On-line electrolytic dissolution of solid metal samples and determination of copper in aluminium alloys by flame atomic absorption spectrometry

A flow-injection system was developed in which alloy metal samples are electrolytically dissolved and the dissolved samples are analysed by flame atomic absorption spectrometry (FAAS). The effects of electrolyte composition and electrolysis parameters on the dissolution of the sample were studied. The method was used for the determination of copper in aluminium alloys. Electrolyte solutions consisting of 0.2–1.0 M nitric acid are better than other electrolytes tested with regard to both alloy sample dissolution and determination of copper by FAAS. The peak height increases linearly with the electrolysis time or current within a certain range. The detection limit depends on the sensitivity of the detector used, and can be improved by increasing the electrolysis time or current. Generally, aluminium alloys containing 0.5–10% copper can give suitable signals for FAAS determination. The reproducibility of electrolysis and determination is about 4% for the same sampling points and 5% for different sampling points on the alloy sample.     

The determination of gallium by atomic absorption spectrometry

The use of a nitrous oxide-acetylene flame for the determination of gallium by atomic absorption spectrometry was compared with the use of air-acetylene flames. The nitrous oxide method provided higher sensitivity and was much less sensitive to acid and base composition and to diverse added salts. Significant matrix and background effects, which occurred when gallium was determined in ore solutions with the air-acetylene flame, were eliminated with the nitrous oxideacetylene flame.     

Preconcentration of copper with dithizone-naphthalene for subsequent determination by atomic absorption spectrometry

A simple and convenient method for the separation and preconcentration of copper from aqueous samples has been developed. The procedure is based on the chemical sorption of copper(II) onto a column packed with immobilized dithizone on microcrystalline naphthalene. The trapped copper is eluted with 10 mL of 4 M nitric acid and determined by flame atomic absorption spectrometry. A preconcentration factor of 200 was obtained for a volume of 2 L. The relative standard deviation for the determination of 5 and 10 μg/L copper was 2.2 and 1.7%, respectively. The procedure was successfully applied to the determination of copper in water and alloy samples. The accuracy was assessed through the analysis of certified reference materials or recovery experiments. The text was submitted by the authors in English.     

The determination of titanium in alloys by atomic absorption spectroscopy

A method is described for the determination of 0.1–1.2 % of titanium in steels, permanent magnet alloys and cast iron using atomic absorption spectroscopy with hydrofluoric acid solutions and a nitrous oxide-acetylene flame. No preliminary separations are required. When the correct conditions are employed there is no interference from the other elements commonly found in these alloys.     

The determination of selenium by atom-trapping atomic absorption spectrometry

The application of atom-trapping atomic absorption spectrometry to the determination of selenium has been studied in detail. The optimum experimental parameters were established and the interference of major elements on the determination of selenium was studied using collection on a cold silica tube. The atom-trapping atomic absorption technique gives a detection limit of 0.03 ppm after 2-min collection on silica in an air—acetylene flame. This compares with ca. 1 ppm by the conventional absorption technique at the same 196.1-nm line. Methods to minimize interferences were examined, including the use of a double tube arrangement, an aluminium oxide-coated silica tube and ion-exchange separation. A combination of combustion in an oxygen flask and collection from an air—acetylene flame on the aluminium oxide-coated silica tube yielded satisfactory results in the analysis of four plant tissue samples.     

The determination of manganese in urine by atomic absorption spectrometry

Urine samples were digested with a mixture of nitric, sulfuric, and perchloric acids containing molybdate as catalyst. A two-point standard addition technique involved extracts of buffered, digested aliquots containing 10- and 20-p.p.b. manganese(II) in the aqueous phase. The extraction system was MIBK-cupferron. Of the substances tested only bismuth, antimony, and thallium interfered. From the same subject, five morning urine samples averaged 3.0 p.p.b. of manganese with a range of 2.0–4.2 p.p.b.; the average deviation was 0.6 p.p.b.     

The determination of sulphate in fertilizers by atomic absorption spectrometry

Methods are described for the determination of sulphate in superphosphate fertilizers. Barium sulphate precipitated from an acidified EDTA solution is filtered onto a membrane filter and redissolved in ammoniacal EDTA, and the barium equivalent to the sulphate is determined by atomic absorption spectrometry. Alternatively, after precipitation of calcium as oxalate during sample solution preparation, and by following a similar sulphate precipitation technique, excess of barium is determined in the filtrate. No interferences were encountered when a nitrous oxide—acetylene flame was used with a potassium ionization buffer.     

The determination of lead in petrol by atomic absorption spectrometry

The lead compounds are extracted into aqueous iodine monochloride, converted to lead nitrate by digestion with nitric acid, and determined by atomic absorption spectrometry against aqueous lead nitrate standards. The procedure is accurate, precise and rapid.     

Fast determination of lead and copper in dairy products by graphite furnace atomic absorption spectrometry

A rapid and direct procedure for determining lead and copper in dairy products by electrothermal atomic absorption spectrometry (ETAAS) is described. Samples are slurried in a medium containing 50% v/v hydrogen peroxide, 1% v/v nitric acid, 0.5% w/v dihydrogen phosphate, and 20% v/v ethanol and directly injected into the furnace with no previous mineralization. Calibration is performed with aqueous standards. Limits of determination were 0.4 and 2.4 ng/mL for copper and lead, respectively. The reliability of the procedure was checked by comparison with the acid mineralization procedure and by analyzing 3 certified reference milk samples.     

The determination of silver in aluminium alloys by atomic absorption spectroscopy

Atomic absorption spectroscopy is used to determine silver in aluminium alloys. The effects of the presence of alloying elements are discussed. The developed procedure is simple and rapid, and results obtained on various samples show satisfactory agreement with those obtained by the normal volumetric procedure.     

The indirect determination of organic compounds by atomic absorption spectrometry

The feasibility of determining indirectly certain organic compounds by precipitation of insoluble silver compounds and determining the excess silver(I) by atomic absorption spectrometry (AAS) has been demonstrated. The determination of other compounds, such as alkylated barbiturates and mercaptans by similar methodology should be possible. Although direct AAS methods are preferable to indirect methods, the insolubility of many silver salts, the inherent sensitivity of the AAS method for silver, and the speed and convenience of AAS methodology suggests that under certain conditions, an indirect AAS method may be appropriate and the method of choice.     

Indirect determination of perchlorate by atomic absorption spectrometry

A liquid-liquid extraction and determination of perchlorate by atomic absorption spectrometry is described. The method involves extraction of perchlorate with the Schiffs base complex [Co(BPTC)₂]⁺, where BPTC = 2-benzoyl pyridine thiosemicarbazone, in methyl isobutyl ketone in acidic medium and subsequent analysis of cobalt in flame AAS, hence indirectly for perchlorate. The extraction efficiency is 98%. The calibration graph was found to be linear for 1.0–11.4 g ClO ₄ ^– per ml of solvent, and the limit of detection is 30 ng ml^–1. The present method is free from interference of large number of foreign ions. The method has been applied for determination of perchlorate in human blood serum samples spiked with perchlorate, urine and commercial potassium chlorate sample.     

The determination of tin by carbon filament atomic absorption spectrometry

The atomic absorption characteristics of tin on a carbon filament atom reservoir are described. The behaviour of tin in aqueous solution astin(II) chloride, in xylene as tin octoate and in oil solutions is studied. The interferenceeffects of a selected range of seven cations, added as chlorides in aqueous solution or as naphthenates in non-aqueous media, and of sulphate and phosphate were examined. In all cases, the signals were measured in the filament reservoir with a surrounding hydrogen diffusion flame. The 1% absorption sensitivity in the organic media at the 286.3-nm line was 10^-10 g and 9·10^-11 g in aqueous solution. In the latter medium, the corresponding sensitivity at 224.6 nm was 6.7·10^-11 g. The linear analytical range lay in the region 0 to 20 ng.     

Indirect determination of vanadium by atomic absorption spectrometry

An indirect method for the determination of vanadium as vanadate by atomic absorption spectrometry is described. In neutral medium, vanadate forms a stable ion-association complex with copper (II) and biguanide, which is extractable into butanol with an efficiency higher than 99%. The copper content in the extract (and hence indirectly VO^?₃) is determined by aspirating it directly into an acetylene flame. The calibration graph is linear up to 3.4 μg ml^?1 of VO^?₃. The limit of detection is 16 ng ml^?1. Only chromium interferes.     

The determination of gold in vegetation by electrothermal atomic absorption spectrometry

A method is described for determining nanogram quantities of gold in vegetation. The sample is digested with fuming nitric acid. After addition of hydrochloric acid, the gold is extracted into 1 ml of 4-methylpentan-2-one; the organic layer is back-extracted with distilled water to remove iron interference, and gold in the organic layer is determined by electrothermal (graphite furnace) atomic absorption spectrometry. Limits of detection depend on the volume of organic phase used but can be as low as 0.2 ng g^?1 for an original sample weight of 1 g.     

The determination of zinc in blood plasma by atomic absorption spectrometry

Atomic absorption spectrometry has been used in the analysis of plasma zinc because of its sensitivity and simplicity. Dilution techniques reduce the viscosity of plasma and facilitate direct analysis, but viscosity differences can produce deviations in aspiration rates between sample and standard, and so cause errors. A direct (1 + 4) dilution of plasma with deionized water is suggested. Working zinc standards are prepared in 5% glycerol to approximate the viscosity characteristics and aspiration rates of the diluted plasma samples. The analytical curves for diluted plasma samples and 5% glycerol working standards proved identical. Plasma zinc concentrations are accurately calculated from a daily working curve. The accuracy of the method exceeds 99% and recovery of added inorganic zinc to a pooled plasma averages 99.8%. The precision is primarily limited by baseline drift. A confidence interval of ± 2 μg/100 ml was achieved by means of six contiguous 10s-integration readings. The method is free of nebulizer clogging and matrix interferences and is not subject to significant day-to-day variations. Because the method is accurate, sensitive, reliable and specific, it should be useful in the clinical laboratory.     

The determination of titanium in iron and steel by atomic absorption spectrometry

A method has been developed for the determination of titanium by atomic absorption spectrometry in a wide range of iron and steels containing <1% aluminium. Interferences are overcome by the addition of aluminium to sample and standard solutions. The accuracy and reproducibility of the method have been established at the 0.05,0.15 and 0.50% levels with British Chemical Standard samples. The procedure is time-saving, particularly as aluminium may be determined on the same initial 2% ($\text{w}\text{v}$) sample solution.     

Indirect determination of pilocarpine by atomic absorption spectrometry

Atomic absorption spectroscopic (AAS) method for microdetermination of pilocarpine alkaloid has been developed. The procedure is based upon the measurement of mercuric content of pilocarpine complex. The experimental conditions as well as the molar ratio were thoroughly studied. The percentage recovery of pilocarpine was found to be (99.15 ± 0.79). The proposed method was applied on pharmaceutical formulations and the results were satisfactory and in good agreement with that given by the official one.     

The determination of lead in copper-base alloys and steel by atomic absorption spectrophotometry

The principle of atomic absorption spectrophotometry has only recently been exploited as an analytical technique and details are given of the development of a procedure for determining lead in copper-base alloys and leaded steels. The recommended method is simple, rapid and provides results as accurate as those obtained by the more time-consuming alternative methods in current use.