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  

Determination of platinum group elements in vanadium-titanium magnetite raw ore by inductively coupled plasma mass spectrometry with antimony fire assay

作　　者：邵坤[1] 范建雄[1] 杨常艳[1] SHAO Kun;FAN Jian xiong;YANG Chang yan(Institute of Multipurpose Utilization of Mineral Resources, CAGS, Chengdu 610041 , China)

机构地区：[1]中国地质科学院矿产综合利用研究所,四川成都610041

出　　处：《冶金分析》2018年第5期18-24,共7页Metallurgical Analysis

摘　　要：考虑到镍锍试金时Os会有损失,铅试金时Ru、Os会有损失,因此采用Sb_2O_3作试金捕集剂,锑扣经灰吹后用50%王水(V/V)溶解合粒,通过加入50mg/L酒石酸抑制锑的水解,建立了锑试金-电感耦合等离子体质谱法(ICP-MS)测定钒钛磁铁矿原矿中铂族元素的分析方法。通过样品还原力测试,确定试金配料组分为8g Na_2CO_3、6g K_2CO_3、6g Sb_2O_3、6g Na_2B_4O_7·10H_2O、4g玻璃粉、0.8g面粉。考察了酒石酸含量和雾化气流速对铂族元素信号强度的影响,最终确定测定介质为5%王水-50mg/L酒石酸,雾化气流速为0.7L/min。讨论了测定同位素的选择及干扰消除,最终确定测定同位素为102 Ru、103 Rh、106Pd、192 Os、193Ir、195Pt;控制灰吹末期锑珠直径在1.5mm左右,采用内标115In校正102 Ru、103 Rh、106 Pd,内标185 Re校正192 Os、193Ir、195Pt,可以有效克服基体效应和信号漂移。方法中各元素校准曲线的相关系数均在0.999以上,方法检出限在0.037~0.18ng/g之间。按照实验方法测定钒钛磁铁原矿样品中铂族元素,结果的相对标准偏差(RSD,n=6)为4.5%~12%,加标回收率在93%~105%之间。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（50 mg/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：8 g of Na2CO3,6 g of K2CO3,6 g of Sb2O3,6 g of Na2B4O7·10H2O,4 g of glass powder,and 0.8 g 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-50 mg/L tartaric acid with atomizing flow rate of 0.7 L/min was selected as the determination medium.The selection of isotopes and the elimination of interference were discussed.102 Ru,103 Rh,106 Pd,192 Os,193 Ir and 195 Pt were selected as the isotopes for determination.The diameter of antimony bead at late stage of cupellation was controlled at about1.5 mm.115 In was used as internal standard for the correction of 102 Ru,103 Rh and 106 Pd,and 185 Re was used as internal standard for the correction of 192 Os,193 Ir and 195 Pt.The matrix effect and signal drift could be effectively solved.The correlation coefficients of calibration curves for each element were higher than0.999.The detection limit was in range of 0.037-0.18 ng/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%.

关 键 词：锑试金 电感耦合等离子体质谱法(ICP-MS) 钒钛磁铁矿 铂族元素 酒石酸 

分 类 号：O657.63[理学—分析化学]