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Modified silicagel (C18) was studied for separation and preconcentration of platinum group metals (Ru, Rh, Pd, Os, Ir and Pt) as ion associates of their chlorocomplexes with cation of onium salt N(1-carbaethoxypentadecyl)-trimethyl ammonium bromide. Sample containing HCl and the onium salt was pumped through the column. After elution with ethanol the eluate was evaporated in the presence of HCl. Resulting aqueous solutions were analysed with inductively coupled plasma atomic emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS). Recovery values of 1-20 mug Pt and Pd from 50 ml of synthetic pure solution were 100+/-3 and 100+/-1%, respectively, however, they diminished with increasing sample volume and in the presence of the real sample matrix or nitrate ions. Samples of engine soot (NIES No. 8), decomposed by low pressure oxygen high-frequency plasma, and airborne particulates from dust filters of meteorological stations, leached with HNO(3) and H(2)O(2), were analysed. A reasonable agreement was found between ICP-MS and ICP-AES results for airborne dust samples and the values comparable with those in literature were determined in NIES No. 8.
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PMID:Preconcentration of platinum group metals on modified silicagel and their determination by inductively coupled plasma atomic emission spectrometry and inductively coupled plasma mass spectrometry in airborne particulates. 1896 26

Problems involved in the determination of Au and the platinum group elements by the nickel sulphide fire assay (NiS-FA) procedure for black shale samples, samples containing magnetite, and samples containing As, Cu, and Fe were studied. The interference of the graphite in black shale samples was eliminated either by roasting the sample prior to fusion or by adding an oxidant to the fusion flux. Addition of a reducing agent to samples, containing the oxygen-rich mineral magnetite, enabled the NiS-FA procedure to be carried out for this sample type. The interference of Cu on Rh in the ICP-MS determination was corrected by establishing a linear correlation between the interference of Cu on (103)Rh and (105)Pd.
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PMID:Determination of gold and the platinum group elements in geological samples by ICP-MS after nickel sulphide fire assay: difficulties encountered with different types of geological samples. 1896 87

The drift in sensitivity due to carbon deposition on the sampling cone, skimmer cone and ion lenses has been a serious problem in gas chromatography/inductively coupled plasma mass spectrometry (GC/ICP-MS). To overcome this problem, a high-speed switching method between a mixed-gas plasma and a pure-argon plasma (named plasma gas-switching method) using an oxygen permeation tube and a switching valve was developed. This enabled both the cleaning of deposited carbon and an enhancement of the sensitivity; as a consequence, both the repeatability and the sensitivity of polybrominated diphenylether (PBDE) were improved by more than 3 and 4 times, respectively. The drifts of sensitivity over a period of 8 h were less than 5% in most cases. Concerning the analytical performance of thermally labile congeners from octa- to deca-BDE, the detection limits, dynamic ranges of the calibration graphs and unequivalent sensitivities were remarkably improved by using a metal capillary separation column coated with a very thin (0.05 micromm) film of immobilized-polydimethylsiloxane. The detection limits ranged from 0.014 pg (BDE-154) to 0.093 pg (BDE-209), which were equal or superior to the lowest values reported hitherto by GC/MS (high resolution). A remarkable loss of sensitivity for highly-brominated congeners, such as nona- and deca-BDE, was observed in an analysis of PBDE technical mixtures when the solvent was methanol. The loss of sensitivity turned out to be due to an activation of the retention gap used for on-column injection; this problem was solved by changing methanol to isooctane in the sample-preparation step before analysis.
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PMID:Plasma gas-switching method for gas chromatography/inductively coupled plasma mass spectrometry and determination of polybrominated diphenylethers with high precision and sensitivity. 1907 60

Reliable determination of arsine (AsH(3)) in gases is of great importance due to stringent regulations associated with health, safety and environmental issues. It is, however, challenging for an analyst to determine trace airborne arsine concentrations without specifically designed collection procedures using adsorption, desorption, dissolution or impinging techniques. To circumvent such technical barrier, we have newly developed a direct analytical method, characterized by introduction of an arsine gas sample into stable plasma stream, followed by gas-phase oxidation of arsine with molecular oxygen in a dynamic reaction cell (DRC) equipped within the inductively coupled plasma-mass spectrometry (ICP/MS) system, followed by subsequent detection of AsO(+) ion. This preliminary work used trace arsine concentrations (161 microg m(-3), 322 microg m(-3), and 645 microg m(-3)) gravimetrically prepared in N(2) balance. The proposed method was optimized for the important experimental parameters such as the flow rates of the reaction gas, the arsine sample, and the carrier gas. This method was then validated by demonstrating good figure-of-merits including the low limit of detection (0.10 microg m(-3)), good linearity (r(2)>0.9915), low measurement uncertainty (0.66%), and high speed of analysis (<6 min). The proposed method is expected to be potentially applicable to the determination of arsine in real workplace air after appropriate modifications are made.
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PMID:Direct determination of arsine in gases by inductively coupled plasma-dynamic reaction cell-mass spectrometry. 1917 46

Recent advances in inductively coupled plasma mass spectrometry (ICP-MS) have included the addition of interference reduction technologies, such as collision and reaction cells, to improve its detection capability for certain elements that suffer from polyatomic interferences. The principle behind reaction cell (RC)-ICP-MS is to remove a particular polyatomic interference by dissociation or formation of a different polyatomic species that no longer interferes with the analyte of interest. However, some interferences cannot be removed by commonly reported reaction gases, such as hydrogen, oxygen, or methane, necessitating using more reactive and hazardous gases, such as ammonia. The current study investigates oxygen as a reaction gas in RC-ICP-MS to specifically react with vanadium analyte ions, rather than the interferents, to produce a polyatomic analyte species and thereby provide a way to analyze for vanadium in complex environmental matrices. The technique has been tested on a series of river water, tap water, and synthetic laboratory samples, and shown to be successful in vanadium analyses in high chloride and sulfate matrices. The zinc isobaric interference on the new vanadium oxide analyte at m/z 67 is also investigated, and can be corrected by using a standard mathematical correction equation. The results of this study further increase the utility of RC-ICP-MS analytical techniques for complex environmental matrices.
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PMID:Determination of vanadium by reaction cell inductively coupled plasma mass spectrometry. 1920 8

Nanomaterials (NM) exhibit novel physicochemical properties that determine their interaction with biological substrates and processes. Three metal oxide nanoparticles that are currently being produced in high tonnage, TiO(2), ZnO, and CeO(2), were synthesized by flame spray pyrolysis process and compared in a mechanistic study to elucidate the physicochemical characteristics that determine cellular uptake, subcellular localization, and toxic effects based on a test paradigm that was originally developed for oxidative stress and cytotoxicity in RAW 264.7 and BEAS-2B cell lines. ZnO induced toxicity in both cells, leading to the generation of reactive oxygen species (ROS), oxidant injury, excitation of inflammation, and cell death. Using ICP-MS and fluorescent-labeled ZnO, it is found that ZnO dissolution could happen in culture medium and endosomes. Nondissolved ZnO nanoparticles enter caveolae in BEAS-2B but enter lysosomes in RAW 264.7 cells in which smaller particle remnants dissolve. In contrast, fluorescent-labeled CeO(2) nanoparticles were taken up intact into caveolin-1 and LAMP-1 positive endosomal compartments, respectively, in BEAS-2B and RAW 264.7 cells, without inflammation or cytotoxicity. Instead, CeO(2) suppressed ROS production and induced cellular resistance to an exogenous source of oxidative stress. Fluorescent-labeled TiO(2) was processed by the same uptake pathways as CeO(2) but did not elicit any adverse or protective effects. These results demonstrate that metal oxide nanoparticles induce a range of biological responses that vary from cytotoxic to cytoprotective and can only be properly understood by using a tiered test strategy such as we developed for oxidative stress and adapted to study other aspects of nanoparticle toxicity.
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PMID:Comparison of the mechanism of toxicity of zinc oxide and cerium oxide nanoparticles based on dissolution and oxidative stress properties. 1920 59

Real time closed loop control of plasma assisted semiconductor manufacturing processes has received significant attention in recent years. Therefore we have developed and tested a customized optical sensor based on buffer gas (argon) actinometry which has been used to determine relative densities of atomic and molecular oxygen in an Ar/O(2) radio-frequency ICP chamber. The operation and accuracy of our optical sensor compared favorably with a high resolution commercial spectrometer but at lower cost and exhibited improved actinometric performance over a low resolution commercial spectrometer. Furthermore, threshold tests have been performed on the validity of buffer gas based actinometry in Ar/O(2) ICP plasmas where Ar is no longer a trace gas through Xe actinometry. The plasma conditions for which this customized optical sensor can be used for closed loop control have been established.
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PMID:Real time sensor for monitoring oxygen in radio-frequency plasma applications. 1955 Jun 63

A F-doped vanadia/titania catalyst has been developed by partly substituting the lattice oxygen of the catalyst with fluorine, using NH(4)F as a precursor. The aim of this novel design was to promote the activity of a catalyst with low vanadia loading in the low-temperature selective catalytic reduction of NO with NH(3). Analysis by N(2) physisorption, XPS, ICP, XRD, ESR and PL spectra showed that fluorine doping facilitated the formation of V(4+) and Ti(3+) ions mainly by charge compensation, promoted the distribution of vanadium on the catalyst surface, and increased the amount of surface superoxide ions. The catalytic activity of NO removal was promoted by F-doping. And the catalyst with [F]/[Ti]=1.35 x 10(-2) showed the highest NO removal efficiency in SCR reaction at low temperatures.
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PMID:The characterization and activity of F-doped vanadia/titania for the selective catalytic reduction of NO with NH3 at low temperatures. 1966 38

In Deinococcus radiodurans, there is a unique RecQ homolog (DR1289) with three-tandem HRDC domains. Deletion of drrecQ resulted in a low doubling rate and sensitivity to hydrogen peroxide. Here, we used cDNA microarray and biochemical assays to explore the physiological changes in the drrecQ mutant. The expressions of genes with predicted functions involved in iron homeostasis, antioxidant system, electron transport, and energy metabolism were significantly altered in response to drrecQ disruption. More reactive oxygen species (ROS) was accumulated in drrecQ mutant strain when compared to wild type. In addition, ICP-MS results showed that the intracellular level of iron was relatively higher, whereas the concentration of manganese was lower in drrecQ mutant than in wild type. Furthermore, our microarray data and pulsed-field gel results showed that DNA suffered more damage in drrecQ mutant than in wild type under 20 mM hydrogen peroxide stress. These results suggested that drrecQ is a gene of pleiotropic functions and contributes to the extraordinary resistance of D. radiodurans against stresses.
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PMID:Pleiotropic effects of RecQ in Deinococcus radiodurans. 1967 78

The flexible, anionic, open-framework material NaLa[(PO(3)H)(2)CH-C(6)H(4)-CH(PO(3)H)(2)].4H(2)O (NaLa(H(4)L)) exhibits an exceptional selectivity for monovalent metal cations. This study elucidates the relationship between the ion-exchange behavior and the framework flexibility of this recently discovered material. The exchange of the Na(+) ions in NaLa(H(4)L) with alkaline-earth, alkaline, and selected transition metal ions was studied. EDX and ICP-OES elemental analysis revealed that ion exchange was successful with monovalent ions, while higher-valent ions were rejected. An explanation for this charge selectivity could be found in the site-specific role of the guest cation. X-ray diffraction and thermogravimetric studies on the reversible hydration and dehydration behavior demonstrate that NaLa(H(4)L) has a flexible framework. Contraction of the channels upon dehydration leads to a decrease in the cell volume of 15%. Rietveld refinement of the structure of the dehydrated form NaLa(H(4)L)(dehyd) revealed the key role played by the guest cation in the channel-shrinking mechanism. In the hydrated, expanded form, each Na(+) ion guest shares three phosphonate oxygens with a La(3+) ion in a lanthanum phosphonate chain that defines part of the wall of a rhombic channel. The Na(+) ion completes its octahedral coordination sphere with two water molecules and a weaker bond to a fourth phosphonate oxygen. In the dehydrated, contracted form, the Na(+) ion loses the two water molecules and moves toward a second La(3+) ion, which is located in an adjacent lanthanum phosphonate chain, to share two more phosphonate oxygens, and becomes 5-coordinate. This results in the formation of an -La-O-Na-O-La- chain and a concomitant shrinking of the channels. A comparison of the monovalent metal (M(I)) ion-exchanged compounds, M(I)La(H(4)L), reveals that both the ionic radius and the enthalpy of hydration of the guest cation affect the equilibrium between the expanded and the contracted forms, and that the framework adapts specifically to the size of the guest cation.
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PMID:Exceptional ion-exchange selectivity in a flexible open framework lanthanum(III)tetrakisphosphonate. 1992 20


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