Determination of platinum group elements in vanadium-titanium magnetite raw ore by inductively coupled plasma mass spectrometry with antimony fire assay
SHAO Kun, FAN Jian-xiong, YANG Chang-yan
Institute of Multipurpose Utilization of Mineral Resources, CAGS, Chengdu 610041, China
Abstract：Considering the Os loss in nickel-sulfur assaying as well as the Ru and Os loss in lead assaying, Sb2O3 was selected as the trapping agent. The antimony button was treated by cupellation and the combined granules were dissolved with 50% aqua regia (V/V). The tartaric acid (50mg/L) was added to inhibit the hydrolysis of antimony. The analysis method of platinum group elements in vanadium-titanium magnetite raw ore by inductively coupled plasma mass spectrometry (ICP-MS) with antimony fire assay was established. Through the tests of reducing power of sample, the components for assaying were determined as below: 8g of Na2CO3, 6g of K2CO3, 6g of Sb2O3, 6g of Na2B4O7·10H2O, 4g of glass powder, and 0.8g of flour. The effect of tartaric acid content and atomizer flow rate on the signal intensity of platinum group elements was investigated. Finally, 5% aqua regia-50mg/L tartaric acid with atomizing flow rate of 0.7L/min was selected as the determination medium. The selection of isotopes and the elimination of interference were discussed. 102Ru, 103Rh, 106Pd, 192Os, 193Ir and 195Pt were selected as the isotopes for determination. The diameter of antimony bead at late stage of cupellation was controlled at about 1.5mm. 115In was used as internal standard for the correction of 102Ru, 103Rh and 106Pd, and 185Re was used as internal standard for the correction of 192Os, 193Ir and 195Pt. The matrix effect and signal drift could be effectively solved. The correlation coefficients of calibration curves for each element were higher than 0.999. The detection limit was in range of 0.037-0.18ng/g. The platinum group elements in vanadium-titanium magnetite raw ore were determined according to the experimental method. The standard deviations (RSD, n=6) of measured results were between 4.5% and 12%. The spiked recoveries were between 93% and 105%.
邵坤, 范建雄, 杨常艳. 锑试金-电感耦合等离子体质谱法测定钒钛磁铁矿原矿中铂族元素[J]. 冶金分析, 2018, 38(5): 18-24.
SHAO Kun, FAN Jian-xiong, YANG Chang-yan. Determination of platinum group elements in vanadium-titanium magnetite raw ore by inductively coupled plasma mass spectrometry with antimony fire assay. , 2018, 38(5): 18-24.
张腾蛟,李佑国,张月娇,等.川西盐边县红格钒钛磁铁矿中镍钴硫化物的铂族元素地球化学特征[J].地质评论,2017,63(4):1050-1063.ZHANG Teng-jiao,LI You-guo,ZHANG Yue-jiao,et al.PGE Geochemical characteristics of massive sulfide in V-Ti magnetite at Hongge Area,Yanbian County,Western Sichuan[J].Geological Review,2017,63(4):1050-1063.
[3]
傅文章.攀西钒钛磁铁矿资源特征及综合利用问题的基本分析[J].矿产综合利用,1996(1):27-34.FU Wen-zhang.Characteristics and current situation of comprehensive utilization of vanadium-titano magnetite resources in Panxi region[J].Multipurpose Utilization of Mineral Resources,1996(1):27-34.
[4]
唐国光.加强攀西战略资源创新开发试验区矿产资源开发[J].四川地质学报,2015,35(2):318-320.TANG Guo-guang.Strengthen exploitation of mineral resources in the pnaxi strategic resources innovation development experimental zone[J].Acta Geologica Sichuan,2015,35(2):318-320.
[5]
赵正,漆亮,黄智龙,等.地质样品中铂族元素的分析测定方法[J].地学前缘,2009,16(1)181-193.ZHAO Zheng,QI Liang,HUANG Zhi-long,et al.The analytical methods for determination of platinum group elements in geological samples[J].Earth Science Frontiers,2009,16(1):181-193.
[6]
孙亚莉,管希云,杜安道.锍试金富集贵金属元素:I.等离子体质谱法测定地质样品中痕量铂族元素[J].岩矿测试,1997,16(1):12-17.SUN Ya-li,GUAN Xi-yun,DU An-dao.Preconcentration of precious metal elements by nickel sulphide fire assay I.determination of platinum group elementsin geological samples by ICP-MS[J].Rock and Mineral Analysis,1997,16(1):12-17.
[7]
蔡树型.铅试金法在贵金属分析中的作用[J].分析试验室,1988,7(9):46-48.CAI Shu-xing.Effect of lead assay in the analysis of precious metals[J].Chinese Journal of Analysis Laboratory,1988,7(9):46-48.
[8]
Gros M,Lorand J P,Luguet A.Analysis of platinum group elements and gold in geological materials using NiS fire assay and Te coprecipitation;the NiS dissolution step revisited[J].Chemical Geology,2002,185:179-190.
[9]
赵素利,张欣,温宏利,等.锍镍试金富集-电感耦合等离子体质谱法测定黑色页岩中的铂族元素[J].岩矿测试,2011,30(6):723-726.ZHAO Su-li,ZHANG Xin,WEN Hong-li,et al.Determination of the platinum group elements in black shale by inductively coupled plasma-mass spectrometry with nickel sulphide fire-assay[J]. Rock and Mineral Analysis,2011,30(6):723-726.
[10]
吕彩芬,何红蓼,周肇茹,等.锍镍试金-等离子体质谱法测定地球化学勘探样品中的铂族元素和金II.分析流程空白的降低[J].岩矿测试,2002,21(1):7-11.L Cai-fen,HE Hong-liao,ZHOU Zhao-ru,et al.Determination of platinum group elements and gold in geochemical exploration samples by nickel sulfide fire assay-ICPMS II.Reduction of reagent blank[J].Rock and Mineral Analysis,2002,21(1):7-11.
[11]
孙中华,章志仁,毛英,等.铅试金-光谱法同时测定地质样品中痕量铂族元素的探索[J].贵金属,2004,25(3):45-48.SUN Zhong-hua,ZHANG Zhi-ren,MAO Ying,et al.An exploration of lead fire assay-AES determination of PGE in geological samples[J].Precious Metals,2004,25(3):45-48.
[12]
林玉南,钟学谊,付育勋,等.锍试金和锑试金富集贵金属[J].分析化学,1974,2(2):31-37.LIN Yu-nan,ZHONG Xue-yi,FU Yu-xun,et al.Preconcentration of precious metal with NiS fire assay and Sb fire assay[J].Chinese Journal of Analytical Spectrometry,1974,2(2):31-37.
[13]
林玉南,胡金星,沈振兴,等.锑试金富集痕量金的研究-地质样品中ng/g级金的测定[J].分析化学,1988,16(1):1-4.LIN Yu-nan,HU Jin-xing,SHEN Zhen-xing,et al.A new fire assay of gold using antimony as a collector-determination of gold at ng/g levels in geochemical materials[J].Chinese Journal of Analytical Spectrometry,1988,16(1):1-4.
[14]
刘军,闫红岭,连文莉,等.封闭溶矿-电感耦合等离子体质谱法测定地质样品中金银铂钯[J].冶金分析,2016,36(7):25-33.LIU Jun,YAN Hong-ling,LIAN Wen-li,et al.Determination of gold,silver,platinum and palladium in geological samples by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2016,36(7):25-33.
[15]
张桢,刘巍,郭颖.电感耦合等离子体质谱法测定镍基高温合金中10种元素[J].理化检验:化学分册,2016,52(10):1201-1205.ZHANG Zhen,LIU Wei,GUO Ying.ICP-MS determination of 10 elements in nickel base superalloy[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2016,52(10):1201-1205.
[16]
梁玉省,谢敏雄,王楠.一种含硫金精矿的火试金方法试验研究及改进[J].世界有色金属,2016(8):79-82.LIANG Yu-sheng,XIE Min-xiong,WANG Nan.A gold sulfur concentrate fire assay method of experimental research and improvement[J].World Nonferrous Metals,2016(8):79-82.
[17]
张志刚,刘凯,陈泓,等.酒石酸络合掩蔽锑-氢醌容量法测定锑矿石样品中常量金[J].岩矿测试,2015,34(4): 454-458.ZHANG Zhi-gang,LIU Kai,CHEN Hong,et al.Determination of gold in antimony ores by hydroquinone volumetric method with antimony tartrate as complexing and masking agent[J].Rock and Mineral Analysis,2015,34(4): 454-458.
[18]
聂西度,何晓梅,李立波,等.有机酸在电感耦合等离子体质谱中基体效应的研究[J].光谱学与光谱分析,2007,27(7):1420-1423.NIE Xi-du,HE Xiao-mei,LI Li-bo,et al.The matrix effects of organic acid compounds in ICP-MS[J].Spectroscopy and Spectral Analysis,2007,27(7):1420-1423.
[19]
张忠亭,邓飞跃,蒋苏琼,等.电感耦合等离子体原子发射光谱法测定炼锑泡渣中碲[J].冶金分析,2011,31(10):46-49.ZHANG Zhong-ting,DENG Fei-yue,JIANG Su-qiong,et al.Determination of tellurium in refined antimony slag by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2011,31(10):46-49.
[20]
张勤,刘亚轩,吴健玲.电感耦合等离子体质谱法直接同时测定地球化学样品中镓铟铊[J].岩矿测试,2003,22(1):21-27.ZHANG Qin,LIU Ya-xuan,WU Jian-ling.Simultaneous determination of gallium, indium and thallium in geochemical samples by inductively coupled plasma mass spectrometry[J].Rock and Mineral Analysis,2003,22(1):21-27.
[21]
陈景.铂族金属络合物稳定性与原子结构的关系[J].贵金属,1984,5(3):1-9.CHEN Jing.The relationship between the stability of platinum group metal complex and the atomic structure[J].Precious Metals,1984,5(3):1-9.
