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电感耦合等离子体发射光谱法(ICP-OES)和微波消解测定钒钛磁铁矿中的铁、钛和钒

[Determination of Fe, Ti and V in vanadium and titanium magnetite by ICP-OES and microwave-assisted digestion].

作者信息

Zhu Xia-ping, Yin Ji-xian, Chen Wei-dong, Hu Zi-Wen, Liang Qing-xun, Chen Tie-yao

机构信息

Institute of Material & Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu 610059, China.

出版信息

Guang Pu Xue Yu Guang Pu Fen Xi. 2010 Aug;30(8):2277-80.

PMID:20939356
Abstract

The method of determination of iron, titanium and vanadium in indissolvable vanadium and titanium magnetite has been established by inductively coupled plasma atomic emission spectroscopy through adding the complexant A and using microwave-assisted digestion. The optimal conditions are confirmed by orthogonal experiment: 0.1 g vanadium and titanium magnetite, 0.04 g complexant A, 12 mL concentrated HC1, 10 min digestion time, and 385 W microwave power. The newly-established method has been applied to digest vanadium and titanium magnetite of Panzhihua Iron and Steel Institute (GBW07226). The iron, titanium and vanadium were detected by ICP-OES, and both comparative error (Er%) and comparative standard deviation (RSD%) met the demand of analytical chemistry, and the complexant A can significantly accelerate the dissolution of vanadium and titanium magnetite through the complexation with the dissolved metal ions, and making the surface of sample and hydrochloric acid medium to update constantly. The determination of the main and trace elements of digestion solution at the same time was achieved by ICP-OES. The method has the advantages of less use of reagents, economy, rapidness, and being friendly to environment, and it meets the requirement for rapid and volume determination. So the method has the value of practical application for the entry-exit inspection and quarantine department of the state and other relevant inspection units.

摘要

通过加入络合剂A并采用微波辅助消解,建立了电感耦合等离子体原子发射光谱法测定难溶钒钛磁铁矿中铁、钛和钒的方法。通过正交试验确定了最佳条件:0.1 g钒钛磁铁矿、0.04 g络合剂A、12 mL浓盐酸、10 min消解时间和385 W微波功率。新建立的方法已应用于攀枝花钢铁研究院钒钛磁铁矿(GBW07226)的消解。采用电感耦合等离子体发射光谱仪(ICP-OES)测定铁、钛和钒,相对误差(Er%)和相对标准偏差(RSD%)均满足分析化学要求,且络合剂A能通过与溶解的金属离子络合显著加速钒钛磁铁矿的溶解,使样品表面和盐酸介质不断更新。通过ICP-OES实现了对消解液中主、微量元素的同时测定。该方法具有试剂用量少、经济、快速、环保等优点,满足快速批量测定的要求。因此,该方法对国家出入境检验检疫部门及其他相关检验单位具有实际应用价值。

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