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Inductively coupled plasma atomic emission spectrometry (ICP-AES) is rapidly overtaking atomic absorption spectrometry (AAS) as the method of choice for the determination of toxic metals in workplace air. However, the few ICP-AES methods that have been published are not well characterised in terms of the effectiveness of the sample dissolution procedures described and their validation status. The International Standards Organization (ISO) is currently engaged in developing ISO 15202, which will describe a generic method for the determination of metals and metalloids in airborne particulate matter by ICP-AES. One part of the proposed standard deals with dissolution procedures. The ISO work has been supported by a project carried out in the authors' laboratory to identify, develop and validate sample dissolution procedures for inclusion in the proposed standard. This paper describes an interlaboratory comparison carried out to assess the performance of selected procedures using samples of airborne particulate matter collected on filters with a multiport sampler. Five dissolution procedures were tested. These included an ultrasonic agitation procedure, two hot-plate procedures (based upon NIOSH 7300 and OSHA ID 125G) and two microwave-assisted procedures (based upon EPA 3052). It was shown that the dissolution procedures selected for use in the trial and used internally at HSL generally gave equivalent performance. As expected, a wider spread of results was obtained by participants in the trial. More specifically, there exists some reservation regarding the ability of the ultrasonic and hot-plate procedures to attack fully on a consistent basis some resistant materials, e.g., chromium containing particulate matter. Above all, the trial demonstrated the usefulness of microwave-assisted dissolution procedures in a modern laboratory.
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PMID:Development of an international standard for the determination of metals and metalloids in workplace air using ICP-AES: evaluation of sample dissolution procedures through an interlaboratory trial. 1152 75

Inductively coupled plasma mass spectrometry (ICP/MS) with direct injection nebulization (DIN) was used to evaluate novel impinger solution compositions capable of capturing elemental mercury (Hg0) in EPA Method 5 type sampling. An iodine based impinger solution proved to be very efficient for Hg0 capture and was amenable to direct analysis by DIN-ICP/MS. Hg0 capture efficiency using aqueous iodine (I3-) was comparable to Hg0 capture using acidified potassium permanganate impinger solutions which were analyzed by cold vapor atomic absorption spectrometry (CVAAS), with greater than 98% capture of Hg0 in the first oxidizing impinger. Using DIN-ICP/MS, it was demonstrated for the first time that iodine can be generated just prior to impinger sampling for efficiently oxidizing Hg0 and retaining it in solution as HgI4(2-). Due to the increased interest in Hg speciation from combustion sources and the potential for using DIN-ICP/MS for multiple metals analyses, an impinger sampling train for gaseous Hg speciation and multiple metals analyses using DIN-ICP/MS analyses is presented. The unique feature of such a sampling train is that each impinger solution in the series is amenable to direct analysis by DIN-ICP/MS. A bituminous coal was combusted in a bench scale coal system, and gaseous Hg species (oxidized and elemental) were determined using the proposed impinger train. The DIN-ICP/MS instrumental detection limit was 0.003 ppb, and MDLs ranged from 0.007 to 0.116 microg/L (ppb) in a variety of impinger solutions used for Hg capture.
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PMID:The development of iodine based impinger solutions for the efficient capture of Hg0 using direct injection nebulization-inductively coupled plasma mass spectrometry analysis. 1178 57

The objective of the work carried out was to recommend protocols for the collection, filtration (0.45 microm) and preservation of surface water samples for the subsequent determination of total 'dissolved' Hg. Cold vapour (CV) ICP-MS was employed to determine Hg; samples were acidified to a strength of 4 mol l(-1) HCl and 1% NaBH4 was used as the reducing agent in-line. Four types of 125 ml bottles were studied (Teflon, fluorinated ethene propene copolymer, FEP; high density polyethylene, HDPE; polyethylene terephthalate copolyester, PET; polypropylene, PP), together with three cleaning methods (EPA Methods 1631, 1638 and a rinse with reverse osmosis deionised water, 'MilliQ'). The transmission properties of the four materials were also studied to evaluate the potential for contamination from atmospheric Hg0. Results of this bottle study (n = 195), all below the detection limit of 0.5 ng l(-1), indicate that the bottles of choice, from an economic and time-saving perspective, are HDPE and PP, the latter being preferable if the sample is to be stored in a contaminated atmosphere. The bottles would be used on a once-only basis, negating the need for labourious and costly cleaning on repeat use. A simple rinse with MilliQ water would suffice prior to use. Twelve 0.45 microm filter systems (mostly Millipore and Gelman) were studied for (a) their potential Hg contamination properties and (b) their retention of Hg, possibly in colloidal form, during filtration. Ottawa River water, spiked at 50 ng l(-1) Hg, was used as a control sample. Again blank values were all negative, indicating contamination was not a concern but different recoveries of Hg were obtained across the different systems. The optimum systems to use, in that they provided maximum recovery (ca 80%) of Hg, are the Millipore Sterivex capsule and the Millipore Millex disc, both based on the hydrophilic Durapore membrane. The lowest recoveries (23-36%) were found with the Gelman AquaPrep systems and the Millipore HN nylon filter. Four control samples, Ottawa, Rideau and Gatineau Rivers, and a MilliQ blank, were used to study three preservation approaches, in the media: 0.5% BrCl, 2% HCl and 0.04% K2Cr2O7 in 1% HNO3. Mercury was stable for 28 days in a medium of 0.5% BrCl in all four samples but the other two media showed a loss of up to ca 20% Hg over this time frame, the loss being sample and time dependent. This may be a species transformation which is not detected by CV-ICP-MS from an HCl medium but this requires further investigation. Mercury was stable over the 28 days in the spiked blank MilliQ sample for all three preservation media.
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PMID:Sample collection, filtration and preservation protocols for the determination of 'total dissolved' mercury in waters. 1208 Oct 47

Regulating arsenic species in drinking waters is a reasonable objective, since the various species have different toxicological impacts. However, developing robust and sensitive speciation methods is mandatory prior to any such regulations. Numerous arsenic speciation publications exist, but the question of robustness or ruggedness for a regulatory method has not been fully explored. The present work illustrates the use of anion exchange chromatography coupled to ICP-MS with a commercially available "speciation kit" option. The mobile phase containing 2 mM NaH(2)PO(4) and 0.2 mM EDTA at pH 6 allowed adequate separation of four As species (As(III), As(V), MMAA, DMAA) in less than 10 min. The analytical performance characteristics studied, including method detection limits (lower than 100 ng L(-1) for all the species evaluated), proved the suitability of the method to fulfill the current regulation. Other parameters evaluated such as laboratory fortified blanks, spiked recoveries, and reproducibility over a certain period of time produced adequate results. The samples analyzed were taken from water utilities in different areas of the United States and were provided by the U.S. EPA. The data suggests the speciation setup performs to U.S. EPA specifications but sample treatment and chemistry are also important factors for achieving good recoveries for samples spiked with As(III) as arsenite and As(V) as arsenate.
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PMID:A study of method robustness for arsenic speciation in drinking water samples by anion exchange HPLC-ICP-MS. 1218 80

Eighteen Dutch soils were extracted in aqueous solutions at varying pH. Extracts were analyzed for Cd, Cu, Ni, Pb and Zn by ICP-AES. Extract dissolved organic carbon (DOC) was also concentrated onto a macroreticular resin and fractionation into three operationally defined fractions: hydrophilic acids (Hyd), humic acids (HA) and fulvic acids (FA). In this manner, change in absolute solution concentration and relative percentage for each fraction could be calculated as a function of extraction equilibrium pH. The soils were also analyzed for solid phase total organic carbon and total recoverable metals (EPA Method 3051). Partitioning coefficients were calculated for the metals and organic carbon (OC) based on solid phase concentrations (less the metal or OC removed by the extraction) divided by solution concentrations. Cu and Pb concentrations in solution as a function of extract equilibrium pH are greatest at low and high pH resulting in parabolic desorption/dissolution curves. While processes such as proton competition and proton promoted dissolution can account for high solution metal concentrations at low pH, these processes cannot account for higher Cu and Pb concentrations at high pH. DOC increases with increasing pH, concurrently with the increase in Cu and Pb solution concentrations. While the absolute concentrations of FA and HA generally increase with increasing pH, the relative proportional increase is greatest for HA . Variation in HA concentrations spans three orders of magnitude while FA concentrations vary an order of magnitude over the pH range examined. Correlation analysis strongly suggests that HA plays a major role in increasing the concentration of solution Cu and Pb with increasing pH in the 18 soils studied. The percentage of the OC that was due to FA was nearly constant over a wide pH range although the FA concentration increased with increasing pH and its concentration was greater than that of the HA fraction at lower pH values (pH = 3-5). Thus, in more acidic environments, FA may play a larger role than HA in governing organo-metallic interactions. For Cd, Ni, and Zn, the desorption/dissolution pattern shows high metal solution concentrations at low pH with slight increases in solution concentrations at extremely high pH values (pH>10). The results presented here suggest that the effects of dissolved organic carbon on the mobilization of Cd, Ni, and Zn may only occur in systems governed by very high pH. At high pH, it is difficult to distinguish in this study whether the slightly increased solution-phase concentrations of these cations is due to DOC or hydrolysis reactions. These high pH environments would rarely occur in natural settings.
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PMID:Correlation of the partitioning of dissolved organic matter fractions with the desorption of Cd, Cu, Ni, Pb and Zn from 18 Dutch soils. 1243 90

Inductively coupled plasma-mass spectrometry (ICP-MS) method EPA 200.8 is gradually finding acceptance as an alternative to uranium analysis. A comparison of the ICP-MS with the accepted radiochemical method EPA 908.0 has been carried out based on data from laboratory control standards, national proficiency test samples, and environmental and drinking water samples from the State of Utah. The method detection limit (MDL) for ICP-MS was determined to be 0.017 microg/L or (0.011 pCi/L), and the minimum reporting limit (MRL) was 0.17 microg/L (MDL x 10) or (0.11 pCi/L). The minimum reporting limit for radiochemical 908.0 method is 1 pCi/L. Our spiked matrix recoveries, spiked blank samples, and reference materials deviate only a few percentage from the listed true values. Results demonstrate that the ICP-MS is a superior analytical tool for the determination of uranium in drinking and environmental waters at concentrations required by the United States Environmental Protection Agency.
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PMID:Comparison of inductively coupled plasma-mass spectrometry and radiochemical techniques for total uranium in environmental water samples. 1252 Nov 66

Coal as well as fuel oil combustion generates emissions of potentially toxic trace pollutants including organic and inorganic chemical compounds besides major pollutants. A study on As, Cd, Co, Cr, Cu, Hg, Fe, Mn, Ni, Pb, Se, and Zn emissions from a 220 MW coal-fired power plant equipped with a electrostatic precipitators (ESPs) and 6 MW oil fired-power plant was carried out, using stack monitoring kit, Envirotech APM 620, which is similar to EPA Method 29. Simultaneous sampling of coal, fuel oil, oil waste, bottom ash, fly ash, flue gases, and particles associated with the gas phase has been performed. This sampling method was used for trace metal sampling. The content of all these metals in coal, oil, oil waste, bottom ash, fly ash have been determined by XRF, whereas their contents in the flue gases, and particles associated with the gas phase has been analyzed with ICP-AES. The mass balances obtained for trace elements were satisfactory in case of fuel oil based power plant, whereas in case of coal fired power plant, the mass balance for all the trace elements were below 50% except for the As, Se, and Hg. The enrichment factors for all trace metals was <1 in both cases. The above sampling method is moderately adequate method for trace element sampling in coal as well as oil fired power plants except for Hg. The results indicate that trace metals emissions were higher in coal-based power plant than the fuel oil-fired power plant.
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PMID:Evaluation of the emission characteristics of trace metals from coal and fuel oil fired power plants and their fate during combustion. 1591 50

The dietary intake of arsenic (As), cadmium (Cd), mercury (Hg), lead (Pb), hexachlorobenzene (HCB), polychlorinated naphthalenes (PCNs), polycyclic aromatic hydrocarbons (PAHs), polychlorinated diphenyl ethers (PCDEs), polybrominated diphenyl ethers (PBDEs), polychlorinated biphenyls (PCBs), and polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) by elite sportsmen and sportswomen of Catalonia, Spain, was assessed. In 2000, food samples were randomly acquired in various cities of Catalonia. Analysis of the above pollutants were determined according to the appropriate analytical techniques (ICP-MS, HRGC/HRMS, HPLC). In general terms, elite sportsmen and sportswomen showed a higher intake of Cd, Hg, Pb, HCB, PCNs, PCDD/Fs and PAHs than the general population, while it was lower for PCDEs (both sexes), and PCBs and PBDEs (women). According to the FAO/WHO provisional tolerable weekly intake (PTWI) for metals, the WHO tolerable daily intake (TDI) for HCB, and the US EPA's reference dose (RfD) for PAHs, the dietary intakes of environmental pollutants should not mean a potential toxic hazard. However, the WHO-TDI for PCDD/Fs and "dioxin-like" PCBs is exceeded in sportsmen. The current results indicate that the consumption of those food groups showing the highest contribution to the intake of these pollutants should be diminished. In relation to this, the reduction of the consumption of dairy products and cereals would be important.
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PMID:Health risks of dietary intake of environmental pollutants by elite sportsmen and sportswomen. 1600 1

An emissions study for arsenic was conducted at a 300 MW coal-fired plant equipped with an electrostatic precipitator. The input and output streams such as coal, slag, ESP ash, and flue gas containing the post-ESP particulates were collected. Gaseous arsenic was sampled using EPA method 29 and the arsenic concentrations in the samples were measured using inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). The mass balance recovery of arsenic estimated in this study was 87.2%. Arsenic concentration in stack gas was 2.5 microg/m3. Approximately 0.53% of the coal-derived arsenic was incorporated into slag, 84.6% of the arsenic was found on the fly ash collected by electrostatic precipitators, and 2.16% was found in the vapor phase. The relationship between arsenic concentration and ash particle size was also assessed, and arsenic is significantly concentrated in the small sized particles.
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PMID:[Characterization of arsenic emissions from a coal-fired power plant]. 1676 77

Waste water pollution in industrial areas is one of the most important environmental problems. Heavy metal pollution, especially chromium species in waste water sources from tannery affects our lives. Kocabas Stream is located in south-west Marmara region and Biga town is positioned in the sub basin on the stream. This water source functions as the water for irrigation in agriculture, drinking water for animals and for human use. Thus, this study is of great importance. Waste water pollution can affect all ecosystems and human health by directly or indirectly as in food chain. The concentration of heavy metals (Pb, Cd, Cu, Zn and Cr) were pre-analysed by ICP-AES method in water samples taken from sub-basin of Kocabas stream. In the results of these analyses, concentrations of the metals except chromium were founded at the limit value. But the total concentration of the Cr was found at high levels of between 0.0082 +/- 0.0001 and 5.7231 +/- 0.0921 mg l(-1) over the limit value (0.05 mg l(-1); WHO, EPA, TSE 266 and inland water quality classification) at sampling points very close to tannery factories. Also physicochemical and microbiological parameters of Kocabas Stream were determined. The effects of the experimental results on environment were investigated.
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PMID:Seasonal variation of some heavy metal pollution with environmental and microbiological parameters in sub-basin of Kocabas Stream (Biga, Canakkale, Turkey) by ICP-AES. 1734 11


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