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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↗

Direct determination of selenium in serum by graphite-furnace atomic absorption spectrometry with deuterium background correction and a reduced palladium modifier: age-specific reference ranges.

We describe the development of a direct method for determination of selenium in serum by graphite-furnace atomic absorption spectrophotometry with deuterium background correction. We include palladium modifier to stabilize selenium in the presence of a strong reducing agent. Spectral interferences from iron are not evident in this system. Because an analysis requires only 20 microL of serum or plasma, the method is applicable to neonatal populations. At a selenium concentration of 0.75 mumol/L (approximately the mean found in our pre-term infants), the within-run CV is 5.3%. For a concentration of 1.83 mumol/L, which approximates our normal adult mean, within-run and between-run CVs are 2.7% and 3.4%. Accuracy is demonstrated by analytical recoveries ranging from 96% to 102%. We present reference values for pre-term and term infants, and age-specific ranges for infants to adults.

Adolescent↗

Total arsenic in foods after sequential wet digestion, dry ashing, coprecipitation with ammonium pyrrolidine dithiocarbamate, and graphite-furnace atomic absorption spectrometry.

A graphite-furnace atomic absorption (GFAAS) method is described for determining total arsenic (organic and inorganic compounds) in foods. Samples ranging from 1 to 40 g (depending on moisture content) were digested with HNO3 and dry-ashed at 500 degrees C overnight after addition of MgO. After dissolution in HCl, the arsenic was reduced with iodide and ascorbic acid and precipitated with ammonium pyrrolidine dithiocarbamate (APDC) in the presence of nickel carrier. Precipitates were collected on 0.3 micron cellulose acetate filters and dissolved in 10% HNO3 containing modifier. Ba(NO3)2 was added to remove a sulfate interference resulting from decomposition of APDC. Arsenic was determined using GFAAS. Accuracy of the method was good for 7 U.S. National Bureau of Standards (NBS) Standard Reference Materials and 3 National Research Council of Canada (NRCC) round-robin samples. Recovery of arsenic(V) from foods averaged 99.2% for peak heights and 97.1% for peak areas, with relative standard deviations (RSD) of 2.2% for peak heights and 3.3% for peak areas for all NBS and NRCC materials. Detection limit of the method was ca 10 ng arsenic.

Arsenic↗

Allergic contact dermatitis from a nonbisphenol A epoxy in a graphite fiber reinforced epoxy laminate.

An employee of the Composites Division of an aircraft engine manufacturing firm developed dermatitis associated with the handling of a graphite fiber reinforced epoxy laminate (epoxy prepreg). Patch test investigation demonstrated that the responsible causal agent was the nonbisphenol A epoxy binder, 4-glycidyloxy-N, N-diglycidylaniline. A patch test with bisphenol A epoxy from a standard patch test screening series was negative. Subsequent interviews with employees of the Composites Division suggested that a relative lack of awareness of the cutaneous hazards of fiber reinforced epoxy laminates, compared with liquid epoxy resin systems, may be an important risk factor for allergic sensitization to these composite materials.

Adult↗

Determination of copper in infant formula by graphite furnace atomic absorption spectroscopy with a L'vov platform.

A rapid method for the determination of sub-part-per-million levels of copper in infant formula, which does not require decomposition of the sample matrix before analysis, has been developed. The method uses L'vov platform graphite furnace atomic absorption spectroscopy (GFAAS), a technique that greatly reduces matrix interferences limiting the applicability of normal GFAAS. The sample preparation consists of dilution of a weighed sample of infant formula to a known volume with a 0.5% solution of Triton X-100 in deionized water. The accuracy of the method, as assessed from the results of overspike recovery studies (96.5-101.3% recovery) for different matrix types and comparison to results generated with alternative methodologies, can be considered excellent. The overall precision of the method ranges from 2.5 to 4.3% RSD for different matrix types.

Copper↗

Determination of cadmium in urine by graphite-furnace atomic absorption spectroscopy.

A simple procedure for graphite-furnace atomic absorption analysis of cadmium in urine, based on the use of a temperature-controlled heating unit, is described. The temperature of the carbon rod is measured by resistance and controlled by electronic feedback. We studied the influence of various heating times and temperatures of ashing and atomization, as well as suitable diluents. Urine samples were diluted with an equal volume of 0.3 mol/liter HNO3, and 1 to 5 microliter of the mixture was analyzed, with background correction. Signals were evaluated electronically, giving values for integrated peaks as well as for peak heights. The detection limit was 1.2 nmol/liter. The method appears to be accurate and reproducible. The CV averaged 8% for concentrations in the range 20 to 100 nmol/liter. Correlations with a chelation-extraction method was 0.994.

Cadmium↗

[Estimation of aluminium in biological fluids by atomic absorption spectrophotometry in a graphite oven (author's transl)].

The possibilities of use of a graphite oven type HGA 74 (Perkin Elmer) for the estimation of aluminium in biological fluids by atomic absorption spectrophotometry are described, with a special study of the stages of drying, mineralisation, atomisation, flow of inert gas, requirement for correction of non-specific absorption, etc. Under fixed experimental conditions, the limit of sensitivity (absorption 1%) was 2.28.10.(-11) grams and the linearity was good up to 100 microgram/l. This method of analysis by direct treatment of the samples required only small volumes of the latter and reduces the risk of contamination.

Aluminum↗

[Microanalysis of serum iron by atomatic absorption spectrophotometry in a graphite oven: improvement and evaluation of this method].

We describe a method of micro-assay of serum iron by atomic absorption without flame, after deproteinisation of the serum by molar hydrochloric acid. In this way, we can assay the serum iron in 10 microliters of serum by injection of the supernatant into a graphite oven. The results show a good correlation with those obtained by conventional techniques of atomic absorption and colorimetric assays using ferrozine and bathophenanthroline. However, great care must be taken in the cleaning of plastic test tubes.

Blood Proteins↗

Analysis of calcium and lead in calcium supplements by inductively coupled plasma-atomic emission spectrometry and graphite furnace atomic absorption spectrophotometry.

A method was developed to analyze various calcium supplements for Ca and Pb content. The analysis involves a dry ash of the supplements followed by wet digestion. The Pb is determined by graphite furnace atomic absorption spectrophotometry (GFAAS). Analysis of Ca is by inductively coupled plasma-atomic emission spectrometry (ICP-AES). Ca supplements fortified with Pb at levels ranging from 0.25 to 10.0 micrograms/g yielded recoveries ranging from 82.7 +/- 4.2 to 105.0 +/- 1.7%. To test accuracy, the method was applied to National Institute of Standards and Technology standard reference materials (NIST SRMs) 1572 citrus leaves and 1486 bone meal. GFAAS analysis of SRM 1572 averaged 13.1 +/- 0.6 micrograms Pb per g (certificate value, 13.3 +/- 2.4 micrograms Pb per g), and analysis of SRM 1486 averaged 1.34 +/- 0.11 micrograms Pb per g (certificate value, 1.335 +/- 0.014 micrograms Pb per g). ICP-AES analysis of SRM 1572 averaged 3.12 +/- 0.01% Ca (certificate value, 3.15 +/- 0.10% Ca by weight), and analysis of SRM 1486 averaged 27.63 +/- 0.27% Ca (certificate value, 26.58 +/- 0.24% Ca). The method's limit of quantitation (LOQ), on supplement Ca basis and a 1 g sample, averaged 0.75 micrograms Pb per 1 g Ca for supplements containing 9 to 35% Ca by weight. At a Pb level of 0.663 micrograms/g Ca, the reproducibility relative standard deviation (RSDr) averaged 7.3% and the repeatability relative standard deviation (RSDR) averaged 8.0%. It is recommended that the method be studied collaboratively.

Calcium↗

Determination of zinc in serum, blood, and ultrafiltrate fluid from patients on hemofiltration by graphite furnace/atomic absorption spectroscopy or flow injection analysis/atomic absorption spectroscopy.

Two methods were optimized for the determination of zinc in samples of blood, serum, and ultrafiltrate fluid from patients with chronic renal impairment undergoing hemofiltration. In the first procedure, after acid digestion of the samples, Zn in blood and serum is determined by a system coupled to flow injection analysis and atomic absorption spectroscopy. The method is rapid, automated, simple, needs small amounts of sample, and has acceptable analytical characteristics. The analytical characteristics obtained were as follows: determination range of method, 0.05-2.0 ppm of Zn; precision as coefficient of variation (CV), 5.3%; recovery, 95-105%; and detection limit (DL), 0.02 ppm. The second method is optimized for ultrafiltrate fluid because the sensitivity of the first procedure is not suitable for the levels of Zn (ppb or ng/mL) in these samples. The technique chosen was atomic absorption spectroscopy with electrothermal atomization in a graphite furnace. The analytical characteristics obtained were as follows: determination range of method, 0.3-2.0 ppb Zn; CV, 5.7%; recovery, 93-107%; and DL, 0.12 ppb. The methods were used to determine zinc in samples of blood, serum, and ultrafiltrate fluid from 5 patients with chronic renal impairment undergoing hemofiltration to discover whether there were significant differences in the zinc contents of blood, serum, and ultrafiltrate fluid after the hemofiltration process. An analysis of variance of the experimental data obtained from a randomly selected group of 5 patients showed that zinc concentrations in the ultrafiltrate fluid, venous blood, and venous serum do not vary during hemofiltration (p < 0.05), whereas in arterial blood and serum, the time factor has a significant effect.

Flow Injection Analysis↗

Determination of platinum in wine by graphite furnace atomic absorption spectrometry.

A method based on graphite furnace atomic absorption spectrometry (GFAAS) was developed for determining platinum in wine. Wine samples were prepared by microwave acid digestion or dry mineralization. The method of standard addition was used for Pt determination in untreated wine samples and mineralized samples. Analyte modifiers and furnace conditions were optimized. Effects of cations (Mg2+, Ca2+, K+, Na+, and NH4+) and anions (PO4(3)-, SO4(2)-) were tested separately and in combination. Analytical characteristics of the method were optimized for analyte recovery and signal enhancement. Recoveries ranged from 92.5 to 102%, and precision reproducibility relative standard deviation varied from 7.5 to 10%. Red, rosé, and white wines from France were analyzed. Platinum levels found in most wines were very low (< 10 micrograms/L).

Calcium↗

Comparison of closed-vessel and focused open-vessel microwave dissolution for determination of cadmium, copper, lead, and selenium in wheat, wheat products, corn bran, and rice flour by transverse-heated graphite furnace atomic absorption spectrometry.

A method is described for the determination of Pb, Cd, Cu, and Se in cereal samples. An atomic absorption spectrometer equipped with a transverse-heated graphite furnace with Zeeman background correction was used for all determinations. Sample preparation was performed by closed-vessel microwave digestion using nitric acid and focused openvessel microwave digestion using nitric acid-hydrogen peroxide. Both techniques were evaluated by using 15 cereal reference materials and comparing results with certified or reference values for each element. Cereal reference standards obtained from the Community Bureau of Reference (Europe), the National Institute of Standards and Technology (USA), the National Institute for Environmental Studies (Japan), the National Research Centre for Certified Reference Materials (People's Republic of China), and the Canadian Grain Commission were used. Application of a series of t-tests, conducted according to Sidak's modified Bonerroni t-procedure, showed that both techniques yielded accurate results for cereal reference materials. Some differences from certified and reference values, however, were found for each element.

Bread↗

Determination of calcium by inductively coupled plasma-atomic emission spectrometry, and lead by graphite furnace atomic absorption spectrometry, in calcium supplements after microwave dissolution or dry-ash digestion: method trial.

A 3-laboratory method trial was conducted to evaluate 2 sample digestion procedures and instrumental determination parameters for analysis of calcium and lead in Ca supplements. Calcium supplements were treated by dry-ash digestion or microwave dissolution prior to spectrometric analysis. In each case, Pb was determined by graphite furnace atomic absorption spectrometry and Ca by inductively coupled plasma-atomic emission spectrometry. Blind duplicates of 6 Ca supplement samples were analyzed after each sample treatment procedure. Matrix pairs contained dissimilar Pb levels to cover the analyte range encountered during method development. Calcium content of the Ca supplement samples also reflected the range seen during method development. Stock solutions of Ca and Pb were supplied to collaborators for preparation of quantitation standards to remove a variable external to the method. National Institute of Standards and Technology Standard Reference Material (NIST SRM) 1486, bone meal, was included to assess method accuracy and recovery at NIST certificate Ca and Pb levels for this material (26.58 +/- 0.24% Ca and 1.335 +/- 0.014 micrograms Pb/g). Analyses of the NIST SRM yielded 25.9 +/- 1.1 and 27.2 +/- 2.3% Ca and 1.53 +/- 0.19 and 1.26 +/- 0.19 micrograms Pb/g for dry-ash and microwave procedures, respectively. Statistical analyses of data indicated acceptable repeatability and reproducibility for determination of Pb and Ca in various Ca supplements. With either sample preparation technique, the method is appropriate for determining Pb or Ca in Ca supplements.

Biological Products↗