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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

After decomposition of plant standard reference materials bush twigs and leaves (GBW07602, GBW07603), poplar leaves (GBW07604) and tea (GBW07605) with either dry ashing method or wet digestion method, all kinds of fine particles left in the solution were collected and examined carefully by a scanning electron microscope (SEM), and their chemical composition were investigated by a SEM-affiliated energy-dispersive X-ray spectrometer at the same time. Moreover, the concentrations of some metal elements distributed among four different tea SRM-originated particle fractions extracted following the BCR sequential extraction procedure were determined by AAS and ICP-AES. It was found that decomposition methods have a great influence on the structure of fine particles. When dry ashing method is used, grey-colored, fluffy and porous partices can be produced, whereas fewer white-colored, compact particles can be produced when another method is used. As for chemical composition, all kinds of fine particles are almost the same, with silicon and aluminium as their main constituents, and calcium, iron, potassium, titanium and so on as their minor ones. The elementaI distribution percentages in four different particle fractions in two kinds of plant-originated particles differ from element to element, which can result in severe negative errors when plant samples are decomposed and determined for elemental concentrations.
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PMID:[Study on the characteristics and compositions of fine particles left in the solution after decomposition of plant samples]. 1682 24

A comparison of slurry sampling (SS)-ETV-ICP-MS and slurry nebulization (SN)-ICP-MS for direct determination of trace impurities in titanium dioxide powder is made. The particle size effect, matrix effect and analytical characteristics of SSETV-ICP-MS and SN-ICP-MS are compared. The results have shown that SSETV-ICP-MS has a lower particle size effect and matrix effect compared to SN-ICP-MS. The analytical performance of the two methods reveals that SSETV-ICP-MS and SN-ICP-MS have similar relative detection limits (in the nanogram per liter level); however, the former has a lower absolute detection limit than the latter. Although the precision for SSETV-ICP-MS is a little worse than that for SN-ICP-MS, it is still acceptable for real sample analysis. The two methods were successfully applied for the determination of trace impurities in titanium dioxide powder samples with particle sizes of less than 50 nm, but only SSETV-ICP-MS could be applied for the determination of trace impurities in titanium dioxide powder samples with a particle size of 1 microm.
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PMID:A comparison of slurry sampling electrothermal vaporization and slurry nebulization inductively coupled plasma mass spectrometry for the direct determination of trace impurities in titanium dioxide powder. 1701 25

We report a simple method that combines dialysis, as a purification method, with the multielement capability of ICP to determine the titanium-to-transferrin mole ratio at physiological pH, under buffer conditions. The method, by means of which titanium and transferrin are determined simultaneously, enabled us to assess the binding capacities of different titanocene complexes.
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PMID:Determination of the titanium content of human transferrin by inductively-coupled plasma-atomic-emission spectroscopy. 1701 77

Nowadays there are many sun-protection cosmetics incorporating organic or inorganic UV filters as active ingredients. Chemically stable inorganic sunscreen agents, usually metal oxides, are widely employed in high-SPF (sun protection factor) products. Titanium dioxide is one of the most frequently used inorganic UV filters. It has been used as a pigment for a long period of cosmetic history. With the development of micronization techniques, it has become possible to incorporate titanium dioxide in sunscreen formulations without the previous whitening effect, and hence its use in cosmetics has become an important research topic. However, there are very few works related to quantitation of titanium dioxide in sunscreen products. In this research, we analyzed the amounts of titanium dioxide in sunscreen cosmetics by adapting redox titration, reduction of Ti(IV) to Ti(III), and reoxidation to Ti(IV). After calcification of other organic ingredients of cosmetics, titanium dioxide is dissolved by hot sulfuric acid. The dissolved Ti(IV) is reduced to Ti(III) by adding metallic aluminum. The reduced Ti(III) is titrated against a standard oxidizing agent, Fe(III) (ammonium iron(III) sulfate), with potassium thiocyanate as an indicator. In order to test the accuracy and applicability of the proposed method, we analyzed the amounts of titanium dioxide in four types of sunscreen cosmetics, namely cream, make-up base, foundation, and powder, after adding known amounts of titanium dioxide (1 approximately 25 w/w%). The percentages of titanium dioxide recovered in the four types of formulations were in the range between 96% and 105%. We also analyzed seven commercial cosmetic products labeled with titanium dioxide as an ingredient and compared the results with those obtained from ICP-AES (inductively coupled plasma-atomic emission spectrometry), one of the most powerful atomic analysis techniques. The results showed that the titrated amounts were well in accord with the analyzed amounts of titanium dioxide by ICP-AES. Although instrument-based analytical methods, namely ICP-MS (inductively coupled plasma-mass spectrometry) and ICP-AES, are best for the analysis of titanium, it is difficult for small cosmetic companies to install such instruments because of their high cost. It was found that the volumetric method presented here gives quantitatively accurate and reliable results with routine lab-ware and chemicals.
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PMID:A novel volumetric method for quantitation of titanium dioxide in cosmetics. 1711 Oct 72

Porous titanium structures hold considerable promise as scaffolds for bone ingrowth in load bearing locations provided they are made osteoinductive by incorporation of bone growth factors. The purpose of the present research was to incorporate soybean trypsin inhibitor (STI) imitating growth factor into a porous Ti scaffold using sol-gel silica as a slow-release protein carrier. Alcohol-free TMOS-based sols (of pH 2 or 5) with dissolved STI were injected into Ti wire scaffolds yielding SiO(2) coating on the wire struts and SiO(2) beads entrapped in-between the wires. The formation of well-polymerized nanoporous SiO(2) was confirmed by FTIR, solid-state NMR, N(2) adsorption/desorption isotherms and BET analysis. In-vitro dissolution of silica and STI release in phosphate buffered saline (PBS) at 37 degrees C were measured by ICP-AES and Bradford assay, respectively. The biochemical activity of released STI protein was assessed by enzymatic assay. STI release was found to follow an attractive pattern of rapid release during the first 5 days followed by steady slow release for over one month. Despite certain conformational changes induced by the encapsulation procedure (detected by Circular Dichroism), the released STI retained most of its biological activity, especially when silica sol was prepared at the high protein-friendly pH = 5.
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PMID:Protein incorporation within Ti scaffold for bone ingrowth using Sol-gel SiO2 as a slow release carrier. 1761 61

A suspension of chrysotile asbestos fibres in aqueous 0.5M oxalic acid was subjected to power ultrasound with the aim to disrupt and detoxify the mineral by the leaching action of oxalic acid on its structural cations acting simultaneously with a vigorous acoustic cavitation. Sonication was performed in a "cavitating tube", a vertical hollow vibrating cylinder made of titanium, operating at 19.2 kHz and 150 W. Treatment lasted from 2.5 to 21 h. Scanning electron microscopy (SEM) showed that the joint action of the chelating agent and ultrasound (though not of either when applied independently) mostly converted asbestos fibres into micrometric aggregates and nano-sized debris, whose morphology totally differed from asbestos fibres. When treated suspensions were filtered through CA membranes (pore size 0.20 microm), more than half of the asbestos went through the filter because it had either been brought in solution or dispersed in the form of extremely small particles. Most of the structural metal ions were brought into solution (ICP-AES). After the treatment the BET surface area of the recovered solid was tenfold greater than the original. The crystalline fraction of residual solids, though resembling the original sample in XRD, was shown by micro-Raman spectra to be made of antigorite, a polymorph form of serpentine. Furthermore, as the length of these antigorite fibrils lay outside the fibre range rated as a health hazard under worldwide regulations, our procedure can be employed for the decontamination of chrysotile-polluted waters and sediments.
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PMID:A new approach to the decontamination of asbestos-polluted waters by treatment with oxalic acid under power ultrasound. 1793 51

The reason of deactivation of titania whiskers used for deep purification of drinking water and the corresponding regeneration methods were presented. AFM, XRD and ICP were carried out to characterize the titanium dioxide. The experimental results suggest that the main reason of deactivation of titania whiskers is the deposition of calcium carbonate on the catalyst surface. The surface of titania whiskers is covered by the insoluble carbonates generated from carbon dioxide produced during the degradation of organics and metal ions such as calcium in the tap water, and the activity of the titania whiskers decreases gradually till deactivation. After washing by 1 mol/L hydrochloric acid for four hours, the photocatalytic activity of the titania whiskers can achieve 95 percent of that before deactivation. The photocatalytic activity of the titania whiskers which regenerated for many times keeps steady.
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PMID:[Deactivation of titania whiskers used for purification of drinking water]. 1799 May 51

The validity of using elemental phosphorus standards to accurately and precisely quantify phosphopeptides by capillary HPLC (capHPLC) coupled to ICP-collison cell-MS is investigated in detail. Operating requirements to maintain stable (31)P sensitivity along the reversed-phase gradient are described. Specifically, the use of an optimum postcolumn makeup flow with a defined acetonitrile content turned out to be necessary to buffer the acetonitrile variation of the capillary chromatographic eluent and ensure plasma stability. Then, a highly pure P-containing standard (bis(4-nitro-phenyl) phosphate, BNPP) was spiked into the samples and used to quantify them with very low absolute errors (2-4%) and excellent precision (3-6%). The capHPLC-ICPMS method showed excellent linearity over 3 orders of magnitude and provided adequate detection limits (110 fmol, 3.4 pg P). Accurate quantification of the phosphopeptides present in a tryptic digest of beta-casein and casein from bovine milk was then attempted. Previously, and in order to be able to close mass balances, total P contents, percentages of inorganic P present, and recoveries from the reversed-phase column used in the separation were computed for each sample. Quantification using the spiked BNPP for the different phosphopeptides detected matched the expected values well validating the quantitative methodology proposed. The capHPLC-ESIMS analysis allowed elucidating amino acid sequences, a requisite still necessary to translate the determined amount of P in each chromatographic peak into amount of phosphopeptide. The great potential of these strategies, based on ICPMS detection, to assess the many procedures proposed and commonly used for purification, preconcentration, and/or isolation of phosphopeptides in phosphoproteomics studies is demonstrated using a commercially available titanium dioxide (TiO(2)) cartridge for phosphopeptide enrichment from complex mixtures. Quantitative results obtained allow one to assess individual phosphopeptide recoveries from the TiO(2) cartridge with unsurpassed accuracy. Of course, this information is essential for reliable absolute quantifications in phosphoproteomics.
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PMID:Absolute and site-specific quantification of protein phosphorylation using integrated elemental and molecular mass spectrometry: its potential to assess phosphopeptide enrichment procedures. 1824 85

This study compared differences in discoloration and dissolution in several titanium alloys with immersion in peroxide- or fluoride-containing solution. Commercially pure titanium (CP-Ti) and six titanium-based alloys were used: Ti-0.15Pd, Ti-6Al-4V, Ti-7Nb-6Al, Ti-55Ni, Ti-10Cu, and Ti-20Cr. Two test solutions were prepared for immersion of polished titanium and titanium alloys: one consisting of 0.2% NaF + 0.9% NaCl (pH 3.8 with lactic acid) and the other of 0.1 mol/l H2O2 + 0.9% NaCl (pH 5.5). Following immersion, color changes were determined with a color meter and released elements were measured using ICP-OES. Discoloration and dissolution rates differed between the two solutions. In the hydrogen peroxide-containing solution, color difference was higher in Ti-55Ni and Ti-6Al-4V than in any of the other alloys, and that Ti-55Ni showed the highest degree of dissolution. In the acidulated fluoride-containing solution, CP-Ti, Ti-0.15Pd, Ti-6Al-4V, Ti-7Nb-6Al, and Ti-10Cu alloys showed remarkable discoloration and dissolution with immersion. On the contrary, Ti-20Cr alloy showed very little discoloration and dissolution in either solution.
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PMID:Discoloration and dissolution of titanium and titanium alloys with immersion in peroxide- or fluoride-containing solutions. 1830 20


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