1. Institute of Material & Chemistry & Chemical Engineering, Chengdu University of Technology, Chengdu 610059, China 2. Department of Mine Inspection, Guangzhou Entry-Exit Inspection and Quarantine Bureau, Guangzhou 510623, China
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.
Key words：Microwave digestion;Vanadium and titanium magnetite;ICP-OES;Complexant A
朱霞萍1，尹继先2，陈卫东2，胡子文1，梁庆勋1，陈铁爻1 . 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(08): 2277-2280.
ZHU Xia-ping1，YIN Ji-xian2，CHEN Wei-dong2，HU Zi-wen1，LIANG Qing-xun1，CHEN Tie-yao1 . Determination of Fe, Ti and V in Vanadium and Titanium Magnetite by ICP-OES and Microwave-Assisted Digestion . SPECTROSCOPY AND SPECTRAL ANALYSIS, 2010, 30(08): 2277-2280.
[1] LING Xue-fang(凌学芳). Minerals and Rocks(矿物岩石), 1990, 10(2): 105. [2] ZHOU Xiao-dong，ZHANG Yun-mei(周晓东, 张云梅). Journal of Yunnan Normal University(云南师范大学学报), 2007，27(5)：67. [3] Kubrakova I V, Toropchenova E S. Inorganic Materials, 2008，44(14)：1509. [4] XIA Zu-xue, LIU Chang-jun, YAN Li-ping, et al(夏祖学, 刘长军, 闫丽萍, 等). Chemical Research and Application(化学研究与应用), 2004，16(4)：441. [5] GU Jin-chuan(谷晋川). Hydrometallurgy of China(湿法冶金), 1998，(3): 50. [6] Harahsheh M A, Kingman S W. Hydrometallurgy, 2004，73：189. [7] ZHANG Lin-lin, XING Xiao-ru, WU Guo-ping, et al(张霖琳, 邢小茹, 吴国平, 等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2009, 29(4): 1115. [8] CHEN Ji-luan, WU Ji-hong, JIANG Ying, et al(陈计峦, 吴继红, 江 英, 等). Spectroscopy and Spectral Analysis(光谱学与光谱分析), 2009，29(2): 496. [9] HUO Jian-zhong(霍建中). Chinese Journal of Analytical Chemistry(分析化学), 2003，31(5): 64. [10] ZHOU Xiao-dong，ZHANG Yun-mei(周晓东, 张云梅). Metallurgical Analysis(冶金分析), 2007, 27(8)：69. [11] YING Hai-song, WANG Yan, LIAO Hai-ping(应海松, 王 艳, 廖海平). Rock and Mineral Analysis(岩矿测试), 2007，26(5): 413. [12] Frank E S, Edward A. Talanta, 1996, 43: 1207. [13] CHEN Zong-hong, SUN Ming-xing, CHU Ming-sheng, et al(陈宗宏，孙明星，楚明生，等). Chemical World(化学世界), 2006，47(7)：401. [14] Irina K. Spectrochimica Acta Part B, 1997, 52: 1469. [15] WU Zheng-zhou, ZHANG Jun-hua(吴政宙，张军华). Metallurgical Analysis(冶金分析), 2005，25(5)：69.
