Determination of Nickel,Manganese, Copper and Zinc in Blood Serum by Atomic Absorption Spectrometry after Deproteinization by Microwave Irradiation

ABSTRACT

Deproteinization of serum was performed by microwave irradiation combined with a small volume of diluted trichloracetic acid. The procedure reduced the protein level of the samples to less than 99% of the total with a small dilution factor (1+1) and allowed the determination of nickel and manganese by electrothermal atomic absorption spectrometry and copper and zinc by flame atomic absorption spectrometry directly without modifiers or matrix interferences. As metallic ions are normally bonded to serum proteins they must be released during protein precipitation. Spiked serum samples were submitted, before the deproteinization, to an incubation treatment to bond the added ions to the proteins. To check the efficiency of the incubation time for each ion, serum samples were ultrafiltered at set time intervals and the metals determined in the ultrafiltrate. The proposed method was compared with the common deproteinization by acids for the separation of the proteins. The reduction of proteins allowed a small dilution of the sample and the use of faster temperature programmes for the determination of nickel and manganese by electrothermal atomic absorption spectrometry and the aspiration of samples more similar to aqueous standards for copper and zinc determination by flame atomic absorption spectrometry. Recoveries from spiked, incubated and deproteinized samples compared to only diluted samples show that the method can satisfactorily be used for atomic absorption spectrometric determination of these elements.     

A Sensitive Indirect Method for the Determination of Titanium by Atomic Absorption Spectrophotometry Using an Air-Acetylene Flame

Abstract

The enhancement of the atomic absorption signal of iron in a fuel-rich air-acetylene flame by small amounts of titanium makes possible the determination of titanium at concentrations of 0.01 to l0ppm. The optimisation of working conditions for the determination of titanium by this indirect method are reported.     

Critical Study of the Determination of Palladium by Graphite Furnace- Atomic Absorption Spectrometry

Abstract

The atomic absorption spectroscopic behaviour of palladium in a graphite furnace has been investigated. The determination is several ordes of magnitude more sensitive than the flame technique. The use of Tantalum coated tubes does not improve considerably the sensitivity but prolongs the lifetime of the furnaces.     

Study of Analytical Methods for Iron Determination in Complex Organic Liquids by Atomic Absorption Spectrometry

Abstract

In the determination of iron in complex organic liquids by atomic absorption spectrometry (A. A. S.), methods of sample preparation, such as dilution with an organic solvent and sample pretreatment to destroy organic material, are investigated. Moreover, methods of analysis using calibration curve and standard additions are presented. The possible cause of error associated with iron determination in organic samples by flame (F-A. A. S.) and graphite furnace (GF-A. A. S.) atomic absorption spectrometry are discussed.

From all of these studies, the use of graphite furnace atomic absorption spectrometry after sample dilution with methyl isobutyl ketone, and the use of the method of standard additions are advised for iron determination.     

Atomic Absorption Spectrometry with an Alternating Current Plasma as an Atomization Source

Abstract

The utilization of an alternating current plasma as an atomization source for atomic absorption spectrometry is described. The analytical performance of this technique has been characterized for the determination of 11 elements. The detection limits (3[sgrave]) were found to be comparable to those determined with existing plasma sources. The accuracy of the method has also been assessed by comparison with flame and graphite furnace atomic absorption spectrometric methods.     

Evaluation of a New Method for the Determination of Elements in Vegetable Foods and Feeds by Atomic Absorption Spectroscopy with Sampling of Carbonaceous Slurry

Abstract

The new method, proposed in a preceeding paper for the determination of elements in plant material by flame atomic absorption spectroscopy (FAAS) with liquid sampling of carbonaceous slurry, was tested on other kinds of organic material such as vegetable foods and feeds. Results are reported for the determination of calcium, magnesium, potassium, iron, manganese, zinc and copper in these materials. Also, the analytical results relative to the determination of cadmium by graphite-tube furnace atomic absorption spectroscopy (GTFAAS) for two matrices are given. In all cases accuracy and precision of the analytical procedure were ascertained.     

Enhancement of Sensitivity for Antimony Determination in Atomic Absorption Spectrophotometry by Introducing Stibine into an Argon-Hydrogen Flame

Abstract

The sensitivity of antimony determination with atomic absorption spectrophotometry is enhanced to a large extent by introducing stibine gas into an argon-hydrogen flame. As a reducing agent, zinc tablet made from the zinc powder paste with water is successfully used for quantitative and rapid productions of stibine from antimony (III) solution. The sensitivity for 1% absorption of the signal is estimated to be about 0.004 ppm of antimony.     

Enhancement of Sensitivity for Selenium Determination in Atomic Absorption Spectrophotometry by Introducting Hydrogen Selenide into an Argon-Hydrogen Flame

Abstract

The sensitivity for selenium determination with atomic absorption spectrophotometry is enhanced to a large extent by introducing hydrogen selenide gas into an argon-hydrogen flame. As a reducing agent, zinc granular and stannous chloride is successfully used for quantitative and rapid productions of hydrogen selenide from selenium(IV) solution. The sensitivity for 1 % absorption of the signal is estimated to be about 0.02 ppm of selenium.     

Application of Ion Chromatography,Nuclear and Spectrochemical Techniques for Trace and Major Element Determination in Seaside Aerosols

Instrumental neutron activation analysis, flame atomic absorption spectrometry, flame atomic emission spectrometry, graphite furnace atomic absorption spectrometry, ion chromatography and visible spectrometry were applied to determine the compositions of atmospheric aerosols, which were collected at a rural site in the Western Black Sea Coast of Turkey. A total of 354 daily aerosol samples were analyzed for about 46 trace and major elements and ions. Sample preparation, quality control procedures, and instrumental operating conditions were reported. Most of the elements measured commonly by the above techniques have very large correlation coefficients and low intercept values indicating the agreement between the results.     

A Sorbent Extraction Procedure for the Preconcentration of Gold,Silver and Palladium on an Activated Carbon Column

ABSTRACT

A preconcentration method based on the use of an activated carbon column has been established for flame atomic absorption spectrometric determinations of gold, silver and palladium. The analytes were sorbed on the column as a complex of dithiophosphoric acid O, O-diethyl ester (DDTP). The sorbed analytes were eluted through the column with 2M NH₃ in acetone. Quantitative recoveries (≥95 %) for gold, silver and palladium were obtained from acidic solutions. The developing method was successfully applied to the determination of trace amounts of gold, silver and palladium in some samples with satisfactory results (relative standard deviation < 7 %; relative error < 3 %).     

A Study of Two Atomic Absorption Methods for the Determination of Sub-Microgram Amounts of Arsenic and Selenium

Abstract

Two atomic absorption accessory units were studied for the determination of arsenic and selenium in waters. One involves a flame mode while the other a flameless mode. Each was analyzed for requirements in speed per analyses, sample sizes required, potential interferences, coefficients of variation, and in overall ease in use.

Although the flameless mode could determine lower levels of arsenic and selenium than the flame mode, it was hampered by some severe interferences. Advantages of these accessories in their use over conventional wet chemical methods included: speed per analysis, elimination of time-consuming concentration steps, and elimination of using fragile equipment and noxious solvents.     

Evaluation of the Uncertainty Associated to the Determination of Heavy Metals in Seawater Using Graphite Furnace Atomic Absorption Spectrometry

Abstract

This work describes the estimation of uncertainty following the “bottom‐up” and the “top‐down” approaches for the determination of several trace metals in seawater when using a classical 1‐pyrrolidinedithiocarbamate/diethyldithiocarbamate/freon extraction method followed by electrothermal atomic absorption spectrometry. A detailed analysis of the uncertainty sources of this method is included, which allows estimating the expanded uncertainties. The results show that the main contribution to the relative overall uncertainty is the extraction step. The estimation of the uncertainty components is shown to be a suitable tool for the experimental design in order to obtain a small uncertainty in the analytical result.     

火焰原子吸收光谱法测定水样中铅含量的不确定度评定

通过采用火焰原子吸收光谱法测定水样中铅的不确定度各项来源和评定方法的分析,建立一种分析实验室不确定度的评定方法,使实验结果更有客观性和准确性.     

Flame Atomic Absorption Spectrometry Assay for Copper Determination in Pharmaceutical Products for Veterinary Use

Abstract

The scope of the present study is to quantify copper in pharmaceutical products of veterinary use, using flame atomic absorption spectometry (f_AAS). The determination is carried out after samples' mineralization in a HCl:HNO₃ (20∶1, v:v) mixture followed by the instrument quantification and the validation of the result. The validation indicates that the interferences from the whole analytical system and their measurement do not influence the results and ensure that there are no other effects which have not been considered.     

Determination of Trace Elements in Aerosol Samples Collected on Polycarbonate Filters by Atomic Absorption Spectrometry

Abstract

The multi-element analysis of aerosol samples collected on polycarbonate filters and the wet digestion procedure in open vessel were investigated. The concentrations of Na, K, Ca, Mg and Zn were determined by flame atomic absorption spectrometry with a micro injection system while Cd, Pb, Cu, Ni and V were determined by graphite furnace atomic absorption spectrometry (AAS).

NIES N[ddot] 8 “Vehicle Exhaust Particulate” Certified Reference Material from the Japan Environment Agency was used to study the decomposition of the samples. Different treatments were applied in order to completely dissolve the aerosol samples. It was found that, from all the methods tested, attack with micro-quantities of HNO₃ and HCIO₄ in an air pressure digestion system was the best procedure for the determination of the elements by AAS.

The recommended method was appropriate for all elements and it was applied to real samples. Two nondestructive analytical techniques for the determination of Na, K, Ca, Mg, Zn and Pb have been compared with the proposed method: proton induced X-ray emission (PIXE) and neutron activation analysis (NAA). Results obtained by the application of these three techniques were similar.     

Use of paper capsules for cadmium determination in biological samples by solid sampling flame atomic absorption spectrometry

In this study, a new device was applied for direct solid sampling flame atomic absorption spectrometry. It was used for trace determination of cadmium in biological samples (bovine and chicken liver). Test samples (0.5 to 7 mg) were weighed into small paper capsules, which were introduced into a quartz cell heated by an air-acetylene flame. Operational conditions for the proposed system were evaluated. There was no significant difference between the results obtained with the proposed system and those obtained after digestion and determination by conventional graphite furnace atomic absorption spectrometry. Good agreement was also obtained with the certified values of two reference materials. Background signals were always low. The characteristic mass was 0.34 ng and relative standard deviation was less than 8%. The limit of detection for the proposed procedure was 1.6 ng or 0.23 μg g^− 1 if a sample mass of 7 mg was used. Excluding the steps for sample preparation (drying, milling and weighing), the proposed system allows the determination of 40 test samples per hour and it can be easily adapted to conventional flame atomic absorption spectrometers.     

Evolved-gas zeeman flame atomic absorption spectrometry for the determination of arsenic compounds

An evolved-gas separation/flame Zeeman atomic absorption spectrometric approach is demonstrated for the speciation and determination of arsenic in oyster tissue. No digestion is needed and separation of inorganic arsenic compounds having similar boiling points is achieved. A stoichiometric or air-rich acetylene/air flame for atomic absorption spectrometry is not generally suitable for arsenic determination because of severe ultraviolet absorption interference at 193.7 nm and low sensitivity; polarized flame Zeeman atomic absorption spectrophotometry with a fuel-rich flame is suitable for the detection of traces of arsenic. The evolved-gas separation/Zeeman atomic absorption approach is simple, based on commercially available instrumentation, and useful for the selective determination of major arsenic compounds. Data are given to demonstrate optimal conditions and to show application to oyster tissue.     

The determination of aluminum by atomic absorption spectroscopy

A study of the determination of aluminum by atomic absorption spectroscopy has been made using a solution of aluminum cupferrate in 4-methyl-2-pentanone to feed oxy-acetylene or oxy-hydrogen flames. Investigations were made on the effect of the variables, viz., slit-width, flow rates, flow ratios and flame positions, on the intensity of aluminum absorption. The data were studied to determine the optimum conditions. These investigations brought out the comparative merits of the two flames for the determination of aluminum, and also elucidated the mechanism of aluminum absorption in an oxy-acetylene flame.     

Chemometrical Interpretation of Lake Waters after their Chemical Analysis by Using Aas,Flame Photometry and Titrimetric Techniques

This article reports the distribution of trace metals and major ions in lake waters of Sultansazl L < L , a reedfield near Kayseri, Turkey. The determination of elements such as Cr, Ni, Cu, Cd and Pb in lake water samples was performed by AAS after a preconcentration step using a column packed with Amberlite XAD-16 resin. Both flame- and graphite furnace-atomic absorption spectrometry was used to determine these metals in lake water samples. The concentrations of the metals bound to humic substances, and free metal ions were determined after their sorption-elution on the resin, separately. The column method optimized with sodium tetraborate reagent was used in determining the free metal ions. In the determinations of Ca²⁺ and Mg²⁺, K⁺ , and SO2-4 , Cl ^m and total hardness, flame atomic absorption spectrometry, flame photometry, and titrimetry were used, respectively. In order to evaluate the analytical data by multivariate statistical techniques which enable feature reduction and grouping of the pollutant sources in lake waters from their chemical composition, principal component analysis (PCA), cluster analysis (CA) and correlation analysis were used. As a consequence of multivariate statistical evaluation, main anthropogenic sources like traffic, industry and agricultural processes were drawn to be responsible from the pollution in the environment investigated.     

Atomic Absorption Spectrometric and Spectrophotometric Trace Analysis of Indium in Environmental Samples

Abstract

Indium (III) was selectively extracted at pH 5.2–5.9 with N-p-methoxyphenyl-2-furylacrylohydroxamic acid (MFHA) into chloroform. BPAR [5-bromo-4(2-pyridylazo) resorcinal] was added to the extract to form an intensely red coloured ternary complex measurable spectrophotometrically at 515 nm (? = 5.81 × 10⁴ 1 mol^?1 cm^?1). The extraction system enabled enrichment of indium and determination of the metal down to 10^?4 ppm (0.1 ppb) levels. For atomic absorption spectrometric determination, indium was extracted with MFHA into methyl isobuyl ketone and measured at 303.9 nm resonance line in the air-acetylene flame. Both the methods were