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PubMed1989

Determination of molybdenum in plasma using graphite furnace atomic absorption spectrometry.

A sensitive method is described for the determination of Mo in plasma or serum by graphite furnace atomic absorption spectrometry. The method involves extraction of the metal as the 8-hydroxyquinoline complex and is free of the interference effects that prevent the direct analysis of plasma for Mo. Recoveries of internal standards were excellent and results from the analysis of a National Institute of Standards and Technology Standard Reference Material were in good agreement with certified values. The sensitivity of the method, based on the analysis of 1 ml of plasma, is ca. 3 ng ml-1.

Animals↗

PubMed1990

Evaluation of biological sample mineralisation methods for the determination of fluorine by graphite furnace molecular absorption spectrometry.

Various mineralisation methods were evaluated as means of treating different liquid and solid biological samples for the determination of fluorine by the formation of aluminium monofluoride in an electrothermal graphite furnace and molecular absorption spectrometry (AIF-MAS). Simple sample dilution and the use of 0.01 M Al3+ + 0.01 M Sr2+ solution as a matrix modifier are sufficient to determine the fluorine content in most liquid samples, although some require the addition of 0.3 M ammonium nitrate to the matrix modifier solution in order to diminish background absorbance. In solid samples, treatment methods routinely used with fluoride ion-selective electrodes such as microdiffusion, furnace ashing - microdiffusion and oxygen flask combustion, were tested for compatibility with AIF-MAS. The results were compared with those obtained with a fluoride ion-selective electrode. The proposed mineralisation methods were checked for applicability to different plants, foodstuffs and other biological materials. Some of the methods gave an over-all precision of better than 10%, which is often acceptable, and all methods gave recoveries above 80%. Differences between labile + ionic fluoride and total fluorine can be established by sample treatment.

Evaluation Studies as Topic↗

PubMed1990

Determination of trace amount of cobalt in feed grains and forages by solvent extraction and graphite furnace atomic absorption spectrometry.

A method is described for the determination of trace amounts of cobalt in feed grains and forages with a detection limit of 1 ng g-1. Samples are ashed in a muffle furnace and complexed with 2-nitroso-1-naphthol. Following solvent extraction, cobalt is determined using graphite furnace atomic absorption spectrometry. The assay can be carried out in a normal analytical laboratory without the need for special "clean" rooms. Reagents have been selected to keep reagent blank values at low levels, and heptan-2-one is used as extracting solvent to avoid problems with evaporation. The assay has been used for diagnostic purposes and to formulate special low cobalt diets for sheep for experimental purposes.

Animal Feed↗

PubMedDate not supplied

Determination of cadmium and lead in foods by graphite furnace atomic absorption spectrometry with Zeeman background correction: test with certified reference materials.

Two methods for the determination of cadmium and lead based on graphite furnace atomic absorption spectrometry (GFAAS) with Zeeman background correction are described. The main difference between the methods is the method of sample destruction, bomb digestion versus dry ashing. The precision and accuracy of the methods has been tested by analysing 16 different reference materials, with cadmium concentrations varying from 2.9 micrograms/kg to 2.7 mg/kg and lead concentrations from 44 micrograms/kg to 13.5 mg/kg. The methods produced results which differ, with a few exceptions, less than 10% from the certified contents, with relative standard deviations of around 5%. The methods are not difficult to carry out, are not very laborious and without modifications are applicable to a large variety of products. The sample solutions obtained can also be used for the determination of other elements, e.g. Al, Cr, Cu, Hg, Mn, Ni and Zn. The detection limits, for test portions of 1 and 5 g (wet products) are 0.5-1 microgram/kg for cadmium and 5-20 micrograms/kg for lead.

Animals↗

PubMed1980

Determination of total tin in environmental biological and water samples by atomic absorption spectrometry with graphite furnace.

Analysis of traces of tin using several analytical techniques (X-ray fluorescence, neutron activation, polarographic techniques and atomic absorption) have been tested. Parameters such as simplicity, rapidity, sensitivity and interferences are compared in order to choose the most useful method for practical purpose. Finally, flameless atomic absorption was chosen for the determination of total tin concentration in different natural samples. Digestion of biological samples (plant, plankton, fish, etc.) was achieved by using Lumatom (a trade organic chemical). Thus, the digested sample is directly injected into the graphite furnace. This digestion technique is suitable and rapid with a minimum of error (contamination and losses). For tin analysis in water samples, a preconcentration of tin is carried out by coprecipitation with 1, 10-phenanthroline and tetraphenyl boron. The precipitate is separated and dissolved in alcohol or in Lumatom. The sensitivity of this method is 0.1 ng absolute tin.

Animals↗

PubMed1986

Determination of ultra trace amounts of cobalt in fish by graphite furnace Zeeman effect atomic absorption spectrometry.

A method is described for determining stable cobalt concentrations in fish flesh and bone using polarized Zeeman effect graphite furnace atomic absorption spectrometry (ZAAS). Cobalt analysis on freshwater fish flesh samples (10 g dry weight) required predigestion and wet-ashing at 70-80 degrees C. Cobalt is chelated with ammonium pyrrolidine dithiocarbamate (APDC) extracted with methyl isobutyl ketone (MIBK) and analysed by ZAAS. The mean cobalt content calculated from the standard additions method using three replicate fish flesh samples was 4.23 +/- 1.0 microgram Co. Kg-1 (dry weight). Analyses were also carried out on flesh and bone samples from similar sized fish, of the same species, taken from three area lakes.

Animals↗

PubMed1991

Graphitized carbon black in quartz tubes for the sampling of indoor air nicotine and analysis by microwave thermal desorption-capillary gas chromatography.

Nicotine in a smoky indoor air environment can be determined using graphitized carbon black as a solid sorbent in quartz tubes. The temperature stability, high purity, and heat absorption characteristics of the sorbent, as well as the permeability of the quartz tubes to microwaves, enable the thermal desorption by means of microwaves after active sampling. Permeation and dynamic dilution procedures for the generation of nicotine in the vapor phase at low and high concentrations are used to evaluate the performances of the sampler. Tube preparation is described and the microwave desorption temperature is measured. Breakthrough volume is determined to allow sampling at 0.1-1 L/min for definite periods of time. The procedure is tested for the determination of gas and paticulate phase nicotine in sidestream smoke produced in an experimental chamber.

Air Pollutants↗

PubMedDate not supplied

Determination of tin in biological materials by atomic-absorption spectrometry with a graphite furnace.

The determination of tin in the blood, liver, kidney, and spleen by atomic-absorption measurement using a graphite furnace was investigated. The presence of 20 micrograms/mL Fe(III) reduced absorbance of 0.2 microgram/mL Sn to 50%. To remove the interference of Fe(III), it was reduced to Fe(II) by 10% ascorbic acid, and Sn(IV) was extracted by methylisobutylketone (MIBK) without a chelating agent. This technique can be applied when 100 micrograms/mL Fe coexists with 0.2 microgram/mL Sn. Four methods for determination of tin in the blood were examined: (a) standard addition, (b) low-temperature ashing/MIBK extraction, (c) wet ashing/MIBK extraction, and (d) direct determination. The results of (a), (b), and (c) showed a high correlation (r greater than 0.86, n = 12), while the values obtained by (d) were scattered widely and showed little correlation with those determined by the other three methods. In methods (b) and (c), the detection limit was 10 ng/mL (0.2 ng Sn) without expansion mode, 2 ng/mL (0.04 ng Sn) with X 5 expansion mode, the recovery more than 90%, and the coefficient of variation 6.6% (n = 8). Method (c) was recommended for large sample sizes, and was also suitable for determination of tin in liver, kidney, and spleen, using 0.5%, instead of 10%, ascorbic acid.

Animals↗

PubMed1983

Microanalysis of platinum in biological media by graphite furnace atomic absorption spectroscopy.

An accurate method for the analysis of platinum in biological matrix is described. The method requires minimal sample handling and pretreatment prior to injection into the graphite furnace. It is reproducible, with average recovery of 97.7% platinum in biological matrix. The data presented also demonstrate that Fe in particular (also NaCl and HNO3) significantly depresses the atomic absorption signal of platinum. Standard addition calibration curves are therefore essential for determination of platinum in biological samples.

Humans↗

PubMedDate not supplied

Graphite calorimeter in water phantom and calibration of ionization chambers in dose to water for 60Co gamma radiation.

A graphite calorimeter similar in size and shape to a Farmer type 0.6-cm3 ionization chamber was developed for direct measurement of absorbed dose at a specified depth in a water phantom irradiated by a beam of 60Co gamma radiation. The accuracy of the absorbed dose determined was estimated to be +/- 1.1% at a dose level of 4 rad/s (4 X 10(-2)Gys-1). The absorbed dose to water at the calibration depth of 5 cm was standardized for our 60Co gamma bean, for a 60-cm SSD and 10 X 10 cm2 field. Farmer type ionization chambers were calibrated against the standardized absorbed dose. The overall accuracy in calibrating the ionization chambers was +/- 1.2%.

Calibration↗

PubMed1991

Determination of dietary cadmium-induced metallothioneins in rabbit kidneys and cadmium in metallothioneins by anion-exchange high-performance liquid chromatography coupled with graphite furnace atomic absorption spectrometry.

A rapid method is described for the determination of dietary cadmium-induced metallothioneins (MTs) in rabbit kidneys by anion-exchange high-performance liquid chromatography. Rabbit kidney MT-I and MT-II were eluted at ca. 15.0 and 18.8 min, respectively, from a DEAE-5PW anion-exchange column with a Tris-HCl buffer (0.01-0.25 M, pH 8.6) and detected by ultraviolet absorbance at 254 nm. A standard calibration curve was constructed using purified standard MT isoforms, which demonstrated an excellent linear correlation between UV absorbance peak heights and the amounts of MT isoforms. Feeding a dose of cadmium for some days resulted in an increase in MT concentrations in rabbit kidneys, but not in the livers. The cadmium concentrations in MT-I and MT-II elutions were determined by graphite furnace atomic absorption spectrometry. MT-I and MT-II showed some differences associated with the oral intake of cadmium. Dietary cadmium also caused zinc to accumulate in kidneys to some extent. The effects of dietary oleic acid on the synthesis of MTs were also studied. Based on the method of standard additions, the recovery of MTs exceeded 93% and replicated injection of samples yielded a relative standard deviation of 2.4% at an MT level of 280 micrograms/g.

Animals↗

PubMed1991

Determination of Cd, Cr, Cu, Pb and Zn in human semen by graphite furnace atomic absorption spectrometry after microwave sample dissolution.

Human semen samples were analyzed by graphite furnace atomic absorption spectrometry, using L'vov platforms and the method of standard additions, to determine their Cd, Cr, Cu, Pb and Zn content. The samples were analyzed directly and after conventional and microwave wet acid dissolution. Matrix modification, using magnesium and palladium nitrates and ammonium biphosphate solutions, was evaluated for the analysis of the microwave-digested samples. The best results were obtained for Cr, Cu and Zn using Pd(NO3)2, and a mixture of Mg(NO3)2 and Pd(NO3)2 solutions. The direct analysis of water-diluted semen produced inaccurate results with unacceptably high standard deviations. The results obtained for the microwave-dissolved samples showed relative standard deviation values within the range 0.63-8.4%. The analysis of spiked semen solutions showed recoveries of the added analytes ranging from 96 to 104%. The accuracy of the measurements was checked against the NIST 1,577a, bovine liver, standard reference material. Sample dissolution time was drastically reduced from 3-4 hours, using the conventional method, to approximately 8 minutes using the microwave-assisted wet acid digestion procedure.

Cadmium↗

PubMed1991

Direct calibration for determining aluminum in bone and soft tissues by graphite furnace atomic absorption spectrometry.

We describe a direct-calibration method for determining aluminum in bone and soft tissues by graphite furnace atomic absorption spectrometry. Aluminum in bone was determined in uncoated tubes, whereas the analytical performance in soft tissue analysis was markedly improved by using pyrolytically coated tubes with a L'vov platform and added calcium. The analytical imprecision (CV) was less than or equal to 5.4% for aluminium concentrations between 12 and 98 micrograms/L, and analytical recoveries of added analyte varied between 94.5% and 103.0%. Detection limits (2 SD of determinations of the zero standard) were 7 and 6 pg for bone and soft tissues, respectively. Characteristic masses (amounts of Al yielding an absorbance signal of 0.0044 A) were 9 and 8 pg, respectively.

Aluminum↗

PubMed1991

Improved sample preparation for accurate determination of low concentrations of lead in whole blood by graphite furnace analysis.

The effect of low concentrations of lead on pre- and post-natal growth and development is a current concern. We describe a simple method of sample preparation for direct determination of lead in whole blood by Zeeman graphite-furnace atomic absorption spectrometry. This procedure improves analytical precision and accuracy of lead determinations at low concentrations as compared with published furnace data. At blood lead concentrations of 0.25, 1.98, and 3.76 mumol/L, within-run CVs were 3.2%, 1.8%, and 1.4% respectively; between-run CVs were 7.3%, 2.9%, and 2.2%. Accuracy, as demonstrated by analytical recovery, ranged from 99% to 102%. Our reproducibility/accuracy score in the 1989 Quebec interlaboratory comparison program was 96% compared with the target, second best of 66 participating laboratories.

Adult↗

PubMed1990

Direct selenium determination in human whole blood by graphite furnace atomic absorption spectrometry with deuterium correction using a L'vov-platform, a Pd/Mg matrix modification and appropriate dilution.

A mixture of palladium/magnesium nitrate was used as matrix modifier in graphite furnace atomic absorption spectrometry for the direct determination of selenium in human whole blood Addition of HCl up to 0.2 M, a twenty-five fold diluted sample and an appropriate furnace program are necessary to eliminate the interference of iron. Reproducibility of less than 3% at the 95 micrograms/L level, a detection limit of 10 micrograms/L and good accuracy, as determined by intercomparison runs and recovery of spiked samples, are obtained. The proposed method can be used for analysing 4 blood samples per hour.

Deuterium↗

PubMed1990

Selenium concentration levels in whole blood of Belgian blood bank donors, as determined by direct graphite furnace atomic absorption spectrometry.

Direct graphite furnace atomic absorption spectrometry after appropriate sample dilution is applied to whole blood of Belgian blood bank donors from different geographical areas. Highest values were obtained for the northern part of the country (Flanders). Different consumption habits may explain the significant difference in selenium level found for the two cultural communities (Flemish and Walloon). No sex difference was obtained in both parts of the country and no influence of age was observed for the two communities. Values obtained are compared with literature data on whole blood selenium content for other European countries.

Adult↗

PubMedDate not supplied

Determination of copper, iron, and nickel in oils and fats by direct graphite furnace atomic absorption spectrometry: summary of collaborative study.

A collaborative study of a method for the determination of copper, iron, and nickel in edible oils and fats by direct graphite furnace atomic absorption spectrometry was recently conducted by the International Union of Pure and Applied Chemistry. The quantitation limits of the method are 5 micrograms/kg for copper and 10 micrograms/kg for iron and nickel. The method has been adopted official first action as an IUPAC-AOAC method.

Copper↗

PubMedDate not supplied

Determination of gold in animal tissue by graphite furnace atomic absorption spectrophotometry.

Historically, compounds that contain gold have been used to treat conditions such as rheumatoid arthritis in humans. However, understanding of the metabolic fate of gold in biological tissues has been limited by lack of sensitive quantitative methods of analysis. We addressed this problem by developing a graphite furnace atomic absorption (GFAA) spectrophotometric method to measure trace amounts of gold. This method was validated on small samples of beef liver, kidney, and bone. The samples were digested in micro-Kjeldahl flasks with a mixture of sulfuric, perchloric, and nitric acids; the residue was treated with aqua regia and extracted into methylisobutyl ketone (MIBK); levels of gold were then measured by GFAA. All the reagents were of an ultra-pure grade and were monitored for gold content. We established that the linear range of quantitation was from 1 to 2500 ppb. Multiple extractions with MIBK were not necessary to recover all the gold, and, in most cases, use of ultra-pure acids was not necessary. A scan of the extracts by inductively coupled argon plasma atomic emission spectrophotometry revealed no appreciable concentration of elements that would be most likely to interfere with the determination of gold. Average recoveries of gold ranged from 102 to 111%, and the overall coefficient of variation was 5.5%.

Animals↗