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Recent spectroscopic work has suggested that only one surface species of sulfate is dominant on hematite. Sulfate is therefore a very suitable anion to test and develop adsorption models for variable charge minerals. We have studied sulfate adsorption on goethite covering a large range of sulfate concentrations, surface coverages, pH values, and electrolyte concentrations. Four different techniques were used to cover the entire range of conditions. For characterization at low sulfate concentrations, below the detection limit of sulfate with ICP-AES, we used proton-sulfate titrations at constant pH. Adsorption isotherms were studied for the intermediate sulfate concentration range. Acid-base titrations in sodium sulfate and electromobility were used for high sulfate concentrations. All the data can be modeled with one adsorbed species if it is assumed that the charge of adsorbed sulfate is spatially distributed in the interface. The charge distribution of sulfate follows directly from modeling the proton-sulfate adsorption stoichiometry since this stoichiometry is independent of the intrinsic affinity constant of sulfate. The charge distribution can be related to the structure of the surface complex by use of the Pauling bond valence concept and is in accordance with the microscopic structure found by spectroscopy. The intrinsic affinity constant follows from the other measurements. Modeling of the proton-ion stoichiometry with the commonly used 2-pK models, where adsorbed ions are treated as point charges, is possible only if at least two surface species for sulfate are used. Copyright 1999 Academic Press.
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PMID:Sulfate Adsorption on Goethite. 1050 84

Inductively coupled plasma atomic emission spectrometry (ICP-AES) was used to study metallic ions in the intestinal mucosa of ICR mice infected with Echinostoma caproni and the mucosa of uninfected control mice. Infected mucosa (n = 9 with about 100 mg wet weight per sample) were examined at 2 weeks p.i. in mice that were infected with about 25 worms per host. Uninfected mucosa (n = 9 with about 100 mg wet weight per sample) were examined in the same time frame as the infected mucosa. Five metals were measured in the mucosa by ICP-AES analysis, as follows: calcium, potassium, magnesium, sodium and zinc. There were no significant differences (Student's t-test, P > 0.05) in the concentrations of calcium, potassium or zinc in infected versus uninfected mucosa. The concentration of sodium was significantly greater (P < 0.05) in the mucosa of infected versus uninfected mucosa, but the situation was reversed in regard to magnesium.
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PMID:Effects of Echinostoma caproni infections on metallic ions in the intestinal mucosa of ICR mice. 1065 9

For selenium speciation analysis, the hyphenation of chromatographic separation with element-specific detection has proved a useful technique. A powerful separation system, which is capable of resolving several biologically and environmentally important selenium compounds in a single column, is greatly needed. However, that has been difficult to achieve. In this paper eight selenium compounds, namely, selenite [Se(IV)], selenate [Se(VI)], selenocystine (SeCys), selenourea (SeUr), selenomethionine (SeMet), selenoethionine (SeEt), selenocystamine (SeCM) and trimethylselenonium ion (TMSe+), were separated by using mixed ion-pair reagents containing 2.5 mM sodium 1-butanesulfonate and 8 mM tetramethylammonium hydroxide as a mobile phase. The separation of these anionic, cationic and neutral organic selenium compounds on a LiChrosorb RP18 reversed-phase column took only 18 min at a flow-rate of 1.0 ml/min with isocratic elution, and baseline separation among the six organic Se compounds was achieved. Inductively coupled plasma mass spectrometry (ICP-MS) was employed as element-specific detection. A comparison of ICP-MS signal intensity obtained with a Barbington-type nebulizer and with an ultrasonic nebulizer (USN) was made. Different signal enhancement factors were observed for the various selenium compounds when a USN was used. The speciation technique was successfully applied to the study on chemical forms of selenium in a selenium nutritional supplement. Selenomethionine was found to be the predominant constituent of selenium in the supplement.
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PMID:Speciation of selenium compounds with ion-pair reversed-phase liquid chromatography using inductively coupled plasma mass spectrometry as element-specific detection. 1076 99

Selenium (Se) is an essential micronutrient for human and animal organisms. Organic selenium complexes and selenium-containing amino acids are considered the most bioavailable. Under appropriate conditions yeasts are capable of accumulating large amounts of trace elements, such as selenium, and incorporating them into organic compounds. It has been found that introduction of water-soluble selenium salt as a component of the culture medium for yeasts produced by conventional batch processing results in a substantial amount of selenium being absorbed by the yeast. Using a culture medium supplemented with 30 microg/mL sodium-selenite added during the exponential growth phase results in selenium-accumulation in the range of 1200-1400 microg/g dried baker's yeast (Saccharomyces cerevisiae) measured by ICP-AES method. In our previous studies it was shown that higher amounts of sodium-selenite in the culture medium have a strong inhibitory effect on the growth of this yeast. As a consequence of variations in cultivation conditions we obtained selenium yeast with different inorganic selenium content. The most important parameters influencing incorporated forms of selenium are pH value and dissolved oxygen level in the culture medium, and depending on these the selenium consumption rate of the yeast. A 0.40-0.50 mg/g h-1 specific selenium consumption rate was found to be appropriate to obtain selenium-enriched bakers' yeast of a high quality. Under suitable conditions the undesirable inorganic selenium content of the yeast could be suppressed to as low as 5-6% at the expense, however, of approximately a 20% decrease in the final biomass.
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PMID:Preparation of selenium yeasts I. Preparation of selenium-enriched Saccharomyces cerevisiae. 1083 33

Macrofungi can accumulate some minerals, including toxic metals if present in the substrate. A periodic monitoring of these elements in mushrooms is recommended when the conditions of cultivation are altered. The aim of this work was to evaluate the mineral content of Pleurotus spp (hiratake and shimeji) and of imported (chilean and italian) dehydrated mushrooms. Fresh fruiting bodies of Pleurotus spp were obtained from cultivators and dehydrated mushrooms were bought in a market. The samples were dried, milled and digested by C1H-NO3H. The content of P, K, S, Ca, Mg, Cu, Fe, Mn, Zn, Na and B were analyzed by ICP-AES and Al, Cd, Cr, Pb, Co, Ni by ICP-OES. The results classify these mushrooms as a source of potassium and copper: Pleurotus spp are also a source of phosphorus (P < 0.05); the chilean mushrooms present high content of iron (P < 0.05). All the evaluated mushrooms were identified as a food without sodium (< 5 mg Na/100 g). So these mushrooms being a source of potassium without Na, answer the needs of hypertension and/or heart diseases patients as a food and/or like a condiment for flavor enhancement. Subsequent studies should include major sampling and the evaluation of the toxic metals, Pb and Cr, employing more accurate methods of analysis, as well as the evaluation of Hg (not analysed in this study), mainly in wild mushrooms, commercialized dehydrated.
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PMID:[Mineral composition of edible mushrooms cultivated in Brazil--Pleurotus spp and other dehydrated species]. 1104 80

A simple and reliable extraction method was developed for quantitative determination of both butyl- and phenyltin compounds in sediments by capillary gas chromatography combined with inductively coupled plasma mass spectrometry (GC-ICP-MS). Both types of organotin compounds were extracted quantitatively from sediment by mechanical shaking into tropolone-toluene and HCl-methanol. After phase separation and pH adjustment, these organotins were ethylated with sodium tetraethylborate. The method was evaluated by analyzing PACS-2 and NIES No. 12 sediment certified reference materials. The dibutyltin (DBT; 1.14 +/- 0.02 micrograms g-1) and tributyltin (TBT; 1.01 +/- 0.04 micrograms g-1) values observed in PACS-2 sediment closely matched the certified values (DBT, 1.09 +/- 0.15; TBT, 0.98 +/- 0.13 microgram g-1 as tin). The monobutyltin (MBT) value was higher (0.62 +/- 0.02 microgram g-1) by more than two fold over the reference value (0.3 microgram g-1 as tin). The concentrations of TBT (0.18 +/- 0.04 microgram g-1) and triphenyltin (TPhT; 0.0099 +/- 0.002 microgram g-1) in the NIES No. 12 sediment were also in good agreement with the certified and reference values of TBT (0.19 +/- 0.03 microgram g-1 as compound) and TPhT (0.008 microgram g-1 as compound), respectively. Recoveries of TBT, tripentyltin (TPeT) and TPhT from spiked sediments were satisfactory (TBT, 102 +/- 3.4%; TPrT, 96 +/- 3.4%; TPhT, 99 +/- 8.5%). The detection limits as tin were in the range 0.23-0.48 ng g-1 for a 0.5 g sample size. It is also noteworthy that clean-up of the extract is not necessary because of the superior selectivity of ICP-MS detection. The present method was successfully applied to marine sediment samples.
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PMID:A quantitative extraction method for the determination of trace amounts of both butyl- and phenyltin compounds in sediments by gas chromatography-inductively coupled plasma mass spectrometry. 1107 May 44

The features of different nebulizer systems (cross-flow-, Meinhard- and GMK-system) in the ICP atomic emission spectrometric analyses of solutions with different contents of different salts were evaluated. As basis for the comparison of the nebulizer systems the recovery rates and noise power spectra were used. Both showed that the GMK-system could be used for the widest diversity of salts (sodium chloride, ammonium sulfate and sodium tetraborate) and concentration range (0-10%, (m/v)) followed by the cross-flow-system and the Meinhard-system in ICP-OES using a 1 kW argon ICP. Of all nebulizer systems the nebulizer according to Meinhard has the lowest performance for the salts investigated. The noise power spectra of all nebulizer systems are dominated by interference noise from the sample introduction system. This noise increases with the salt concentration of the solution and the GMK-system shows the lowest increase, followed by the cross-flow- and Meinhard-system.
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PMID:Noise power spectra and recovery rates obtained with different nebulizer systems in ICP atomic emission spectrometric analyses in the case of different types of salts and salt contents. 1122 May 73

The simultaneous injection of volatile hydride species and hydrogen gas, originating in reagent decomposition, was monitored during the operation of a continuous hydride generation manifold employed for the determination of trace arsenic by HG-ICP-AES. Line and background intensities as well as the FWHM of the hydrogen Hgamma and Hdelta lines were measured, and electron number densities (ne) estimated from Stark broadening of the line profiles. Results were compared with those obtained by conventional pneumatic injection of aqueous solutions. Overlapping with atomic nitrogen lines at 410 nm and 411 nm tends to distort the Hdelta line profile for the hydrogen-seeded plasma, rendering unreliable results. The N I lines seem to be quenched by the presence of water aerosol. More consistent results were obtained with the Hgamma line. When no solutions are pumped through the hydride generation manifold ("dry" plasma), the measured ne value was (1.57 +/- 0.22) x 10(15)cm(-3). Conversely, when the reducing reagent flow was replaced by pure water (corresponding to the injection of water vapor in equilibrium that is swept by the argon carrier gas passing through the phase separator), the electron concentration is 25% higher. In that case the ne value agrees between the experimental error with that obtained for a plasma in which a water aerosol is introduced at a flow rate of 1 mL/min. An enhancement of 52% relative is observed in ne when the system is operated under optimized conditions for arsine generation, employing sodium tetrahydroborate in acidic medium as reducing agent (i.e. hydrogen seeded plasma). It was also observed that the continuum emission near 410 nm for the hydrogen containing plasma correlates with the measured electron number density, suggesting that the background enhancement under hydride generation conditions may respond to the ion-electron recombination mechanism.
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PMID:Evaluation of hydrogen line emission and argon plasma electron concentrations resulting from the gaseous sample injection involved in hydride generation-ICP-atomic emission spectrometric analysis. 1122 63

A method to separate and quantify two inorganic arsenic species As(III) and As(V) and two organic arsenic species, monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA), by HPLC-ICP/MS has been developed. The separation of arsenic species was achieved on the anionic exchange column IonPac AS11 (Dionex) with NaOH as mobile phase. The technique was successfully applied to analyze extracts of two contaminated soils, sampled at a former tannery site (soil 1) and a former paint production site (soil 2). The soils were extracted at pH values similar to the natural environment. Extractions were performed at different pH values with 0.3 M ammonium oxalate (pH = 3), milli-Q water (pH = 5.8), 0.3 M sodium carbonate (pH = 8) and 0.3 M sodium bicarbonate (pH = 11). No organically bound arsenic was found in the extracts. As(V) was the major component. Only up to 0.04% of the total arsenic contained in soil 1 were mobilized. The highest amount of extracted arsenic was found at the highest pH. In the milli-Q water extract of soil 1 As(III) and As(V) were found. High amounts of As(V) were found in the extracts of soil 2. Up to 20% of the total arsenic bound to soil 2 constituents were released. The results show that the mobilization of arsenic depended on the pH value of the extraction solution and the kind of extracted soil. Dramatic consequences have to be expected for pH changes in the environment especially in cases where soils contain high amounts of mobile arsenic.
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PMID:Speciation of As(III), As(V), MMA and DMA in contaminated soil extracts by HPLC-ICP/MS. 1122 33

In the field of industrial hygiene, besides the necessity of monitoring phosphine with direct reading apparatus to prevent accidents, there is a need for a method of sampling and analysing phosphine to control workers' exposure. The use of filters impregnated with silver nitrate to collect arsine, phosphine and stibine in workplace air has been described in the literature. Having previously chosen this type of filter to collect arsine, we studied its characteristics for phosphine capture. A filter impregnated with sodium carbonate was used both as a prefilter to collect the particles and to trap arsenic trioxide. After dissolving the silver compounds in nitric acid, ICP emission spectrometry was used to carry out the analysis. This article describes the comparative sampling we performed in a microelectronic laboratory and in a fumigation chamber (130 samples) to determine the concentration of AgNO3 impregnation solution to be used, the detection limit of the method and the retention capacity of the impregnated filters. Interference with other gases reacting with silver nitrate was studied and the storage time for sampled filters and analysis solutions was checked. The detection limit of the adopted method is better than 1 microg per filter, and the retention capacity exceeds 300 microg per filter. The problem of how to sample phosphine when H2S, NH3, or HCl is present has been solved, but the problem of sampling phosphine in atmospheres where acetylene evolves remains. Sampled filters and filter solutions are stable for more than three months at ambient temperature.
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PMID:Phosphine sampling and analysis using silver nitrate impregnated filters. 1125 53


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