].分析测试技术与仪器,2012,18(1):38-43.
[11]RKWinge,VAFassle,VJPeterson,等.电感耦合等离子体发射光谱图册.北京:中国光学学会光谱学会翻译,1986.
[2]YS/T 514-2009中国人民共和国有色金属行业标准.高钛渣、金红石化学分析方法[S].
[3]仵利萍,刘卫.熔融制样-X射线荧光光谱法测定钒钛磁铁矿中主次组分含量[J].理化检验-化学分册,2013,49(9):1107-1113.
[4]张争京,王凯,张永文.X射线荧光光谱法测定钒钛磁铁矿中的主次量元素[J].理化检验-化学分册,2014,50(10):1274-1277.
[5]成勇.微波消解样品-电感耦合等离子体质谱法测定钒钛磁铁矿中杂质元素[J].理化检验-化学分册,2011,47(44):1329-1332.
[6]魏轶,谈建安,余志峰,等.ICP-AES测定钛铁矿、钒钛磁铁矿中钛[J].光谱试验室,2013,30(3):1492-1495.
[7]肖军,宁燕平.ICP-AES法测定矿石及原料中痕量钒钛[J].钢铁钒钛,1998,19(1):62-65.
[8]关雄俊,李德芳,张兰,等.ICP-AES测定钢铁样中硅、磷、锰、铬、镍、铜和铝[J].分析测试学报,1998,17(2):69-71.
[9]成勇.微波消解-电感耦合等李字体原子发射光谱法测定富钛料中14种杂质元素[J].冶金分析,2012,32(3):59-63.
[10]成勇,袁金红,胡金荣,等.微波消解-ICP-OES测定钛渣中常量或微量杂质[J].分析测试技术与仪器,2012,18(1):38-43.
[11]RKWinge,VAFassle,VJPeterson,等.电感耦合等离子体发射光谱图册.北京:中国光学学会光谱学会翻译,1986.