碰撞反应池-电感耦合等离子体质谱(ICP-MS)法测定三氧化钨中钠钾铜砷钼锑磷硫

Determination of Sodium,Potassium,Copper,Arsenic,Molybdenum,Antimony,Phosphorus and Sulfur in Tungsten Trioxide by Inductivity Coupled Plasma Mass Spectrometry with Collision Reaction Cell

三氧化钨作为制备纯钨的原料,对其杂质元素含量的把控是非常有必要的。采用氨水溶解三氧化钨,通过柠檬酸对其不稳定杂质元素络合,用电感耦合等离子体质谱仪对其杂质元素进行测定。选择^(23)Na、^(39)K、^(65)Cu、^(75)As、^(95)Mo、^(121)Sb为待测同位素,通过调节氦气流量、以氦气碰撞模式消除质谱干扰;对于S和P两种元素,由于氨水环境中存在^(14)N^(16)OH^(+)及^(16)O_(2)^(+)的干扰,通过EXPEC 7350三重四极杆ICP-MS(ICP-MS/MS)中CRC可控的化学反应有效、可靠地消除多原子干扰。采用O_(2)作为反应气体在质量转移模式下分别测定质量数为47和48处的P(以^(31)P^(16)O^(+)形式测定)和S(以^(32)S^(16)O^(+)形式测定),配合内标元素Sc、Rh来消除基体效应,建立了碰撞反应池-电感耦合等离子体质谱法测定三氧化钨中钠、钾、铜、砷、钼、锑、磷、硫8种杂质元素的方法。在优化实验条件下,采用氨水对三氧化钨进行溶解,8种元素的检出限为0.01~0.17 mg/kg,定量限为0.03~0.56 mg/kg。8种元素测定结果相对标准偏差(RSD,n=6)均小于7.8%,加标回收率在97.0%~111%。方法可以快速、准确测定三氧化钨中钠、钾、铜、砷、钼、锑、磷、硫8种杂质元素,适用于工业生产流程中对三氧化钨质量的把控。

As a raw material for preparing pure tungsten,it is necessary to control the content of impurity elements in tungsten trioxide.In this study,tungsten trioxide was dissolved by ammonia water and the impurity elements were complex by citric acid.The impurity elements in tungsten trioxide were determined by inductively coupled plasma mass spectrometry.^(23)Na,^(39)K,^(65)Cu,^(75)As,^(95)Mo and ^(121)Sb were selected as the isotopes to be measured,and the mass spectrum interference was eliminated by adjusting the helium flow rate and using the helium collision mode.For the elements S and P,due to the interference of ^(14)N ^(16)OH^(+) and ^(16)O^(2)^(+) in ammonia environment,the multi-atomic interference was effectively and reliably eliminated through the controlled chemical reaction of collision reaction cell(CRC)in EXPEC 7350 ICP-MS(ICP-MS/MS).O 2 was used as the reaction gas to measure P(in the form of ^(31)P ^(16)O^(+))and S(in the form of ^(32)S ^(16)O^(+))at the mass 47 and 48 respectively in the mass transfer mode.The matrix effect was eliminated by combining with internal standard elements scandium and rhodium.A collision-reaction cell inductively coupled plasma mass spectrometry(ICP-MS)method was developed for the determination of eight impurity elements in tungsten trioxide,including sodium,potassium,copper,arsenic,molybdenum,antimony,phosphorus and sulfur.Under the optimized experimental conditions,tungsten trioxide was dissolved with ammonia water,the detection limits of eight elements were in the range of 0.01-0.17 mg/kg,and the limits of quantification were in the range of 0.03-0.56 mg/kg.The relative standard deviation(RSD,n=6)of determination results for eight elements were all less than 7.8%.The recoveries were between 97.0%and 111%.As a result,this method can be used for the rapid and accurate determination of eight impurity elements in tungsten trioxide,including sodium,potassium,copper,arsenic,molybdenum,antimony,phosphorus and sulfur.It is suitable for the quality control of tungsten trioxide in industrial production process.