炭素中微量元素分析研究进展

介绍了炭素材料中微量元素的测定方法,内容包括国际标准、国外先进标准、中国国家标准和行业标准。测定方法涵盖了重量法、分光光度法、原子吸收光谱法、电感耦合等离子体原子发射光谱(ICP-AES)、电感耦合等离子体质谱法(ICP-MS)、X射线荧光光谱分析法(XRF)等。并阐述了铝用炭素中微量元素测定标准样品的研制。     

ICP-AES和ICP-MS法测定光学玻璃中的15种稀土元素

采用Na₂O₂熔融分解样品,运用电感耦合等离子体发射光谱法（ICP-AES）和电感耦合等离子体质谱法（ICP-MS）测定光学玻璃中的稀土元素。采用该方法对国家一级标准物质GBW07158、GBW07159、GBW07160和GBW07161进行测定,其结果表明与标准值相符。方法选择性好、灵敏度好、定量准确,适用于光学玻璃中稀土元素的测定,结果令人满意。     

X射线荧光光谱测定石墨烯粉体中的杂质元素

石墨烯粉体是我国已具备规模化生产能力的主要石墨烯材料,针对其关键物理化学特性建立准确可靠的测量方法极为重要.开发了一种利用X射线荧光光谱（XRF）技术对石墨烯粉体中杂质进行快速、无损分析的检测方法,可实现对石墨烯粉体产品质量的便捷初判.研究了石墨烯粉体样品的不同测试形态,并通过将XRF测量结果与电感耦合等离子体-原子发射光谱（ICP-OES）、电感耦合等离子体-质谱（ICP-MS）和X射线能谱（EDX）等检测技术的测量结果进行对比,结果表明XRF可对石墨烯粉体样品中的非金属杂质S、Cl、Si、P及金属杂质Na、Mg、Ca、Fe、Cu、Ti、W、Cr等可靠检出,可实现对石墨烯粉体中杂质元素的快速、简便、无损低成本的定量测量.     

乙酸乙酯萃取-氢化物发生-原子荧光光谱法测定高纯金中硒和碲

硒和碲是高纯金中的主要有害杂质元素,依据国家标准GB/T 25933-2010规定高纯金中硒和碲是必检项目,所用仪器为电感耦合等离子体原子发射光谱仪(ICP-AES)[1-2]和电感耦合等离子体质谱仪(ICP-MS)[3],而这两种仪器成本和运行费用十分昂贵,且检出限较高。氢化物发生-原子荧光光谱法(AFS)具有灵敏度高、检出限低、仪器相对便宜的优点,已广泛应用于冶金、地质和生物样品分析[4-5]。     

电感耦合等离子体原子发射光谱法及电感耦合等离子体质谱法在二次资源分析中的应用进展

综述了2005-2012年间国内利用电感耦合等离子体原子发射光谱法(ICP-AES)和电感耦合等离子体质谱法(ICP-MS)测定二次资源中有关元素、特别是重金属元素的分析的最新进展,从样品前处理方法、仪器测定条件优化、技术联用等方面阐述了上述两种方法在二次资源重金属分析中的应用(引用文献40篇)。     

电感耦合等离子体原子发射光谱(ICP-AES)法测定镧玻璃废粉中稀土元素总量及配分量

建立了电感耦合等离子体原子发射光谱(ICP-AES)法测定镧玻璃废粉中稀土元素总量和配分量的分析方法。样品经碱熔融后分离硅、铝等元素及钠盐,用硝酸和高氯酸破坏滤纸和溶解沉淀,用ICP-AES法测定稀土元素总量和配分量。讨论了溶解样品条件、共存元素干扰等影响测定的各种因素。实际样品的稀土总量与草酸盐重量法测定结果一致,配分量与X-射线荧光光谱(XRF)法、电感耦合等离子体质谱(ICP-MS)法测定结果一致。RSD(n=11)在0.15%~1.1%,加标回收率为97%~105%。测定范围为:La_2O_3/REO(80%~98%);CeO_2/REO(2%~20%);REO(16%~70%)。方法能快速准确地测定镧玻璃废粉中稀土元素总量及配分量。     

化学计量及分析测试技术发展动态

介绍国内外标准物质、分析测试技术的发展状况,重点介绍了美国、加拿大近几年在痕量有机分析、光谱化学分析、高准确度库仑分析、电感耦合等离子质谱、炉内原子化等离子体发射光谱等方面的研究动态。     

氟化氢铵消解-电感耦合等离子体质谱(ICP-MS)法测定地球化学样品中的锂铷铯

建立了氟化氢铵消解样品,电感耦合等离子体质谱(ICP-MS)法测定地球化学样品中锂、铷和铯的方法。方法经国家土壤和水系沉积物标准参考物质验证,方法的检出限锂0.012μg/g、铷0.038μg/g、铯0.045μg/g,相对标准偏差锂0.41%～1.3%、铷0.32%～0.94%、铯1.3%～2.5%,能够满足地球化学样品分析测试的质量要求。并且有效地避免了铷和铯在样品消解过程中的挥发损失。方法具有操作简便、测试成本低、分析效率高等特点,适合于批量样品的分析测试。     

碱熔-电感耦合等离子体原子发射光谱(ICP-AES)法测定水泥标准物质中的氧化物含量

电感耦合等离子体原子发射光谱(ICP-AES)法与内标法的结合扩展了ICP-AES法的分析范围。采用氢氧化钠熔融样品,ICP-AES-内标法测定各类水泥标准物质样品中SiO_2、Al_2O_3、TFe_2O_3、MgO、TiO_2等氧化物的含量。实验结果表明,标准物质测定值与标准值吻合,6次平行样品测定相对标准偏差小于1.4%。方法一次熔样,纵向测定主常量元素,操作简单,快速,准确,为水泥标准物质的研制提供了另一种定值方式。     

超细样品的地质分析应用

采用X-射线荧光(XRF)、电感耦合等离子体光谱和质谱(ICP-AES/MS)技术,研究了超细地质分析样品(约800目)的分析方法和条件.结果表明,对于超细样品,XRF可直接粉末压片制样而不必高温熔融制样进行高精度的主、次组分测定;ICP-AES/MS的取样量可降至2 ～5 mg(仅为-200目样品的1/20 ～1/50),试剂用量大大减小,样品更易消解,不仅可节约成本,降低能耗,还显著减小了对环境的影响.讨论了发展超细样品分析的意义及对地质分析技术发展的可能影响.     

Trace element analysis of Geological Survey of Japan silicate reference materials: Comparison of SSMS with ICP-MS data and a critical discussion of compiled values

The concentrations of 29 trace elements have precisely been determined in 15 international silicate reference materials of the Geological Survey of Japan by spark source mass spectrometry (SSMS) and inductively coupled plasma-mass spectrometry (ICP-MS). The samples span a wide range of concentration levels. Most of the SSMS and ICP-MS values agree within analytical error down to the ppb concentration range. Of particular interest are the data for Nb, Y, Zr, Th, U in samples with low trace element concentrations (<1–10 ppm), for which published data are quite variable. The results obtained generally agree with those of modern sensitive analytical techniques (such as ICP-MS, HPLC), but are often much lower than standard XRF and compiled reference values. It is suggested that these discrepancies arise from calibration and analytical problems for standard XRF and ICP-MS and incorporation of these data into compiled values. More judicious selection of data based on analytical methodology and geochemical behaviour is required for samples which challenge the detection limits of standard analysis.     

Determination of metals in biofluids and tissues: sample preparation methods for atomic spectroscopic techniques

Several sample preparation methods unique to each instrumental technique exist for the elemental analysis of biological specimens, but no review or book has dealt with them. The present review is an attempt to fill this void and focuses on sample preparation methods unique to atomic and X-ray spectroscopic techniques. The techniques covered are: flame and electrothermal AAS, inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS) and X-ray fluorescence spectrometry (XRF) since these are most commonly used in trace element analysis of biological materials. The intent is not to present the procedural details for the various tissues or elements, but rather to highlight the methods which are unique to each instrument. The bibliography accompanying this review should aid the analytical chemist in his/her search for the detailed preparation protocols.     

Human albumin as a reference material for trace elements

Summary An investigation through interlaboratory comparison using different analytical techniques has been carried out in order to assess the suitability of a plasma protein solution as a source for a trace element reference material in clinical analysis. Reasonable agreement was obtained for a number of elements from the range studied: Al, Ba, Cr, Cu, Fe, Mg, Mn, Mo, Ni, Se, Sr, V and Zn. The techniques used included flame and furnace atomic absorption spectrometry (FAAS and ETA-AAS), furnace atomic emission spectrometry (ETA-AES), inductively coupled plasma atomic emission spectrometry (ICP-AES), inductively coupled plasma mass spectrometry (ICP-MS), and simultaneous multi-element atomic absorption spectrometry (SIMAAC). Results indicated that this plasma protein solution may prove useful as a source for a reference material covering trace element levels outwith the range found in normal human plasma.

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Humanalbumin als Referenzmaterial für Spurenelemente

     

Multielement analytical procedure coupling INAA, ICP-MS and ICP-AES: Application to the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco)

Instrumental neutron activation analysis (INAA), inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) were used for the determination of major and trace elements in sediment samples of the Bouregreg river (Morocco). The reliability of the results was checked, by using IAEA Soil-7 certified reference material. Results obtained by the three techniques were compared to control digestions efficiencies. A general good agreement was found between INAA and both ICP-MS and ICP-AES after alkaline fusion (ICPf). The ICP-MS technique used after acid attack (ICPa) was satisfactory for a few elements. A principal component analysis (PCA) has been used for analyzing the variability of concentrations, and defining the most influential sites with respect to the general variation trends. Three groups of elements could be distinguished. For these groups a normalization of concentrations to the central element concentration (that means Mn, Si or Al) is proposed.     

Matrix Digestion of Soil and Sediment Samples for Extraction of Lead,Cadmium and Antimony and Their Direct Determination by Inductively Coupled Plasma-Mass Spectrometry and Atomic Emission Spectrometry

An environmentally friendly and simple method has been developed for complete digestion of lead, cadmium and antimony from soil samples using a magnesium nitrate assisted dry ashing procedure. Statistical data for a series of experiments with standard reference materials are presented, and precision values are found to be comparable for inductively coupled plasma-mass spectrometry and for inductively coupled plasma-atomic emission spectrometry. From a single digest solution all analytes are quantified without involving any pre-concentration routes. Inter-method comparison of inductively coupled plasma-mass spectrometry (ICP-MS) and inductively coupled plasma-atomic emission spectrometry (ICP-AES) shows that the probability of the results being different is less than 99%.     

Double pulse laser induced breakdown spectroscopy applied to natural and artificial materials from cultural heritages : A comparison with micro-X-ray fluorescence analysis

The laser-induced breakdown spectroscopy (LIBS) is an applied physical technique that has shown in recent years its great potential for rapid qualitative analysis of materials. Thanks to the possibility to implement a portable instrument that perform LIBS analysis, this technique is revealed to be particularly useful for in situ analysis in the field of cultural heritages. The purpose of this work is to evaluate the potentiality of LIBS technique in the field of cultural heritages, with respect to the chemical characterization of complex matrix as calcareous and refractory materials for further quantitative analyses on cultural heritages. X-Ray Fluorescence (XRF) analyses were used as reference. Calibration curves of certified materials used as standards were obtained by XRF analyses. The LIBS measurements were performed with a new mobile instrument called Modì (Mobile Double pulse Instrument for LIBS Analysis). The XRF analyses were performed with a portable instrument ArtTAX. LIBS and XRF measurement were performed on both reference materials and samples (bricks and mortars) sampled in the ancient Greek–Roman Theatre of Taormina. Although LIBS measurements performed on reference materials have shown non linear response to concentrations, and so we were not able to obtain quantitative results, an integrated study of XRF and LIBS signals permitted us to distinguish among chemical features and degradation state of measured building materials.     

Double pulse laser induced breakdown spectroscopy applied to natural and artificial materials from cultural heritages: A comparison with micro-X-ray fluorescence analysis

The laser-induced breakdown spectroscopy (LIBS) is an applied physical technique that has shown in recent years its great potential for rapid qualitative analysis of materials. Thanks to the possibility to implement a portable instrument that perform LIBS analysis, this technique is revealed to be particularly useful for in situ analysis in the field of cultural heritages. The purpose of this work is to evaluate the potentiality of LIBS technique in the field of cultural heritages, with respect to the chemical characterization of complex matrix as calcareous and refractory materials for further quantitative analyses on cultural heritages. X-Ray Fluorescence (XRF) analyses were used as reference. Calibration curves of certified materials used as standards were obtained by XRF analyses. The LIBS measurements were performed with a new mobile instrument called Modì (Mobile Double pulse Instrument for LIBS Analysis). The XRF analyses were performed with a portable instrument ArtTAX. LIBS and XRF measurement were performed on both reference materials and samples (bricks and mortars) sampled in the ancient Greek–Roman Theatre of Taormina. Although LIBS measurements performed on reference materials have shown non linear response to concentrations, and so we were not able to obtain quantitative results, an integrated study of XRF and LIBS signals permitted us to distinguish among chemical features and degradation state of measured building materials.     

微波辅助消解-原子荧光法测定玻璃中的镉砷铅

光学玻璃中的各种元素对玻璃的光学性能有不同的影响。如加入镉可以提高玻璃折射率;砷的引入能增加玻璃的透光度,含铅玻璃具有低成本、高折射性等优点。但是镉、砷、铅均为有毒元素,玻璃加工和处理过程以及毒废弃物的处理都可能引起水、土壤、大气的污染并给人体带来一定的危害     

Assessment of the ICP-MS method using the interlaboratory QA study of two Polish soil RMs

 Under an international collaborative certification programme, two new Polish soil reference materials, PL-1 (loess) and BPGM-1 (sandy loam soil), were analysed for 34 trace elements including all the rare earth elements using the acid decomposition method and inductively coupled plasma - mass spectrometry (ICP-MS). After the certification by the organisers, the analytical data obtained at our institute were compared with the certified data. 'Z-score' values calculated for individual trace elements helped in the assessment of the quality of the data. While the majority of the data obtained on ICP-MS was very precise and accurate, some of the data especially for elements such as Zr, Hf and Nb suffered from incomplete dissolution of the sample and spectroscopic interferences. For some trace elements, certified data are not available for comparison. These features together with the usefulness of interlaboratory collaborative programmes and ICP-MS for the certification of soil reference materials are discussed. Received: 6 August 1999 / Accepted: 28 February 2000