同位素稀释多接收电感耦合等离子体质谱法测定血铅

采用同位素稀释多接收电感耦合等离子体质谱（ID-MC-ICP-MS）法测定血铅。运用同位素稀释法测得整个实验的流程空白Pb的浓度平均值为5.6 ng。对SRM 955b level 1和SRM 955b level 3标准血样进行分析,测得血样浓度分别为40.2、207.8 μg•L^-1,测定值落在血样参考值范围之内,证明该方法有效、可靠。利用建立的血铅分析方法,参加了络合型血铅标准物质的定值,得到3种血铅标准样中铅的浓度分别为（102.7±5.5）、（181.7±4.0）、（304.1±3.9） μg•L^-1。     

多接收电感耦合等离子体质谱法测定Nd同位素标准物质

The precision and accuracy of Nd isotope analysis using multicollector-inductively coupled plasma mass spectrometry (MC-ICPMS) is verified through repeated measurements of standard reference materials of JMC Nd2O3 and GBW04419. A mixed solution of Nd separated from hundreds of geological samples is measured for 143Nd/144Nd ratio, which produces excellent long-term repeatability. This solution, named as CAGS-Nd-1, can be used as an in-house reference material for monitoring instrument stability during Nd isotope measurements.     

多接收电感耦合等离子体质谱法测量UTB系列铀同位素工作标准同位素比值

In order to analyze uranium isotopic ratios accurately by mass spectrometry, reference materials are used to correct the mass bias and detector bias. Isotopic ratios of UTB U Series working reference material which have been developed in our country last century were measured by multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS). In this report, the isotopic ratios were corrected by measuring CRM U series reference material. Hydride rate UH^＋/U⁺ of different sample introduction devices were studied. The linearity of the Daly detector was also investigated. Preliminary results have indicated that there is no significant difference between the measurement value and reference value.     

多接收电感耦合等离子体质谱法测量钐同位素丰度

多接收电感耦合等离子体质谱(MC-ICPMS)作为第三代等离子源质谱计在近年来得到了国内外质谱界的关注,它在同位素丰度比的测量中发挥着越来越重要的作用.虽然在测量精度方面已经可以和最先进的TIMS相媲美,而由于干扰因素过多,系统偏差较大,使人们对它的测量准确性存在着诸多的疑问[1,2].为研究MC-ICPMS在同位素丰度测量中系统偏差的校正及其可溯源性,本工作拟选用具有7个同位素的钐作为研究对象,采用高浓缩同位素混合的绝对测量法对其系统偏差进行校正,并与表面热电离质谱(TIMS)的测量结果进行比较.     

多接收电感耦合等离子体质谱法测量痕量钚同位素

The isotopic analysis of 232Pu plutonium in 5×10-12 g/g samples using a multi-collector inductively coupled plasma mass spectrometry (MC-ICPMS) is described. IRMM-290b and uranium (UTB750) were used to correct the metrical data, and the analytical precision is about 0.5%.     

多接收电感耦合等离子体质谱法精确测量

经过核燃料后处理得到的铀产品中含有极微量钚杂质, 对其同位素组成进行分析有利于对应铀材料的溯源。本工作在铀钚化学分离的基础上,对影响MC-ICP-MS法精确测量痕量钚同位素丰度比值的仪器条件进行了优化,研究了仪器分辨率、离子提取模式的选择、“背景和干扰”等参数的影响,探索研究了MC-ICP-MS上质量偏倚的校正方法。对选择的两个后处理铀产品中痕量钚同位素比进行了测量,当铀钚比例达10¹⁰时,测得的²³⁹Pu/²⁴⁰Pu相对不确定度优于5％。并且建立了在MC-ICP-MS上测量ng•L^-1量级钚同位素丰度比值的方法。     

高分辨电感耦合等离子体质谱法测定大气气溶胶中铅同位素比值

采用高分辨电感耦合等离子体质谱技术(HR-ICP-MS)分析了48个不同季节大气气溶胶颗粒样品中铅同位素比值,为中国城市铅污染源研究提供数据.样品采至中国北京和长岛地区(2002年～2003年期间).206Pb/207Pb和208Pb/207Pb的10次测定标准偏差为0.05%～0.19%.     

多接收电感耦合等离子体质谱法测定79Se

The analysis of ⁷⁹Se in high radioactive waste using a multi-collector inductively coupled plasma mass spectrometry (MC-ICP-MS) is described, Hexapole collision cell was used to remove argide-based interferences, which have always presented a problem to the measurement of certain elements, such as Ca, Cr, Fe, and Se. ⁷⁸SeH was deducted from the measurement of ⁷⁹Se.     

多接收电感耦合等离子体质谱法测量分离样品中Li同位素丰度比

Isotopic abundance ratios in chemical exchange separation sample were determined using GV IsoProbe multicollector-inductively coupled plasma mass spectrometry (MC-ICP-MS). GV IsoProbe MC-ICP-MS was calibrated by the lithium nature isotope reference material. Calibrated GV IsoProbe MC-ICP-MS was used to determine lithium isotope abundance ratio which was produced through chemical change separation.     

电感耦合等离子体质谱法测定土壤中的多元素

A method was studied for determination of multi-elements in soil by using microwave digestion-ICP-MS. The digestion condition was optimized from digestion system, proportion of acids and digestion procedure. The potential interference was eliminated. The method detection limits for all elements were between 0.000 5-38.08 μg/g.     

多接收双聚焦等离子体质谱法测定高精度同位素比

采用 VG Axiom型多接收双聚焦等离子质谱仪 ( MC-ICPMS)测定 Nd、Pb、U同位素比值 ,应用指数公式对测定的结果进行质量歧视校正。结果表明 :测定参考物质 Ames Nd获得的钕同位素比值为 14 3 Nd/14 4 Nd=0 .5 1 2 1 44± 0 .0 0 0 0 1 5 (确认值为 0 .5 1 2 1 3 5 )、14 5Nd/14 4 Nd=0 .3 4841 7± 0 .0 0 0 0 1 9(确认值为 0 .3 4841 8) ;测定参考物质 NIST SRM981获得的铅同位素比值为 2 0 8Pb/2 0 4Pb=3 6.71 1 4± 0 .0 0 81、2 0 7Pb/2 0 4Pb=1 5 .4886± 0 .0 0 3 8、2 0 7Pb/2 0 6Pb=0 .91 44 5 6± 0 .0 0 0 0 3 9、2 0 6Pb/2 0 4Pb=1 6.93 82± 0 .0 0 3 1、2 0 8Pb/2 0 6Pb=2 .1 660 1± 0 .0 0 0 1 6;测定参考物质 NIST SRM 0 1 0获得的铀同位素比值为 2 3 4 U/2 3 8U =0 .0 0 0 0 5 46±0 .0 0 0 0 0 0 3 (确认值为 0 .0 0 0 0 5 46)     

热表面电离同位素稀释质谱法测定红酒中痕量铅

采用热表面电离同位素稀释质谱法 ( TI-IDMS)对国际计量委员会 ( CIPM)物质量咨询委员会 ( CCQM)组织的“CCQM-P1 2国际比对 -红酒中痕量铅”进行了准确测量。研究了铅含量低、样品前处理和空白污染等方面的问题 ,建立了适用于热表面电离同位素质谱分析的红酒中痕量铅化学前处理方法 ,同时对测量结果的不确定度进行了分析和评定     

碰撞池-多接收电感耦合等离子体质谱分析硅同位素的方法研究

通过更换仪器进样系统、改变溶液基体、调节碰撞气的种类和流量以及调节质量分辨率等参数,建立了碰撞池-多接收电感耦合等离子体质谱（Collision Cell-MC-ICP-MS）测定硅同位素丰度组成的分析方法。实验结果表明:使用PFA雾化器、Pt锥和蓝宝石材质的矩管可有效降低仪器本底;调节狭缝宽度、中心杯位置等可提高仪器的质量分辨率,实现硅同位素离子与同量异位素干扰离子在一定程度上的分离;选择氖气（Ne）和氩气（Ar）的混合气作为碰撞气、降低溶液中四甲基氢氧化铵（TMAH）浓度等能有效降低多原子离子的干扰。在此基础上,分析了样品WASO 04和GBW(E)080272中硅同位素的丰度组成,同位素丰度比R_30/28的测量精度达到0.02%。将样品WASO 04作为参考标准时,样品GBW(E)080272中的硅同位素分馏系数δ³⁰Si为-1.57‰。     

仪器对液相色谱-同位素稀释质谱测试结果的影响

以同位素稀释质谱法测定奶粉中氯霉素为例,比较了近几年商品化的API5000、Q-trap5500、Agilent 6490、Waters XEVO TQS 4种高效液相色谱-串联三重四极杆质谱仪（LC-MS/MS）的关键指标,并重点研究了由于离子源设计导致的样品基质中残留化合物对氯霉素及其氘代同位素试剂测量的基质效应差异。通过比较测量氯霉素的线性、灵敏度和精密度等指标,发现这4种仪器测量氯霉素的线性和检测灵敏度差异不大。在0.2~1.0 ng/g痕量浓度范围分析时,在低浓度点时,不同仪器上两种化合物的离子化差异较大,测量精密度在1.0%~9.8%之间;在高浓度时,仪器对目标物响应的影响较小。考察了各仪器对不同基质溶液所产生的基质效应,发现在所有仪器上被测物与其同位素稀释剂的响应均存在差异,且随浓度增大差异越来越明显;不同预处理方法下得到的样品基质溶液,在不同仪器可能出现抑制或增强两种相反的基质效应现象,且强度差异也较大。表明基质中不同类型的干扰物在不同类型的离子源上的离子化模式与机理可能存在较大差异,从而导致同位素试剂之间响应的差异,在准确测量中必须分别进行基质效应的验证与确认。     

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用同位素稀释电感耦合等离子体质谱法测定海水中的痕量铅

5 -磺基 -8-羟基喹啉用作微柱流动注射在线分离、富集和电感耦合等离子体质谱分析流程中的螯合剂 ,与铅反应生成铅螯合物被硅酸镁吸附剂吸附 ,实现痕量铅的分离、富集。对联用系统的参数如螯合剂用量、淋洗条件、洗脱条件和进样量等进行最优化 ,测定标准水样和加标海水的铅回收率分别为 1 0 1 %和 97.9% ,相对标准偏差为± 0 .98% ,检测限为 0 .2 0 4 μg/ L。可应用于生物、环境等高盐样品中铅的在线分离测定