Abstract:Silicon content is an important control index in metallurgical process.In this paper,the self-produced nickel ore was used as an example to discuss the experimental conditions affecting the coloring of silicon molybdenum yellow as well as common interference of Fe3+ and F- in metallurgical samples.The sample was treated by sodium hydroxide melting.The filtrate was taken as the solution to be tested after dry filtration.The acidity was stabilized with sulfuric acid,and the absorbance was measured after adding ammonium molybdate solution for coloring.The results showed that the maintaining of proper coloring acidity was the key to determination,and the addition of other reagents were unnecessary.Taking SiO2 as the unit of measurement,the linear range of calibration curve was 1.00%-40%.The limit of detection was about 1.00%.The apparent molar absorption coefficient was 1.1×104 L·mol-1·cm-1.When the mass concentration of F- in test solution was higher than 65 mg/L,it would influence on the coloring of silicon-molybdenum heteropoly acid.When the mass concentration of Fe3+ in test solution was less than 7.5 mg/L,it had no influence on the determination.The content of silica in nickel raw ore was determined according to the experimental method,and the relative standard deviation(RSD,n=8) of the determination results was less than 0.6%.The recoveries were between 95% and 100%.As the mass fraction of silica was in range of 20%-40%,the estimation error was 0.4%.Moreover,a method to measure the matching between samples and standard matrix series was also recommended in this study.
[1] 贺国春,王飞龙,龚强.含镁硅酸盐矿物在硫化铜镍矿浮选分离体系中的行为机理研究[J].世界有色金属,2018(9):88-90. HE Guochun,WANG Feilong,GONG Qiang.Behavior mechanism of magnesium silicate minerals in flotation separation system of copper nickel sulfide ore[J].World Nonferrous Metals,2018(9):88-90. [2] 冯博,汪惠惠,周利华.新疆某难选硫化铜镍矿浮选工艺[J].有色金属工程,2016,6(1):49-53. FENG Bo,WANG Huihui,ZHOU Lihua.Flotation technology of a refractory copper-nickel sulfide ore in Xinjiang[J].Nonferrous Metals Engineering,2016,6(1):49-53. [3] 张振强,赵俊学,崔雅茹,等.镍闪速熔炼新渣型的物化性质研究[J].有色金属(冶炼部分),2013(5):5-9. ZHANG Zhenqiang,ZHAO Junxue,CUI Yaru,et al.Study on physico-chemical property of new slag type for nickel flash smelting[J].Nonferrous Metals(Extractive Metallurgy),2013(5):5-9. [4] 陈卫.二氧化硅定量分析常用方法对比探讨[J].中国非金属矿工业导刊,2023(4):60-63. CHEN Wei.Comparison of common methods for quantitative analysis of silica[J].China Non-metallic Minerals Industry,2023(4):60-63. [5] 沙德仁.提高硅钼黄比色溶液稳定性的研究[J].玻璃纤维,2010(4):18-28,41. SHA Deren.Study of improving the stability of colorimetric solution of silicon molybdenum yellow[J].Fiber Glass,2010(4):18-28,41. [6] 王纪华,江美珍,唐书天.冶金炉渣中SiO2分析方法的研究及应用[J].冶金分析(Metallurgical Analysis),2000,20(3):48-49. [7] 刘克清.浅谈采用硅钼黄分光光度示差法测定碳酸盐中SiO2含量[J].玻璃(Glass),2002(1):27-29. [8] 翟庆洲,裘式纶,魏波,等.硅钼黄光度法测定沸石分子筛中硅[J].理化检验(化学分册),2000(12):553-554. ZHAI Qingzhou,QIU Shilun,WEI Bo,et al.Molybdenum yellow-photometric determination of silicon in zeolite molecular sieves[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2000(12):553-554. [9] 张晓莲.分光光度法测定SiO2-Al2O3型耐火原料中硅的含量[J].金属矿山,2001(5):39-41. ZHANG Xiaolian.Measurement of SiO2 content in SiO2-Al2O3 series raw refractory materials by spectrophotometric method[J].Metal Mine,2001(5):39-41. [10] 徐寿昌.有机化学[M].2版.北京:高等教育出版社,1993:86-93. [11] 张薇薇,杨怡,陈培超,等.钼酸铵分光光度法测定水发产品中过氧化氢残留量[J].现代预防医学,2008(8):1556-1558. ZHANG Weiwei,YANG Yi,CHEN Peichao,et al.Spectrophotometric determination of residual hydrogen peroxide in soaking solution of waterborne products[J].Modern Preventive Medicine,2008(8):1556-1558. [12] 李玉娇.硅酸钠水溶液特性研究[J].钻采工艺,2007(4):116-118,1. LI Yujiao.Study on characteristics of sodium silicate solution[J].Drilling & Production Technology,2007(4):116-118,1. [13] 中国轻工业联合会,全国造纸工业标准化技术委员会.GB/T 1914—2017化学分析滤纸[S].北京:中国标准出版社,2017. [14] 王风云,夏明珠,雷式.现代大学化学[M].北京:化学工业出版社,2015:21-35. [15] 吴争平,尹周澜,陈启元,等.β型四钼酸铵的制备及结晶过程[J].中南工业大学学报(自然科学版),2001(2):135-138. WU Zhengping,YIN Zhoulan,CHEN Qiyuan,et al.The preparation of ammonium β-tetramolybdate and the crystallization process[J].Journal of Central South University of Technology(Natural Science),2001(2):135-138. [16] 王朝霞,李彦岗.分光光度分析在水泥及其原材料化学分析中的应用[J].山西煤炭管理干部学院学报,2012,25(4):156-158. WANG Chaoxia,LI Yan′gang.Application of spectrophotometric analysis in chemical analysis of cement and its raw materials[J].Journal of Shanxi Coal-Mining Administrators College,2012,25(4):156-158. [17] 王弦,张军伟,彭奇均.硅钼黄分光光度法测定柠檬酸液中的溶硅[J].应用化工,2012,41(8):1462-1465. WANG Xian,ZHANG Junwei,PENG Qijun.Determination of nanocolloidal silicon in citric acid solution by molybdosilicate yellow spectrophotometry[J].Applied Chemical Industry,2012,41(8):1462-1465. [18] 乔蓉.分光光度法测定炉渣中的二氧化硅[J].金属材料与冶金工程,2009,37(5):57-59,64. QIAO Rong.Determination of silicon dioxide in slag by the spectrophotometric method[J].Metal Materials and Metallurgy Engineering,2009,37(5):57-59,64. [19] 中华人民共和国水利部.SL 91.1—1994 二氧化硅(可溶性)的测定(硅钼黄分光光度法)[S].北京:中国标准出版社,1994. [20] 冉敬,杜谷,杨乐山,等.关于检出限的定义及分类的探讨[J].岩矿测试,2008(2):155-157. RAN Jing,DU Gu,YANG Leshan,et al.Discussion on the definition and classification of detection limit[J].Rock and Mineral Analysis,2008(2):155-157. [21] 《分析化学》编委会.分析化学(上册)[M].北京:地质出版社,1995:265. [22] 同济大学应用数学系.概率统计简明教程[M].北京:高等教育出版社,2003:121-125.