小体积外循环进样ICP-AES直接测定薄膜样品成份

本文试用小体积外循环进样系统,不称样重、不计试液体积,用归一计算法(或摩尔比法)ICP-AES直接进行小试样样品的成份测定,方法简便、快速,分析结果满意。     

有机溶液进样大功率微波诱导空气等离子体发射光谱法测定金属离子的研究

研究了由Okamoto腔产生的大功率微波诱导空气等离子体的分析性能以及用该等离子体直接有机溶液进样测定有机溶剂或含有大量有机溶剂的废水中的金属污染物的可行性。用本方法测定了几种工业废水中的金属污染物,并与原子吸收光谱法的测定结果进行了比较。     

电感耦合等离子体原子发射光谱法中悬浮液直接进样技术的研究与应用的进展

对电感耦合等离子体原子发射光谱法(ICP-AES)中的悬浮液直接进样技术的研究及应用的进展作了评述。文中引用文献涉及年份为1988~2005年。主要的评述内容包括试样制备方法、仪器装置、校准方法、影响悬浮液进样中的传输效率和雾化效率及分析结果可靠性的因素,以及此技术的分析应用(引用文献47篇)。     

ICP-AES法的固体进样方法

电感耦合等离子体激发原子发射光谱法(ICP-AES)如今已发展成为现代分析试验室的一种十分有效的重要分析手段。虽然研究过将试样引入电感耦合等离子体(ICP)的多种进样方法,但是目前大多数研究者和商品仪器都是借助于气体动力或超声波使液体试样雾化,以气-液气溶胶形式将试样溶液引入ICP。溶液进样方法,特别是气动雾化系统日趋成熟,已成为普遍采用的溶液进样装置。然而,日常分析工作中,还经常遇到难溶解或不易完全溶解的试样,如某些氧化物、耐腐蚀的合金试样、地质矿物试样等。分析者希望能直接将这类固体试样(不经转化为溶液)引进ICP中进行分析。另外,固体试样直接进样有利于减少沾污,降低空白,提高分析效率,而且避免了转变为溶液时带来的稀释因素等。     

流动注射-电感耦合等离子体发射光谱联用技术研究——Ⅳ.痕量钪的快速测定

本文提出了用流动注射-电感耦合等离子体发射光谱(FIA-ICP-AES)测定工艺流程Sc试液中痕量钪的新方法。考察了基体Fe和Ti的光谱干扰;对常规进样和FIA进样中的基体效应进行了比较。当采用0.5ml体积进样,以Sc 363.075nm为分析线,Sc的检出限为8.4ng/ml,R.S.D.为2.5％。此法可以直接用于基体浓度在Fe≤30mg/ml和Ti≤10mg/ml范围内痕量钪的测定,而无需分离基体或在标样和试样之间进行基体浓度匹配。本法分析速度快(90个样/小时)、操作简便和精密度好,可以作为工艺流程中测定痕量Sc的快速的分析方法。     

电感耦合等离子体-发射光谱法测定纯锑中硫的含量

建立了用电感耦合等离子体-发射光谱法(ICP-AES)测定锑锭中硫元素含量的分析方法。样品用王水溶解,加入适量的酒石酸作为稳定剂,稀释定容后直接进行ICP-AES分析。硫元素的测定下限为0.0008%;0.20μg/mL的硫标准溶液平行7次进样的相对标准偏差为3.7%。利用所建立的方法,对两个批次的锑锭进行了分析,加标回收率分别为96.0%和100.6%,并与国标分析方法进行了实验数据比对。     

原子荧光光谱进样技术的研究进展

原子荧光光谱已成为检测金属或类金属的重要手段,其仪器进样方式与所用原子化器类型直接相关。根据进样原理的不同,综述了原子荧光光谱仪器的直接进样、喷雾进样、化学蒸气发生进样和电热蒸发进样4种进样技术,详细介绍了原子荧光光谱各进样技术特别是化学蒸气发生进样和电热蒸发进样的发展历程、原理及优缺点,展望了原子荧光仪器进样技术的发展前景。引用文献75篇。     

ICP-AES中三种进样方式对基体干扰影响研究

本文介绍了ICP-AES中基体干扰的研究工作,主要是通过比较流动注射、蠕动泵、气动提升三种进样方法的酸效应和化学干扰的特点和程度,发现蠕动泵进样法的酸效应仍相当严重,流动注射进样法的酸效应干扰比蠕动泵进样法轻得多。另方面,三种进样法的化学干扰特点很相似。由此结果对ICP-AES中基体干扰的机理作了初步探讨,并得到了一些新结论。     

离线二氧化碳发生原位再溶解-电感耦合等离子体原子发射光谱法测定水样中无机碳

基于二氧化碳在水中具有较大的溶解度,提出了在电感耦合等离子体原子发射光谱法(ICP-AES)测定水样中无机碳含量时,用离线二氧化碳发生及原位再溶解作为样品溶液的制备方法。取一定量水样与4mL盐酸(1+9)溶液反应,使样品中碳酸盐及碳酸氢盐转化为二氧化碳,并在原溶液中原位再溶解。样品溶液的总体积为50mL,经过仪器上常规采用的单管进样装置导入于仪器中,经气液分离器在172.4kPa压力条件下,使试液中的二氧化碳分离析出,用ICP-AES测定其浓度。二氧化碳质量浓度在400mg·L-1以内与测定信号之间呈线性关系,方法的检出限(3s/k)为0.087mg·L-1。在20mg·L-1浓度水平做重复性试验,计算其相对标准偏差(n=10)为0.97%。应用此方法分析了4个水样,所得二氧化碳的测定值与滴定法测定值相一致。     

ICP-AES法测定加氢催化剂中的元素

本文论述了应用ICP-AES法测定加氢催化剂中的主要及次要组分的分析技术。考察了样品处理、测定条件及各种干扰。并确定在硝酸溶液中以H_2O_2为氧化剂、醋酸为催化剂,使S直接氧化成硫酸根的方法。ICP-AES同时测定试液中的S,P,Zn,Mo,Co,Ni,Cu,Ti,Fe及As。其含量为1—30%时,相对标准偏差<5%;1%以下时,相对标准偏差<13%。     

FI溶剂萃取与ICP-AES联机的研究水样中微量铜的测定

本文建立了用FI-溶剂萃取-ICP-AES测定水样中微量铜的分析方法。选择了ICP-AES、超声雾化发生器及FIA的最佳工作条件。研究了溶液pH对用打萨腙-四氯化碳体系萃取铜的影响;有机相流速与水相流速之比例;萃取盘管长度等因素对萃取过程及等离子体放电的影响。分析了自来水样品及美国标准局标准水样中铜含量。统计了分析方法的精密度、检出限与实验条件下的富集倍数。     

Application of a microwave-based desolvation system for multi-elemental analysis of wine by inductively coupled plasma based techniques

Elemental wine analysis is often required from a nutritional, toxicological, origin and authenticity point of view. Inductively coupled plasma based techniques are usually employed for this analysis because of their multi-elemental capabilities and good limits of detection. However, the accurate analysis of wine samples strongly depends on their matrix composition (i.e. salts, ethanol, organic acids) since they lead to both spectral and non-spectral interferences. To mitigate ethanol (up to 10% w/w) related matrix effects in inductively coupled plasma atomic emission spectrometry (ICP-AES), a microwave-based desolvation system (MWDS) can be successfully employed. This finding suggests that the MWDS could be employed for elemental wine analysis. The goal of this work is to evaluate the applicability of the MWDS for elemental wine analysis in ICP-AES and inductively coupled plasma mass spectrometry (ICP-MS). For the sake of comparison a conventional sample introduction system (i.e. pneumatic nebulizer attached to a spray chamber) was employed. Matrix effects, precision, accuracy and analysis throughput have been selected as comparison criteria. For ICP-AES measurements, wine samples can be directly analyzed without any sample treatment (i.e. sample dilution or digestion) using pure aqueous standards although internal standardization (IS) (i.e. Sc) is required. The behaviour of the MWDS operating with organic solutions in ICP-MS has been characterized for the first time. In this technique the MWDS has shown its efficiency to mitigate ethanol related matrix effects up to concentrations of 1% (w/w). Therefore, wine samples must be diluted to reduce the ethanol concentration up to this value. The results obtained have shown that the MWDS is a powerful device for the elemental analysis of wine samples in both ICP-AES and ICP-MS. In general, the MWDS has some attractive advantages for elemental wine analysis when compared to a conventional sample introduction system such as: (i) higher detection capabilities; (ii) lower ethanol matrix effects; and (iii) lower spectral interferences (i.e. ArC(+)) in ICP-MS.     

Tandem on-line continuous separations for atomic spectroscopic indirect analysis: Iodide determination by ICP-AES

A sensitive and selective indirect determination of iodide by inductively coupled plasma emission spectrometry (ICP-AES) based on the principle of tandem on-line continuous separations as an alternative means of introducing samples into plasmas is proposed. Iodide is continuously extracted as an ion-pair into xylene by mixing the sample with Hg(II) and dipyridil solutions. The organic phase (containing the analyte in [Hg(Dipy)₂]I₂ form) is on-line continuously mixed with NaBH₄ (in DMF) and acetic acid solutions. Mercury vapour continuously generated from this organic phase is separated in a classical U-type gas-liquid separation device. The system has been optimized for the continuous extraction of KI, for the direct generation of cold mercury vapour from xylene and for the final ICP-AES determination of mercury. The optimised method has been applied to the determination of iodide (detection limit 20 ng/ml of iodide) in table salt and in synthetic samples. Very good agreement between found and certified results was observed. The usefulness and convenience of such alternative sample chemical pretreatment/presentation to the ICP is thus demonstrated for indirect determinations to be carried out by atomic spectroscopy methods.     

Inductively coupled plasma-atomic emission spectrometry: Analytical assessment of the technique at the beginning of the 90's

The main application of the inductively coupled plasma (ICP) today is in atomic emission spectroscopy (AES), as an excitation spectrochemical source, although uses of an ICP for fluorescence as just an atomiser, and specially for mass spectrometry, as an ionization source, are rocketing in the last few years.Since its inception, only a quarter of a century ago, ICP-AES has rapidly evolved to one of the preferred routine analytical techniques for convenient determination of many elements with high speed, at low levels and in the most varied samples. Perhaps its comparatively high kinetic temperature (capable of atomising virtually every compound of any sample), its high excitation and ionisation temperatures, and its favourable spatial structure at the core of the ICP success.By now, the ICP-AES can be considered as having achieved maturity in that a huge amount of analytical problems can be tackled with this technique, while no major or fundamental changes have been adopted for several years. Despite this fact, important driving forces are still in operation to further improve the ICP-AES sensitivity, selectivity, precision, sample throughput, etc. Moreover, proposals to extend the scope of the technique to traditionally elusive fields (e.g. non-metals and organic compound analysis) are also appearing in the recent literature.In this paper the state of the art, the last developments and the expectations in trying to circumvent the limitations of the ICP-AES (on the light of literature data and personal experience) are reviewed.     

Tandem on-line continuous separation and determination of arsenic by inductively coupled plasma atomic emission spectrometry

The principle of tandem on-line continuous separation techniques as an alternative means of introducing samples into plasmas was applied to the development of a sensitive, selective and convenient method for the determination of arsenic by inductively coupled plasma atomic emission spectrometry (ICP-AES). Arsenic is continuously extracted as AsI₃ into xylene from the sample dissolved in 0.1 M potassium iodide solution in 7.2 M hydrochloric acid. The xylene phase (containing the analyte) is continuously mixed on-line with NaBH₄ in dimethylformamide and acetic acid solutions. Arsine is thus continuously generated directly from the organic phase and is separated in a gas—liquid separation device which prevents most of the xylene phase vapour from reaching the ICP. The system was optimized for the continuous extraction of AsI₃, the direct generation of arsine from xylene and the final ICP determination of arsenic. Finally, the tandem on-line continuous separation ICP detection system was applied to the determination of arsenic in real samples (white metal, cast iron, cupro-nickel and orchard leaves standard materials). Very good agreement between the experimental results and the certified values was obtained.     

Determination of different oxidation states of arsenic and selenium by inductively coupled plasma-atomic emission spectrometry with ion chromatography

Recent regulation in Japan requires more sensitive trace analysis methods for the determination of arsenic and selenium and their oxidation states As(III) and (V), Se(IV) and (VI). The hydride generation (HG) technique is usually used in combination with AAS and ICP-AES to increase sensitivity. However, hydrochloric acid is mostly used to acidify the sample solution in HG. Isobaric interferences due to chlorine-related species cause mass spectral problems when the same solution is used for the determination of these elements by ICP-MS. In this study, different oxidation states of As and Se were determined by coupling ion chromatography (IC) to an ICP-AES instrument. An HG technique was used to introduce test samples into the ICP. Nitric acid was employed to acidify the samples for HG. The concentrations of acid and base were kept as low as possible to reduce contamination. The formation of As and Se hydrides could be achieved without HCl, if the concentrations of acid and alkaline solutions were optimized. However, HCl was necessary for additional reduction of Se(VI) to Se(IV).     

Determination of different oxidation states of arsenic and selenium by inductively coupled plasma-atomic emission spectrometry with ion chromatography

Recent regulation in Japan requires more sensitive trace analysis methods for the determination of arsenic and selenium and their oxidation states As(III) and (V), Se(IV) and (VI). The hydride generation (HG) technique is usually used in combination with AAS and ICP-AES to increase sensitivity. However, hydrochloric acid is mostly used to acidify the sample solution in HG. Isobaric interferences due to chlorine-related species cause mass spectral problems when the same solution is used for the determination of these elements by ICP-MS. In this study, different oxidation states of As and Se were determined by coupling ion chromatography (IC) to an ICP-AES instrument. An HG technique was used to introduce test samples into the ICP. Nitric acid was employed to acidify the samples for HG. The concentrations of acid and base were kept as low as possible to reduce contamination. The formation of As and Se hydrides could be achieved without HCl, if the concentrations of acid and alkaline solutions were optimized. However, HCl was necessary for additional reduction of Se(VI) to Se(IV).     

Direct determination of major elements in solid plant materials by electrothermal vaporization inductively coupled plasma atomic emission spectrometry

The present work demonstrates the capability of electrothermal vaporization (ETV) to become an important tool of solid sample introduction in ICP-AES for plant sample analysis. Direct determination of Al, Ca, Fe, K, Mg, Mn, Na and Zn was investigated in powdered plant samples. Obtaining good results for major elements in plant samples was governed by some special operating conditions. The sensitivity of the method necessitated the use of ICP in radial view configuration. The behavior of elements during vaporization was studied between 500 and 2600 °C. External calibration was carried out using solid external (cellulose) spiked with aqueous standard solutions. However, performances of the analytical method were found dependent of argon flow rates. Analytical accuracy of the method was tested in three reference materials. Analytical results agreed with certified values when cellulose was used in calibration. However, K could not be determined because of excessive sensitivity. Without cellulose, it was found that Fe results were underestimated and Zn results overestimated. Relative standard deviations varied from 3 to 23%. Limits of detection varied from 1 to 80 ng g⁻¹ from one element to the other for a typical mass sample of 2 mg.     

Determination of rare earth elements in geological samples by inductively coupled plasma atomic emission spectrometry with flow injection liquid-liquid extraction.

A direct sampling with organic solvent extracts for simultaneous multi-element determination implemented with inductively coupled plasma atomic emission spectrometry (ICP-AES) associated with a flow injection liquid-liquid extraction (FI-LLE) sample preconcentration method was studied. The "robustness" of the plasma discharge with tributyl phosphate (TBP) loading was diagnosed by using the Mg II 279.55 nm and Mg I 285.21 nm lines intensity ratio. A FI-LLE preconcentration system for rare earth elements (REEs)-nitrate-TBP was established by using a laboratory-designed phase separator. For these elements, an average sensitivity enhancement factor of 64 was obtained with respect to ICP-AES sampling with aqueous solutions. The precision of the method was characterized by a relative standard deviation (%RSD) of 1.8 - 5.2%. A throughput of 27 samples per hour can be achieved with an organic solvent consumption of less than 200 microl per determination. Good results were obtained for the analysis of standard reference materials.     

电感耦合等离子体光发射光谱分析中无机酸基体效应研究(Ⅰ)无机酸基体效应及其机理

介绍了电感耦合等离子体光发射光谱分析中无机酸对分析结果的影响,并对产生酸基体效应的主要因素进样系统及等离子炬激发性能方面的研究现状进行综述,引用文献34篇。