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

样品经~（107）Ag&gt;、~（116）Cd&gt;、~（65）Cu&gt;、~（61）Ni&gt;、~（206）Pb&gt;、~（203）Tl&gt;和~（68）Zn&gt;等添加剂处理后，<HNO_3>在HC<10_4>和HF混合溶剂中于低温、高压下分解。将分解的样品加热至干燥，并将获得的残留物溶解在稀溶液中<HNO_3>。重金属以双硫腙的形式从溶液中萃取到氯仿中，并应用于质谱仪通过测量&lt;^（205）Tl&gt; / &lt;^（203）Tl&gt;，&lt;^（109）Ag&gt; / &lt;^（107）Ag&gt;，&lt;^（63）Cu&gt; / &lt;^（65）Cu&gt;、&lt;^（114）Cd&gt; / &lt;^（116）Cd&gt;、&lt;^（208）Pb&gt; / &lt;^（206）Pb&gt;、&lt;^（58）Ni&gt; / &lt;^（61）Ni&gt;和&lt;^（66）Zn&gt; / &lt;^（68）Zn&gt;。本方法可以测量微小的量，即，&lt;10^（-9）&gt; - &lt;10^（-11）&gt; g，准确度为1%。 ...更多信息 在超净通风室和100级加压室中的工作台上进行试验，后者由不锈钢双层壁构成，并具有甲氧基树脂覆盖的地板。试剂和水均采用亚沸蒸馏法提纯，质谱仪可检测到元素发射的质谱发射电流&lt;10^（-19）&gt; A，测量同位素比，变异系数精度为0.1%，加标物从田纳西州橡树岭国家实验室进口，美国，将每种掺料溶解在稀溶液中<HNO_3>并储存在紧塞的聚四氟乙烯或石英瓶中。将每个加标物的同位素丰度和摩尔浓度标准化为参比物质。该方法已成功应用于岩石、植物、动物、极地冰和海洋沃茨等环境样品以及工业材料的分析。少

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