Determination of phosphorus in waste-waters by inductively-coupled plasma atomic emission spectrometry

Inductively coupled plasma—atomic emission spectrometry offers a simple and rapid method for the determination of total phosphorus in waste-waters: the optimum operating conditions are described. The detection limits are 0.02, 0.04, and 0.11 μg ml^-1 at the 213.618, 214.914, and 253.565-nm lines, respectively. Interferences by other elements are negligible at the concentration levels of these elements in environmental and waste-waters, except for the spectral interference of copper on the lines at 213.618 and 214.914 nm. Differences in emission response for various inorganic and organic phosphorus compounds are small. Analytical results for phosphorus in municipal and industrial waste-waters agree well with those obtained by standard methods.     

Determination of sulfur in biological samples by vacuum-ultraviolet inductively-coupled plasma atomic emission spectrometry

Sulfur is most sensitively determined at 180.7 nm, the detection limit being 10 μg l^?1. A comparison of digestion procedures shows that acid digestion in a teflon bomb gives least loss of analyte. Only calcium interferes spectrally at this wavelength. Results for various reference materials are presented.     

Determination of cadmium by suction-flow liquid-liquid extraction combined with inductively-coupled plasma atomic emission spectrometry

The flow manifold described permits suction-flow liquid-liquid extraction of cadmium in a discrete aqueous sample as its diethyldithiocarbamate into carbon tetrachloride. The organic extract is fed into the nebulizer of an inductively-coupled plasma atomic emission spectrometer by a peristatic pump. An increase in sensitivity of ca. 250-fold is achieved in comparison with direct aspiration of the aqueous solution. The sampling frequency is 20 h^?1 and the consumption of carbon tetrachloride and 5% (w/v) sodium diethyldithiocarbamate solution are each 0.6 ml min^?1. The 3σ detection limit is 0.4 ng ml^?1 cadmium, and the calibration is linear up to 300 ng ml^?1. The relative standard deviation for 10 replicate measurements is 1.5% for 50 ng ml^?1 cadmium. The flow interferences observed can be decreased or eliminated by the addition of citrate to the buffer solution. Results of analysis of some certified biological reference materials are given.     

Determination of rare-earth elements by high-performance liquid chromatography/inductively-coupled plasma/atomic emission spectrometry

Liquid chromatography coupled on-line to a sequential ICP/AES system is applied for the determination of 14 rare-earth elements (REEs) in samples with widely different concentrations of REEs and matrix elements. The REEs are separated on a cation-exchanger by applying an α- hydroxyisobutyric acid gradient. The determination limits were the same as those obtained by continuous nebulization of single-element standard solutions. The chromatographic separation precludes mutual spectral interferences between the REEs. The practical value of the method developed is demonstrated by the determination of REE impurities in Specpure rare-earth oxides, by its demonstrated potential to evaluate real spectral interferences, and by the analysis of geological samples (natural phosphates) with relatively low total REE contents. The detection limits of REEs in these natural phosphates ranged between 0.005 and 0.4 μg g^?1.     

Determination of arsenic by inductively-coupled plasma atomic emission spectrometry enhanced by hydride generation from organized media

A method is described for the determination of arsenic, which combines a continuous flow hydride generation technique with an inductively coupled plasma atomic emission detection system. Some atomic absorption preliminary studies are described as well. Arsine is generated with NaBH(4) from a didodecyldimethylammonium bromide (DDBA) vesicular medium. The analytical performance of this vesicles-enhanced method is superior to the generation of the hydride from aqueous media: the detection limit (0.6 ppb) is improved by a factor of 2 and greater tolerance to interferences is observed for arsine generation from DDBA vesicles. Precision of As determinations is also improved. The proposed method has been validated for low As levels determinations in two Certified Reference Materials (CRM) sediments with satisfactory results. The potential of organized media to improve hydride generation is addressed.     

Determination of boron in geological materials by inductively-coupled plasma emission spectrometry

Determination of boron in international silicate reference materials with an argon plasma is demonstrated. Detection limits are about 5 ppm for rock samples.     

Simultaneous multielement analysis of zeolite catalysts by inductively-coupled plasma atomic emission spectrometry

Summary A method comprising digestion of zeolites with an acid mixture followed by inductively-coupled plasma atomic emission spectrometry (ICP-AES) has been established for the simultaneous determination of Al, Na, La and Si in various zeolite samples. Various aspects including sample digestion, instrumental interference effects as well as analytical performance and applicability of the established method have been investigated in detail. The results indicated that aqua regia in combination with hydrofluoric acid was effective for decomposition of a wide variety of zeolite samples. The effects of borate and fluoride ions in the digested sample solution on the ICP-AES determination have been carefully investigated. The method established will be generally applicable for the simultaneous determination of Al, Na, La and Si in zeolite with a precision of 5%. The analytical results obtained were checked by comparison with classical wet chemistry methods and found to be in reasonably good agreement. Application to the kinetic study of La-NaY exchange reaction was also performed.

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Simultane Multielementanalyse von Zeolit-Katalysatoren durch ICP-AES

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Dedicated to Prof. Dr. W. Fresenius on the occasion of his 75th birthday     

Determination of trace elements in sea water by inductively-coupled plasma emission spectrometry

Pb, Zn, Cd, Ni, Mn, Fe, V and Cu in sea water are determined by extraction of their complexes with sodium diethyldithiocarbamate into chloroform, decomposition of the chelates and inductively-coupled plasma emission spectrometry. When 1-l water samples are used, the lowest determinable concentrations are: 0.063 μg Mn l^-1, 0.13 μg Zn l^-1, 0.25 μg Cd l^-1, 0.25 μg Fe l^-1, 0.38 μg V l^-1, 0.5 μg Ni l^-1, 0.5 μg Cu l^-1, and 2.5 μg Pb l^-1. Above these levels, the relative standard deviations are better than 12% for the complete procedure.     

Determination of arsenic in glycerine by flow injection,hydride generation and inductively-coupled plasma/atomic emission spectrometry

The determination of low concentrations of arsenic in glycerine is investigated with flow injection for the introduction of analyte and tetrahydroborate reagent for arsine generation, separation in a vapor-liquid flow cell, and inductively-coupled plasma/atomic emission spectrometry (i.c.p./a.e.s.). Peak areas are used to quantify arsenic in the concentration range 0.12–3.0 μg ml^?1. Peak areas for prepared standards exhibited average deviations of about 1.4% for this concentration range. The slope and intercept for a least- squares fit of area (nanocoulombs) vs. concentration (μg ml^?1) were 10.9 ± 0.17 and 0.46 ± 0.3, respectively.     

Determination of uranium in organic solutions by inductively coupled plasma atomic emission spectrometry

The determination of uranium in organic solutions by inductively coupled plasma atomic emission spectrometry is reported. The conditions for achieving plasma stability were determined as well as the optimum conditions (RF power, observation height and argon flow) of a spectrometer for analysis of U(II) 367.007 nm in three organic solvents, xylene, kerosine and benzene. The effects of RF power and observation height on signal-to-back-ground ratio and the detection limits are considered. Spectral interferences due to CN band are discussed.A part of this work was presented at the Second Karlsruhe International Conference on Analytical Chemistry in Nuclear Technology Karlsruhe, FRG, June 5–9, 1989.     

Determination of traces of boron in semiconductor amorphous silicon film by filament-vaporization inductively-coupled plasma/atomic emission spectrometry

Silicon is dissolved from the platinum substrate by nitric/hydrofluoric acids. The recovery of boron on direct analysis was poor, but was increased to >95% by the addition of 500–5000 μg ml^?1 phosphorus as phosphoric acid. The results compared well with the molar ratio of the gases (B₂H₆/(Ar + H₂) used to form the film and the intensity ratio of ¹¹B⁺ and ³⁰Si⁺ obtained by secondary-ion mass spectrometry.     

Screening for selected toxic elements in urine by sequential-scanning inductively-coupled plasma atomic emission spectrometry

A rapid screening method for nine elements (Se, As, Cr, Zn, Cd, Pb, Ni, Mn, and Cu) in human urine is described. A sequential-scanning inductively-coupled plasma atomic emission spectrometer, incorporating a cross-flow nebulizer, was used. Internal standardization with yttrium compensated for the differences between the aqueous calibration standards and the undiluted urine specimens. Accuracy was evaluated with aqueous (NBS SRM 1643a, EPA 378-13, and EPA 476-3) and urine (NBS SRM 2670 and Fisher Urichem Level II) reference and control materials. Detection limits for the system were evaluated from analyses of normal urine materials found to contain low levels of the elements investigated.     

Determination of traces of zirconium in silicate rocks by inductively-coupled plasma emission spectrometry

The sample is fused with a mixture of sodium and potassium carbonates. Zirconium is separated from the large amounts of sodium and potassium by precipitation of hydrated oxides before nebulization. The detection limit is 0.32 μg Zr g^-1. Results for seven standard rocks are in accord with recommended values.     

Determination of phosphorus death profiles in semiconductor silicon by chemical etching and filament vaporization inductively-coupled plasma atomic emission spectrometry

Silicon slices are dissolved by anodizin and removal of the silica film by hydrofluoric acid. The phosphorus in the etching solution is determined by the filament vaporization technique and the depth of silicon is measured by determining the silicon content in the etching solution by conventional inductively-coupled plasma atomic emission spectrometry. A lower limit of 10¹⁸ phosphorus atoms cm^?3 can be determined by sectioning intervals of 30–50 nm.     

Determination of rare earths in lanthanum oxide by inductively-coupled plasma emission derivative spectrometry

Rare-earth elements (REE) at ppm levels in lanthanum oxide can be determined without prior separation and preconcentration by use of high-resolution inductively-coupled plasma emission derivative spectrometry (ICPEDS). The calibration graphs are all linear and pass through the origin, even in the presence of large amounts of lanthanum, except those for dysprosium, holmium and ytterbium. The detection limit for each REE is 1-10 mug g in lanthanum oxide. Investigation of various physical and/or spectral interferences shows that good selectivity is obtained by ICPEDS.     

Determination of minor and trace elements in silicate rocks by inductively-coupled plasma emission spectrometry

Samples (0.5 g) are decomposed with mixed acids in a sealed teflon vessel. After suitable treatment, barium, cobalt, chromium, copper, lithium, nickel, scandium. strontium, vanadium and zirconium are determined sequentially. The method is satisfactory for a variety of standard silicate materials.     

Reduction of tin and germanium to hydrides for determination by inductively-coupled plasma atomic emission spectrometry

The effect of a range of acids on the reduction of tin and germanium to their hydrides in aqueous solutions by means of sodium tetrahydroborate(III) solution in a continuous flow system is investigated. Interference effects in hydrochloric acid and tartaric acid reaction media are tabulated. Tartaric acid decreases many interference effects. Detection limits for both elements are low (ca. 0.2 μg l^-1) and the linear calibration ranges span nearly four orders of magnitude.     

Determination of trace concentrations of antimony by the introduction of stibine into an inductively-coupled plasma for atomic emission spectrometry

A simple, rapid and sensitive method is described for the determination of trace concentrations of antimony by inductively-coupled plasma atomic emission spectrometry with hydride generation. Hydrochloric acid (1 M) is the best medium for stibine generation, but antimony(III) is also effectively reduced to stibine in 1 M malic acid or 0.5 M tartaric acid, whereas antimony(V) gives no significant signal in either of these acids. This permits the differential determination of Sb(III) and Sb(V). Most of the inter-element interference effects can be minimized by thiourea, bur standard additions are recommended for accurate determinations. Thiourea is also effective in prereducing Sb(V) to Sb(III). The detection limit is 0.19 ng Sb ml^?1 and the calibration graph is linear up to 100 μg ml^?1. The r.s.d, at 1 and 100 ng Sb ml^?1 are 3.8 and 2.1%, respectively. The method is applied to copper metal and to speciation of antimony in waste water.     

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。     

电感耦合等离子体发射光谱法同时测定玻璃中的硫和磷

通过对玻璃试样中硫、磷的分解方法、分析线选择、共存元素光谱干扰和仪器最佳分析条件等方面的研究, 建立了ICP-AES 测定玻璃中硫、磷的方法. 选用紫外区谱线S 181.972 nm、 P 177.434 nm, 避免了基体元素对硫、磷的干扰, 该法能够准确、快速地测定玻璃样品中的硫、磷量, 测定结果的相对标准偏差小于2.9%, 方法的检出限分别为 S 0.07 μg/mL, P 0.08 μg/mL, 已用于玻璃样品的分析.