3520ICP发射光谱仪维修二例

３５２０ＩＣＰ发射光谱仪维修二例房毅卓，原力（中国科学院青海盐湖研究所西宁８１０００８）３５２０型电感耦合等离子顺序扫描发射光谱仪，是由瑞士应用研究实验室（ＡＲＬ）生产的高速自动分析装置，主要应用于冶金、地质、石油、卫生和科研等部门的元素分析。以下介...     

美国热电公司获三项年度创新产品奖并已成为中国最大的分析仪器产品和服务供应商

世界领先的分析仪器研发和制造商“Thermo”公司在“2004--2005年度仪器新产品发布论坛”荣获三项新品奖，包括DFS高分辨双聚焦磁质谱、LTQ Orbitrap组合式质谱仪和iCAP-6000系列等离子体发射光谱仪。这次评选以“聚焦仪器新产品，促进科技创新”为主题，旨在帮助国内仪器用户、厂商及业内人士及时了解近年在中国市场推出的仪器新品，这些仪器被广泛用于环境、石化、冶金、食品饮料、医药医学、地球化学和水泥行业。     

ICP-AES法测定10种蒙成药中四种重金属元素的含量

目的测定十种蒙成药中As、Pb、Hg、Cd 4种重金属元素的含量。方法采用V（HNO3）＋V（H2O2）=5＋3为溶样试剂,微波消解与电感耦合等离子体发射光谱仪联用。结果表明测定的各元素检出限介于0.048-1.036μg·L^-1之间,加标回收率在94.5%-103.6%之间,RSD〈2.4%。结论该法简单、快速、准确,适合同时测定食品中的元素。     

用国产单道扫描电感耦合等离子体发射光谱仪分析海绵铂

铂族元素具有相似的电子层结构和化学性质,使很多试剂能同时与多种铂族元素发生相似反应并产生相互干扰,很难找到特效的试剂,因此分离和测定十分困难.我国贵金属行业测定海绵铂纯度用直流电弧发射光谱法或进口电感耦合等离子体原子发射光谱仪.     

美国ESA公司推出新型LeadCareⅡ血铅检测仪

美国ESA生物科学公司最近推出一种新型LeadCareⅡ血铅检测仪，可以快速测量患者血液中的铅含量，能在3min之内得到结果。这种检测仪主要用于筛查儿童和成人血液中对人体有害的铅，可以使用手指血或者静脉全血。用该仪器检测患者当场就能够得到结果，而传统血液检测方法则需要2周。     

偏硼酸锂-四硼酸锂熔融-电感耦合等离子体原子发射光谱(ICP-AES)法测定石膏中多组分含量

石膏在我国储量丰富,应用广泛,快速准确分析其成分含量对石膏资源的综合利用具有重要意义。针对酸溶法无法测定SiO2,碱熔法无法测定K2O、Na2O的问题,本文建立一种偏硼酸锂-四硼酸锂熔融-电感耦合等离子体发射光谱法同时测定石膏中CaO、SO3、Al2O3、Fe2O3、MgO、TiO2、K2O、Na2O、SiO2含量。实验优化了熔剂用量、熔融温度,结果表明采用试样与偏硼酸锂-四硼酸锂混合熔剂质量比例1：5,在铂金坩埚中1000 ℃熔融10 min,在超声条件下,于50 mL 10 %盐酸中浸取熔融物,能够有效分解试样而浸取待测组分。向标准溶液系列中加入偏硼酸锂-四硼酸锂-盐酸基体溶液以消除基体对测试结果的影响。各待测组分的校准曲线的相关性系数均大于0.9990,方法检出限在3~292 μg/g范围内;采用实验方法分别对国家一级标准物质GBW03109a、GBW03110和实际样品进行测定,标准物质的5次平行测试的相对标准偏差在0.14 %~8.86 %之间,测定结果的相对误差在0.03~8.75 %之间,测试结果与标准值无显著性差异;实际样品中各成分测定值的RSD（n=5）为0.24~8.80 %。该方法操作简单、准确度高、精密度好、检出限低,可以同时测定石膏中的多组分含量,能够为石膏资源综合利用调查评价提供一定的技术支撑 。     

科学家成功研制全半导体室温太赫兹时域光谱仪

英国的研究人员已经公布了全半导体室温太赫兹时域光谱仪。该小组认为,这是第一个使用全半导体结构的光谱仪,相比于传统的基于超激光的设计,具有节约成本和规模小的优势。南安普敦大学的VasileiosApostolopoulos在optics.org提到:传统的太赫兹时域光谱仪是基于钛蓝宝石激光器的基础上设计的,它虽然具有优良的性能,但成本昂贵、规模较大。目前使用的是由南安普敦的AnneTropper研究小组开发的一种微型半导体激光源,它有非常高的重复率,并在未来的一两年内,可能会产生低于200飞秒的脉冲。通过全半导体的方法,研究小组开始制造垂直外腔表面发射激光器(VECSEL),在波长为1044nm时可以发射480飞秒的脉冲。腔体包括一个光学斯塔克半导体可饱和吸收镜(SESAM)作为锁模元件。垂直外腔表面发射激光器用于传统的时域光谱设置,它可以照亮一组光敏天线。Apostolopoulos和他的同事们报告说,他们可以检测到超过带宽0.1至0.8THz的辐射,并有充分确定水吸收谱线的方案。Apostolopoulos评论说:“同样的技术可被用来制造太赫兹光敏天线和垂直外腔表面发射激光器的元件,如量子阱增益样品和半导体...     

元素缺乏分四阶段

起始缺乏阶段：其特征为由于摄人不足而引起的元素本身的代谢变化，这是在供应不足的一段时问内所起的代偿变化，因此检查不出生物结构和功能紊乱。起始缺乏阶段在增加元素摄入后可恢复到正常状态；如果摄入量仍然保持在边缘水平，可能持续整个生命期；当摄人更严重限制时可导致第二阶段。起始缺乏阶段本身对健康没有不利后果，但它代表缺乏的危险性增加，安全界限降低。     

元素缺乏分四阶段

起始缺乏阶段：其特征为由于摄入不足而引起的元素本身的代谢变化,这是在供应不足的一段时间内所起的代偿变化,因此检查不出生物结构和功能紊乱。起始缺乏阶段在增加元素摄入后可恢复到正常状态;如果摄入量仍然保持在边缘水平,可能持续整个生命期;当摄入更严重限制时可导致第二阶段。起始缺乏阶段本身对健康没有不利后果,但它代表缺乏的危险性增加,安全界限降低。     

氢化物发生与ICP/AES联用后等离子体的性质研究

本文通过测量电子密度ｎｅ,电子温度Ｔｅ,激发温度Ｔｅｘｃ及谱线强度,将氢化物进样同水溶液常规气动雾化进样对比,研究了氢化物进入ＩＣＰ后,对等离子体性质的影响。结果表明,由于氢化物的引入,ＩＣＰ的激性能得到了改善。     

Bestimmung von Wolfram mit dem induktiv gekoppelten Plasma (ICP)

Zusammenfassung Die relativen Intensitäten von 231 Spektrallinien des Wolframs im Ar-ICP werden angegeben. Anregungs- und Gastemperaturen unter den Meßbedingungen sowie die Einflüsse von Generatorleistung, Beobachtungshöhe und Alkaligehalt sind beschrieben. Zur Wolframbestimmung werden die Linien W I 400,875 nm, W I 407,436 nm, W II 257,144 nm und W II 239,709 nm empfohlen und ihre spektralen Störungen angegeben. Die Nachweisgrenzen liegen für verschiedene Matrices im Bereich um 0,02g/ml W. Probenvorbereitungen für Legierungen, Konzentrate und Gesteine werden mitgeteilt.

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Determination of tungsten with the inductively coupled plasma (ICP)

Summary The relative intensities of 231 tungsten lines in the Ar-ICP are listed. Excitation and gas temperatures under the measurement conditions have been determined and the influences of generator power, observation height and alkali concentration on the intensities investigated. The lines W I 400,875 nm, W I 407,436 nm, W II 257,144 nm and W II 239,709 nm are recommended for analytical use and their spectral interferences are specified. The detection limits are about 0.02g/ml W in various matrices. Sample preparations for alloys, concentrates and silicate rock are described.

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Wir danken der Deutschen Forschungsgmeinschaft und dem Fonds Der Chemischen Industrie für finanzielle Udterstützung.     

Bestimmung von Hafnium mit dem induktiv gekoppelten Plasma (ICP)

Zusammenfassung Die relativen Intensitäten von 198 Spektrallinien des Hafniums im Ar-ICP von 2 kW werden angegeben. Für die 9 analytisch geeignetsten wurden Koinzidenztabellen mit allen Störlinien im Abstand von ±60 pm erstellt. Sie enthalten die im ICP gemessenen Werte IEC (interferent equivalent concentration) und CCR (critical concentration ratio) für insgesamt 115 Linien von allen 34 möglicherweise störenden Elementen. Keine hinreichend intensive Hf-Linie ist frei von jeglicher spektraler Störung. Am Beispiel zweier NBS-Referenzproben werden Beispiele zur Errechnung der jeweils am wenigsten schlechten Hf-Linie gegeben. Die aus NBS-Intensitäten für das ICP umgerechneten CCR-Daten weichen von den gemessenen Werten oft um 1 bis 2 Größenordnungen ab und erweisen sich als wenig brauchbar. Parametereinflüsse auf das Linie/Untergrundverhältnis werden diskutiert.

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Determination of hafnium with the inductively coupled plasma (ICP)

Summary The relative intensities of 198 hafnium lines in the Ar-ICP are listed. Spectral interference tables are given for the 9 analytically best lines, covering the range of ±60 pm around the Hf-lines. They include measured (not calculated) data of the interferent equivalent concentrations (IEC) and the critical concentration ratios (CCR) for 115 lines of all 34 possibly interfering elements. In many cases, these IEC- or CCR-data differ by 1 or 2 orders of magnitude from those calculated from intensities observed in the NBS-copper arc. Since no intense Hf-line is free from spectral interferences, examples are given for the calculation of the most suitable line for a known matrix.

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Herrn Prof. Dr. H. Monien zum 60. Geburtstag gewidmet

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Die Publikation beruht auf der Diplomarbeit von K. Pose [26]. Wir danken der Deutschen Forschungsgemeinschaft und dem Fonds der Chemischen Industrie für finanzielle Unterstützung.     

电感耦合等离子体光谱仪器技术进展与现状

介绍了电感耦合等离子体光谱分析仪器技术的发展历程及主要技术特点,并分别评述了目前三种典型ICP光谱仪器及其技术现状和新进展,它们分别是：顺序扫描型ICP光谱仪、同时型ICP光谱仪及顺序-同时型ICP光谱仪。最后介绍了几种有较好应用前景的光谱新光源：静态高灵敏ICP(SHIP)光源,高功率微波等离子体光源,电容耦合等离子体光源,炬内进样短炬管等。     

Multielementbestimmung der Seltenen Erden durch Atomemissionsspektrometrie (AES) im induktiv gekoppelten Plasma (ICP)

Summary Multielement analysis of rare earth elements by use of AES-ICP is investigated in detail for monazite sand, xenotime and gadolinite. After dissolution of the minerals the analysis is carried out without chemical separation. Optimum conditions are selected. The influence of interfering elements is checked separately and characterized by IEC values. The method is most suitable for the analysis of solutions, because this can be performed immediately (i.e., without chemical separation) and takes little time.Furthermore, a method of multielement analysis of the lanthanides on the basis of their natural abundance is described and discussed. In this method only several selected elements are analyzed directly, whereas the concentrations of the other elements are determined by interpolation. The application of this method is also demonstrated for the minerals mentioned above.

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Herrn Prof. Dr. W. Fresenius aus Anla\ seines 75. Geburtstages gewidmet     

Introducing wet aerosols into the static high sensitivity ICP (SHIP)

A demountable design of the static high sensitivity ICP (SHIP) for optical emission spectrometry is presented, and its use as an excitation source with the introduction of wet aerosols was investigated. Aerosols were produced by standard pneumatic sample introduction systems, namely a cross flow nebulizer, Meinhard nebulizer and PFA low flow nebulizer, which have been applied in conjunction with a double pass and a cyclonic spray chamber. The analytical capabilities of these sample introduction systems in combination with the SHIP system were evaluated with respect to the achieved sensitivity. It was found that a nebulizer tailored for low argon flow rates (0.3–0.5 L min⁻¹) is best suited for the low flow plasma (SHIP). An optimization of all gas flow rates of the SHIP system with the PFA low flow nebulizer was carried out in a two-dimensional way with the signal to background ratio (SBR) and the robustness as optimization target parameters. Optimum conditions for a torch model with 1-mm injector tube were 0.25 and 0.36 L min⁻¹ for the plasma gas and the nebulizer gas, respectively. A torch model with a 2-mm injector tube was optimized to 0.4 L min⁻¹ for the plasma gas and 0.44 L min⁻¹ for the nebulizer gas. In both cases the SHIP system saves approximately 95% of the argon consumed by conventional inductively coupled plasma systems. The limits of detection were found to be in the low microgram per litre range and below for many elements, which was quite comparable to those of the conventional setup. Furthermore, the short-term stability and the wash out behaviour of the SHIP were investigated. Direct comparison with the conventional setup indicated that no remarkable memory effects were caused by the closed design of the torch. The analysis of a NIST SRM 1643e (Trace Elements in Water) with the SHIP yielded recoveries of 97–103% for 13 elements, measured simultaneously. Photo of the SHIP-III during operation     

Inductively coupled plasma mass spectrometry (ICP MS): a versatile tool

Inductively coupled plasma (ICP) mass spectrometry (MS) is routinely used in many diverse research fields such as earth, environmental, life and forensic sciences and in food, material, chemical, semiconductor and nuclear industries. The high ion density and the high temperature in a plasma provide an ideal atomizer and element ionizer for all types of samples and matrices introduced by a variety of specialized devices. Outstanding properties such as high sensitivity (ppt-ppq), relative salt tolerance, compound-independent element response and highest quantitation accuracy lead to the unchallenged performance of ICP MS in efficiently detecting, identifying and reliably quantifying trace elements. The increasing availability of relevant reference compounds and high separation selectivity extend the molecular identification capability of ICP MS hyphenated to species-specific separation techniques. While molecular ion source MS is specialized in determining the structure of unknown molecules, ICP MS is an efficient and highly sensitive tool for target-element orientated discoveries of relevant and unknown compounds. This special-feature, tutorial article presents the principle and advantages of ICP MS, highlighting these using examples from recently published investigations.     

高盐食品中痕量铅的流动注射-氢化物发生-等离子体原子发射光谱(FI-HG-ICP-AES)在线测定

本文报道流动注射（ＦＩ）－氢化物发生（ＨＧ）与多道等离子体光谱仪联用在线测定高盐食品中痕量铅．考察了氯化钠对铅信号的影响及实验参数的选择．铅的检出限和相对标准偏差分别为１．６ｎｇ／ｍＬ和１．２％，进样频率为７５ｈ－１．方法用于两种盐制蔬菜中铅的测定，加入回收率为９７－１０１％．