Abstract：During the determination of titanium by ammonium ferric sulfate titration method, the presence of chromium had interference. The samples from flotation-metallurgy process of heavy placer mineral from Mozambique contained chromium, which should be pre-separated for the determination of titanium by ammonium ferric sulfate titration.The sample was firstly fused with sodium peroxide. Then the crucible after cooling was transferred into 300 mL beaker containing 100-150 mL of water. The beaker was heated on high-temperature electric furnace. The solution was boiled for 5-8 min to dissolve the melt and remove hydrogen peroxide. At this time, titanium existed in precipitate in the form of titanium hydroxide, while chromium existed in solution in the form of chromate. After filtration, chromium existed in filtrate and could be determined by ammonium ferrous sulfate titration using N-phenylanthranilic acid as indicator. Titanium existed in precipitate on filter paper and was then washed into conical flask with hot hydrochloric acid (1+1) and water. The content of titanium was determined by ammonium ferric sulfate titration using potassium thiocyanate as indicator. The interference mechanism of chromium to the determination of titanium was studied and discussed. During the determination of titanium, bivalent chromium was possibly generated, which consumed the standard solution of ammonium ferric sulfate and influenced on the determination of titanium. The experimental method was applied to the determination of titanium dioxide and chromic oxide in standard sample, concentrate ore (6-6-1 concentrate) and tailings ore (6-6-1 tailings) after roasting-magnetic separation. The determination results of titanium dioxide were consistent with the certified values. The relative standard deviation (RSD, n=7) was 0.082 %-0.81%. The determination results of chromic oxide were consistent with the certified values or those obtained by ammonium ferrous sulfate titration without filtration separation. The RSD (n=7) was 0.25%-1.79%.
刘艳花,孙湘莉. 莫桑比克某重砂矿选冶流程样品中钛和铬的联合测定[J]. 冶金分析, 2017, 37(7): 37-44.
LIU Yan-hua,SUN Xiang-li. Combined determination of titanium and chromium in the samples from the flotation-metallurgy process of heavy placer in Mozambique. , 2017, 37(7): 37-44.
高本恒,王化军,曲媛.印尼某海滨砂矿精矿直接还原-磨矿-磁选提铁试验研究[J].矿冶工程,2012,32(5):44-46.GAO Ben-heng,WANG Hua-jun,QU Yuan,et al.Experimental research on extracting iron from beach placer concentrate in indonesia by direct reduction-grinding-magnetic separation[J].Mining Metallurgical Engineering,2012,32(5):44-46.
[2]
张立刚.某重砂矿氧化焙烧-磁选提钛降铬试验研究[J].矿冶工程,2016,36(2):44-49.ZHANG Li-gang.Oxidizing roasting-magnetic separation technique adopted for upgrading titanium and degrading chrome in heavy mineral sands[J].Mining Metallurgical Engineering,2016,36(2):44-49.
[3]
郑小敏,汪雪梅,杨平.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.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.
[4]
刘冠龙,许俊鸿.重铬酸钾滴定法快速测定钛铁矿中钛铁含量[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]
巨力佩,季伟,张旺强.电感耦合等离子体发射光谱法测定钒钛铁矿中二氧化钛[J].分析测试技术与仪器,2013,19(2):88-91.JU Li-pei,JI Wei,ZHANG Wang-qiang.Determination of TiO2 in sefstromite by inductively coupled plasma atomic emission sepectrometry[J].Analysis and Testing Technology and Instruments,2013,19(2):88-91.
[6]
马光强,邹敏,霍红英.二安替比林甲烷光度法测定高钛型高炉渣中钛[J].冶金分析,2013,33(7):77-80.MA Guang-qiang,ZOU Min,HUO Hong-ying.Spectrophotometric determination of titanium in high-Ti-bearing blast-furnace slag with diantipyrylmethane[J].Metallurgical Analysis,2013,33(7):77-80.
[7]
胡德新,马德起,潘宏伟,等.电位滴定法测定铬矿石中三氧化二铬的微波溶样法研究[J].冶金分析,2011,31(2):63-66.HU De-xin,MA De-qi,PAN Hong-wei,et al.Study on microwave dissolution of sample for the determination of chromium sesquioxide in chrome ore by potentiometric titration[J].Metallurgical Analysis,2011,31(2):63-66.
[8]
梁述忠,李智.恒电流库仑分析法测定铬矿中三氧化二铬[J].冶金分析,2006,26(4):47-49.LIANG Shu-zhong,LI Zhi.Determination of Cr2O3 content in chromium mineral by the constant current coulometric analysis[J].Metallurgical Analysis,2006,26(4):47-49.
[9]
靳丽波,田凤英.电感耦合等离子体发射光谱法测定铬铁矿中三氧化二铬[J].化工矿产地质,2013,35(3):188-192.JIN Li-bo,TIAN Feng-ying.Quantification of chromium oxide in chromite by inductive coupled plasma-atomic emission[J].Geology of Chemical Minerals,2013,35(3):188-192.
[10]
李传启,王露,杨崇秀.高氯酸处理-硫酸亚铁铵滴定法测定铜合金中铬[J].冶金分析,2016,36(2):71-74.LI Chuan-qi,WANG Lu,YANG Chong-xiu.Determination of chromium in copper alloy by ferrous ammonium sulfate titration after perchloric acid treatment[J].Metallurgical Analysis,2016,36(2):71-74.
[11]
曹晨,焦凤菊,郭英英.硫酸亚铁铵滴定法测定氮化铬铁中铬[J].冶金分析,2016,36(6):77-81.CAO Chen,JIAO Feng-ju,GUO Ying-ying.Determination of chromium in nitrogen-bearing ferrochromium by ammonium ferrous sulfate titrimetry[J].Metallurgical Analysis,2016,36(6):77-81.
[12]
周海波,李玉茹,吴爱华,等.快速测定铬铁矿中铬的溶样方法研究[J].中国无机分析化学,2011,1(4):29-32.ZHOU Hai-bo,LI Yu-ru,WU Ai-hua,et al.Study on the sample dissolution method for rapid determination of chrominum in chromite[J].Chinese Journal of Inorganic Analytical Chemistry,2011,1(4):29-32.
[13]
成勇,袁金红,彭慧仙,等.微波消解-电感耦合等离子体原子发射光谱法测定钒钛磁铁矿中锆铌钒铬[J].冶金分析,2013,33(12):43-46.CHENG Yong,YUAN Jin-hong,PENG Hui-xian,et al.Determination of zirconium,niobium,vanadium and chromium in vanadium titano-magnetite ore by microwave digestion inductively coupeld plasma atomic emission spectrometry[J].Metallurgical Analysis,2013,33(12):43-46.
黄舜华.二价铬镀锌白钝化:理论与实践[J].电镀与环保,1989,9(1):38-41.HUANG Shun-hua.Cr2+ galvanized passivation:theory and practice[J].Electroplating and Environmental Protection,1989,9(1):38-41.
[16]
马国军,范巍,徐之浩,等.不锈钢厂烟尘中铬及其他元素的分布规律[J].过程工程学报,2010,10(增刊1):68-72.MA Guo-jun,FAN Wei,XU Zhi-hao,et al.Distribution behavior of chromium and other elements in the stainless steel plant dust[J].Journal of Process Engineering,2010,10(supplement 1):68-72.
