Determination of impurities in magnesium niobate by slurry introduction axially viewed inductively coupled plasma optical emission spectrometry

A simple preparation scheme is described for the quantitative analysis of a magnesium niobate sample using slurry introduction axially viewed inductively coupled plasma optical emission spectrometry. Relationships between the stability of slurries and the conditions, such as particle size, pH, dispersant and amount of dispersant, were investigated experimentally. The MgNb₂O₆ slurry sample was prepared by adding the dispersant sodium polyacrylate and agitation in an ultrasonic bath to ensure good dispersion. Under optimization of pH and amount of dispersant, an analysis of minor and trace impurities (Ba, Ca, Cr, Cu, Fe, Mn, Ni, Pb) in magnesium niobate was accomplished. Applying a paired t test, we showed that the results were in agreement at a 95% confidence level with the reference values obtained by a fusion method for a magnesium niobate sample, which verified that the calibration curves could be established by aqueous standards. Analytical results demonstrate that the factors that affected the accuracy of determination for MgNb₂O₆ are mainly the particle size of the sample and the stability of slurry.     

悬浮液进样电感藕合等离子体发射光谱中颗粒的输运和蒸发行为

以碳化硼为例,研究了悬浮液雾化进样中的粒子在传输和蒸发过程中的行为,并对分析结果出现负偏离的原因进行了详细探讨.对比悬浮液颗粒的原始粒径分布和经过传输过程后的粒径分布,获得到达等离子体的颗粒粒径上限小于10 Am.样品中存在的部分超大粒径的颗粒(d>>10 μm)会严重影响可传输区域颗粒(d<10 μm)的质量运输效率...     

电感耦合等离子体发射光谱法测定植物油中的磷

用电感耦合等离子体发射光谱法(ICP-AES)测定了植物油中的磷.采用多谱线拟合技术(MSF)校正了铜对P213.617 nm和P214.914 nm光谱干扰.比较了活性炭炭化灰化法和微波消解法两种样品前处理方法对分析结果的影响.结果表明这两种前处理方法所得结果都能与国标磷钼蓝分光光度法的分析结果吻合,其中活性炭炭化灰化法的方法检出限(0.053 mg/kg)较微波消解法的方法检出限(0.42 mg/kg)更低,所以对低含量的磷的检测结果其相对误差及精密度更好.该法应用于植物油中磷的测定.     

ICP-AES中乙醇作用机理的定量研究Ⅰ.乙醇干扰函数和各种干扰因素的相对贡献

本文应用Einstein-Boltzmann-Saha方程和Raoult-Clausius-Clapeyron方程,定量地考察了乙醇对电感耦合等离子体(ICP)中各种干扰因素的影响及各干扰因素对乙醇干扰效应(用干扰因子表示)的相对贡献。实验结果表明,Boltzman因子项和活度系数项的变化是乙醇增敏效应的主要来源。由实验结果分别提出了提升量、校正提升量变化后的干扰因子和活度系数项与乙醇浓度的关系方程。     

Hair analysis and the early detection of imbalances in trace elements for members of expeditions in Antarctica

In the framework of the Human Biology and Medicine Project of the National Program for Research in Antarctica (Programma Nazionale di Ricerche in Antartide, PNRA) a study was undertaken to explore the suitability of trace element determination in human hair as a tool for the early detection of the impact of extreme environmental conditions on the health of members of the Italian and French expeditions. This study included three campaigns, namely, the 1995–1996 expedition to the Italian base of Terra Nova Bay, as well as the 1997–1998 and 1998–1999 expeditions to both the Italian base of Terra Nova Bay and the Italian–French base of Dome C. Sampling of hair of participants in the expeditions was carried out both prior to departure and at the end of the period spent at the bases. As regards storage, pre-treatment and analysis of hair samples they were performed in accordance with previously established procedures. Acid-assisted microwave digestion was adopted as the best approach for preparing solutions for subsequent analysis by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry. In the first part of this study, only the elements Ca, Cu, Fe, Mg and Zn were selected, while at a later stage it was decided to also include Co, Cr, Mn, Mo and Ni. Experimental results were subjected to basic statistical analysis to detect possible significant differences in element concentrations that occurred during the sojourn at the bases, with a view to identify possible remedial action to minimize adverse consequences.     

利用多功能LB-HG型雾化氢化物发生器与电感耦合等离子体原子发射光谱联用测定人发中砷、锑、汞、铅

采用多功能ＬＢ－ＨＧ型雾化氢化物发生器与ＩＣＰ－ＡＥＳ联用，测定砷、锑、铅。较传统的气动雾化法，检出限降低了１０～１００倍。标准人发样品的分析结果与推荐值相吻合。     

ICP－AES中无机酸效应与OH带强度相关性研究

本文用干扰因子法对ＩＣＰ－ＡＥＳ中无机酸的非光谱干扰进行了讨论，特别是对元素干扰因子与ＯＨ带干扰因子之间的相关性作了较深入探讨。由此建立了元素干扰因子与ＯＨ带干扰因子之间的线性回归方程，并以ＯＨ带作为通用内参比线来校正无机酸效应引起的干扰。为了验证此种校正方法是否可行，我们对不同酸浓度的人工合成样品进行校正，校正后的回收率在８０％—１２０％之间，基本符合痕量分析要求，证明此种校正方法是可行的。     

Determination of rhodium: Since the origins until today: ICP-OES and ICP-MS

Rh is contained in catalyst in much smaller quantities than Pt. For this reason, the database for this metal with respect to emissions from catalytic converters is much smaller than that for platinum, thus precluding a quantitative risk assessment.Accurate determinations of the rhodium have always been difficult tasks. The metal is often present at trace levels in sample types of complex composition. This situation has improved recently due to developments of instrumental methods and their applications to analyses of rhodium in a variety of matrices. The purpose of this review is to describe the analytical sensitive methods by inductively coupled plasma spectrometry.     

乙醇溶液电感耦合等离子体发射光谱研究 Ⅲ.关于背景和氰分子辐射的某些观察

乙醇导入ICP导致等离子体连续辐射(即复合辐射和轫致辐射)强度减小和分子带(主要是CN带)强度增大。分子带的影响随波长而异,所以在正常分析区不同波长处的总背景强度随乙醇浓度增大有三种变化趋势:单调增大、单调减小或在某个乙醇浓度时出现最小值。详细研究了CN带强度与ICP工作参数的关系以及CN带对稀土元素和钪灵敏线的干扰,指出适当增加炬管的外管长度可以有效地抑制CN带。     

Influence of hydrogen gas over the interference of acids in inductively coupled plasma atomic emission spectrometry

The effect of hydrogen gas on the plasma and its influence on acid interferences in plasma atomic emission spectrometry was studied. The study was performed with HCl and HNO₃ in the concentration range of 0–2 mol l⁻¹. Vanadium and magnesium were used as test elements, the study was extended to other several elements. The effects of hydrogen gas on the plasma were studied by measuring excitation temperature, electron number density and the ionic-to-atomic line intensity ratio. The net effect of hydrogen was an increase in electron density and ionic to atomic line intensity ratio. A small increase in the excitation temperature was observed. The signal suppression for ionic lines causes by mineral acid was reduced when small amounts of hydrogen was introduced into the plasma as sheathing gas. This effect was attributed to the increase in plasma electron density.     

电感耦合等离子体光谱/质谱联机同时测定多金属结核中常量、微量、痕量元素

采用电感耦合等离子体质谱(ICP-MS)与等离子体光谱(ICP-OES)联机同时测定多金属结核样品中常量、微量、痕量元素。样品经高压密封溶样弹消解后,一次气动雾化进样,ICP-OES测定常量和微量元素,ICP-MS测定微量和痕量元素。详细探讨了不同浓度范围元素的测定方式、元素分析信号的采集模式、多原子离子干扰的校正因子。采用ICP-MS与ICP-OES二种方式同时测定Co、Cu、Ni、Zn、V、Ba、Sr,分析结果表明具有较好的一致性。所建立的ICP-MS与ICP-OES联机检测技术用于多金属结核标准样品的分析(Nod-A-1,GSPN-1,GSPN-2,GSPN-3),分析结果与推荐值符合,相对标准偏差小于10％。     

电感耦合等离子体质谱法测定黄沙土壤中铅同位素比

用电感耦合等离子体质谱法（ＩＣＰ—ＭＳ）测定了５个黄沙原土样品中铅同位素比２０７Ｐｂ／２０６Ｐｂ、２０８Ｐｂ／２０６Ｐｂ，样品来自被认为是黄沙气溶胶源地区，为了使铅同位素测量中质量偏差和漂移减至最少，在样品中加入了铊标准溶液，测量２０５Ｔｌ／２０３Ｔｌ比，校正质量数差别选择的影响．同时，采用ＩＣＰ—ＭＳ和电感耦合等离子体原子发射光谱法（ＩＣＰ一ＡｌＳ）测定了随粒径变化样品中１２种元素浓度的变化．     

Direct solid analysis of powdered tungsten carbide hardmetal precursors by laser-induced argon spark ablation with inductively coupled plasma atomic emission spectrometry

The potential of the laser-induced argon spark atomizer (LINA-Spark atomizer) coupled with ICP-AES as a convenient device for direct analysis of WC/Co powdered precursors of sintered hardmetals was studied. The samples were presented for the ablation as pressed pellets prepared by mixing with powdered silver binder containing GeO₂ as internal standard. The pellets were ablated with the aid of a Q-switched Nd:YAG laser (1064 nm) focused 16 mm behind the target surface with a resulting estimated power density of 5 GW cm^–2. Laser ablation ICP-AES signals were studied as a function of ablation time, and the duration of time prior to measurement (pre-ablation time) which was necessary to obtain reliable results was about 40 s. Linear calibration plots were obtained up to 10% (m/m) Ti, 9% Ta and 3.5% Nb both without internal standardization and by using germanium as an added internal standard or tungsten as a contained internal standard. The relative uncertainty at the centroid of the calibration line was in the range from ±6% to ±11% for Nb, Ta and Ti both with and without internal standardisation by Ge. A higher spread of points about the regression was observed for cobalt for which the relative uncertainty at the centroid was in the range from ±9% to ±14%. Repeatability of results was improved by the use of both Ge and W internal standards. The lowest determinable quantities calculated for calibration plots were 0.060% Co, 0.010% Nb, 0.16% Ta and 0.030% Ti with internal standardization by Ge. The LA-ICP-AES analyses of real samples led to good agreement with the results obtained by solution-based ICP determination with a relative bias not exceeding 10%. The elimination of the dissolution procedure of powdered tungsten (Nb, Ta, Ti) carbide is the principal advantage of the developed LA-ICP-AES method.     

电感耦合等离子体原子发射光谱法（ICP-AES）测定RoHS指令聚合物中的铅和镉

本文引入微波技术消解聚合物塑料样品,使用电感耦合等离子体原子发射光谱仪（ICP-AES）测定聚合物中的铅（Pb）和镉（Cd）含量,并建立了优化的样品消解程序和测定方法,得到满意的测定结果。[摘要应包括目的、方法、结果、结论,请修改,同时修改英文]该方法具有效率高、污染小的优点。检测结果具有良好的精密度。     

电热蒸发进样/电感耦合等离子体原子发射光谱的蒸发过程研究

本文考察了电热蒸发进样 ETV/ICP-AES 技术中蒸发电流对不同挥发性元素的信号强度及峰形的影响;探索了蒸发器体积及其结构对分析物蒸发行为和信号的影响;本文还探索了平台技术在 ETV-ICP-AES 中的应用。并相应得出了一些有益的结论。     

Slurry nebulization ICP-AES spectrometry method for the determination of tin in organotin(IV) complexes

This paper proposes a quick, novel method for tin determination in organotin chemicals by slurry nebulization inductively coupled plasma atomic emission (ICP-AES) spectrometry. The method was tested by the measurement of five organotin carboxylate complexes of known composition for obtaining simple stoichiometric data. The slurries were prepared by first dissolving the organotins in an adequate solvent (methanol, pyridine or acetone) well miscible with water and then adding this solution drop-by-drop to a 0.005% TX-100 tenzide solution while maintaining intensive mixing. Dynamic laser light scattering experiments showed that the average equivalent particle size in the resulting slurry was ≈0.3 μm for all samples and solvents. Under suitable ICP-AES measuring conditions, the signal recoveries were found to be between 101.8 and 106.6%, which allowed direct nebulization and calibration against aqueous solutions. Typically, 70 μg l⁻¹ detection limit and 1–5% relative S.D. on five replicates can be achieved by the described method.     

A pilot study on the feasibility of the preparation of a new certified reference material based on the Antarctic Scallop Adamussium Colbecki

As foreseen by the Italian National Programme of Research in Antarctica, a preliminary investigation was performed to ascertain the feasibility of the production of a new Certified Reference Material for trace elements based on the bivalve Adamussium colbecki. The scallops sampled in Antarctica during the 1999–2000 Italian scientific expedition were analyzed by inductively coupled plasma atomic emission spectrometry and high-resolution inductively coupled plasma mass spectrometry for their content in selected trace elements (As, Cd, Cr, Cu, Fe, Hg, Mn, Mo, Ni, V and Zn). The certification campaign will be undertaken on the basis of the findings of this feasibility study in close cooperation with the Institute for Reference Materials and Measurements, Joint Research Centre of the European Commission.     

Determination of cadmium, lead, iron, nickel and chromium in selected food matrices by plasma spectrometric techniques

In the frame of a study aimed at investigating the transfer of metal contaminants through the food chain and the effects of food processing, five elements, namely Cd, Pb, Fe, Ni and Cr, were accurately determined in (i) durum wheat grain and derived products, (ii) wheat-based reference materials, (iii) drinking water, used both as an ingredient and for technological purposes in the investigated industrial process. Microwave closed vessel digestion was selected as the dissolution technique for solid samples, whereas water samples were acidified with ultrapure nitric acid and analysed directly. As several analytes had to be quantified at trace or ultratrace levels, inductively coupled plasma mass spectrometry (ICP-MS) was resorted to for analytical determinations. Overall, this straightforward analytical approach enabled to detect the often small changes in element concentration associated with the different technological steps of processing. Nevertheless, detection of heavily interfered elements, especially Cr, as well as analyte quantification at ultratrace-level level in water, posed analytical challenges that required suited analytical solutions.Changes in the sample introduction system and complementary use of inductively coupled plasma atomic emission spectrometry (ICP-AES) straightforwardly overcame the difficulties in determining the analytes in the selected food matrixes. The benefits of ultrasonic nebulization in reducing the effects of problematic spectral interferences were demonstrated. Overall, a robust and high-throughput analytical method was outlined.     

Determination of Arsenic,Cadmium, Cobalt,Chromium, Nickel,and Lead in Cosmetic Face-Powders: Optimization of Extraction and Validation

An analytical method for the quantification of toxic metals in face-powders is presented and discussed. Acid digestion with HNO₃-H₂O₂ or HNO₃-HCl was performed and compared with total digestion by HF. The digestion with HNO₃-H₂O₂ was the most suitable for these purposes. Analyses were performed by inductively coupled plasma atomic emission spectrometry (ICP-OES) and inductively coupled plasma mass spectrometry (ICP-MS), whose performances were compared by analyzing three different certified reference materials. The analysis of five commercial face-powders revealed the presence of all the considered metals in the range 0.06–8.0 µg/g. To simulate the bioaccessibility of metals in physiological conditions, a digestion with a simulated sweat solution was performed. In this case, the analysis of the same face-powder samples provided results below the limit of quantification, suggesting low bioaccessibility of the considered trace elements.