光谱学与光谱分析, 2010, 30 (8): 2277, 网络出版: 2011-01-26  

微波消解ICP-OES快速测定难溶钒钛磁铁矿中铁、 钛、 钒

Determination of Fe, Ti and V in Vanadium and Titanium Magnetite by ICP-OES and Microwave-Assisted Digestion
作者单位
1 成都理工大学材料与化学化工学院, 四川 成都610059
2 广州出入境检验检疫局化矿处, 广东 广州510623
摘要
建立了添加络合剂A进行微波消解难溶钒钛磁铁矿, 电感耦合等离子体发射光谱(ICP-OES)测定其中铁、 钛、 钒的方法。 通过正交实验确定的最优消解条件是: 0.1 g钒钛磁铁矿; 12 mL浓盐酸; 0.04 g络合剂A; 消解时间10 min; 微波功率385 W。 用新建立的方法对攀枝花钢铁研究院的钒钛磁铁矿(GBW07226)进行消解, 用ICP-OES法对Fe, Ti, V进行测定, 测定的相对误差和相对标准偏差均达到分析化学的要求。 新建立的方法中, 添加络合剂与溶解出的金属离子络合, 使得试样与溶解介质盐酸的接触面不断更新, 显著加速了矿物的溶解, 用ICP-OES法测定消解液, 实现了多种主量、 微量元素同时测定。 该法试剂用量少、 经济; 样品消解、 测定迅速; 对环境友好; 适合大批量样品快速测定。 建立的方法对国家商检部门、 相关分析测试单位等具备实际应用价值。
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 HCl, 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.

朱霞萍, 尹继先, 陈卫东, 胡子文, 梁庆勋, 陈铁爻. 微波消解ICP-OES快速测定难溶钒钛磁铁矿中铁、 钛、 钒[J]. 光谱学与光谱分析, 2010, 30(8): 2277. ZHU Xia-ping, YIN Ji-xian, CHEN Wei-dong, HU Zi-wen, LIANG Qing-xun, CHEN Tie-yao. Determination of Fe, Ti and V in Vanadium and Titanium Magnetite by ICP-OES and Microwave-Assisted Digestion[J]. Spectroscopy and Spectral Analysis, 2010, 30(8): 2277.

关于本站 Cookie 的使用提示

中国光学期刊网使用基于 cookie 的技术来更好地为您提供各项服务,点击此处了解我们的隐私策略。 如您需继续使用本网站,请您授权我们使用本地 cookie 来保存部分信息。
全站搜索
您最值得信赖的光电行业旗舰网络服务平台!