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The determination of lead in tinplate by ICP-AES was presented in this paper. The tinplate samples were pretreated with NaOH-H2O2 for dissolving tin and lead,and the spectral interferences from iron could thus be avoided. The lead content in the sample was determined in the range of 0.14-0.38 microg/cm2. The recovery and the relative standard deviation (RSD) were in the ranges of 96.1%-103.2% and 2.6%-3.8%, respectively. The method was simple,rapid and efficient.
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PMID:[Determination of lead in tinplate by ICP-AES]. 1581 66

Hazardous shipyard wastewater is a worldwide problem, arising from ship repair. In this study an experimental programme was undertaken to establish the suitability of dolomite and dolomitic sorbent materials to remove contaminants from wastewater arising from a commercial shipyard. Experimental data indicate that dolomite and dolomitic sorbents have the ability to significantly reduce the COD concentration of the shipyard effluent (98% reduction). The data gained from trials at a shipyard indicated that the dolomite treatment process could be undertaken in a 8000 L pilot scale reaction vessel. Analysis of the wastewater using ICP-MS during the pilot trial indicated that the dolomite significantly reduced the concentrations of metallic impurities. The concentration of Sn ions, which is indicative of organo-tin complexes commonly found in shipyard wastewater, was reduced by 80% from its initial concentration in the pilot trial. The mechanism for the removal process using dolomite has been ascribed to a metal complexation/sorption process.
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PMID:Treatment of hazardous shipyard wastewater using dolomitic sorbents. 1595 26

An accurate and sensitive multi-species species-specific isotope dilution GC-ICP-MS method was developed for the simultaneous determination of trimethyllead (Me3Pb+), monomethylmercury (MeHg+) and the three butyltin species Bu3Sn+, Bu2Sn2+, and BuSn3+ in biological samples. The method was validated by three biological reference materials (CRM 477, mussel tissue certified for butyltins; CRM 463, tuna fish certified for MeHg+; DORM 2, dogfish muscle certified for MeHg+). Under certain conditions, and with minor modifications of the sample pretreatment procedure, this method could also be transferred to environmental samples such as sediments, as demonstrated by analyzing sediment reference material BCR 646 (freshwater sediment, certified for butyltins). The detection limits of the multi-species GC-ICP-IDMS method for biological samples were 1.4 ng g(-1) for MeHg+, 0.06 ng g(-1) for Me3Pb+, 0.3 ng g(-1) for BuSn3+ and Bu3Sn+, and 1.2 ng g(-1) for Bu2Sn2+. Because of the high relevance of these heavy metal alkyl species to the quality assurance of seafood, the method was also applied to corresponding samples purchased from a supermarket. The methylated lead fraction in these samples, correlated to total lead, varied over a broad range (from 0.01% to 7.6%). On the other hand, the MeHg+ fraction was much higher, normally in the range of 80-100%. Considering that we may expect tighter legislative limitations on MeHg+ levels in seafood in the future, we found the highest methylmercury contents (up to 10.6 microg g(-1)) in two shark samples, an animal which is at the end of the marine food chain, whereas MeHg+ contents of less than 0.2 microg g(-1) were found in most other seafood samples; these results correlate with the idea that MeHg+ is usually of biological origin in the marine environment. The concentration of butyltins and the fraction of the total tin content that is from butyltins strongly depend on possible contamination, due to the exclusively anthropogenic character of these compounds. A broad variation in the butylated tin fraction (in the range of <0.3-49%) was therefore observed in different seafood samples. Corresponding isotope-labeled spike compounds (except for trimethyllead) are commercially available for all of these compounds, and since these can be used in the multi-species species-specific GC-ICP-IDMS method developed here, this technique shows great potential for routine analysis in the future.
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PMID:Simultaneous multi-species determination of trimethyllead, monomethylmercury and three butyltin compounds by species-specific isotope dilution GC-ICP-MS in biological samples. 1613 5

For the first time we are able to report the identification and quantification of several unexpected alkylated tin compounds such as dimethyldiethyltin, trimethylethyltin and propyltrimethyltin in European municipal waste deposits, by using GC-ICP-MS. Future studies will reveal whether their origin is from the degradation of butyl-, or octyltin compounds or simply products of de novo synthesis within the landfill environment.
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PMID:Municipal landfills exhale newly formed organotins. 1625 54

Methylated species of antimony, arsenic and tin were examined in urban soils of the Ruhr basin, near the cities of Duisburg and Essen, Germany. The main aim of this study was to investigate the occurrence of mono-, di- and trimethylated species of these elements in urban soils. The influence of historical and present land use upon the species content was examined. The distribution of inorganic As, Sb and Sn and their methylated species along the profile depth was investigated. As, Sb and Sn speciation was performed by pH-gradient hydride generation purge and trap gas chromatography, followed by inductively-coupled plasma mass spectrometry (HG-PT-GC/ICP-MS). Species' structures were confirmed by GC-EI/MS-ICP-MS. Monomethylated Sb and As were the dominant species detected: the concentration of these metal(loid) species varied between <0.07-56 microg kg(-1) per dry mass. All dimethylated species and monomethyltin concentrations were between <0.01-7.6 microg kg(-1) per dry mass, and for the trimethylated species of all examined elements, concentrations between <0.001-0.63 microg kg(-1) per dry mass were detected. The highest organometal(loid) concentrations were observed in agricultural soils and garden soils; lower concentrations were found in the soils of abandoned industrial sites (wasteland, primary forest and grassland) and a flood plain soil of the Rhine. This result can be ascribed to both the cultivation and the increased biological activity of the agricultural soils, and the generally higher contamination, the disturbed structure and the artificial substrates (deposits from industrial sources) of the abandoned industrial soils. Due to periodical sedimentation, the flood plain profile was the only one where no depth dependence of organometal(loid) species concentration was detected. The other soil profiles showed a decrease of species content with increasing depth; this was particularly noticeable in soils with a clear change from a horizon with an organic character towards a mineral horizon, i.e. decreasing vitality from profile top to bottom. It is not as yet clear whether the organometal(loid) species are formed in the mineral horizons of the profiles or whether they are displaced from the organic, biologically-active horizons towards the mineral horizons. Field studies revealed that soil parameters like pH, water content or temperature did not correlate significantly with the degree of biomethylation observed. In contrast to the lower in vitro biomethylation efficiency of Sb vs. As in microbial incubations, we consistently detected higher proportions of transformed Sb compounds in situ in soil samples. These data may indicate a need to re-examine the currently accepted model of Sb biogeochemical cycling in the real environment.
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PMID:Methylated arsenic, antimony and tin species in soils. 1630 70

A survey of 12 metals including lead (Pb), copper (Cu), cadmium (Cd), mercury (Hg), arsenic (As) and platinum (Pt) was carried out using ICP-MS in 34 samples of wild fungi and 48 samples of wild blackberries collected from sites across the UK. On a fresh weight basis (mg/kg) levels of Pb were in the range 0.003-5.990, Cu 0.596-34.800, Cd<0.001-19.6, Hg<0.001-4.150, As 0.001-0.972 and Pt (microg/kg) 0.006-0.200, with higher concentrations found in fungi than in blackberries. The results of the survey showed that the concentrations of the metals were consistent with previous studies, where available. Concentrations in wild fungi of Pt, tin (Sn), and titanium (Ti) were significantly higher at urban sites than at rural sites. Urban blackberries had significantly higher levels of Pb, Ti, and Cd than rural ones, but lower levels of manganese (Mn). Pb, Ti and Sn concentrations were significantly higher in blackberries sampled near main roads rather than in rural areas.
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PMID:Multi-element survey of wild edible fungi and blackberries in the UK. 1644 56

Personal and area samples for airborne lead were taken at a lead mine concentrator mill, and at a lead-acid battery recycler. Lead is mined as its sulfidic ore, galena, which is often associated with zinc and silver. The ore typically is concentrated, and partially separated, on site by crushing and differential froth flotation of the ore minerals before being sent to a primary smelter. Besides lead, zinc and iron are also present in the airborne dusts, together with insignificant levels of copper and silver, and, in one area, manganese. The disposal of used lead-acid batteries presents environmental issues, and is also a waste of recoverable materials. Recycling operations allow for the recovery of lead, which can then be sold back to battery manufacturers to form a closed loop. At the recycling facility lead is the chief airborne metal, together with minor antimony and tin, but several other metals are generally present in much smaller quantities, including copper, chromium, manganese and cadmium. Samplers used in these studies included the closed-face 37 mm filter cassette (the current US standard method for lead sampling), the 37 mm GSP or "cone" sampler, the 25 mm Institute of Occupational Medicine (IOM) inhalable sampler, the 25 mm Button sampler, and the open-face 25 mm cassette. Mixed cellulose-ester filters were used in all samplers. The filters were analyzed after sampling for their content of the various metals, particularly lead, that could be analyzed by the specific portable X-ray fluorescence (XRF) analyzer under study, and then were extracted with acid and analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES). The 25 mm filters were analyzed using a single XRF reading, while three readings on different parts of the filter were taken from the 37 mm filters. For lead at the mine concentrate mill, all five samplers gave good correlations (r2 > 0.96) between the two analytical methods over the entire range of found lead mass, which encompassed the permissible exposure limit of 150 mg m(-3) enforced in the USA by the Mine Safety and Health Administration (MSHA). Linear regression on the results from most samplers gave almost 1 ratio 1 correlations without additional correction, indicating an absence of matrix effects from the presence of iron and zinc in the samples. An approximately 10% negative bias was found for the slope of the Button sampler regression, in line with other studies, but it did not significantly affect the accuracy as all XRF results from this sampler were within 20% of the corresponding ICP values. As in previous studies, the best results were obtained with the GSP sampler using the average of three readings, with all XRF results within 20% of the corresponding ICP values and a slope close to 1 (0.99). Greater than 95% of XRF results were within 20% of the corresponding ICP values for the closed-face 37 mm cassette using the OSHA algorithm, and the IOM sampler using a sample area of 3.46 cm2. As in previous studies, considerable material was found on the interior walls of all samplers that possess an internal surface for deposition, at approximately the same proportion for all samplers. At the lead-acid battery recycler all five samplers in their optimal configurations gave good correlations (r2 > 0.92) between the two analytical methods over the entire range of found lead mass, which included the permissible exposure limit enforced in the USA by the Occupational Safety and Health Administration (OSHA). Linear regression on the results from most samplers gave almost 1 ratio 1 correlations (except for the Button sampler), indicating an absence of matrix effects from the presence of the smaller quantities of the other metals in the samples. A negative bias was found for the slope of the button sampler regression, in line with other studies. Even though very high concentrations of lead were encountered (up to almost 6 mg m(-3)) no saturation of the detector was observed. Most samplers performed well, with >90% of XRF results within +/- 25% of the corresponding ICP results for the optimum configurations. The OSHA algorithm for the CFC worked best without including the back-up pad with the filter.
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PMID:A comparison of portable XRF and ICP-OES analysis for lead on air filter samples from a lead ore concentrator mill and a lead-acid battery recycler. 1652 23

A method was developed for high-throughput determinations of 7 elements in food samples, namely antimony (Sb), arsenic (As), cadmium (Cd), chromium (Cr), lead (Pb), mercury (Hg), and tin (Sn). The samples were digested by closed-vessel microwave-assisted digestion using concentrated nitric acid (HNO3) as the medium, followed by microwave- assisted evaporation to concentrate the sample solutions before dilution to the desired volume. The microwave-assisted evaporation procedure effectively reduced the final acid concentration to around 8% before analysis by inductively coupled plasma-mass spectrometry (ICP-MS). This reduction allows determination by ICP-MS to proceed without further sample dilution, which would affect the detection limit. The method was validated, and method recoveries for As, Cd, Cr, Pb, and Hg were within the certified ranges of the chosen certified reference materials. Recoveries of the 7 elements from spiked samples ranged from 93.1 to 103.6%. The standard uncertainties of precision for the 7 elements were between 3.1 and 4.3%. Interlaboratory comparison studies for As, Cd, and Pb gave z-scores ranging from -0.2 to 0.3.
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PMID:High-throughput determination of seven trace elements in food samples by inductively coupled plasma-mass spectrometry. 1664 Feb 96

'Metal ash' presents a waste disposal problem in most of the developing countries as the industries employ obsolete technologies. In this paper we describe analysis of tin ash, zinc ash and aluminium ash by means of optical methods, such as X-ray diffraction (XRD), inductively coupled plasma mass spectrometry (ICP-MS), electron probe micro analysis (EPMA), scanning electron microscopy (SEM) and chemical methods. The results of tin ash obtained by XRD method matched well with the cassiterite, a naturally occurring mineral of tin. ICP-MS studies reveal the presence of a large number of tracer metals, which may cause pollution by tertiary dispersion and this aspect is discussed. Conversely, the data generated by chemical methods are limited. However, the methods are simple and cost-effective. Then, they can easily be adopted by low-budget industries. Simple and cost-effective process to recover tin from tin ash is described. It is based on heating tin ash with sodium cyanide to about 900 degrees C to separate tin component from the metal ash. The process recovers good quality tin and offers a very high yield. The process can be scaled up to small pilot plant.
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PMID:Optical and chemical methods of metal ash analysis and tin recovery. 1705 54

Among the "traditional" hydride-forming elements, lead is probably the most difficult, and its determination in this form has rarely been reported in the literature. In this paper a simple and rapid method, axial-view inductively-coupled plasma optical-emission spectrometry using on-line hydride generation (HG-ICP-OES) from samples prepared as slurry, is proposed for determination of lead in environmental samples. The samples (20-50 mg, particle size <or=120 microm) were treated with 1 mL aqua regia in a 40-kHz ultrasonic bath for 60 min. The slurry was diluted to a final volume of 50 mL with a 10% m/v solution of (NH(4))(2)S(2)O(8). The concentrations of NaBH(4), tartaric acid, and (NH(4))(2)S(2)O(8), used for on-line plumbane generation were optimized by means of a complete factorial analysis applied to an aqueous standard solution and to the slurry of a sediment certified reference material (CRM). External calibration against aqueous standards in the concentration range 10-100 microg L(-1) was used for analysis of six CRM--three marine sediments, one river sediment, and two sewage sludges. Analysis of the filtered slurry showed that Pb was only partially extracted into the liquid phase. Several major concomitants tested did not affect the Pb signal. The detection limit (3s, n = 10) for 20 mg sample in a final volume of 50 mL was 5.0 microg g(-1). Tin was the only other hydride-forming analyte that could be determined satisfactorily with Pb; for tin the detection limit was 1.0 microg g(-1). The values obtained for Pb and Sn were not significantly different from the certified concentrations, according to the t-test at the 95% confidence level. Nine river sediments collected locally were also analyzed and the concentrations were in agreement with results obtained after total digestion.
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PMID:Determination of lead in sediments and sewage sludge by on-line hydride-generation axial-view inductively-coupled plasma optical-emission spectrometry using slurry sampling. 1724 88


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