Atomic-absorption determination of lead in geological materials

A method is described for the determination by atomic-absorption spectrophotometry of lead, tip to the milligram level, in samples of geological materials. After attack with perchloric-hydrofluoric acid mixture and the removal of perchlorate ion by precipitation as potassium perchlorate, lead is separated from matrix elements by means of anion-exchange in 2M hydrobromic acid on the strongly basic anion-exchange resin Dowex 1 x 8. Lead is adsorbed on the resin column while practically all other accompanying elements pass into the effluent. For the elution of lead 6(M) hydrochloric acid is used and after evaporation of the eluate lead is determined by atomic-absorption spectrophotometry. The method was tested by analysing numerous samples with contents ranging from a few ppm to milligram amounts of lead. In most cases very good agreement of results was obtained.     

Atomic absorption spectrometric determination of copper,zinc, and lead in geological materials

An atomic absorption spectrometric method is described for the determination of copper, zinc, and lead in geological materials. The sample is digested with HF—HCl—H₂O₂; the final solution for analysis is in 10 % (v/v) HCl. Copper and zinc are determined directly by aspirating the solution into an air—acetylene flame. A separate aliquot of the solution is used for determination of lead; lead is extracted into TOPO-MIBK from the acidic solution in the presence of iodide and ascorbic acid. For a 0.50-g sample, the limits of determination are 10–2000 p.p.m. for Cu and Zn, and 5–5000 p.p.m. for Pb. As much as 40 % Fe or Ca. and 10 % Al, Mg, or Mn in the sample do not interfere. The proposed method can be applied to the determination of copper, zinc, and lead in a wide range of geological materials including iron- and manganese-rich, calcareous and carbonate samples.     

Atomic-absorption determination of manganese, cobalt and copper in whole blood and serum, with a graphite atomizer

A new and rapid method is described for the determination of Mn, Co and Cu by atomic absorption with a graphite atomizer and deuterium compensation, on very small samples of whole blood and serum, with no preliminary manipulations. The metal concentrations in blood serum from healthy donors have been found to be Mn 9 +/- 4.3 ng ml ; Co 7.7 +/- 1.9 ng ml and Cu 1.2 +/- 0.16 mug ml .     

Atomic-absorption determination of beryllium in geological materials by use of electrothermal atomization

A method is described for the atomic-absorption determination of beryllium in geological materials, that utilizes electrothermal atomization after a separation by solvent extraction. Samples are decomposed with hydrofluoric acid and nitric acid in Teflon-lined pressure decomposition vessels. Beryllium is isolated by its extraction as beryllium acetylacetonate at pH 8 into xylene and back-extraction in 3M hydrochloric acid. The method has been successfully applied to the determination of beryllium in 14 U.S. Geological Survey standard rocks. Four subsamples from four bottles of each standard sample were analysed in random order. The mean beryllium contents (ppm) are: AGV-1, 1.98; PCC-1, 0.024; MAG-1, 2.84; BHVO-1, 0.90; DTS-1, 0.026; SCo-1, 1.74; SDC-1, 2.52; BCR-1, 1.44; GSP-1, 1.22; SGR-1, 0.86; QLO-1, 1.83; RGM-1, 2.21; STM-1, 8.75; G-2, 2.29. An analysis of variance shows that all the samples may be considered homogeneous at F(0.95) except AGV-1 and DTS-1 which may be considered homogeneous at F(0.99).     

Simultaneous preconcentration of copper, nickel, cobalt and lead ions prior to their flame atomic absorption spectrometric determination

A sensitive and simple method for the simultaneous preconcentration of nutritionally important minerals in real samples has been reported. The method is based on the adsorption of Cu2+, Ni2+, Co2+ and Pb2+ on 4-propyl-2-thiouracil (PUT) loaded on activated carbon. The metals on the complexes are eluted using 5 mL 3 M HNO3 in acetone. The influences of the analytical parameters including pH and sample volume were investigated. The effects of matrix ions on the retentions of the analytes were also examined. The recoveries of analytes were generally higher than 95%. The detection limits for Cu2+, Ni2+, Co2+ and Pb2+ were 1.6, 1.3, 1.2, 2.3 ng ml(-1), respectively. The method has been successfully applied for these metals content evaluation in some real samples including natural water samples.     

Electrothermal atomic absorption spectrometric determination of cobalt, copper, lead and nickel traces in aragonite following flotation and extraction separation

A method of determination of Co, Cu, Pb and Ni in nanogram quantities from aragonite is presented. Flotation and extraction of Co, Cu, Pb and Ni is suggested as methods for elimination matrix interferences of calcium. The method of flotation is performed by iron(III) hexamethylenedithiocarbamate, Fe(HMDTC)(3), as a colloid precipitate collector. The liquid-liquid extraction of Co, Cu, Pb and Ni is carried out by sodium diethyldithiocarbamate, NaDDTC, as complexing reagent into methylisobutyl ketone, MIBK. The electrothermal atomic absorption spectrometry (ETAAS) is used for determination of analytes. The detection limits of ETAAS followed by flotation are: 7.8 ng.g(-1) for Co, 17.1 ng.g(-1) for Cu, 7.2 ng.g(-1) for Pb and 9.0 mug.g(-1) for Ni. The detection limits of ETAAS followed by extraction are found to be: 12.0 ng.g(-1) for Co, 51.0 ng.g(-1) for Cu, 24.0 ng.g(-1) for Pb and 21.0 ng.g(-1) for Ni.     

Simultaneous spectrophotometric determination of traces of cobalt,nickel and copper with dithio-oxamide

The cobalt, nickel and copper complexes of dithio-oxamidc have been characterized in terms of color, effect of pH, structure in solidion, order of addition of reagents, adherence to Beer's law and sensitivity. The reactivity of the reagent to other ions has been reported. A method for the simultaneous spectrophotometric determination of cobalt, nickel and copper has been developed. the results of the application of this procedure to synthetic samples and to several National Bureau of Standards Samples are given.     

Simultaneous spectrophotometric determination of cobalt, nickel and copper with 2,3-quinoxaline- dithiol

In aqueous ethanol cobalt(II), nickel(II) and copper(I) react instantaneously with 2,3-quinoxalinedithiol at pH 2 to form strongly coloured complexes exhibiting absorption maxima at 510, 606 and 665, and 625 nm, respectively. At pH 6 the reaction of copper can be virtually eliminated, while the cobalt and nickel reactions show only small decreases in sensitivity. This behaviour has been made the basis of a rapid method for the simultaneous determination of these three elements. The absorbances of the complexes have been found to be additive for all combinations of these elements in which the individual concentrations have been varied from approximately 0.1 to 1 ppm. A least-squares estimate of the concentration of any of the elements may be readily obtained by using a simple linear equation based on the absorbance readings and a set of constants derived from the spectrophotometric data. The analyses of seven synthetic solutions and four NBS Standard Reference Materials yielded a maximum error of 6.0% and an average error of 1.6%.     

Colorimetric determination of copper, nickel and cobalt in their respective soaps

Summary The metal ion content of heavy metal soaps can be successfully determined colorimetrically using their dilute solutions in pyridine. Measurements with copper and nickel soaps (myristates and palmitates) could be carried out at 675 and 650 nm respectively, those for the corresponding cobalt soaps (myristate and palmitate) at 550 nm.

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Zusammenfassung Der Metallgehalt von Schwermetallseifen kann mit gutem Erfolg colorimetrisch bestimmt werden, wenn man die verdünnte Lösung der Substanz in Pyridin verwendet. Messungen an Kupfer- und Nickelseifen (Myristate und Palmitate) wurden bei 675 bzw. 650 nm, an Kobaltseifen (ebenfalls Myristat und Palmitat) bei 550 nm durchgeführt.

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Thanks are due to Prof. A. R. Kidwai for providing facilities and to the Council of Scientific and Industrial Research, India for the award of a fellowship to one of us (R. H.) to carry out this work.     

Gravimetric determination of cobalt and nickel,and their separations from copper with n-benzoylphenylhydroxylamine

N-Benzoylphenylhydroxylamine can be used for the gravimetric determination of cobalt and nickel. The precipitates can be weighed as such, or ignited and weighed as cobalt sulphate or nickclous oxide. Cobalt or nickel can be separated from copper with the reagent.     

Atomic-absorption spectrometric determination of metals and silicon in tar-sands fly-ash

Atomic-absorption spectrometric methods are described for the determination of metals and silicon in a fly-ash which is produced during oil recovery from Alberta tar sands. The techniques of standard additions and matrix matching are compared. An experimental design for the detection, estimation and correction of interference effects arising in the determination of specific elements in the fly-ash is presented.     

The determination of aluminum,nickel, cobalt,copper, and iron in alnico

A method has been developed for the determination of the major constituents of Alnico based on an anion exchange separation of the chloride complexes and the subsequent determination of aluminum, nickel, copper, cobalt and iron with EDTA. The method is more convenient than conventional classical methods.     

Simultaneous determination of iron, cobalt, nickel and copper by UV-visible spectrophotometry with multivariate calibration

A method for the simultaneous spectrophotometric determination of the divalent ions of iron, cobalt, nickel and copper based on the formation of their complexes with 1,5-bis(di-2-pyridylmethylene) thiocarbonohydrazide (DPTH) is proposed. The resolution of quaternary mixtures of these metallic ions was accomplished by several chemometric approaches. A comparative study of the results obtained for simultaneous determinations in mixture by using principal component regression (PCR) and partial least-squares regression (PLS-1 and PLS-2) for absorbance, first-derivative and second-derivative data is presented. In general, the best recovery values are obtained by the PLS-2 method for absorbance data. This procedure allows the simultaneous determination of the cited ions in alloys and biological materials Good reliability of the determination was proved.     

激光热透镜光谱分析法同时测定铜、钴和镍研究

基于2-(5-NO2-吡啶-2-偶氮)-1-羟基-8-氨基萘-3，6-二磺酸与铜(Ⅱ)、钴(Ⅱ)和镍(Ⅱ)反应酸度的差异及热透镜信号强度的加和性，建立了激光热透镜光谱法同时测定铜、钴和镍的新方法。测定铜、钴和镍的线性范围依次为0～200ng/mL、0～200ng/mL和0～100ng/mL，检出限依次为2ng/mL，2．5ng/mL和1ng/mL。方法已用于合成样品及人发样中铜、钴和镍的同时测定。     

Direct atomic absorption spectrometric determination of copper,nickel and vanadium in coal and petroleum coke

The solid sampling technique is used to determine copper, nickel and vanadium in coals and a petroleum coke. The National Bureau of Standards SRM 1632a, Trace Elements in Coal, and aqueous solutions of the elements were employed as standards. The contents of copper, nickel and vanadium were in the ranges 1–17, 3–130 and 20–140 ppm, respectively.     

Atomic-absorption determination of gold in blister copper and speiss products

Summary The determination of gold at 10^–3–10^–4% levels in black copper and speiss is based upon selective dissolution of the samples with sulphuric acid and separation of the matrix elements by filtration. Gold is determined in the solid residue by flame atomic absorption spectrometry. Relative standard deviation was 7%–10% for about 20 g Au/t.

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AAS-Bestimmung von Gold in Rohkupfer und Speiseprodukten