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Metal Fe or Cu doped P25 titania was prepared using the photodeposition method and characterized by TEM, ICP, XRD and UV-Vis, further tested for photocatalytic nitrate reduction and TN removal, under 20 W UV lamp irradiation. The influencing factors such as the pH values of solution, stirring gas, metal loadings, hole scavenger formic acid amount and co-doped Ag-Cu/TiO2 are investigated and discussed in detail. The experimental results after 2 h reaction indicated that with the increase of Cu loadings, nitrate conversion increases too, while a loading of 0.5% is optimal for highest N2 selectivity and TN (total nitrogen) removal. Using N2 as stirring gas and under acidic conditions, the N2 selectivity is lower (62%), but the highest conversion of nitrate and removal of TN can reach 36.9% and 23.2% respectively. Using CO2 as stirring gas, the highest selectivity for nitrogen 88.4% is obtained with 0.5% Cu/TiO2, 0.06 mol/L formic acid. Under the same conditions, using the prepared bimetallic titania (1%, 1:1 Ag/Cu), the conversion of nitrate and removal of TN are 48.1%, 34.2%, and N2 selectivity is 72.2%.
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PMID:[Photocatalytic reduction of nitrate using metal-doped titania]. 1906 39

This paper describes the use of a pervaporation (PV) technique in a flow injection (FI) system for selective improvement in iodide analysis. Iodide in the sample zone is oxidized to iodine, which permeates through a hydrophobic membrane. Detection of the diffused iodine is achieved using the chemiluminescent (CL) emission at 425nm that results from the reaction between iodine and luminol. The method was applied for the analysis of some pharmaceutical products, such as nuclear emergency tablets and multivitamin tablets. Ascorbic acid present in multivitamin samples interfered seriously with the analysis, and off-line sample treatment using anion exchange resin was employed to successfully remove ascorbic acid before the analysis. Ascorbic acid was flushed from the column using 0.4M sodium nitrate followed by elution of iodide with 2M sodium nitrate. The detection limit (3S.D.) of the system was 0.5mgl(-1), with reproducibility of 5.2% R.S.D. at 5mgl(-1). Sample throughput was determined as 30injectionsh(-1). There was good agreement between iodide concentrations from extracted samples determined using four different methods, i.e., PV-FI, gas diffusion-flow injection, potentiometry and ICP-MS. A comparison of the analytical features of the developed pervaporation system with these of the previously reported chemiluminescence gas diffusion-flow injection previously reported is also described.
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PMID:Pervaporation-flow injection with chemiluminescence detection for determination of iodide in multivitamin tablets. 1907 65

The intent of this work was to gain further insight on the fungus-assisted degradation/solubilization of humic acid and the related changes in metal-binding profiles. In the experimental design, Aldrich reagent humic acid (HA) or HA enriched with Cu, Pb, and Ni (HA(Me)) was added to Fusarium oxysporum f. sp. lycopersici cultures in vitro. The cultures were supplied by different carbon- and nitrogen-containing nutrients (glucose, Glc, or glutamate, Glu and ammonium, NH4+, or nitrate, NO3-, ions, respectively) in order to examine their possible effect on HA and HA(Me) decomposition. During the first 48 h of fungus growth, gradual acidification to pH 2 was observed in medium containing Glc + NH4+, while for other cultures, alkalinization to pH 9 occurred and then, the above conditions were stable up to at least 200 h. Size exclusion chromatography (SEC) with UV/Vis detection showed progressive degradation and solubilization of both HA and HA(Me) with the increasing time of fungus growth. However, the molecular mass distributions of HA-related soluble species were different in the presence of metals (HA(Me)) as referred to HA and were also influenced by the composition of growth medium. The solubilization of Pb, Cu, and Ni and their association with HA molecular mass fractions were studied using inductively coupled plasma mass spectrometry (ICP-MS) detection. Under acidic conditions, relatively high concentrations of low-molecular-mass metallic species were found in culture supernatants, while in alkaline media, metal solubilization was generally poorer. In contrast to low pH culture, SEC-ICP-MS results obtained in alkaline supernatants indicated metal binding to degradation products of humic substances of MM > 5 kDa. In summary, the results of this study suggest that fungus-assisted degradation of HA and HA(Me) might be controlled using appropriate N- and C- sources required for fungus growth, which in turn would affect molecular mass distribution of soluble metallic species thus potentially influencing their actual bioaccessibility.
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PMID:Effect of Fusarium oxysporum f. sp. lycopersici on the degradation of humic acid associated with Cu, Pb, and Ni: an in vitro study. 1954 55

A Working Ring Test (WRT) was organised in the framework of the EU Regulation (EC) No 2152/2003 ("Forest Focus") and of the UN/ECE Program "ICP Forests" to evaluate the overall performance of the laboratories monitoring atmospheric deposition and soil solution in European Forests. Seven natural samples of atmospheric deposition and soil solutions and 5 synthetic solutions were distributed to 52 laboratories, which analysed them using their routine methods. Thirteen variables are considered in this paper: pH, conductivity, calcium, magnesium, sodium, potassium, ammonium, sulfate, nitrate, chloride, total alkalinity, total dissolved nitrogen and dissolved organic carbon. For each variable, the relative standard deviation of the results was evaluated, after outlier rejection, to estimate the analytical error of the measurements. The results are evaluated considering the Quality Assurance/Quality Control (QA/QC) procedure included in the ICP Forests monitoring manual: consistency check of the data and use of control charts and internal standards. A Data Quality Objective (DQO) is defined for each of the variables and the number of data meeting the DQOs are discussed in relation to the QA/QC procedures adopted. Although 38% of the results did not meet the DQO, the laboratories adopting QA/QC procedures produced a larger proportion of results meeting the objective and a consistent part of the outliers could be detected a posteriori checking analyses consistence.
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PMID:Influence of QA/QC procedures on non-sampling error in deposition monitoring in forests. 1955 24

The paper describes a research of possible application of UTEVA and TRU resins and anion exchanger AMBERLITE CG-400 in nitrate form for the isolation of uranium and thorium from natural samples. The results of determination of distribution coefficient have shown that uranium and thorium bind on TRU and UTEVA resins from the solutions of nitric and hydrochloric acids, and binding strength increases proportionally to increase the concentration of acids. Uranium and thorium bind rather strongly to TRU resin from the nitric acid in concentration ranging from 0.5 to 5 mol L(-1), while large quantities of other ions present in the sample do not influence on the binding strength. Due to the difference in binding strength in HCl and HNO(3) respectively, uranium and thorium can be easily separated from each other on the columns filled with TRU resin. Furthermore, thorium binds to anion exchanger in nitrate form from alcohol solutions of nitric acid very strongly, while uranium does not, so they can be easily separated. Based on these results, we have created the procedures of preconcentration and separation of uranium and thorium from the soil, drinking water and seawater samples by using TRU and UTEVA resins and strong base anion exchangers in nitrate form. In one of the procedures, uranium and thorium bind directly from the samples of drinking water and seawater on the column filled with TRU resin from 0.5 mol L(-1) HNO(3) in a water sample. After binding, thorium is separated from uranium with 0.5 mol L(-1) HCl, and uranium is eluted with deionised water. By applying the described procedure, it is possible to achieve the concentration factor of over 1000 for the column filled with 1g of resin and splashed with 2L of the sample. Spectrophotometric determination with Arsenazo III, with this concentration factor results in detection limits below 1 microg L(-1) for uranium and thorium. In the second procedure, uranium and thorium are isolated from the soil samples with TRU resin, while they are separated from each other on the column filled with anion exchanger in alcohol solutions. Anion exchanger combined with alcohol solutions enables isolation of thorium from soil samples and its separation from a wide range of elements, as well as spectrophotometric determination, ICP-MS determination, and other determination techniques.
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PMID:Determination of uranium and thorium in complex samples using chromatographic separation, ICP-MS and spectrophotometric detection. 1978 36

Arsenic volatilization in the environment is thought to be an important pathway for transfer from terrestrial pools to the atmosphere. However, this phenomenon is not well characterized due to inherent sampling issues in trapping, quantifying and qualifying these arsine gases; including arsine (AsH(3)), monomethyl arsine (MeAsH(2)), dimethyl arsine (Me(2)AsH) and trimethyl arsine (TMAs). To quantify and qualify arsines in air we developed a novel technique based on silver nitrate impregnated silica gel filled tubes. The method was characterized by measuring the recovery of trapped arsines after elution of this chemo-trap with hot boiling diluted nitric acid. Results from three separate experiments, measured by ICP-MS, showed that the method is reproducible and quantitative. Arsine species recovery ranged from 80.1 to 95.6%, with limit of detection as low as 3.8 ng per chemo-trap tube. Moreover, HPLC-ICP-MS analysis of hot boiling water eluted traps showed that the corresponding oxy ions of the arsines were formed with the As-C bonds of the molecule intact, hence, allowing qualification of trapped arsine species. A microcosm study examining volatile arsenic evolution from field contaminated Bangladeshi paddy soils (24.2 mg/kg arsenic) was used to show the application of silver nitrate chemo-trapping approach. Traps were placed on the inlet and the outlet of microcosms containing the soils that were either (cattle derived) manured or not, or flooded or not, in a factorial design. The headspace was purged with air at a flow rate of 12 mL/min. Results showed that as much as 320 ng of arsenic (0.014% of total soil content) could be emitted in a 3 week period for manured and flooded soils and that TMAs was the dominant species evolved, with lesser quantities of Me(2)AsH. No volatile arsenic evolution was observed for nonmanured treatments, and arsine release from the nonflooded, manured treatment was much less than the flooded treatment.
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PMID:Quantitative and qualitative trapping of arsines deployed to assess loss of volatile arsenic from paddy soil. 1992 55

Stabilization/solidification (S/S) is one of the most employed techniques for treating liquid wastes containing heavy metals. Magnesium potassium phosphate cements have been used in recent years as stabilizing agents with positive results. However, little information is available about the retention of the metals by magnesium potassium phosphate cements matrices with the exception of the results of compliance tests. In this work, several pastes were prepared by reaction between low grade MgO and KH(2)PO(4) in the presence of different heavy metal nitrate solutions (containing Cd(II), Cr(III), Cu(II), Ni(II), Pb(II) or Zn(II)). In all cases, the initial metal content of the dissolution was 25 g dm(-3) and the oxide-phosphate ratio of the pastes was (50:50) in weight. Four different leaching tests were conducted on magnesium potassium phosphate cement pastes: simple batch test (EN 12457-2), equilibrium leaching test, availability test (NEN 7371) and acid neutralization capacity test (ANC). The metal leachate concentration was determined by means of ICP-MS. The stabilization of metals was successful in all cases, although the immobilizing system shows a better behaviour for Pb(II) and Cr(III) under acidic or neutral conditions.
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PMID:Leaching behaviour of magnesium phosphate cements containing high quantities of heavy metals. 1993 57

Long term trend analysis of bulk precipitation, throughfall and soil solution elemental fluxes from 12 years monitoring at 10 ICP Level II forest sites in the UK reveal coherent national chemical trends indicating recovery from sulphur deposition and acidification. Soil solution pH increased and sulphate and aluminium decreased at most sites. Trends in nitrogen were variable and dependant on its form. Dissolved organic nitrogen increased in bulk precipitation, throughfall and soil solution at most sites. Nitrate in soil solution declined at sites receiving high nitrogen deposition. Increase in soil dissolved organic carbon was detected - a response to pollution recovery, changes in soil temperature and/or increased microbial activity. An increase of sodium and chloride was evident - a possible result of more frequent storm events at exposed sites. The intensive and integrated nature of monitoring enables the relationships between climate/pollutant exposure and chemical/biological response in forestry to be explored.
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PMID:Chemical fluxes in time through forest ecosystems in the UK - soil response to pollution recovery. 1996 1

Volatile arsenic compounds in natural gas, existing in the form of trimethylarsine (TMAs), have been determined using gas cryo-trapping gas chromatography coupled to inductively coupled plasma-mass spectrometry (CT-GC-ICP-MS). The results from a number of different gas wells revealed a huge concentration spread ranging from below the detection limit of 0.2 up to 1800 microg/m(3) TMAs (as As) in the gas. Due to the toxicity and corrosive nature of these arsines, they need near real time monitoring via a method that can easily be implemented on site, i.e. during gas exploitation. Here, we introduce a novel method which utilises silver nitrate impregnated silica gel tubes for quantitative chemotrapping of trimethylarsine (TMAs) from a natural gas matrix. Subsequent elution with hot nitric acid followed by online photo-oxidation hydride generation atomic fluorescence spectrometry (HG-AFS) is used for the determination of TMAs gas standards in nitrogen and natural gas samples, respectively. The chemotrapping method was validated using CT-GC-ICP-MS as a reference method. The recovery of arsenic from nitrogen or natural gas matrix ranged from 85 to 113% for a range of 20 to 2000 ng As. Trapping efficiency was >98%, from the methods LOD of 20 ng to 4.8 microg (absolute amount As) with sample sizes of 0.02 and 2 L gas. Method performance was established by comparing the results obtained for eight natural gas samples containing between 1 and 140 microg As/m(3) with those achieved by the reference method (CT-GC-ICP-MS).
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PMID:Chemotrapping-atomic fluorescence spectrometric method as a field method for volatile arsenic in natural gas. 2002 20

The effects of hydraulic retention time (HRT, 7 h, 13.5 h and 18 h) and pH (7.5 and 8.0) on the denitrification performance and the extent of inorganic precipitation, in a H2-driven non-porous membrane biofilm reactor for autotrophic denitrification were investigated. The membrane was cleaned periodically to evaluate the solids contents generated in the system and identify the precipitants. The reactor that was operated under the longer HRT contained more inert solids than when operated under shorter HRT, and showed lower specific nitrate removal rates, even though the generation of volatile solids was almost identical in all tested cases. A lower pH level at shorter HRT, due to higher influent dilution rates, resulted in improved denitrification rates. However, aggressive pH control, by adding additional phosphate buffer, was not beneficial because of extensive precipitation of up to 76% of total solids. Inorganic precipitation was strongly and linearly related to the denitrification performance, indicating the inhibitory effect of inorganic precipitants on the transfer of gases or substrates in a membrane biofilm reactor. The sloughed-off solids from the reactors were characterized by ICP analysis and revealed an abundance of various calcium-related precipitants, which were found to be responsible for the increase in the inert solids content. Calcium phosphate precipitation was identified as the major reason for the inhibition of system performance in this study. Operation under long HRT increases the potential to generate substantial amounts of diverse, inhibitory inorganic precipitants.
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PMID:Inorganic precipitation during autotrophic denitrification under various operating conditions. 2008 14


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