Simultaneous multielement AAS with carbon furnace atomization for the analysis of biological samples

Summary A continuum source AAS spectrometer coupled with a graphite furnace atomizer was employed for the determination of trace elements in biological materials (enzymes, blood serum). With proper furnace conditions, accurate multielement determinations can be made simultaneously.

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Simultane Multielement-AAS mit Graphitofen-Atomisierung zur Analyse biologischer Proben

Zusammenfassung Eine Kontinuum-Lichtquelle in Verbindung mit einem Graphitofen-Atomiser wurde zur Bestimmung von Spurenelementen in biologischen Materialien (Enzyme, Blutserum) eingesetzt. Die erreichte Genauigkeit ist mit der bei der Isotopenverdünnungs-MS erzielbaren vergleichbar. Matrixeffekte können reduziert werden.

     

Synthetic multielement standard samples for serial neutron activation analysis of biological materials

New synthetic standard samples (SSB-1 and SSB-2), produced on the basis of phenol-formaldehyde resin in the shape of tablets are suggested. The samples are intended for INAA of biological materials. SSB-1 and SSB-2 samples contain Se, Cr, Au, Sb, Ag, Rb, Fe, Zn, Co and Ca, Ba, Hg, Sn, Br, Cs, Ni, Sc and Na. The concentrations of these elements are chosen so that the maximum statistical error of -quantum registration by the semiconductor detector should not exceed 3% when irradiating samples in a neutron flux of 10¹³ n·cm^–2·s^–1.     

An accurate procedure for multielement neutron activation analysis of trace elements in biological materials

A procedure for radiochemical neutron activation analysis of biological materials for As, Cd, Co, Cu, Ga, Hf, Mg, Mn, Na, Sb, Sc, Se, Zn, and the rare-earth elements (REE) has been developed. Maximum control over accuracy has been emphasized. Samples are digested under reflux in the presence of carrier for every element determined, and a chemical yield is measured for every element assayed. The procedure has been tested by replicate analysis of National Bureau of Standards bovine liver sample (SRM-1577). Values agree to within their uncertainties with those given by NBS for the 9 elements of this group that they have analyzed. Accuracies at the 90% confidence level for elements in the liver sample are estimated as better than ±10% for Cu, Na, and Zn, between ±10 and ±25% for As, Co, Hg, La, Mn, and Se, and between ±25 and ±50% for Cd, Sb, Sc, and Sm.     

Trace multielement analysis in boron materials by epithermal neutron activation analysis

A method, based on epithermal neutron activation analysis using a boron filter is described for the determination of ～60 trace elements in boron and its compounds. The method has an accuracy of ～20%, a precision of ～15% RSD and limits of detection for most elements are either at the sub-ppm or low ppm levels. The method requires no sample preparation and is economical in effort.     

Automated wet ashing and multi-metal determination in biological materials by atomic-absorption spectrometry

Ohne Zusammenfassung

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Automated wet ashing and multi-metal determination in biological materials by atomic-absorption spectrometry

     

Simultaneous multielement determination of rare earth elements by substoichiometric activation analysis

This paper presents simultaneous substoichiometric separation of four rare earth elements; samarium, europium, terbium and ytterbium. The elements are separated simultaneously and substoichiometrically by forming their complexanates with substoichiometric DTPA and extracting their unreacted parts with HTTA. Application to the determination of these elements by substoichiometric neutron activation is also presented.     

New Polish certified reference materials for multielement inorganic trace analysis

Summary An overview of the activities of the Polish Institute of Nuclear Chemistry and Technology in the field of preparation and certification of reference materials for multielement trace analysis is presented. A general strategy has been worked out and is briefly described with more detailed emphasis on the problem of data evaluation. Two geological-environmental materials recently issued [i.e. an Apatite Concentrate (CTA-AC-1) and Fine Fly Ash (CTA-FFA-1)] which were certified for 25 and 40 elements, respectively, are described. The preparation and testing of a new CRM of biological origin Oriental Tobacco Leaves (CTA-OTL-1) is presented in detail, including study of the optimum methods for drying, checking homogeneity, radiation sterilization etc. Interlaboratory comparison, in which 61 laboratories participated, yielded results enabling recommended (certified) values for 29 elements and information values for further 11 elements to be established.     

Simultaneous multielement analysis of various human tissues by inductively-coupled plasma atomic-emission spectrometry

Human soft tissues were analysed by inductively-coupled plasma atomic-emission spectrometry (ICP-AES) for twelve elements. The tissues had been vacuum-dried for storage and were dry-ashed at low temperature and then digested with nitric acid prior to analysis. Accuracy and precision were examined by analysing NBS Standard Reference Material 1577 Bovine Liver. For P, K, Na, Mg, Ca, Fe, Cu, Zn and Cd, the concentrations obtained were within 4% of the certified or informational values. It was found that cerebrum, cerebellum, heart, kidney, liver, pancreas, spleen and muscle samples in portions of less than 1 g dry weight could be conveniently analysed for these elements.     

Simultaneous multielement analysis of zeolite catalysts by inductively-coupled plasma atomic emission spectrometry

Summary A method comprising digestion of zeolites with an acid mixture followed by inductively-coupled plasma atomic emission spectrometry (ICP-AES) has been established for the simultaneous determination of Al, Na, La and Si in various zeolite samples. Various aspects including sample digestion, instrumental interference effects as well as analytical performance and applicability of the established method have been investigated in detail. The results indicated that aqua regia in combination with hydrofluoric acid was effective for decomposition of a wide variety of zeolite samples. The effects of borate and fluoride ions in the digested sample solution on the ICP-AES determination have been carefully investigated. The method established will be generally applicable for the simultaneous determination of Al, Na, La and Si in zeolite with a precision of 5%. The analytical results obtained were checked by comparison with classical wet chemistry methods and found to be in reasonably good agreement. Application to the kinetic study of La-NaY exchange reaction was also performed.

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Simultane Multielementanalyse von Zeolit-Katalysatoren durch ICP-AES

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Dedicated to Prof. Dr. W. Fresenius on the occasion of his 75th birthday     

Simultaneous determination of mercury and selenium in biological materials by radiochemical neutron activation analysis

A simple and sensitive radiochemical neutron activation analysis (RNAA) method has been developed for the simultaneous determination of mercury and selenium in biological materials. The radiochemical procedure is based upon the digestion of irradiated samples with sulphuric and nitric acids followed by subsequent extractions of mercury and selenium into toluene, first of mercury from 7.5 M H₂SO₄-0.01M HBr media and after of selenium from 7M H₂SO₄-1 M HBr media. After washing of the organic phases with similar media, the mercury bromide was back-extracted into 0.034M EDTA in 5% aqueous ammonia and the selenium bromide into 0.14M H₂O₂ in aqueous solution. The¹⁹⁷Hg and the⁷⁵Se were counted on a Ge(Li) detector. The precision and accuracy of the method was checked by analysing NBS Standard Reference Materials: orchard leaves and bovine liver.     

Comparison of instrumental neutron activation analysis of geological materials with other multielement techniques

Results obtained for 12 elements in approximately 1600 rocks by instrumental neutron activation analysis (INAA) are compared with those obtained by ICP emission spectrometry (ICP-ES), XRF, and atomic-absorption spectrometry (AAS). Sample duplicates and two controls are used to evaluate the precison of the methods investigated. Application of a method (Maximum Likelihood Functional Relationship) to determine and quantify rotational and translational bias is demonstrated. The elements Na, Fe, Ba, Co, Cr, La, Ni and Rb can be determined in rocks by INAA with sufficient sensitivity and precision, whereas the determination of Ag, Yb, Zn and Zr suffers from inadequate sensitivity. Good agreement is seen in the results for Na (by INAA, ICP-ES and XRF) and AG (INAA and AAS). A significant positive bias (13% or less) is evident in the comparison of results by INAA and ICP-ES or XRF for Cr, Ba, Ni and Fe over a wide range of concentration. A similar trend, though less significant, is observed for the elements Yb, Rb, La and Co; the upper limit of concentration for satisfactory determination is within a decade of the highest detection limit for these elements. Rotational and translational bias is evident for Zn in the comparison of data obtained by INAA and ICP-ES, the results by INAA being appreciably lower above about 400 ppm Zn.     

Simultaneous determination of arsenic, manganese, and selenium in biological materials by neutron-activation analysis

A new method was developed for the simultaneous determination of arsenic, manganese, and selenium in biological material by thermal-neutron activation analysis. The use of (81 m)Se as indicator for selenium permitted a reduction of activation time to 1 hr for a 1 g sample, and the possibility of loss of volatile compounds during irradiation could be dismissed. No pretreatment of the sample is required, and the radiochemical separation scheme is based on simple chemical operations, completed in less than 3 hr. A systematic experimental investigation of the performance characteristics of the method was carried out, including studies of the accuracy of the results. The actual precision achieved in routine application of the method in the analytical laboratory was in good agreement with the calculated precision, and the results are therefore well suited for statistical evaluation of differences at the ppM level in samples of biological tissue.     

Use of standard reference materials as multielement irradiation standards in neutron activation analysis

Standard reference materials, normally used to check accuracy and precision of analytical methods or for interlaboratory comparisons, are proposed for use as multielement irradiation standards in neutron activation analysis (NAA). The advantages are simplicity of operation, and elimination of errors inherent in the preparation of a large number of synthetic standards at the trace element level. Examples of the approach are illustrated in the analysis of geological materials, soils, sediments, meteorites, lunar samples, coal and fly ash using the USGS diabase W-1 as the irradiation standard. Plant materials and animal tissue are analyzed using NBS Orchard Leaves as the irradiation standard. Best values for four popular SRM's (W-1, Bowen's Kale, Orchard Leaves, and Bovine Liver) are tabulated to facilitate further use of the proposed approach to multielement neutron activation analysis.     

Hot-injection procedures for the rapid analysis of biological samples by electrothermal atomic-absorption spectrometry

The combination of palladium/hydrogen matrix-modification and injection of samples into a graphite tube at 120 degrees has allowed the accurate determination of copper, iron, lead and nickel in biological reference materials (urine, milk powder and bovine liver). Palladium modification allowed the use of a standard ashing temperature of 1000 degrees for all four elements. Direct aqueous calibration was applied without the need for standard additions. The total heating cycle, from the start of sample injection, took 45 sec.     

Resonance activation analysis of biological materials

An istrumental method is developed for the determination of As, Br, Cd, I, Mg, Mo, Sb, Si, Sn and Sr in biological materials based on resonance neutron activation analysis. Samples were irradiated inside cadmium and boron shields with reactor neutrons and counted on Ge(Li) detector after a delay of about 5 min. The interfering activities of²⁴Na,³⁸Cl and⁵⁶Mn were significantly reduced particularly in the boron shield. The advantage factors of the various elements are compared for boron and cadmium shields. The method is especially useful for the determination of As, Cd, I and Sn.     

Simple method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer

A method for determination of selenium in biological materials by flameless atomic-absorption spectrometry using a carbon-tube atomizer is described. The sample is burned by an oxygen-flask combustion procedure, the resulting solution is treated with a cation-exchange resin to eliminate interfering cations, the selenium is extracted with dithizone in carbon tetrachloride and the resulting selenium dithizonate is combined with nickel nitrate in the carbon tube to enhance the sensitivity for selenium and avoid volatilization losses. The method measures selenium concentrations as low as 0.01 mug/g with a relative standard deviation of 8%.     

Solvent extraction-electrothermal atomic-absorption analysis

The review discusses the problems of rational combination of solvent-extraction separation and preconcentration of trace elements with their determination by electrothermal atomic-absorption spectrometry.     

Determination of multielement in optical waveguide and standard reference materials by instrumental neutron activation analysis

Trace amounts of transition elements (Co, Cr, Cu, Fe, Mn and V) and other seven elements in optical waveguide samples were determined by INAA. The contents of impurities in ultra-pure materials are less than those of high-purity materials and of G.R. grade. The increase of contamination of trace transition elements and iridium from furnace or crucible are observed in the production of optical glass fibers. Up to seventeen elements were determined in five NBS biological standard reference materials: Oyster Tissue: SRM-1566, Brewers Yeast: SRM-1569, Spinach: SRM-1570, Orchard Leaves: SRM-1571 and Tuna Fish, and in four Japanese biological standard reference materials: Tea Leaves B&C, Pepperbush and Shark Meat. The analytical results in NBS and Japanese standard reference materials are in good agreement with published values and certified values by NBS.