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The argon supported inductively coupled plasma--atomic emission spectrometer (ICP--AES) is found to be an attractive analytical tool for the simultaneous multi-element determination of major, minor and trace elements in human liver and kidney specimens. The sample is digested with a mixture of HNO3--HClO4. The damp residue is taken up in HCl, aspirated into the plasma and the resulting emission signals are detected by a polychromator where the analytical lines of the 20 elements determined are included as fixed channels. The method is rapid, precise, sensitive, less subject to interferences and cost-effective. A total of 20 elements in about 40 autopsy samples of human kidney (cortex and medulla) and liver taken from Canadian adults living in the Great Lakes Region of Ontario were determined using the wet digestion-ICP--AES technique.
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PMID:Simultaneous determination of 20 elements in some human kidney and liver autopsy samples by inductively-coupled plasma atomic emission spectrometry. 711 97

The purpose of the study was utilization of emission atomic absorption spectrometry with excitation in induction-coupled plasma, and molecular spectrometry for determination of lead in milk and dairy products after condensation in ammonia atmosphere. Two methods were proposed for lead condensation on lanthanum carrier--in form of hydroxide or sulphide. By coprecipitation of lead on lanthanum in ammonia atmosphere lead separated and selectively condensed. Other metals (Zn, Cd, Cu) coexistent in food products remained as amino complexes in the solution. The sediment remaining after lead condensation was dissolved in 2 mol/dm3 hydrochloric acid solution. The selected conditions of lead separation and condensation make possible determination of the metal in the concentrations from 0.01 mcg/ml to 0.2 mcg/ml by the ICP-ARS and dithizone methods. The method of condensation and determination was used for lead determination in milk and dairy products in concentrations below 1.5 x 10(-5)%. The studied food products were mineralized with concentrated HNO3, H2SO4 and perhydrol. This mineralization method makes it possible to determine in one mineralisate directly copper and zinc by ICP-ARS and dithizone methods, and lead after condensation. The obtained results were precise and reproducible.
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PMID:[Determination of lead (II) in food using the ICP-AES method after condensation on the lanthanum carrier]. 748 2

The method of the atomic emission spectrometry with an excitation in the inductively coupled plasma ICP-AES has been applied to the simultaneous analysis of the elements: Al, Cd, Cr, Cu, Fe, Li, Mg, Mn, Ni, P, Pb, S, Sr and V in the tobacco leaves samples CTA-OTL-1. The spectrometric analyses have been carried out on the emission spectrometer Spectroflame ICP M. About 300 mg of the sample and 1 cm3 of the concentrated HNO3 acid have been sealed in the quartz tube and mineralized by the pressure method. Since the ICP-AES technique is the most suitable to the direct analysis of the solutions, the main problem to solve was a mineralization of the sample. An application of the HNO3 acid alone did not give satisfactory results--unsolved residue remained. As a consequence the results for Mg, Ni, Pb were too low, whereas for the Al-nearly twice lower than the respective values given in the sample reference data. It has been observed that an addition of the conc. HF acid helps to dissolve the residue and, consequently, the optimalization of the mineralization process in the presence of the HNO3-HF mixture has been carried out. The results show that the appropriate amount of the HF acid to be added is 0.25 cm3. The other methods of mineralization using various mixtures of acids did not give good results. Only HNO3-HF mixture used in appropriate proportions give results in agreement with provided sample characteristics.(ABSTRACT TRUNCATED AT 250 WORDS)
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PMID:[Use of the ICP-AES method for multi-element analysis of tobacco leaves]. 748 4

A microwave digestion procedure, followed by Inductively Coupled Argon Plasma Spectroscopy, is described for the determination of boron (B) in human plasma. The National Institute of Standards and Technology (NIST) currently does not certify the concentration of B in any substance. The NIST citrus leaves 1572 (CL) Standard Reference Material (SRM) and wheat flour 1567a (WF) were chosen to determine the efficacy of digestion. CL and WF values compare favorably to those obtained from an open-vessel, wet digestion followed by ICP, and by neutron activation and mass spectrometric measurements. Plasma samples were oxidized by doubled-distilled ultrapure HNO3 in 120 mL PFA Teflon vessels. An MDS-81D microwave digestion procedure allows for rapid and relatively precise determination of B in human plasma, while limiting handling hazards and sources of contamination.
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PMID:Microwave digestion preparation and ICP determination of boron in human plasma. 768 26

A speciation method for vanadium(IV) and vanadium(V) is presented that uses a combination of HPLC and ICP-AES. In this method, 1 mM HNO3 solution and 100 mM HNO3 solution were applied in sequence as eluent. A vanadium(IV) and vanadium(V) mixture was injected into a HPLC anion-exchange column; and vanadium(IV) cation was then eluted by 1 mM HNO3, while vanadium(V) oxoacid anion was trapped on the column. After this separation, vanadium(V) was eluted as a cation from the column by 100 mM HNO3. Vanadium was detected by ICP-AES. In this separation, about 15% of vanadium(V) interfered with vanadium(IV), and trace vanadium(IV) interfered with vanadium(V). This interference could be estimated by simple calculation based on standard observations, and the speciation of vanadium(IV) and vanadium(V) was performed. The lower determination limit was 1 microgram/mL, which is insufficient to speciate vanadium sampled by conventional sampling methods in a working environment. However, impurity of the other valent vanadium species in a vanadium(V) reagent can be determined by the present method, which should be valuable in precisely assessing the toxicities of vanadium species.
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PMID:Speciation of vanadium(IV) and vanadium(V) using ion-exchange chromatography and ICP-AES. 769 4

The method of the emission atomic spectrometry with an excitation in the inductively coupled plasma (ICP-AES) has wide range of applications due to the possibility of the simultaneous determination of several elements in various materials. This technique allows to carry out a multi-element analysis at relatively low consumption of the sample which is an additional advantage of the method. In this paper we report an application of the ICP-AES method for a direct determination of the element Al, Cu, Fe, Mn, Sn and Zn in the samples of milk. Several types of pressure mineralization (teflon bomb, sealed quartz tubes) as well as the pressureless technique with the use of the H2SO4, HNO3 and H2O2 agents have been studied. The determinations have been carried out with the use of the Spectroflame M sequential spectrometer with the excitation in ICP plasma made by Spectro Analytical Instruments at the Frequency of 27.12 MHz. The milk samples after mineralization have been diluted to the same volume and directly introduced into the ICP plasma with the help of the pneumatic nebulizer of Meinhard type. On the basis of the obtained results it has been concluded that with an application of the aforementioned mineralization method the average values for the determination of the particular elements are comparable. Generally the most "repeatable" results have been obtained for the sample mineralized in the quartz tubes.(ABSTRACT TRUNCATED AT 250 WORDS)
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PMID:[Simultaneous determination of metals in milk by the ICP-AES technique]. 779 17

ICP-MS is a powerful analytical technique for the determination of trace and ultra-trace elements in biological materials. Results are given of the analysis of human serum and of several biological reference materials (bovine liver, milk powder, wheat flour and pig kidney). Because concentrations of many trace metals of interest in these materials are low, dilution should be kept as limited as possible, although concentrations of certain concomitant elements (e.g. Na, K) can be high enough to cause significant suppression or enhancement of the ion signal. The result is that the dissolution procedure becomes a critical step in the analysis. Microwave digestion, wet digestion with several acids (HNO3, HClO4, HF) and simple dilution are compared with each other. In addition, three possible approaches to overcome these problems are discussed, namely the internal standardization method, the standard addition method and the isotope dilution method. Furthermore, ICP-MS is also more susceptible than initially expected to isobaric interferences arising from the plasma, the acids used in the sample preparation or the sample itself. These interferences are generally less important above a mass number of 80. Nevertheless, several researchers have investigated the possibility of removing the trace metals from the matrix or of using correction formulae based on the isotopic abundances of the elements. Some of these are evaluated. The need for identifying and quantifying chemical species, not just the elements, is well recognized. One of the reasons why elemental determination may not suffice is that different species of the same element may have a different chemical and toxicological behaviour. Arsenic (As(III), As(V)) and mercury (organomercury) are typical examples.(ABSTRACT TRUNCATED AT 250 WORDS)
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PMID:A review of the capabilities of ICP-MS for trace element analysis in body fluids and tissues. 815 84

Various canned foods were digested sequentially with HNO3 and HCl, diluted to 100 mL, and filtered, and then tin was determined by inductively coupled plasma atomic emission spectrometry (ICP/AES). Samples of canned Satsuma mandarin, peach, apricot, pineapple, apple juice, mushroom, asparagus, evaporated milk, short-necked clam, spinach, whole tomato, meat, and salmon were evaluated. Sample preparations did not require time-consuming dilutions, because ICP/AES has wide dynamic range. The standard addition method was used to determine tin concentration. Accuracy of the method was tested by analyzing analytical standards containing tin at 2 levels (50 and 250 micrograms/g). The amounts of tin found for the 50 and 250 micrograms/g levels were 50.5 and 256 micrograms/g, respectively, and the repeatability coefficients of variation were 4.0 and 3.8%, respectively. Recovery of tin from 13 canned foods spiked at 2 levels (50 and 250 micrograms/g) ranged from 93.9 to 109.4%, with a mean of 99.2%. The quantitation limit for tin standard solution was about 0.5 microgram/g.
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PMID:Inductively coupled plasma atomic emission spectrometric determination of tin in canned food. 828 77

Rare earth elements (REEs) in a blood serum reference sample, which is a freeze-dried sample issued from the National Institute for Environmental Studies, Japan, have been determined by inductively coupled plasma mass spectrometry (ICP-MS) after sample digestion and concentration pretreatment. The freeze-dried serum sample (ca. 0.8 g), which corresponded to 10 ml of original blood serum, was digested with HNO3 with heating on a hot plate. The digested sample was then diluted with 100 ml of 0.1 M HNO3, and REEs in the diluted solution were adsorbed on chelating resin (Chelex 100). The resin was then filtered with a glass filter. Finally, REEs on the resin were dissolved with 10 ml of 2 M HNO3 aqueous solution, and the sample solution was analyzed by ICP-MS. The concentrations of all the REEs were successfully determined by the present method. The recovery values of REEs were in the range of 70-80%, and the relative standard deviation of the recovery values in repeated experiments (n = 3) was less than 5% for all REEs. In addition, 20 other elements were also determined by ICP-MS and ICP-AES.
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PMID:Determination of rare earth elements in blood serum reference sample by chelating resin preconcentration and inductively coupled plasma mass spectrometry. 884 90

The concentrations of Cd, Co, Cu, Mn, Ni, Pb, and Zn in natural and sea waters are too low to be directly determined with by flame atomic absorption spectrometry (FAAS) or graphite furnace atomic absorption spectrometry (GFAAS). Specific sample preparations are requested that make possible the determination of these analytes by preconcentration or extraction. These techniques are affected by severe problems of sample contamination. In this work Cd, Co, Cu, Mn, Ni, Pb, and Zn were determined by inductively coupled plasma mass spectroscopy (ICP-MS) or by atomic absorption spectrometry, in fresh and seawater samples, after on-line preconcentration and following solvent elution with a flow injection system. Bonded silica with octadecyl functional group C18, packed in a microcolumn of 100-μl capacity, was used to collect diethyldithiocarbamate complexes of the heavy metals in aqueous solutions. The metals are complexed with a chelating agent, adsorbed on the C18 column, and eluted with methanol directly in the flow injection system. The methanolic stream can be addressed to FAAS for direct determination of Cu, Ni, and Zn, or collected in a vial for successive analysis by GFAAS. The eluted samples can be also dried in a vacuum container and restored to a little volume with concentrated HNO3 and Milli-Q water for analysis by ICP-MS or GFAAS.
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PMID:Determination of Cd, Co, Cu, Mn, Ni, Pb, and Zn by Inductively Coupled Plasma Mass Spectroscopy or Flame Atomic Absorption Spectrometry after On-line Preconcentration and Solvent Extraction by Flow Injection System 897 55


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