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Leaching and runoff of arsenic (As) from the contaminated soil of an old wood impregnation plant, and fate in a recipient freshwater ecosystem, was studied in soil-water-sediment mesocosms in laboratory (0.9 m3; total water volume 200 l). During the 4-month experiment total leaching and discharge of As from regularly irrigated soil was approximately 40 mg, i.e. approximately 0.6% of total initial As content in the soil. Of the total As load, 7.5% remained in the water; 44% settled down to the shallow (water depth 5-30 cm) sediment zone; and 48.5% to the deeper (water depth 80 cm) sediment zone. The different arsenic species; arsenite [As(III)], arsenate [As(V)], monomethylarsonic acid (MMAA) and dimethylarsinic acid (DMAA), were analysed from irrigation and discharge water; mesocosm pool water; and sediment pore water using ion chromatography-inductively coupled plasma-mass spectrometry (IC-ICP-MS). The total amounts of arsenic in soil, water and sediment were determined by ICP-MS. Arsenic was leached out from the soil as As(V). In mesocosm water As(V) was the predominant dissolved species, but DMAA and particle bound species, were also detected. In shallow sediment, As(V) was the most abundant species together with some DMAA, whereas in deep sediment As(III) was the dominant species.
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PMID:Leaching, runoff and speciation of arsenic in a laboratory mesocosm. 1100 86

Aluminium speciation was studied in forest soil extracts by size exclusion chromatography (SE) with UV and inductively coupled plasma-atomic emission spectrometric (ICP-AES) detection and cation exchange fast protein liquid chromatography (FPLC) with ETAAS detection. Size exclusion chromatography was performed on a Superdex HR75 10/30 column. Isocratic clution with 0.15 mol dm(-3) NaCl in TRIS-HCl buffer (pH = 5.5) was applied over 100 min at a flow rate of 0.35 cm(3) min(-1). The chromatographic run was followed at 278 nm and separated Al species also determined 'off line' in 0.875 cm3 fractions by ICP-AES. The analytical procedure enabled speciation of high molecular weight Al complexes. Cation exchange FPLC was performed on a Mono S HR 5/5 column. Aqueous 8 mol dm(-3) NH4NO3 linear gradient elution was applied over 10 min at a flow rate of 1 cm3 min(-1). Separated Al species were collected in 0.5 cm3 fractions and Al determined 'off line' by ETAAS. The analytical procedure enabled speciation of some positively charged monomeric Al species. Negatively charged species were eluted with the solvent front. The combination of the two analytical techniques was successfully employed in speciation of Al in forest soil extracts. Water was used as an extracting solution. It was found experimentally that 80-95% of Al in aqueous extracts of forest soils exists in monomeric Al forms. Water soluble Al (30-40%) is bound to high molecular weight complexes with humic substances. The remaining monomeric Al in the low molecular weight fraction exists as AIF2+, Al-oxalate and Al-citrate species.
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PMID:Speciation of aluminium in forest soil extracts by size exclusion chromatography with UV and ICP-AES detection and cation exchange fast protein liquid chromatography with ETAAS detection. 1100 89

The purpose of this study was to examine whether oral exposure to aluminum (Al) can affect the human immune system. Eighteen healthy volunteers (mean age 42, 28-57 yr) were divided into a test group (9 females, 4 males) and a referent group (3 females, 2 males). Over 6 weeks, the test subjects ingested 10 ml of antacid (aluminum hydroxide, 59 mg Al/ml) three times daily. Aluminum was analyzed in urine before and during the exposure period (ICP-MS). Blood samples were used for analysis of lymphocyte subpopulations, mitogen-induced lymphocyte proliferation and in vitro production and circulating plasma concentrations of immunoglobulin (Ig) A, IgG, IgM, interleukin (IL) -2 and IL-4. Urinary Al concentration in the test subjects was approximately 10- to 20-fold higher than in the referent group during exposure. This indicates that ingestion of an Al-containing antacid is associated with an Al absorption far above that originating from food and drinking water. In both referents and test subjects the lymphocyte subpopulations, lymphocyte proliferation and the in vitro Ig and IL production showed similar, time-dependent changes before as well as during the exposure period. No major differences were seen between the referent and test groups regarding the immune parameters, except for a slightly smaller CD8+CD45R0+ population (primed cytotoxic T-cells), in the exposed individuals as compared to the referents. The results also show that subjects on antacid therapy may constitute a suitable population for studying biological effects of high-dose oral exposure to Al.
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PMID:Influence of aluminium on the immune system--an experimental study on volunteers. 1101 99

The selenium supply in almost all European countries, including Austria and Germany, is below the recommended daily intake. In these countries, selenium fortification of foods and the use of selenium supplements are quite popular to compensate for low Se intake from diets. In general, wheat (Triticum aestivum) is known to be a good source for bioavailable selenium, and many studies have been performed to enrich selenium in wheat by selenium fertilization of the soil. In the present work, the process of sprouting was investigated as an alternative to enrich selenium in wheat. Sprouting was chosen because it additionally improves the nutritional value of seeds, for example, by a higher vitamin content, a better quality of protein, and some other parameters. Wheat, alfalfa (Medicago sativa), and sunflower (Helianthus annuus) seeds were germinated for 5 and 7 days in solutions containing selenate. The selenium sensitivity of the sprouts was tested by measuring visible germination levels and seedling development. Uptake rates were studied by determination of total selenium using inductively coupled plasma mass spectrometry (ICP-MS). Metabolism of the absorbed selenium was analyzed by determination of selenium species in extracts of the sprouts using anion exchange HPLC coupled to ICP-MS. It was shown that sunflower sprouts were the most resistant and had the highest uptake rates (up to 900 mg/kg), but almost 100% of the selenium was extracted with water and found to be nonmetabolized selenate. Wheat and alfalfa were less resistant and enriched selenium up to concentrations of 100 and 150 mg of Se/kg of dry mass, respectively. The metabolism of the selenate was inversely related to the total uptake rates. At low Se enrichment (approximately 1-2 mg of Se/kg), <20% of the total selenium content within the sprouts remained as inorganic selenium, indicating a high metabolism rate. With increasing uptake the amount of selenate increased to approximately 40-50%. However, with the method used it is possible to produce sprouts containing certain amounts of selenium, which might provide substantial proportions of bioavailable selenium. In combination with the generally high nutritional value of sprouts, they might serve for production of improved cereal-based diets.
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PMID:Selenium-enriched sprouts. A raw material for fortified cereal-based diets. 1108 86

Controlling of elements content in drugs is indispensable for drug quality evaluation. Zinc was selected for study because zinc contents in drugs span a wide range. Numerous multi-mineral preparations used and nutritional supplements to make up for the microelemental deficiencies in humans and animals, contain less than 0.001% zinc, i.e., trace amounts of zinc. On the other hand, external application drugs such as ointments and suppositories usually contain more than 0.1% of zinc. Zinc was determined out in Technilab's "Hemacort HC" ointments and suppositories, in Nattermann's "Dolovit Multimineral" tablets, and in Richter Pharma's "Minerasol" parenteral veterinary solution. These preparations were selected for investigation not only in view of differentiated zinc contents, but also because of the various drug forms and various procedures involved in sample preparation procedures. The tablets were dissolved with the aid of microwave energy, the ointment and suppositories were extracted, and the parenteral solution was diluted with water or with and aqueous 1% nitric acid. Atomic absorption spectrometry with graphite-tube (AAS), inductively coupled plasma mass spectrometry (ICP-MS), adsorptive stripping voltammetry (AdSV), square-wave voltammetry (SWV), and differential pulse polarography (DPP) were used for the determinations. Zinc was determined within concentration ranges of 20-40 ppb, 0.5-20 ppb, and 10-50 ppb by AAS, ICP-MS and AdSV, respectively. In the AAS and ICP-MS, zinc recoveries were contained within the limits of 101.8-114.2% and 111.0-114.2% respectively. The errors of determination (RSD) were 3.37-5.74% in AAS, 0.28-4.47% in ICP-MS and 0.19-2.50% in the electrochemical method.
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PMID:The AAS, ICP-MS and electrochemical determinations of zinc in selected pharmaceutical preparations. 1112 13

The choice of the analytical method for the determination of actinide isotopes in leachate solutions has to be made considering several parameters: detection limit for each isotope, sample preparation procedure in terms of duration and complexity, counting time and interferences. A leachate solution obtained by keeping a pellet of UO2 doped with 238Pu in contact with distilled water was investigated for the content of U and Pu isotopes by radiometric methods (alpha-, gamma-spectrometry and liquid scintillation counting). The results of the radiometric methods were compared with those obtained from the analysis performed by inductively coupled plasma mass spectrometry on-line to a system for chromatographic separation (IC-ICP-MS). The comparison confirmed that IC-ICP-MS is a powerful method for the detection of long-lived radionuclides. The radiometric methods have a detection limit two orders of magnitude lower than IC-ICP-MS in the case of short-lived radioisotopes mostly due to the low background in the detector. On the other hand, the sample preparation and the analysis duration are more time-consuming compared to IC-ICP-MS; moreover, not all isotopes can be determined by using only one radiometric technique.
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PMID:Ion chromatography inductively coupled plasma mass spectrometry (IC-ICP-MS) and radiometric techniques for the determination of actinides in aqueous leachate solutions from uranium oxide. 1122 Aug 37

An on-line zinc preconcentration and determination system implemented with inductively coupled plasma atomic emission spectrometry (ICP-AES) associated with flow injection (FI) was studied. The zinc was retained as zinc-2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Zn-(5-Br-PADAP)) complex at pH 9.2. The zinc complex was removed from the knotted reactor (KR) with 30% v/v nitric acid. An enrichment factor of 42 was obtained for the KR system with respect to ICP-AES using pneumatic nebulization. The detection limit for the preconcentration of 10 mL of aqueous solution was 0.09 microg/L. The precision for 10 replicate determinations at the 5 microg/L Zn level was 2.3% relative standard deviation (RSD), calculated with the peak heights obtained. The calibration graph using the preconcentration system for zinc was linear with a correlation coefficient of 0.9997 at levels near the detection limits up to at least 100 microg/L. The method was succesfully applied to the determination of zinc in river water samples.
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PMID:On-line complexation of zinc with 5-Br-PADAP and preconcentration using a knotted reactor for inductively coupled plasma atomic emission spectrometric determination in river water samples. 1122 29

For the major component analysis of Mo-Si (-B) alloys by ICP-AES, an appropriate dissolution method is necessary. The general procedure using a HNO3-HF mixture cannot be applied for Mo-Si (-B) alloys due to Si volatilization followed by violent reaction and due to MoO2 precipitation in the preparation of a Mo standard solution from metallic Mo. Good results were obtained with a mixture of 10 mL H2SO4, 1 mL HNO3, 2 mL HF and 12 mL H2O for Mo-Si (-B) alloys. The samples were completely dissolved at room temperature without any losses. A sequential correction method is also suggested to correct several errors in ICP-AES analysis such as fluctuation in the emission intensities, spectral interferences, non-spectral interferences and blank values.
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PMID:Dissolution of molybdenum-silicon (-boron) alloys using a mixture of sulfuric, nitric and hydrofluoric acids and a sequential correction method for ICP-AES analysis. 1122 63

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

The chemical analysis with inductively coupled plasma-mass spectrometry (ICP-MS) can help to examine the purity of ultra pure water (UPW) down to 10 part per trillion (ng/L) and lower. For a proper determination of a high number of samples per week the analysis must be divided into two parts: the routine analysis and the reference water analysis. The routine analysis is done by direct measurement of the ultra pure water samples. Applying a standard addition method under particular clean conditions, the reference water analysis leads to the definition of the accurate zero. A quick evaluation scheme is also presented for the reference water analysis. The method is tested for its fitness for application by examining LOD (for relevant element < 2 ng/L), reproducibility and linearity of calibration. The ICP-MS was optimized according to the methodology of G. Taguchi to improve reproducibility and LOD.
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PMID:Routine analysis of ultra pure water by ICP-MS in the low- and sub-ng/L level. 1122 18


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