Development of Isotope Dilution Surface Ionization Mass Spectromety and its Use as the Absolute Analytical Method for Heavy Metals in Standard Reference Materials

同位素稀释表面电离质谱的发展及其作为标准参考物质中重金属的绝对分析方法

• 批准号: 59470023
• 负责人: MUROZUMI Masayo
• 金额: $ 4.35万
• 依托单位: Muroran Institute of Technology
• 依托单位国家: 日本
• 项目类别: Grant-in-Aid for General Scientific Research (B)
• 财政年份: 1984
• 资助国家: 日本
• 起止时间: 1984 至 1986
• 项目状态: 已结题
• 来源: https://kaken.nii.ac.jp/en/grant/KAKENHI-PROJECT-59470023/
• 关键词: Isotope Dilution; Mass Spectrometry; Surface Ionization Mass Spectrometry; 絶対分析法

After spiking with <^(107)Ag> , <^(116)Cd> , <^(65)Cu> , <^(61)Ni> , <^(206)Pb> , <^(203)Tl> and <^(68)Zn> , the spiked sample was decomposed in a mixture of <HNO_3> ,HC <10_4> and HF at low temperature under pressure. The decomposed sample was heated to dryness and the residue obtained was dissolved in a dilute <HNO_3> solution. The heavy metals were extracted from an aliquot of the solution as their dithizonates into chloroform and applid to the mass spectrometer(Hitachi RMU-6) equipped with a surface ionization device incorporating a Re single filament.Their concentrations in the sample could be successively determined by measuring <^(205)Tl> / <^(203)Tl> , <^(109)Ag> / <^(107)Ag> , <^(63)Cu> / <^(65)Cu> , <^(114)Cd> / <^(116)Cd> , <^(208)Pb> / <^(206)Pb> , <^(58)Ni> / <^(61)Ni> and <^(66)Zn> / <^(68)Zn> with raising ionization temperature. The present method could measure minute amounts, i.e., <10^(-9)> - <10^(-11)> g of the above elements with an accuracy of 1%.Samples were all pr … More epared in a ultra clean draft chamber and on benches set in a class 100 pressurized room,the latter being constructed of stainless steel double walls and having a methoxy-resin covered floor. Reagents and water were all purified by sub-boiling distillation method.The mass spectrometer could detect an emitter current of <10^(-19)> A for the mass spectrum emitted by an element and measure the isotopic ratio with an accuracy of 0.1% in the coefficient of variations.The spikes were imported from the Oak Ridge National Laboratory, Tenn., U.S.A., and each spike was dissolved in a dilute <HNO_3> solution and stored in a tightly stoppered teflon or quartz bottle. The isotopic abundance and molar concentration of every spike were standardized to the reference materials. The working composite spike solution was prepared by mixing the stock solutions just prior to the use.The method has been applied with a good success to the environmental samples such as rocks,plants,animals,Polar ice and oceanic waters as well as industrial materials. Less

在添加了&lt；^(107)Ag&>、&lt；^(116)Cd&>；、&lt；^(65)Cut&>；、&lt；^(61)Ni&>；、&lt；^(206)Pb&>；、&lt；^(203)Tl&>；和&lt；^(68)Zn&>；之后，将添加的样品分解成&lt；HNO_3&>t；、HC&lt；10_4&gt；的混合物；在加压下的低温下，氢氟酸。分解的样品被加热到干燥，得到的残留物被溶解在稀释的硝酸溶液中。将样品中的重金属以二硫代萃取物的形式提取到氯仿中，在配有单丝表面电离装置的日立RMU-6质谱仪上，通过测量~(203)Tl&gt；、~(109)Ag&gt；/&lt；^(107)Ag&gt；/&lt；^(63)Cu&gt；/&lt；，&lt；^(114)Cd；/&lt；^(116)Cd&>；，&lt；^(208)Pd&>；/&lt；^(206)Pb&>；，&lt；^(58)Ni&>；^(61)Ni&>；和&lt；^(66)Zn&>；/&lt；^(68)Zn&>；随电离温度升高。本方法可以测定上述元素中的微量，即10^(-9)&gt；10^(-11)&gt；g，准确度为1%。样品均为Pr…更多的是在超净的通风室和设置在100级加压房间的长凳上，后者由不锈钢双层墙建造，地板上覆盖着甲氧基树脂。试剂和水都是用亚沸腾蒸馏法提纯的。质谱仪可以检测元素发射的发射极电流为~lt；10^(-19)&gt；A，并测量同位素比率，变异系数的精度为0.1%。这些尖峰从美国田纳西州橡树岭国家实验室进口，每个尖峰都溶解在稀释的&lt；HNO_3&gt；溶液中，储存在密闭的特氟龙或石英瓶中。将每一峰的同位素丰度和摩尔浓度与标准物质进行了标准化。在使用前将原液混合制成工作复合尖峰溶液，该方法已应用于岩石、植物、动物、极地冰层和海洋以及工业材料等环境样品中，取得了良好的效果。较少

项目成果

室住正世,中村精次,川原伸一郎: 分析化学.

室住正代、中村精二、川原真一郎：分析化学。

同位体希釈表面電離質量分析法の開発と標準物質中の重金属の絶対分析法の研究,室住正世: 文部省科学研究費補助金・一般研究B(昭和59〜61年度)報告書, 140 (1987)

同位素稀释表面电离质谱法的开发及标准物质中重金属绝对分析的研究，室住正世：文部科学省科学研究补助金/一般研究B（1980-1981） ）报告，140（1987）

室住正世: 分析化学. 35. 759-765 (1986)

室澄正世：分析化学。35. 759-765 (1986)

Bunseki Kagaku; M.Murozumi;Seiji Nakamura;S.Kawahara: "Isotope Dilution Surface Ionization Mass Spectrometry of Tl,Ag,Cu,Cd,Pb,Ni and Zn in purified water" Bunseki Kagaku. 35. 759-765 (1986)

文石化学；

室住正世,中村精次: 日本化学会誌.

Masayo Murozumi、Seiji Nakamura：日本化学会杂志。