Determination of platinum and palladium in dead catalysts using inductively coupled plasma atomic emission spectrometry after sample digestion by high-temperature fusion

A technique for the determination of platinum and palladium in dead catalysts using ICP-AES after sample digestion by high-temperature fusion with potassium pyrosulfate is described. The technique is universal; it offers the possibility to analyze various brands of catalysts and their mixtures at a content of platinum and palladium of 0.1% to whole units of percent in a short time. The accuracy of results of determination of platinum and palladium is confirmed by comparison with the data of interlaboratory control. The relative standard deviation in the developed technique is 4–2.5% for the content of platinum and palladium of 0.1 to 0.5% and 2–1% for higher concentrations of these elements.     

Analysis of pure scandium,yttrium, and their oxides using methods of inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry

The analytical possibilities of direct detection of rare earth and non-rare-earth impurities in pure scandium, yttrium, and their oxides using the ICP-AES and ICP-MS methods are investigated. The analytical lines and isotopes of the sought elements that are the most free from folding are selected. The effect of the sought impurities of the matrix elements on the analytical signal is studied. The detection and determination limits for impurities in scandium and yttrium are estimated. The lower limits of determining impurities in scandium, yttrium, and their oxides at the level of n × 10⁴ mass fractions, %, are reached using the ICP-AES method; those at the level of n × 10⁻⁶ mass fractions, %, are reached using the ICP-MS method. The joint application of the ICP-AES and ICP-MS methods for the analysis of standard specimens of yttrium and scandium oxide is implemented. The control of the validity is accomplished by comparing the obtained results with the certified values of standard specimens and by the method of addition.     

Sorption-atomic-absorption determination of platinum,palladium, and rhodium in dead autocatalysts

The conditions for determination and group concentration of platinum metals (PMs) in the presence of matrix components using new S,N-containing complex-forming sorbents in solutions obtained after decomposition of decontaminated autocatalysts are proposed. The technique of atomic-absorption determination of PMs from a solution (n × 10⁻⁴−n × 10⁻²; s _r = 0.15–0.07) and a solid phase (n × 10⁻⁵−n × 10⁻⁴; s _r = 0.20–0.12) is developed.     

Nanosemiconductor-based photocatalytic vapor generation systems for subsequent selenium determination and speciation with atomic fluorescence spectrometry and inductively coupled plasma mass spectrometry

We reported novel Ag-TiO(2)- and ZrO(2)-based photocatalytic vapor generation (PCVG) systems as effective sample introduction techniques for further improving the sensitivity of the atomic spectrometric determination of selenium for the first time, in which the conduction band electron served as a "reductant" to reduce selenium species including Se(VI) and convert them directly into volatile H(2)Se, which was easily separated from the sample matrix and underwent more effectively subsequent atomization and/or ionization. These two PCVG systems helped us to overcome the problem encountered in the most conventional KBH(4)/OH(-)-H(+) system, in that Se(VI) was hardly converted into volatile selenium species without the aid of prereduction procedures. The limits of detection (LODs) (3σ) of the four most typical Se(IV), Se(VI), selenocystine ((SeCys)(2)), and selenomethionine (SeMet) species were, respectively, down to 1.2, 1.8, 7.4, and 0.9 ng mL(-1) in UV/Ag-TiO(2)-HCOOH, and 0.7, 1.0, 4.2, and 0.5 ng mL(-1) in UV/ZrO(2)-HCOOH with the relative standard deviations (RSDs) lower than 5.1% (n = 9 at 1 μg mL(-1)) when using atomic fluorescence spectrometry (AFS) under flow injection mode. They reached 10, 14, 18, and 8 pg mL(-1) in UV/Ag-TiO(2)-HCOOH, and 6, 7, 10, and 5 pg mL(-1) in UV/ZrO(2)-HCOOH with the RSDs lower than 4.4% (n = 9 at 10 ng mL(-1)) when using inductively coupled plasma mass spectrometry (ICPMS). After the two PCVG systems were validated using certified reference materials GBW(E)080395 and SELM-1, they were applied to determine the total Se in the selenium-enriched yeast sample and used as interfaces between high-performance liquid chromatography (HPLC) and AFS or ICPMS for selenium speciation in the water- and/or enzyme-extractable fractions of the selenium-enriched yeast.     

Determination of phosphorous and sulfur in environmental samples by electrothermal vaporization inductively coupled plasma atomic emission spectrometry

From the viewpoint of selective introduction of the analyte from its solvent and matrices, electrothermal vaporization (ETV) is useful for the sample introduction into the inductively coupled plasma (ICP). By using a tungsten boat furnace (TBF) vaporizer system, the loss of analyte phosphorus, which normally occurs during the drying and ashing stages, is suppressed. The phosphate ion is reacted with the tungsten supplied from the surface of the TBF to form stable tungsten phosphate species. Regarding the determination of sulfur, additional chemical modifiers such as copper(II), lead(II), etc., are necessary to retain the analyte on the TBF. The furnace-fusion (FF) method or wet-digestion technique on the TBF is applied to unify the chemical forms of the analytes. Various oxidative and reductive inorganic compounds as well as organic compounds of phosphorus and sulfur show the same sensitivities after the FF digestion with hydrogen peroxide. The detection limits are 1.5 ng and 0.12 ng for phosphorous and sulfur, respectively. The repeatabilities in terms of the relative standard deviations of 10 replicate measurements of phosphorus and sulfur are 4.2% and 2.0%, respectively. Finally, the established method is applied to the determination of several environmental waters.     

Direct atomic-absorption determination of platinum,palladium, and rhodium in dead ceramic-based autocatalysts

The data on the effect of different concentrations of components of dead automobile catalysts on determination of platinum, palladium, and rhodium using the method of ETAAS are obtained and systematized. The conditions for direct atomic-absorption determination of Pt, Pd, and Rh are optimized. The technique of atomic-absorption determination of PM in secondary raw and technogenic materials is developed (n × 10⁻⁴−n × 10⁻¹ wt %, s _r = 0.12–0.07).     

Development and application of acousto-optic background correction for inductively coupled plasma atomic emission spectrometry

In two configurations, a solid-state acousto-optic (AO) deflector or modulator is mounted in a 0.5 m monochromator for background correction with inductively coupled plasma atomic emission spectrometry (ICP-AES). A fused silica acousto-optic modulator (AOM) is used in the ultraviolet (UV) spectral region applications while a glass AO deflector (AOD) is used for the visible (VIS) region. The system provides rapid sequential observation of adjacent on- and off-line wavelengths for background correction. Seventeen elements are examined using pneumatic nebulization (PN) and electrothermal vaporization (ETV) sample introduction. Calibration plots were obtained with each sample introduction technique. Potable water and vitamin tablets were analyzed. Flame atomic absorption (FAA) was used to verify the accuracy of the AO background correction system.     

Sample preconcentration using ion-exchange polymer film for laser ablation sampling inductively coupled plasma atomic emission spectrometry

An efficient sample pretreatment/introduction technique for the inductively coupled plasma atomic emission spectrometry (ICP-AES) using ion exchange for analyte preconcentration and matrix separation and laser ablation sampling for sample introduction has been developed. Ammonium pyrrolidine dithiocarbamate (APDC)-polystyrene films are coated on glass plates for analyte preconcentration. Repetitive laser ablation sampling of the polymer film removes the ion-exchanged metal ions from the polymer film as fine particles for sample introduction into the ICP. After immersing the sample probe in a sample solution for 5 min, the ICP emission intensity for laser ablation of the polymer film is a few times larger than that after solution nebulization. The sample probe removes only a small fraction of the sample solution and, therefore, in principle, does not disturb the original solution significantly. Single-pulse laser ablation of the polymer film shows that the ion-exchanged metal ion concentration in the film reduces exponentially with the depth of the polymer film. Ion exchange to the polymer film is probably limited by the rate of metal ion diffusion into the film. Calibration curves for Cu, Hg, Pb, and Zn show linear dynamic range of ～1-2 orders of magnitude. The linear dynamic range for Cu increases to >3 orders of magnitude when using Pb as an internal standard. RSD of the ICP emission intensity is ～8%.     

A graphite furnace electrothermal vaporization system for inductively coupled plasma atomic emission spectrometry

An improved graphite furnace electrothermal vaporization device equipped with an autosampler for inductively coupled plasma atomic emission spectrometry is presented. The transport losses of eight selected analytes in the individual segments of the device were determined by means of the radiotracer technique by applying amounts traced comparable to those to be determined in real samples. The results obtained from the radiotracer study were the basis for further improvement of the interface design, leading to considerable increase of the total transport efficiency, which finally was found to be between 26 (for Cr) and 57% (for Ga). The whole system consists of a graphite furnace vaporizer, a power supply, a gas flow box, and an autosampler with incorporated microbalance. The temperature program, gas flows, and autosampler functions are controlled by a data station which also provides the data acquisition and processing of the transient signals. The performance parameters of the developed system were evaluated using aqueous standard solutions. Absolute limits of detection for most analytes were between 0.1 and 1 ng, and for As, K, Ni and Pb, they were between 2 and 3.2 ng.     

电感耦合等离子体原子发射光谱法测定银中硒、碲含量的不确定度评定

采用电感耦合等离子体原子发射法测定银中的硒、碲含量,对测定结果的不确定度进行评定.通过对测量过程中测量重复性、标准曲线变动性、试液体积、试料质量、标准溶液浓度和移取体积等影响因素进行分析,结果表明,测量重复性和标准曲线变动性对总不确定度影响较大.因此,在测定中应适当增加样品和标准溶液重复测定次数,不断优化仪器参数,准确...     

Indirect inductively coupled plasma atomic emission determination of fluoride in water samples by flow injection solvent extraction

An indirect determination of fluoride in water by inductively coupled plasma atomic emission spectrometry combined with flow injection coupled with solvent extraction is reported in this paper. A manifold for rapid determination of fluoride has been designed that uses a single coil for complex formation and extraction. The method involves the formation of lanthanum/alizarin complexone/fluoride complex and its extraction into hexanol containing N,N-diethylaniline. The concentration of fluoride is determined indirectly by introduction of the organic layer into the plasma and measurement of the emission intensity of the La II 333.75-nm line. The optimum experimental conditions for the determination are described. A coiled groove phase separator fitted with a grid and PTFE porous membrane was used in this work. The sampling rate was 36 samples per hour and the calibration graphs were linear from 0.03 to 1.3 micrograms/mL. The relative standard deviation found was 2.16% for 200 microL of 1 microgram/mL of fluoride. The method is selective and has been applied satisfactorily to the determination of fluoride in water samples.     

Microwave sample preparation of facing materials for analysis using the method of atomic emission spectroscopy with inductively coupled plasma

A technique for microwave decomposition of the powder for plasma-jet hard-facing and determination of boron, iron (III), and chromium (III) by ICP-AES is presented. The solvent composition and parameters of the microwave decomposition of the samples in an autoclave are optimized. The detection limits for B, Cr (III) and Fe (III) are 3.0 × 10⁻³, 7.6 × 10⁻⁵, and 2.0 × 10⁻² wt %, respectively.     

Determination of impurities in aluminum isopropoxide by inductively coupled plasma atomic emission spectrometry

A procedure has been developed for the determination of impurities in aluminum isopropoxide by inductively coupled plasma atomic emission spectrometry. The matrix effect has been compensated by adding a Bi internal standard. The detection limits of impurities are 10⁻⁷ to 10⁻⁵ wt %.     

Signal fluctuations due to individual droplets in inductively coupled plasma atomic emission spectrometry

Large emission intensity fluctuations are observed from analyte species in inductively coupled plasmas. Relative standard deviations are as large as 71% when emission is viewed with time resolution of 10 microseconds. Low in the plasma, peaks in atom emission intensity are accompanied by depressions in ion emission. This behavior appears to be due to local cooling by aerosol droplets. High in the plasma, peaks in atom emission are followed by peaks in ion emission. These emission spikes result from atomization and ionization of analyte from vaporizing particles. Laser light scattering experiments show that droplets or particles exist in a conventional 1.0-kW plasma up to 20 mm above the load coil. Emission signals detected high in the plasma correlate with laser light scattering signals below.