Determination of titanium dioxide in red mud by ammonium ferric sulfate titrimetry
ZHU Xiao-bo1,2, LI Wang1, GUAN Xue-mao1
1. School of Materials Science and Engineering, Henan Polytechnic University, Jiaozuo 454000, China; 2. Henan Key Discipline Open Laboratory of Mining Engineering Materials, Jiaozuo 454000, China
Abstract：The red mud sample was heated and fused in muffle furnace with sodium hydroxide using its strong basicity and ablation property. The fusant was firstly leached in worm water followed by dissolution with 30 mL of hydrochloric acid. Then, the aluminum sheet was added for reduction in presence of sodium bicarbonate solution for protection. Finally, the content of titanium dioxide in red mud was determined by ammonium ferric sulfate titrimetry using ammonium thiocyanate solution as indicator. The effect of sample dosage, particle size, sodium hydroxide dosage, roasting condition, sample dissolution condition and protection solution on the determination was investigated. The results showed that the optimal experimental conditions were as follows: the dosage of sodium hydroxide dosage was 6 g, the roasting temperature was 650 ℃, the roasting time was 20 min, the reducing agent was 2.2 g of aluminum sheet, the protection solution was saturated sodium bicarbonate solution, and the placing time before titration was less than 15 min. The proposed method was applied to the determination of titanium dioxide in actual red mud sample, and the found results were consistent with those obtained by inductively coupled plasma atomic emission spectrometry. The relative standard deviation (RSD, n=5) was less than 0.2%.
Agatzini L S, Oustadakis P, Tsakiridis P E,et al. Titanium leaching from red mud by diluted sulfuric acid at atmospheric pressure [J]. Journal of Hazardous Materials, 2008, 157: 579-586.
[2]
Indrani G, Saumyen G R, Balasubramaniam A V, et al. Leaching of metals from fresh and sintered red mud [J]. Journal of Hazardous Materials, 2011, 185: 662-668.
[3]
周晓东, 张云梅. 钛铁矿中钛的测定[J]. 理化检验: 化学分册,2007, 43(3):544-546.ZHOU Xiao-dong,ZHANG Yun-mei.Determinationof titanium in ilmenite[J]. Physical Testing and Chemical Analysis Part B: Chemical Analysis,2007, 43(3):544-546.
[4]
刘冠龙, 许俊鸿. 重铬酸钾滴定法快速测定钛铁矿中钛含量[J]. 冶金分析,2012, 32(3):74-76.LIU Guan-long,XU Jun-hong.Rapid determination of titanium and iron in ilmenite by potassium dichromate titrimetry[J]. Metallurgical Analysis, 2012, 32(3):74-76.
[5]
梁庆勋, 朱霞萍, 尹继先. 重铬酸钾滴定法测定钛铁时钒钛磁铁矿试样的微波消解研究[J]. 冶金分析, 2010, 30(7):44-47.LIANG Qing-xun,ZHU Xia-ping,YIN Ji-xian.Study on microwave digestion of vanadium-titaniummagnetite sample in the determination of titanium and iron by potassium dichromate titration[J].Metallurgical Analysis, 2010, 30(7):44-47.
[6]
郑小敏, 汪雪梅, 杨平, 等. 硫酸高铁铵滴定法测定制备金属钛的电解质熔盐中Ti2+和Ti3+[J]. 冶金分析,2011, 31(10):29-33.ZHENG Xiao-min,WANG Xue-mei,YANG Ping,et al.Determination of Ti2＋and Ti3＋ in electrolyte fused salt for preparing metallic titanium by ammonium ferric sulfate titration[J].Metallurgical Analysis,2011,31(10):29-33.
[7]
耿新, 康宝军, 窦成, 等. 电感耦合等离子体原子发射光谱法测定金属锰中痕量钛[J]. Metallurgical Analysis, 2013, 33(9):53-56.GENG Xin,KANG Bao-jun,DOU Cheng,et al.Determination of trace titanium in manganese by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis, 2013, 33(9):53-56.
[8]
于媛君, 杨丽荣, 顾继红, 等. 电感耦合等离子体原子发射光谱法测定帘线钢中痕量钛[J]. 冶金分析,2009, 29(1):52-55.YU Yuan-jun , YANG Li-rong , GU Ji-hong , et al. Determination of trace titanium in tire cord steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis, 2009, 29(1):52-55.
[9]
邵海舟,刘成花.电感耦合等离子体原子发射光谱法测定铌铁中铌钛钽硅铝磷[J]. 冶金分析,2011, 31(12):54-57.SHAO Hai-zhou,LIU Cheng-hua.Determination of niobium,titanium,tantalum,silicon,aluminium and phosphorus in ferroniobium byinductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis, 2011, 31(12):54-57.
[10]
彭洪,吴文斌,濮国荣, 等. ICP-AES法测定铀水冶萃取原液中的钛[J]. 铀矿冶, 2012, 31(3):140-142.PENG Hong,WU Wen-bin,PU Guo-rong,et al. Determination of titanium content in feed solution in uranium hydrometallurgical processby ICP-AES method[J]. Uranium Mining and Metallurgy, 2012, 31(3):140-142.
[11]
韦斌, 付晓恒, 王龙龙, 等. 微波消解ICP-AES法测量赤泥中的钠、铁、铝、钛 [J]. 环境科学与工程,2008(12):59-61.WEI Bin,FU Xiao-heng,WANG Long-long.The microwave resolution technology and ICP-AES to survey in the red mud the sodium,the iron,the aluminum,the titanium[J].Journal of Environmental Science and Engineering, 2008(12):59-61.
