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A method for determining atmospheric diborane in concentrations higher than 1/10 of TLV, i.e., 0.01 ppm, has been developed using the adsorption sampling method. Silica gel impregnated with potassium permanganate, synthetic resin activated carbon impregnated with or without mercury(II) chloride and activated carbon impregnated with chromate salt showed adsorption capacities larger than 18 l of 3 ppm diborane test gas when the test gas was drawn at 300 ml/min. Complete desorption of the adsorbed diborane was possible only from silica gel impregnated with potassium permanganate into a hydroxylamine hydrochloride solution. As methods for determining the desorbed boron, both the chromotropic acid-HPLC method and ICP-AES were applied. The former was more sensitive, but the latter was less influenced by coexistent substances. The most sensitive and reproducible procedure for diborane determination was as follows: diborane is collected with silica gel impregnated with potassium permanganate (0.05% (w/w)) and desorbed into hydroxylamine hydrochloride solution (400 micrograms/ml) followed by the determination of boron by the chromotropic acid-HPLC method. When diborane in 3 l of 0.1 ppm test gas was collected, the desorption efficiency was 105.3% with an RSD of 13.5%. The limit of quantitation of this method was 0.0026 ppm in 3 l air. Much lower concentrations can be determined by sampling larger amounts of air.
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PMID:Determination of diborane by adsorption sampling using modified silica gel and the chromotropic acid-HPLC method. 131 78

The reaction of [Mo(3)S(4)(H(2)O)(9)](4+) with Bi(III) in the presence of BH(4)(-) (rapid), or with Bi metal shot (3-4 days), gives a heterometallic cluster product. The latter has been characterized as the corner-shared double cube [Mo(6)BiS(8)(H(2)O)(18)](8+) by the following procedures. Analyses by ICP-AES confirm the Mo:Bi:S ratio as 6:1:8. Elution from a cation-exchange column by 4 M Hpts (Hpts = p-toluenesulfonic acid), but not 2 M Hpts (or 4 M HClO(4)), is consistent with a high charge. The latter is confirmed as 8+ from the 3:1 stoichiometries observed for the oxidations with [Co(dipic)(2)](-) or [Fe(H(2)O)(6)](3+) yielding [Mo(3)S(4)(H(2)O)(9)](4+) and Bi(III) as products. Heterometallic clusters [Mo(6)MS(8)(H(2)O)(18)](8+) are now known for M = Hg, In, Tl, Sn, Pb, Sb, and Bi and are a feature of the P-block main group metals. The color of [Mo(6)BiS(8)(H(2)O)(18)](8+) in 2.0 M Hpts (turquoise) is different from that in 2.0 M HCl (green-blue). Kinetic studies (25 degrees C) for uptake of a single chloride k(f) = 0.80 M(-)(1) s(-)(1), I = 2.0 M (Hpts), and the high affinity for Cl(-) (K > 40 M(-)(1)) exceeds that observed for complexing at Mo. A specific heterometal interaction of the Cl(-) not observed in the case of other double cubes is indicated. The Cl(-) can be removed by cation-exchange chromatography with retention of the double-cube structure. Kinetic studies with [Co(dipic)(2)](-) and hexaaqua-Fe(III) as oxidants form part of a survey of redox properties of this and other clusters. The Cl(-) adduct is more readily oxidized by [Co(dipic)(2)](-) (factor of approximately 10) and is also more air sensitive.
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PMID:Preparation and Properties of the Corner-Shared Double Cube [Mo(6)BiS(8)(H(2)O)(18)](8+) as a Derivative of [Mo(3)S(4)(H(2)O)(9)](4+) in Aqueous Acidic Solutions. 1166 43

ICP-MS has been used for the determination of over 30 geochemically significant trace elements (Sc, V, Cr, Co, Ni, Cu, Zn, Ga, Rb, Sr, Y, Zr, Nb, Cs, Ba, Hf, Ta, Pb, Th, U and REEs) in anorthosites and related rock reference samples. Open acid digestion, pressure decomposition using HF, HNO(3) and HClO(4), and a fusion method using lithium metaborate and subsequent dissolution in dil. HNO(3) were adopted for the decomposition of these rock samples before analysis. The dissolution problems and interference effects are discussed. Rh and Bi were used as internal standards. The first set of data on several rare earths and other trace elements in the Russian anorthosite reference sample, MO-6 are presented along with data on other samples. The data are compared with the available data. The results obtained with different dissolution methods were found to be in good agreement for the majority of the trace elements. The accuracy and precision achieved (better than 6% RSD in most cases) suggested that the data obtained by ICP-MS for such samples are best suited for geochemical interpretations.
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PMID:Comparitive study of the sample decomposition procedures in the determination of trace and rare earth elements in anorthosites and related rocks by ICP-MS. 1504 36

The E.U. Directive on incineration of waste regulates the harmful emissions of particles and twelve toxic elements, including copper, chromium, and arsenic. More information is critically needed on the speciation and behavior of these trace elements during combustion, including the effects of different process variables, as well as of different fuels and fuel mixtures. Using a 15 kW pellets-fueled grate burner, experiments were performed to determine the fate of copper, chromium, and arsenic during combustion of chromate copper arsenate (CCA) preservative wood. The effects of co-combustion of CCA-wood with peat were also studied since peat fuels previously have proved to generally reduce ash related problems. The fate and speciation of copper, chromium, and arsenic were determined from analysis of the flue gas particles and the bottom ash using SEM-EDS, XRD, XPS, and ICP-AES. In addition, chemical equilibrium model calculations were performed to interpret the experimental findings. The results revealed that about 5% copper, 15% chromium, and 60% arsenic were volatilized during combustion of pure CCA-wood, which is lower than predicted volatilization from the individual arsenic, chromium, and copper oxides. This is explained by the formation of more stable refractory complex oxide phases for which the stability trends and patterns are presented. When co-combusted with peat, an additional stabilization of these phases was obtained and thus a small but noteworthy decrease in volatilization of all three elements was observed. The major identified phases for all fuels were CuCrO2(s), (Fe, Mg, Cu)(Cr, Fe, Al)04(s), Cr2O3(s), and Ca3(AsO4)2(s). Arsenic was also identified in the fine particles as KH2AsO4(s) and As2O3(s). A strong indication of hexavalent chromium in the form of K2CrO4 or as a solid solution between K3Na(CrO4)2 and K3Na(SO4)2 was found in the fine particles. Good qualitative agreement was observed between experimental data and chemical equilibrium model calculations.
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PMID:Fate of Cu, Cr, and As during combustion of impregnated wood with and without peat additive. 1794 5

In this work, different analytical speciation schemes have been used to study the reduction of Cr(VI) by a chromate-resistant strain of filamentous fungi Ed8 (Aspergillus sp), indigenous to contaminated industrial wastes. As demonstrated previously, this strain has the capability to reduce chromate present in the growth medium without its accumulation in the biomass, yet the reduced chromium end-products have not been characterized. Liquid growth medium, initially containing 50 mg L(-1) Cr(VI), was analyzed for Cr(III)/Cr(VI) and for total Cr at different time intervals (0-24 h) after inoculation with fungi. Three hyphenated procedures, based on the Cr(III)-EDTA formation and species separation by anion-exchange or ion-pairing reversed-phase chromatography with ICP-MS or DAD detection were used. The results obtained for Cr(VI) in each case were consistent, demonstrating efficient reduction of chromate during 24 h of Ed8 growth. However, pre-column complexation with EDTA did not ensure complete recovery of the reduced forms of chromium in the above procedures. An alternative speciation scheme, based on extraction of Cr(VI)-benzyltributylammonium bromide (BTAB) ion pairs into chloroform and subsequent determination of residual chromium by ICP-MS has provided evidence on the effective conversion of chromate into reduced chromium species in the growth medium. The results indicate the feasibility of using Ed8 strain for chromate bioremediation purposes. Analytically it can be concluded that speciation of chromium in biological systems should not be limited to its two most common oxidation states, because the actual reduced chromium species are not converted quantitatively to Cr(III)-EDTA.
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PMID:Analytical speciation of chromium in in-vitro cultures of chromate-resistant filamentous fungi. 1866 54

In order to implement a simpler, less expensive and more safe sample dissolution procedure, we have substituted the HF-HClO(4) mixture by NH(4)F. By testing three certified reference materials, lichen 336, basalt BE-N, soil 7, it was found that the three-reagents digestion without HF and HClO(4) (HNO(3)+H(2)O(2)+NH(4)F was used) was very effective for the pretreatment of ICP-MS measurement. The comparison was based on the measurement results and their uncertainties. All are reference material for amount contents of different trace elements. The accuracy and precision of the developed method were tested by replicate analyses of reference samples of established element contents. The accuracy of the data as well as detection limits (LODs) vary among elements but are usually very good (accuracy better than 8%, LODs usually below 1 microg/g in solids). ICP-MS capabilities enable us to determine routinely 13 and 16 minor and trace elements in basalt and soil.
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PMID:Relevance of NH4F in acid digestion before ICP-MS analysis. 1880 58

A hydrogen reduction and activated sintering process was proposed to prepare chromic oxide green pigment. Through ICP, XRD, SEM, FT-IR, UV, and CIE-L*a*b* colorimetric analysis, key factors and mechanism that influenced preparation of chromic oxide green pigment were studied. The results revealed that lower hydrogen reduction temperature, suitable addition of Al and Ba, were beneficial to obtaining the high quality chromic oxide green pigment. Typically, when the hydrogen reduction temperature was kept at 450-500 degrees C, physicochemical properties and color performance of the prepared chromic oxide green pigment doped with about 0.1-0.2 wt % Al and 0.2-0.5 wt % Ba conformed to commercial pigment standards. Additionally, characteristics of the green process were discussed. About 90 wt % KOH was reused directly and about 90 wt % Cr(VI) was conversed to Cr(III) directly from potassium chromate to chromic oxide green pigment. Integrating the proprietary green metallurgical process from chromite ore to potassium chromate of this laboratory, more than 99 wt % Cr(VI) could be conversed to Cr(III) compounds and about 99 wt % KOH could be recycled to use. The whole green process, ranging from chromite ore to chromic oxide green pigment, eventually not only provided the possibility for producing the high quality chromic oxide green pigment, but could reach comprehensive utilization of resources, inner recycle of KOH, and zero emission of Cr(VI).
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PMID:A green process to prepare chromic oxide green pigment. 1893 51

A method for speciation of vanadium in soil is presented in this work. The sequential extraction analysis procedure of Tessier et al. for heavy metals was used for the vanadium separation. The method consists of sequential leaching of the soil samples to separate five fractions of metals: (1) exchangeable, (2) bound to carbonates, (3) bound to Fe-Mn oxides, (4) bound to organic matter and (5) residual. The leaching solutions of Tessier were used for the vanadium extraction, only for the residual fraction the HClO(4) was replaced with H(2)SO(4). The optimum conditions for leaching of vanadium from soil (weight of sample, concentration and volume of extractants, time of extraction) were chosen for each fraction. A sensitive, spectrophotometric method based on the ternary complex V(IV) with Chrome Azurol S and benzyldodecyldimethylammonium bromide (epsilon=7.1x10(4) l mol(-1) cm(-1)) was applied for the vanadium determination after separation of V(V) by solvent extraction using mesityl oxide and reduction of V(V) using ascorbic acid. This method was applied for vanadium speciation in soil from two different regions of Poland: Upper Silesia (industrial region) and Podlasie (agricultural region). The content of vanadium in the fractions of Upper Silesia soil was respectively (in 10(-3)%): I, 3.39; III, 4.53; IV, 10.70; V, 8.70 and it was the highest in the organic fraction, indicating input by anthropogenic activities. The content of vanadium in Podlasie soil was clearly lower and it was (in 10(-3)%): I, 2.07; III, 0.92; IV, 0.69; V, 1.23. The concentration of vanadium in fraction 2 of both soils was less than detection limit of applied method. The total content of vanadium in the five soil fractions was in good correlation with the total content of this element in both soils found after HF-H(2)SO(4) digestion. Analysis using the ICP-AES method gave comparable results.
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PMID:Speciation of vanadium in soil. 1896 78

A procedure for the determination of chromium is described based on synergistic pre-concentration of the chromate anion at a carbon paste electrode modified in situ with quarternary ammonium salts such as 1-ethoxycarbonylpentadecyltrimethylammonium bromide (Septonex((R))), cetyltrimethylammonium bromide (CTAB) or cetylpyridinium bromide (CPB). The proper electrochemical detection utilises the reduction Cr(VI) --> Cr(III) performed in the differential pulse cathodic voltammetric mode. In discussion, considerable attention has been paid to the accumulation mechanism at the carbon paste electrode in the presence of surfactants. Furthermore, after optimising the corresponding experimental conditions (0.1-0.3M HCl + 0.1M NaCl as the supporting electrolyte, 2.5-25muM as the total concentration of modifier, pre-concentration at +0.7V versus Ag/AgCl and the stripping from +0.7 to -0.4V), the analytical performance of the method has been evaluated. The signal of interest was reproducible within +/-8% and proportional to the concentration in a range of 0.5-50muM CrO(4)(2-), with a limit of detection (S/N = 3:1) of about 5x10(-8)M CrO(4)(2-) (with accumulation for 300s). Interference studies were focused mainly on the species capable of forming ion-pairs with the modifier; i.e., TlCl(4)(-), AuCl(4)(-), PdCl(4)(2-), PtCl(6)(2-), VO(4)(3-), MnO(4)(-) and I(-). Practical applicability of the method was tested on model solutions via the recovery rates (typically 90-110%) or using selected certified reference materials (tea, bush leaves, clover) and two samples of black tea when the respective results were compared to those obtained by the reference determinations with ICP-AES.
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PMID:A study on the determination of chromium as chromate at a carbon paste electrode modified with surfactants. 1896 79

Resin-derived contaminants added to samples during column chemistry are shown to cause matrix effects that lead to inaccuracy in multi-collector inductively coupled plasma mass spectrometry measurement of small natural variations in Cd and Zn isotopic compositions. These matrix effects were evaluated by comparing pure Cd and Zn standards and standards doped with bulk column blank from the anion exchange chromatography procedure. Doped standards exhibit signal enhancements (Cd, Ag, Zn and Cu), instrumental mass bias changes and inaccurate isotopic compositions relative to undoped standards, all of which are attributed to the combined presence of resin-derived organics and inorganics. The matrix effect associated with the inorganic component of the column blanks was evaluated separately by doping standards with metals at the trace levels detected in the column blanks. Mass bias effects introduced by the inorganic column blank matrix are smaller than for the bulk column blank matrix but can still lead to significant changes in ion signal intensity, instrumental mass bias and isotopic ratios. Chemical treatment with refluxed HNO(3) or HClO(4)/HNO(3) removes resin-derived organic components resulting in matrix effects similar in magnitude to those associated with the inorganic component of the column blank. Mass bias correction using combined external normalization-SSB does not correct for these matrix effects because the instrumental mass biases experienced by Cd and Zn are decoupled from those of Ag and Cu, respectively. Our results demonstrate that ion exchange chromatography and associated resin-derived contaminants can be a source of error in MC-ICP-MS measurement of heavy stable element isotopic compositions.
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PMID:Matrix effects on the multi-collector inductively coupled plasma mass spectrometric analysis of high-precision cadmium and zinc isotope ratios. 1911 Jan 12


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