电感耦合等离子体原子发射光谱法在铋矿石化学物相分析中的应用  

Application in the Phase Analysis of Bismuth Ores by Inductively Coupled Plasma Atomic Emission Spectrometry

作　　者：马海萍[1] 马玲[1] 黄勤[1] MA Haiping;MA Ling;HUANG Qin(Anhui Research Institute of Geological Experiment,Hefei 230001,China)

机构地区：[1]安徽省地质实验研究所

出　　处：《理化检验（化学分册）》2019年第12期1412-1416,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：国家重点研发计划“国家质量基础的共性技术研究与应用”重点专项(2016YFF020110304)

摘　　要：取铋矿石试样(0.5000g),用抗坏血酸0.5g和1mol·L-1盐酸溶液50mL,于25℃振荡提取30min,经致密滤纸过滤。取其滤液制成含20%(体积分数,下同)盐酸的试液100.0mL,用电感耦合等离子体原子发射光谱法(ICP-AES)测定其中的氧化矿铋的含量。将上述过滤中的滤纸及其不溶物用盐酸羟胺0.5g和50%盐酸溶液25mL于100℃水浴中浸取1h后,加水25mL并过滤,取其滤液制成含20%盐酸的试液100.0mL,用ICP-AES测定其中的辉铋矿铋。将上述过滤后所得滤纸及其不溶物移入瓷坩埚中,升温至800℃灰化2h。冷却后,将坩埚中的不溶物用盐酸-硝酸-水(3+1+2)混合酸20mL加热溶解并蒸缩至约10mL,加入20%盐酸溶液10mL并定容至50.0mL,用原子荧光光度计(AFS)测定其中自然铋矿铋的含量。另取铋矿石样品0.5000g,用上述混合酸20mL加热溶解并蒸缩至约10mL,加入20%盐酸溶液20mL,并定容至100.0mL,用ICP-AES测定其全铋量。ICP-AES校准曲线的线性范围在10.00mg·L-1以内,铋的检出限(3S/N)为3.0μg·g-1。用所提出方法和常用的比色法对3个样品中的全铋、氧化矿铋和辉铋矿铋分别进行测定,两种方法所得结果相互一致。A portion(0.500 0 g)of bismuth ore was extracted with 0.5 g of ascorbic acid and 50 mL of 1 mol·L-1 HCl solution by shaking for 30 min,at 25 ℃.After filtration on fine texture filter paper,the filtrate containing bismuth of oxide ore was collected to prepare a testing solution with a volume of 100.0 mL and containing20%(volume fraction,the same below)by volume of HCl,which was used for inductively coupled plasma atomic emission spectrometry(ICP-AES)determination for its Bi-content.The filter paper containing the insolubles was taken and extracted with 0.5 g of NH2OH·HCl and 25 mL of 20% HCl solution by heating in a water bath at100℃for 1 h.After which 25 mL of H2O were added and the mixture was filtered.The filtrate containing bismuth of bismuthinite was collected and made its volume to 100.0 mL containing 20% by volume of HCl,which was used for ICP-AES determination for its Bi-content.The filter paper with insolubles on it was transferred to a porcelain crucible and ashed for 2 hat 800℃.After cooling,the residue in the crucible was dissolved by heating with 20 mL of an acid mixture of HCl-HNO3-H2O(3+1+2),and when the solution was concentrated to a volume of ca.10 mL,10 mL of HCl(1+1)solution were added and its volume was made up to 50.0 mL with H2O.The solution was used for determination bismuth of native bismuth ore by AFS.Another portion(0.500 0 g)of the bismuth ore sample was taken and dissolved by heating with 20 mL of the above mentioned mixed acid.When the volume of the solution was reduced to ca.10 mL during the heating and evaporation,the heating was stopped and 20 mL of HCl(1+1)solution were added to the sample solution and its volume was made up to 100.0 mL,which was used for ICP-AES determination of total bismuth in the ore sample.Linearity range of the standard curve for ICP-AES determination was found within 10.00 mg·L-1,with detection of bismuth(3 S/N)3.0μg·g-1.Three bismuth ore samples were analyzed by the present method and the conventional colorimetric method separately,giving consist

关 键 词：电感耦合等离子体原子发射光谱法 铋矿石 化学物相 

分 类 号：O657.3[理学—分析化学]