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 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 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.     

Determination of aluminum oxide in and on high-purity aluminum by a phenol dissolution method

A simple rapid determination of aluminum oxide in aluminum is described. Aluminum reacts with phenol at 180°C forming aluminum phenoxide but aluminum oxide does not. After the reaction, the aluminum oxide is filtered off and brought into aqueous solution by fusion with potassium hydrogensulfate for determination by atomic absorption spectrometry or by the 8-quinolinol spectrophotometric method. The reaction between aluminum and phenol is stoichiometric. The procedure is applicable to the determination of aluminum oxide in commercial aluminum metals of various forms. The method is relatively rapid and appears to be superior to the conventional bromine—methanol method.     

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 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.     

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 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.     

Preconcentration by dithiocarbamate extraction for determination of trace elements in natural waters by inductively-coupled plasma atomic emission spectrometry

Preconcentration by dithiocarbamate extraction into 2-ethylhexyl acetate for simultaneous determination of trace elements in natural water is described. After 250-fold concentration, the organic phase is used directly for inductively-coupled plasma atomic emission spectrometry. Thirteen elements (As, Se, Mo, Zn, Cd, Ni, Co, Sn, Fe, Cr(VI), Pb, V and Cu) are simultaneously concentrated at pH 4.3 with the combination of ammonium tetramethylenedithiocarbamate and dibenzylammonium dibenzyldithiocarbamate and are determined in the extract; Mn and Cr(III) are also determined after preconcentration at pH 6.9 with the same chelating agents. Lake waters are analyzed by this method.     

Determination of phosphorous in organic compounds and metal complexes by inductively-coupled plasma atomic emission spectrometry

Phosphorus is determined by inductively-coupled plasma atomic emission spectrometry at 213.618 nm. Different types of organic and inorganic phosphorus compounds and metal complexes were examined after direct dissolution in water, aqueous ethanol or acid, or after decomposition by oxygen flask combustion or Kjeldahl digestion; results were within the usual limit of precision and accuracy for such determinations. The effect of small (<20%) ethanol concentrations in the aqueous solution on the signals obtained from a low-power (1200 W) argon plasma is examined and discussed.     

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.     

Application of hydride generation to the determination of trace concentrations of arsenic by inductively-coupled plasma atomic emission spectrometry

A method is described for the determination of traces of arsenic, based on sodium tetrahydroborate reduction of arsenic and introduction of the arsine formed to a relatively low-powered (1.6 kW) inductively-coupled plasma where the arsenic atomic emission is generated, Inter-element interference effects are described; many can be eliminated by addition of potassium iodide to the sample solutions, but the standard additions method is recommended for accurate arsenic determination. Potassium iodide is also used for prereducing arsenic(V) to arsenic(III). The method has a detection limit of 0.1 ng As ml^-1 and the linear calibration range spans nearly four orders of magnitude. The proposed method is applied to the determination of ng ml^-1 levels of arsenic in waste waters.     

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.     

Iminodiacetic acid/ethylcellulose as a chelating ion exchanger: Part 2. Determination of trace metals by inductively-coupled plasma atomic emission spectrometry

A chelate-forming cellulose, iminodiacetic acid/ethylcellulose (IDAEC), is applied to the collection of metals from ammonium citrate and acetate solutions. A method is devised for the i.c.p./a.e.s. determination of metal contaminants in magnesium by separation and preconcentration of the metals with IDAEC.     

膜去溶-ICP-MS法测定高纯Eu_2O_3中14种痕量稀土杂质

研究了不需基体分离,膜去溶-ICP-MS法直接测定高纯Eu2O3中的14种痕量稀土杂质的分析方法。讨论了Eu基体产生的多原子离子对被测元素的质谱干扰。使用膜去溶后,待测元素灵敏度提高3倍左右,EuO/Eu产率从去溶前的0.016%降低为0.0007%。建立了Tm的数学校正方程,通过膜去溶结合数学校正可将Eu基体对Tm干扰完全消除。14种稀土杂质的检出限和(∑RE)为70 ng/L,测定下限和(∑RE)为0.54μg/g。对6N高纯Eu2O3样品进行了分析,样品回收率为96%~109%,RSD小于10%。所建立的方法对Eu2O3标准样品的测定结果与国家标准方法测定结果相一致。     

Emission efficiency for particulate forms of iron and aluminum in rain-water measured by inductively-coupled plasma atomic emission spectrometry

The bulk emission efficiency for particulate forms of iron and aluminum in rain-water was evaluated. The efficiencies for iron and aluminum were >80% for particles 0.4–1 μm in diameter and about 17% for particles >8 μm; relative standard deviations were <20%. A procedure is described by which the concentrations of particulate forms of iron and aluminum in rain-water are determined. Fluctuation of particles in rain-water during a rainfall event can be monitored in detail.     

Simultaneous multi-element determination of trace metals in sea water by inductively-coupled plasma atomic emission spectrometry after coprecipitation with gallium

Coprecipitation with gallium hydroxide is studied for the preconcentration of trace metals in sea water before multi-element analysis by inductively-coupled plasma/atomic emission spectrometry. Gallium precipitates at pH 9 only when magnesium is present. Optimum conditions are established for multi-element preconcentration and removal of matrix elements. The method is almost free from contamination because of the use of highly pure gallium meetal and only a small amount of sodium hydroxide for pH adjustment. Spectral interferences from gallium are negligible and a concentratioin factor of more than 200 can be obtained. Detection limits range from a few ng l^?1 to 150 ng l^? for Al, Co, Cr, Fe, La, Mn, Ni, Ti, V, Zn, Y and Pb. Artificial and natural sea-water samples can be analyzed with adequate precision.     

石墨炉原子吸收法测定高纯硒中痕量铁

研究了石墨炉原子吸收直接进样法和石墨炉内富集法测定高纯硒中痕量铁的条件,建立了石墨炉原子吸收法直接测定高纯硒中痕量铁的分析方法.直接进样法的检出限为0.008 μg/g,石墨炉内富集法的检出限为0.004 μg/g,相对标准偏差分别为:5.2%和4.6%,两种方法检测样品结果基本一致.测定含铁0.3 μg/g的高纯硒,测定值的RSD为4.6～5.2%.     

Preconcentration and determination of trace chromium(III) by flow injection/inductively-coupled plasma/atomic emission spectrometry

A manifold incorporation an activated alumina (basic form) minicolumn is used to preconcentrate chromium(III), which is then eluted with 2 M nitric acid for detection. Calibration is linear up to 1000 μg l^? Cr, and the limit of detection for a 10-ml sample is 0.05 μg l^?1. The determination of chromium(III) in human urine is discussed.     

Determination of trace impurities in high-purity cadmium by high-resolution inductively coupled plasma mass spectrometry.

Trace impurities in high-purity cadmium were determined by high-resolution inductively coupled plasma mass spectrometry (HR-ICP-MS). To overcome some potentially problematic spectral interference, measurements were acquired in both medium and high-resolution modes. The matrix effects due to the presence of excess HCl and cadmium were evaluated. The optimum conditions for the determination were tested in this experiment and discussed. The detection limits ranged from 0.01 to 0.27 microg g-1, depending on the elements. The results for the determination of 22 trace elements in high-purity cadmium are presented.