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The selenium determination in biological materials by the classical fluorometric method (FM) is time-consuming and also hazardous, as it requires the destruction of the organic matrix samples with hot HNO3/HClO4 mixtures prior to analysis. Accordingly, commercial analytical laboratories are increasingly using faster instrumental methods; for sample digestion, avoid using HClO4. Because of these procedural changes, the results obtained by commercial laboratories may be unreliable, especially for samples containing Se in organic forms. One such "difficult" substrate is Se yeast, which contains most of its Se as selenomethionine. To establish which methods for Se analysis and sample digestion are applicable, samples of Se yeast and of selenomethionine standards were sent to laboratories employing either flame atomic absorption spectrometry (FAAS), inductively coupled plasma-mass spectrometry (ICP-MS), or hydride generation atomic absorption spectrometry (HGAAS). The results were compared with those obtained by FM and non-destructive instrumental neutron activation analysis (INAA). ICP-MS, after microwave digestion of sample with HNO3/H2O2, produced results within 5% of the expected values, as did those obtained by FM and INAA. With FAAS, acceptable results were obtained after digestion with HNO3/HCl. With HGAAS, sample digestion with HNO3/H2O2 produced values that were systematically elevated by about 10% and exhibited standard deviations of > or = 10%. Thus, current methods of sample digestion are applicable for Se yeast analysis by ICP-MS and FAAS, but not by HGAAS.
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PMID:Evaluation of methods for total selenium determination in yeast. 1229 28

In the event of a nuclear incident it is essential that analytical information on the distribution and level of contamination is available. An ICP-MS method is described which can provide data on plutonium contamination in food within 3 h of sample receipt without compromising detection limits or accuracy relative to traditional counting methods. The method can also provide simultaneous determinations of americium and neptunium. Samples were prepared by HNO3 closed-vessel microwave digestion, evaporated to dryness and diluted into a mobile phase comprising 1.5 M HNO3 and 0.1 mM 2,6-pyridinedicarboxylic acid. A commercially available polystyrene-divinylbenzene ion chromatography column provides on-line separation of 239Pu and 238U reducing the impact of the 238U1H interference. Oxidation of the sample using H2O2 ensures all Pu is in the Pu(+4) state. The oxidation also displaces Np away from the solvent front by changing the oxidation state from Np(+3) to Np(+4) and produces the insoluble Am(+4) ion. Simultaneous Pu, Am and Np analyses therefore require omission of the oxidation stage and some loss of Pu data quality. Analyses were performed using a magnetic sector ICP-MS (Finnigan MAT Element). The sample is introduced to the plasma via an ultrasonic nebuliser-desolvation unit (Cetac USN 6000AT+). This combination achieves an instrumental sensitivity of 238U > 2 x 10(7) cps/ppb and removes hydrogen from the sample gas, which also inhibits the formation of 238U1H. The net effect of the improved sample introduction conditions is to achieve detection levels for Pu of 0.020 pg g(-1) (4.6 x 10(-2) Bq kg(-1)) which is significantly below 1/10th of the most stringent EU (European Union) legislation, currently 0.436 pg g(-1) (1 Bq kg(-1)) set for baby food. The new method was evaluated with a range of biological samples ranging from cabbage to milk and meat. Recovery of Pu agrees with published values (100% +/- 20%).
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PMID:A rapid and accurate method for the determination of plutonium in food using magnetic sector ICP-MS with an ultra-sonic nebuliser and ion chromatography. 1261 74

The aim of this in vitro study was to evaluate mineral content of root canal dentin after treatment with several endodontic irrigation solutions. Sixty mandibular anterior teeth extracted for periodontal reasons used. The crowns of the teeth were removed at the cemento-enamel junction. Pulp tissues were removed and the teeth were randomly divided into six groups including 10 teeth each. Root canals were enlarged with gates-glidden burs (# 1, 2, and 3). The groups were treated as follows: group 1, 0.2% chlorhexidine gluconate for 15 min; group 2, 3% H2O2 for 15 min; group 3, 17% EDTA for 15 min; group 4, 5.25% NaOCl for 15 min; group 5, 2.5% NaOCl for 15 min; and group 6, distilled water (control). Dentin chips were obtained using gates-glidden burs (# 4, 5, and 6). The levels of five elements calcium, phosphorus, magnesium, potassium, and sulfur in each specimens were analyzed using ICP-AES (Inductively Coupled Plasma Atomic Emission Spectrometry) technique. Changes in the levels of the chemical elements were recorded. The results were then statistically analyzed by one-way ANOVA and Tukey tests. There was a significant decrease in the calcium and phosphorus levels after treatment with all irrigation solutions except for 5.25% NaOCl when compared with the control group (p < 0.05). The K, Mg, and S level changes were not statistically significant (p > 0.05). It has been concluded that endodontic irrigation solutions have an effect on mineral contents of root dentin.
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PMID:Effects of endodontic irrigation solutions on mineral content of root canal dentin using ICP-AES technique. 1573 66

A new method has been developed for simultaneous derermination of 16 elements in decoction solution of Chinese herbal medicine by ICP-AES after pretreatrment the solution with HNO3-H2O2. This method has low and stable blank value. The detection limits of 0.1-5ng/ml for most elements and recoveries of 85-103% were obtained. This method has been applied to the determination of 16 elements in decoction solution of chinese herbal medicine with satisfactory reswls.
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PMID:[Simultaneous determination of 16 elements in decoction solution of Chinese herbal medicine by ICP-AES]. 1581 Mar 69

The determination of lead in tinplate by ICP-AES was presented in this paper. The tinplate samples were pretreated with NaOH-H2O2 for dissolving tin and lead,and the spectral interferences from iron could thus be avoided. The lead content in the sample was determined in the range of 0.14-0.38 microg/cm2. The recovery and the relative standard deviation (RSD) were in the ranges of 96.1%-103.2% and 2.6%-3.8%, respectively. The method was simple,rapid and efficient.
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PMID:[Determination of lead in tinplate by ICP-AES]. 1581 66

A method for the determination of iodine in iodo-calcium pieces by ICP-AES was studied. I- was turned to I2 by HClO4 and H2O2. The detection limit of iodine is 1 ng/mL. The sample was dissolved with water and was directly determined without seperating the precipitate in the bottom of volume flask. It was found that the precipitate attracted with I2 and the quantity of attracting would increase with delay time.
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PMID:[Study on the determination of iodine by ICP-AES]. 1581 61

The determination of metal elements in Chinese medicine wild jujube seed decoction was studied by ICP-AES after HNO3-H2O2 digestion. The average recoveries of the method for Ca, Cr, Al, Fe, K, Mg, Mn and Zn in wild jujube seed decoction were found to be 95.5%-106.8%, while RSD (n=5) was found to be 1.7%-3.9% for these metal elements. The method was applied to the analysis of some practical samples and the results obtained were satisfactory.
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PMID:[Study on the determination of metal elements in wild jujube seed decoction by ICP-AES]. 1582 55

Three treatment media, used for the removal of arsenic from drinking water, were sequentially extracted using 10 mM MgCl2(pH 8), 10 mM NaH2PO4(pH 7) followed by 10 mM (NH4)2C2O4(pH 3). The media were extracted using an on-line automated continuous extraction system which allowed the arsenic in each of the extraction fluids to be speciated on-line using IC-ICP-MS. The 10 mM MgCl2 preferentially extracted As(III) from each of the media. The percentage of the arsenic extracted by the MgCl2, relative to a HNO3/H2O2 digestion of the media, ranged from 0.1-2.3% for the three solids. The next sequential extraction fluid, 10 mM NaH2PO4, extracted some of the residual As(III) remaining on each of the media but the predominant species extracted was As(V). The 10 mM NaH2PO4 extracted 15.3 to 42.8% of the total arsenic relative to a total digested concentration for each of the media. The As(III) and As(V) stability studies conducted in these two extraction fluids indicated that conversion between As(III) and As(V) was not significant for the short extraction fluid sample contact time associated with the on-line continuous flow extraction cell. Finally, the 10 mM (NH4)2C2O4 extraction fluid was utilized in an off-line analysis mode because the Fe and As concentrations extracted from the media were not compatible with direct ICP-MS detection. The (NH4)2C2O4 extracted 2.9-29% As(III) for all three media and caused an oxidation of As(III) to As(V) during the extraction period for one of the three media. The sum of the arsenic from each of the three extraction fluids represented 92%, 44% and 53% of the available total arsenic for the three media, respectively. The speciation results for each media were obtained by adding all the speciation results from all three extraction fluids together and the resulting distribution of As(III)/As(V) compared well with the speciation results obtained via XANES.
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PMID:Investigation of arsenic speciation on drinking water treatment media utilizing automated sequential continuous flow extraction with IC-ICP-MS detection. 1625 57

APM was collected and trace elements existing in the particles were monitored since May 1995 in this study. APM sample was collected separately by size (d < 2 microm, 2-11 microm and >11 microm) on the roof of the university building (45 m above ground) in the campus of Faculty of Science and Engineering, Chuo University, Tokyo, Japan, using an Anderson low volume air sampler. The collected sample was digested by HNO3, H2O2 and HF using a microwave oven, and major elements (Na, Mg, Al, K, Ca and Fe) were measured by ICP-AES, and trace elements (Li, Be, Ti, V, Cr, Mn, Co, Ni, Cu, Zn, As, Se, Mo, Cd, Sb, Ba and Pb) were measured by ICP-MS. It was observed that the APM concentration was higher between the winter and the spring, compared to during the summer. The enrichment factor was calculated for each element in each set of APM (d < 2 microm, 2-11 microm and >11 microm). Seasonal trends of enrichment factors were examined, and the elements were classified into 3 groups according to the common seasonal behavior. It is likely that the elements in the same group have common origins. Toxic pollutant elements (Sb, Se, Cd, Pb and As) were found in small particles with d of <2 microm in concentrated levels. Antimony (Sb) had the highest enrichment factor, and the results suggested that Sb level in APM was extremely high. The origins of Sb were sought, and wastes from plastic incineration and brake pad wears of automobiles were suspected. Each set of APM (d < 2 microm, 2-11 microm and >11 microm) was classified by the shape, and the shape-dependent constituents of a single APM particle were quantitatively measured by SEM-EDX. High concentration of Sb was found in APM <2 microm and square particles. Particles less than 2 microm and square shaped particles were major particles produced by actual car braking experiments. From these experimental results it was concluded that the source of Sb in squared APM <2 microm is considered to be from brake pad wear.
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PMID:Concentrations, enrichment and predominant sources of Sb and other trace elements in size classified airborne particulate matter collected in Tokyo from 1995 to 2004. 1630 66

A method is presented for the simultaneous determination of Cr(III) and Cr(VI) in yeast using species-specific double-spike isotope dilution (SSDSID) with anion-exchange liquid chromatography (LC) separation and sector field inductively coupled plasma mass spectrometric (SF-ICP-MS) detection. Total Cr is quantitated using ID SF-ICP-MS. Samples were digested on a hot plate at 95+/-2 degrees C for 6 h in an alkaline solution of 0.5 M NaOH and 0.28 M Na2CO3 for the determination of Cr(III) and Cr(VI), whereas microwave-assisted decomposition with HNO3 and H2O2 was used for the determination of total Cr. Concentrations of 2,014+/-16, 1,952+/-103 and 76+/-48 mg kg-1 (one standard deviation, n=4, 3, 3), respectively were obtained for total Cr, Cr(III) and Cr(VI) in the yeast sample. Significant oxidation of Cr(III) to Cr(VI) (24.2+/-7.6% Cr(III) oxidized, n=3) and reduction of Cr(VI) to Cr(III) (37.6+/-6.5% Cr(VI) reduced, n=3) occurred during alkaline extraction and subsequent chromatographic separation at pH 7. Despite this significant bidirectional redox transformation, quantitative recoveries for both Cr(III) and Cr(VI) were achieved using the SSDSID method. In addition, mass balance between total Cr and the sum of Cr(III) and Cr(VI) concentrations was achieved. Method detection limits of 0.3, 2 and 30 mg kg-1 were obtained for total Cr, Cr(VI) and Cr(III), respectively, based on a 0.2-g sub-sample.
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PMID:Application of double-spike isotope dilution for the accurate determination of Cr(III), Cr(VI) and total Cr in yeast. 1695 11


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