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Acetic acid was used to enhance the efficiency of chemical vapor generation (CVG) of copper. The volatile product was formed at room temperature following merging of the sample solution with a flowing stream of 0.1% NaBH4; ICP-OES was used for detection. A precision of 1.6% RSD (n=11, 0.2 mg/L) was realized at sampling frequencies of about 90/h. A detection limit of 0.4 ng/mL (3sigma) was obtained. Sensitivity was enhanced approximately 8-fold over conventional pneumatic nebulization sample introduction. Compared with CVG in an optimized HCl or HNO3 medium, sensitivity was increased by an order of magnitude using acetic acid and the reductant concentration was reduced to only 10% of that required with HCl or HNO3. The generation efficiency was estimated to be 18% or 70%, depending on the method used to evaluate it. The methodology was successfully used to the determine copper in human hair and low alloy steel certified reference materials.
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PMID:Chemical vapor generation of Cu: optimization of generation media. 1623 83

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

The potential of quadrupole-based ICP-MS as a tool for B-isotopic analysis of wines and its usefulness in provenance determinations were assessed. A precision of 0.1-0.25% RSD (corresponding to a relative standard deviation of the mean of three replicate measurements of 0.06-0.12%) was sufficient to establish small differences in the B isotope ratios in wines from different geographical origins. Each sample measurement was bracketed by measurements of a standard and mass bias drift correction made by interpolation. Sample preparation was kept to a minimum to avoid possible fractionation. Dilution of the wine samples by a factor of 100 with 0.65% HNO3 was found to reduce matrix-induced mass discrimination substantially. Wines from three wine-producing regions, Stellenbosch, Robertson, and Swartland, in the Western Cape Province of South Africa, and wines from specific regions in France (Bergerac) and Italy (Valpolicella) were analyzed by ICP-QMS for their B-isotopic compositions. It was concluded that the 11B/10B ratios can be used to characterize wines from different geographical origins. Average 11B/10B ratios in red wines from South Africa (Stellenbosch), France (Bergerac), and Italy (Valpolicella) were found to differ by between 0.5 and 1.5%.
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PMID:Classifying wine according to geographical origin via quadrupole-based ICP-mass spectrometry measurements of boron isotope ratios. 1625 41

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

Capillary liquid chromatography (cLC) and capillary electrophoresis (CE) have been critically compared for the separation of metalloproteins when using collision-cell inductively coupled plasma mass spectrometry (ICP-CC-MS) as detection system. For cLC separation, the selected column was a C8 (0.3 mm I.D.) and the separation conditions involved a gradient up to 80% methanol in 10mM ammonium acetate buffer (pH 7.4). The low flow rate used (3 microL min(-1)) permitted the utilization of a high methanol content maintaining the sensitivity along the whole chromatographic run. For this purpose, a new low-flow interface has been developed based on a total consumption nebulizer. Similarly, CE has been studied as separation technique using a 75 microm I.D. fused silica capillary and a running buffer of 20 mM Tris-HNO3 (pH 7.4) and working at 30 kV. Metallothionein (mixture of MT-I and -II) and superoxide dismutase (SOD) have been used as protein models in order to evaluate the separation/detection capabilities using the same injection volumes in both systems (20 nL). For both hybrid systems, separation parameters such as retention factor, numbers of theoretical plates, tailing factor and resolution have been critically compared. Also, the analytical performance characteristics of both hybrid systems have been evaluated and tested by analyzing the Cu-, Zn-species present in red blood cell extracts in order to explore more adequate separation methodology for the analysis of metalloproteins in complex matrices.
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PMID:Direct comparison of capillary electrophoresis and capillary liquid chromatography hyphenated to collision-cell inductively coupled plasma mass spectrometry for the investigation of Cd-, Cu- and Zn-containing metalloproteins. 1651 92

Nanometer titanium dioxide immobilized on silica gel (immobilized nanometer-scale TiO2 particles) was prepared by a sol-gel method and characterized by X-ray diffraction and scanning electron microscopy. The adsorptive behavior of Cr(III) and Cr(VI) on immobilized nanometer TiO2 was assessed. Cr(III) was selectively sorbed on immobilized nanometer TiO2 in the pH range of 7-9, while Cr(VI) was found to remain in solution. A sensitive and selective method has been developed for the speciation of chromium in water samples using an immobilized nanometer TiO2 microcolumn and inductively coupled plasma atomic emission spectrometry. Under optimized conditions (pH 7.0, flow rate 2.0 mL/min), Cr(III) was retained on the column, then eluted with 0.5 mol/L HNO3 and determined by ICP-AES. Total chromium was determined after the reduction of Cr(VI) to Cr(III) by ascorbic acid. The adsorption capacity of immobilized nanometer TiO2 for Cr(III) was found to be 7.04 mg/g. The detection limit for Cr(III) was 0.22 ng/mL and the RSD was 3.5% (n = 11, c = 100 ng/ mL) with an enrichment factor of 50. The proposed method has been applied to the speciation of chromium in water samples with satisfactory results.
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PMID:Speciation of chromium by selective separation and preconcentration of Cr(III) on an immobilized nanometer titanium dioxide microcolumn. 1652 98

A 234U and 230Th determination method based on an extraction chromatographic separation on a flow injection system coupled to a quadruple ICP-MS was developed. Two-milliliter UTEVA (Eichrom Co.) cartridges were applied as separation tool and 236U and 229Th as spikes. Loading and washing steps were carried out in 3 M HNO3 solution and 0.05 M ammonium oxalate applied to elute both uranium and thorium. The method was applied initially to the IAEA-327 soil reference sample and NIST SRM 4357 ocean sediment reference material, with the obtained 234U and 230Th concentrations in agreement with the reference levels. Samples from a deep-sea sediment core (2450 m water depth) were analyzed and based on 230Th/234U dating, a mean sedimentation rate of 3.3 cm ky(-1) was calculated. Samples from two sediment layers were also dated by 14C-AMS and the observed ages agree with the 230Th/234U results.
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PMID:234U and 230Th determination by FIA-ICP-MS and application to uranium-series disequilibrium in marine samples. 1654 93

A method is described for determination of selenium in sediment by isotope-dilution inductively coupled plasma mass spectrometry with an octapole reaction cell (ID-ICP-ORCMS). Sediment samples were digested with HNO3, HClO4, and HF, and the digestion included an elaborate evaporation process to remove bromine from the digested solution. Simple strong cation-exchange disk filtration was used to remove rare earth elements (REE) from the digested solution, because REE2+ seriously interfere with Se isotopes (i.e. 156Gd2+ with 78Se+, 160Gd2+ with 80Se+). Addition of acetic acid to the filtrate was examined to improve the sensitivity of ICP-ORCMS measurement of Se+ by means of a carbon-enhancement effect. The interfering Ar2+ for selenium isotopes were almost eliminated by use of H2 as reaction gas. Interference from BrH+ formed in the reaction cell was negligible because the Br was removed in the evaporation process. Approximately 99.5% of REE were removed by cation-exchange disk filtration yet more than 99% of Se remained in the filtrate solution. The intensity for Se+ was enhanced approximately fourfold by addition of 5% (v/v) of acetic acid whereas that for Ar2+ was barely enhanced. Measured 80Se/78Se ratios in unspiked digested solutions of the sample were in good agreement with that for an Se standard solution. The analytical results for Se in the certified reference materials MESS-3 and PACS-1 were in good agreement with their certified values, with small uncertainties.
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PMID:Determination of selenium in sediment by isotope-dilution inductively coupled plasma mass spectrometry with an octapole reaction cell. 1655 8

A method was developed for high-throughput determinations of 7 elements in food samples, namely antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), lead (Pb), mercury (Hg), and tin (Sn). The samples were digested by closed-vessel microwave-assisted digestion using concentrated nitric acid (HNO3) as the medium, followed by microwave- assisted evaporation to concentrate the sample solutions before dilution to the desired volume. The microwave-assisted evaporation procedure effectively reduced the final acid concentration to around 8% before analysis by inductively coupled plasma-mass spectrometry (ICP-MS). This reduction allows determination by ICP-MS to proceed without further sample dilution, which would affect the detection limit. The method was validated, and method recoveries for As, Cd, Cr, Pb, and Hg were within the certified ranges of the chosen certified reference materials. Recoveries of the 7 elements from spiked samples ranged from 93.1 to 103.6%. The standard uncertainties of precision for the 7 elements were between 3.1 and 4.3%. Interlaboratory comparison studies for As, Cd, and Pb gave z-scores ranging from -0.2 to 0.3.
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PMID:High-throughput determination of seven trace elements in food samples by inductively coupled plasma-mass spectrometry. 1664 Feb 96

Soil metal surveys were conducted in Baltimore, MD (1976-1979), Minnesota (1981-1988) and most recently, New Orleans, LA (1989-present). The unique characteristic of New Orleans is that it has two surveys; Survey I was completed in 1992 and Survey II was completed in 2000. This paper seeks to determine if there is a perceptible change in the amount of metals during less than a decade that separated these surveys. The Survey I collection was 4,026 samples stratified by 283 census tracts. All samples were collected in residential neighborhoods at least one block from a busy street. The Survey II collection was 5,467 samples stratified by 286 census tracts (plus City Park). The Survey II collection included busy streets as a category of samples. For comparison, the busy street category of 1,078 samples was excluded from Survey II for a total of 4,388 samples. The extraction methods of the two surveys used the same protocol for strength of acid (1 M HNO3), shaker-time (2 hours), and room temperature (approximately 22 degrees C). However, Survey II differed in amount of sample used in extraction. For Surveys I and II, 4.0g and 0.4g were used respectively. The same ICP-AES was used to measure 8 metals in both surveys. To evaluate the analytical results of the two methods, reference soi 1 samples (n=36) from the Wageningen Evaluating Programs for Analytical Laboratories, International Soil-analytical Exchange (WEPAL; ISE) were used. The relationship between the 4.0 and 0.4 g results were linear and the Survey I results were adjusted for sample:acid ratio. Further evaluation was done by creating interpolated Multiple Metal Accumulation (MMA) maps based on the median MMA for each census tract. A new map was created by dividing Survey II MMA by Survey I MMA. The ratio indicates increases of soil metals in the inner city and decreases of soil metals in the outlying areas of Metropolitan New Orleans. Comparing fresh parent alluvium from the Mississippi River with urban soil metal quantities demonstrates that the soils of New Orleans have undergone a massive accumulation of metals. The preliminary results provide ideas about methods needed to further evaluate the changes between these surveys.
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PMID:Changes of multiple metal accumulation (MMA) in New Orleans soil: preliminary evaluation of differences between survey I (1992) and survey II (2000). 1670 33


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