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PubMed2000

The effect of oxidation and acidification on the speciation of heavy metals in sulfide-rich freshwater sediments using a sequential extraction procedure.

The speciation of metals in a contaminated, anoxic, sulfide-rich, freshwater sediment was determined experimentally, using a sequential extraction procedure based on the method of Tessier et al. Taking into account the advantages and disadvantages of sequential extractions, the applied methodology allowed the investigation of the influence of aeration and acidification on the distribution of various metals in the sediment. Aeration caused Zn and Cd to be released from sulfides. Carbonates were partly dissolved by the oxidation process, causing mobilisation of Ca. Fe became less mobile owing to a stronger binding to organic matter. The speciation of K, Al, Ni, Pb and Mn and to a lesser extent of Cu was not affected by aeration. As a result of acidification of the aerated sediment, Ca, Mn, Ni, Zn and Cd became more mobile owing to the dissolution of carbonates.

Environmental Monitoring↗
PubMed1992

Overview of analytical methods for elemental speciation.

This paper describes a selection of the major developments in the field of analytical methodology for elemental speciation over the period from January 1986 to December 1990. Methods for a number of elements will be highlighted. Judging by the number and diversity of published reports, there has been increasing interest and activity in the development of new and modified analytical methods. Further, it is very encouraging to observe the number of papers concerned with the accuracy and precision of such analytical methods, and with comparisons between two or more methods. Among electrochemical methods of analysis, anodic stripping voltammetry has provided an important basis for measurements of concentrations of labile metals in aqueous media. The fastest growing area of method development is the coupling of separation methods, usually chromatography, with a single- or multi-element detector. Most importantly, inductively coupled plasma mass spectrometry has recently been described as a very sensitive, multi-element detector. The success of a 'coupled' method is greatly dependent on a suitable interface. Several papers have been published recently describing useful interfaces. Chemical extraction procedures continue to occupy an important place. Applications of analytical elemental speciation methods have included environmental, biological, clinical and geological samples. A number of methods for elements most frequently studied will be discussed.

Animals↗
PubMed1995

Use of a model gut system to study the effects of dietary fibre and multivitamins on the speciation of copper, zinc and iron.

A gut model has been used to examine the speciation of three dietary available elements, Cu, Zn and Fe and their complexation with fibre and multivitamins. The analytical system consisted of an FI-ICP-MS interface for the determination of soluble and insoluble elemental distributions in samples. Solubility of elements was found to increase in the gut whereas in the intestinal tract they were seen to decrease. Experimental details are given for both the gut model and the speciation methodology used. The presence of fibre in the model had the greatest influence on elemental solubility in the intestinal tract whilst multivitamins have a less pronounced effect. The reduction in solubility of elements was most notable for zinc whilst the effect on iron and copper was notably less.

Copper↗
PubMed2001

The relevance of speciation in the remediation of soils and sediments contaminated by metallic elements--an overview and examples from Central Scotland, UK.

The environmental impact of metallic contaminants in soils and sediments is dependent both on the chemical speciation of the metal and the response of the matrix to biological and physicochemical conditions. These factors are responsible for the mobilisation of the metal from the solid into the aquatic phase and hence transport within the immediate vicinity, impacting on the rate of dispersal, dilution, uptake and transfer into living systems. The impact of changing environmental conditions on the contaminant inventory can be to enhance or moderate these phenomena, with subsequent consequences for the broader risk assessment of the contaminants. Remediation of metallic contaminants can only be brought about by their removal from the site or by establishing conditions which favour their retention in the solid phase. A wide range of in situ and ex situ approaches are available and a summary overview is presented. The examples show assessment at both the field and laboratory scale and demonstrate an equally wide range of success in achieving remediation targets. This can be attributed to limitations in ensuring that the desired conditions for the initial removal or immobilisation process are met and maintained over a suitable period of time. Three areas are reviewed which include: the transport and release of metallic contaminants in estuarine sediments and the assessment of their potential to impact on biota; terrestrial contamination systems involving the release of chromium from waste ore contaminating urban environments; the response of metal-contaminated wastes to changing environmental conditions and the impact of natural bioremediation. The focus of the discussion is to highlight the generation of reliable speciation information and the problems associated with impact and risk assessment. Particular issues of concern are the laboratory to field scale evaluation of contaminant behaviour and the approach used to assess the reliability of remediation options. In conclusion, part of a recent initiative in risk assessment and the development of pilot scale experimental systems to study long-term behaviour are addressed as future goals to fill gaps in current research.

Animals↗
PubMed2001

Sulfur speciation monitored in situ with solid state gold amalgam voltammetric microelectrodes: polysulfides as a special case in sediments, microbial mats and hydrothermal vent waters.

Sulfur speciation was determined in real time in salt marsh microbial mats, subtidal sediments and hydrothermal vent diffuse flow waters using solid state gold-amalgam voltammetric microelectrodes. Chemical species were measured in situ without any sample manipulation or processing. The partially oxidized sulfur species detected were polysulfides, thiosulfate, elemental sulfur and tetrathionate. Fe(III) oxidation of hydrogen sulfide does not occur within the mats where microbially mediated processes are responsible for oxidation of H2S. In sediments and diffuse flow vent waters, Fe(III) phases are the direct oxidant of H2S. Sulfur speciation determined in this work is due to in situ biogeochemical processes and is not due to artefacts of sample manipulation. The voltammetric data show that polysulfides are the first detectable intermediate during sulfide oxidation which is consistent with previous laboratory studies.

Electrodes↗
PubMed2001

Monitoring of the natural environment by chemical speciation of elements in aerosol and sediment samples.

The development of a monitoring network for chemical speciation of elements of aerosol and sediment samples collected at Lake Balaton has been carried out. Sequential leaching procedures for the determination of the distribution of elements in aerosols (3 steps) and sediments (4 steps) were used. These methods were recently successfully applied to describe environmentally mobile and stable fractions of toxic metals. In aerosol matrices the partition of elements was accomplished by particle size and chemical bonding. In sediments the distribution was performed by chemical bonding. The processes are called fractionation of elements. Particular attention was paid to distinguishing between environmentally mobile and environmentally immobile fractions because these represent the two extreme modes by which the metals are bound to solid matrices. The monitoring objectives were to assess pollution effects on man and his environment and to identify any possible cause and effect relationship between pollutant concentrations and health effects. The results of dry and wet deposition rates showed that most of the toxic metals were dissolved in an aqueous phase and the wet deposition played an important role. It has been found that, while the concentration of Cd and Pb in aerosols is low (0.7 and 29 ng m(-3), respectively), environmentally mobile fractions are considerable. Based upon the data it can be concluded that the effect of the anthropogenic sources on the quality of the lake is minor. This has been the first attempt to correlate speciation results between aerosols and sediments.

Aerosols↗
PubMed2001

Speciation of arsenic using solid phase extraction cartridges.

Various solid phase extraction (SPE) cartridges were investigated for speciation of arsenite [As(III)], arsenate [As(v)], monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA). Cartridges containing different types of sorbent materials were tested for arsenic retention and elution characteristics. Alumina cartridges were found to completely retain all the four target arsenic species, and are suitable for removal and preconcentration purposes. For speciation analysis, different arsenic species were separated on the basis of their selective retention on and elution from specific cartridges. DMA was retained on a resin-based strong cation exchange cartridge and eluted with 1.0 M HCl. MMA and As(v) were both retained on a silica-based strong anion exchange cartridge and sequentially eluted with 60 mM acetic acid (for MMA) and 1.0 M HCl [for As(v)]. As(III) was not retained on either cartridge and remained in solution. Arsenic species in solution and those eluted from the cartridges were subsequently quantified by using flow injection with hydride generation atomic fluorescence spectrometry (FI-HGAFS) and hydride generation atomic absorption spectrometry (FI-HGAAS). A detection limit of 0.05 microg L(-1) arsenic in water sample was achieved using HGAFS. An application of the method was demonstrated at a drinking water treatment facility. As(III) and As(v) species were determined in water at various stages of treatment. The method is suitable for routine determination of trace levels of arsenic in drinking water to comply with more stringent environmental regulations.

Adsorption↗
PubMed2001

Chemical speciation and sequential extraction of Mn in workroom aerosols: analytical methodology and results from a field study in Mn alloy plants.

Workers in the Mn alloy producing industry are exposed to aerosols containing a variety of Mn compounds (MnO, MnO,, Mn2O3, Mn3O4, FeMn and SiMn). This paper reports a novel four-step chemical speciation/ fractionation procedure developed for characterisation of workroom aerosols collected in Mn alloy producing plants. The following components of the aerosol have been quantified: "water soluble" Mn dissolved in 0.01 M ammonium acetate: Mn0 and Mn2+ dissolved in 25% acetic acid; Mn3+ and Mn4+ dissolved in 0.5%) hydroxylamine hydrochloride in 25%) acetic acid; and "insoluble" Mn digested in aqua regia and hydrofluoric acid. Dissolution of pure Mn compounds with well-defined stoichiometries were essentially complete in the respective leaching steps with detectable amounts of < 1% in others. Recoveries of a mixed quality control sample were also acceptable in the range 92-97% for the different oxidation states. The levels measured in the inhalable and respirable fractions in three Mn alloy producing plants were approximately 300 and 35 microg m(-3) of total Mn, respectively. The most obvious feature of the speciation results is that none of the work areas is characterised by a single Mn contaminant. The predominant oxidation states in the inhalable aerosol fraction are Mn0 and Mn2+ independent of job functions/departments. The occurrence of insoluble Mn compounds in both the inhalable and respirable aerosol fractions is significantly higher during production of SiMn.

Aerosols↗
PubMed2001

Speciation of nickel in airborne particulate matter by means of sequential extraction in a micro flow system and determination by graphite furnace atomic absorption spectrometry and inductively coupled plasma mass spectrometry.

A four-stage sequential extraction procedure for the speciation of nickel has been applied to ambient aerosol samples. The determination of the soluble, sulfidic, metallic and oxidic Ni fractions in particulate matter was carried out by graphite furnace (electrothermal) atomic absorption spectrometry (ETAAS) and inductively coupled plasma mass spectrometry (ICP-MS). An EDTA solution, a mixture of diammonium citrate and hydrogen peroxide, and a KCuCl3 solution were used as leaching agents for the determination of the soluble, sulfidic and metallic species, respectively, and nitric acid was used for the determination of oxidic compounds after microwave digestion of particulate matter sampled on filters. A new micro scale filter holder placed in a closed flow injection analysis (FIA) system for use in nickel speciation by means of sequential extraction, and the results of the optimisation of the extraction conditions are described. The temperature program for ETAAS was optimised for all extraction solutions with the aid of temperature curves. Pyrolysis temperatures of 900. 600 and 1,000 degrees C were found to be optimum for EDTA, hydrogen peroxide plus ammonium citrate and KCuCl3-containing solutions, respectively. Airborne dust was sampled on lilters at two locations near to a metallurgical plant in Dortmund, Germany. Concentrations in the low ng m(-3) range down to the detections limits (0.1-0.3 ng m(-3)) and various nickel species were found to be present in the collected dust. The mean fractions of total nickel (sampling period of one month) were found to contain 36+20% of soluble, 6 +/- 4% of sulfidic, 11 +/- 15% of metallic and 48 +/- 18% of oxidic nickel.

Air Pollutants↗
PubMed2002

Speciation of arsenic in plants by HPLC-HG-AFS: extraction optimisation on CRM materials and application to cultivated samples.

A recently developed method for the determination of arsenic species (arsenite, arsenate, monomethylarsonate, MMAA, and dimethylarsinate, DMAA) has been applied to the study of arsenic speciation in plants. This method uses ion-exchange liquid chromatography coupled on-line to atomic fluorescence spectrometry through continuous hydride generation. Various extraction procedures have been studied in detail using three plant certified reference materials. None of the procedures tested revealed fully satisfying results with all kinds of plant samples; microwave assisted extraction with 0.3 mol dm-3 orthophosphoric acid was found to be the most convenient for dealing with terrestrial plants. Species stability appears good. This method was applied to real world cultivated plant parts. Arsenate appears to predominate in soils, roots and leaves; unidentified species (probably arsenosugars) play an important role (60%) in rice fruits. Carrot was found to be the most contaminated edible plant part, containing 1 mg kg-1 essentially as arsenate species. MMAA was detected in all soils and some plant parts especially shallots at low levels, whereas DMAA was found only in one soil sample and in hot pepper leaves. Arsenite is a minor component of all soils; it is also present in some plant parts at low levels. However, no evident relationships were found between As speciation in the various plant parts and much more detailed studies will be necessary to elucidate As behaviour in plants.

Arsenates↗
PubMed2002

Antimony speciation by inductively coupled plasma mass spectrometry using solid phase extraction cartridges.

A novel and simple method for inorganic antimony speciation is described based on selective solid phase extraction (SPE) separation of antimony(III) and highly sensitive inductively coupled plasma mass spectrometric (ICP-MS) detection of total antimony and antimony(V) in the aqueous phase of the sample. Non-polar SPE cartridges, such as the Isolute silica-based octyl (C8) sorbent-containing cartridge, selectively retained the Sb(III) complex with ammonium pyrrolidine dithiocarbamate (APDC), while the uncomplexed Sb(V) remained as a free species in the solution and passed through the cartridge. The Sb(III) concentration was calculated as the difference between total antimony and Sb(V) concentrations. The detection limit was 1 ng L(-1) antimony. Factors affecting the separation and detection of antimony species were investigated. Acidification of samples led to partial or complete retention of Sb(V) on C8 cartridge. Foreign ions tending to complex with Sb(III) or APDC did not interfere with the retention behavior of the Sb(III)-APDC complex. This method has been successfully applied to antimony speciation of various types of water samples.

Antimony↗
PubMed2003

Chromium redox speciation in natural waters.

Dissolved hexavalent chromium concentrations were determined in river, estuarine and coastal waters of the Humber catchment in north-east England. Samples were collected, filtered, extracted on site and after storage for up to eight days. Hexavalent chromium concentrations did not change by more than 0.05 microg l(-1) (not significant, p = 0.05) over this period. Total chromium concentrations in the catchment were less than 1.0 microg l(-1). This is low in relation to the proposed Environmental Quality Standard. Hexavalent chromium accounted for between 27% and 100% of the total dissolved concentration, with an average of approximately 50%. The proportion of Cr(III) and Cr(VI) in the rivers and estuary were of the same range as previously measured in 1993. The addition of Cr(III) and Cr(VI) to fresh and saline water samples illustrates the complexity of the factors controlling chromium speciation in natural waters. The presence of oxidisable organic matter and the stabilising role of complexing organic ligands are proposed as the main controlling influences of redox speciation in filtered samples.

Carcinogens, Environmental↗
PubMed2003

Aluminium speciation in effluents and receiving waters.

The respective speciation of aluminium in sewage effluent and in river water receiving effluent, has been examined. Results showed that concentrations of reactive aluminium changed over a timescale of hours and were controlled predominantly by pH. A minimum concentration of reactive aluminium occurred at a pH of approximately 6.8, coinciding with the prevalence of non-reactive, insoluble Al(OH)3 species. For receiving waters of low pH value, typically < pH 5, a large proportion of the 'naturally present' aluminium can be present in a reactive form at concentrations higher than the proposed Environmental Quality Standard (EQS). Mixing of waters of this type with effluent of a higher pH value leads to the precipitation of aluminium hydroxide. Mixing of effluent of pH value in the range 7.5-8.0 with river water in the same (or slightly higher) pH range appears to result in no appreciable change in the proportion of reactive aluminium; the change in concentration tends to be related simply to dilution. On the basis of a theoretical knowledge of aluminium speciation, results obtained in this work indicate that it is possible to make predictions about the proportion of reactive aluminium present in a receiving water, based on the pH values of the effluent water mixture and the concentration in the effluent. Reasonable comparisons between measured and predicted values were obtained at higher pH values, but the relationship was less certain at pH values less than 6.5 for which levels of reactive metal tended to be higher than the quality standard value.

Aluminum↗
PubMed2004

Liquid chromatography-hydride generation-atomic absorption spectrometry for the speciation of tin in seafoods.

Liquid chromatography with hydride generation atomic absorption spectrometry as the detection system was applied to the separation and determination of inorganic tin, tributyltin, dibutyltin, monobutyltin, diphenyltin and monophenyltin. A reversed phase C18 column and a methanol/water/acetic acid (70:27:3, v/v/v) mixture containing 0.05%(v/v) triethylamine and 0.1%(w/v) tropolone as the mobile phase (isocratic elution) were used. Extraction of organotins from the samples was carried out using methanol containing 0.05%(w/v) tropolone, a process that was repeated twice. The supernatants were shaken with water and dichloromethane in a separating funnel and the organic phase was collected and evaporated to dryness. When the method was applied to the speciation of tin in fresh and canned mussels, no organotins above the detection limits were identified in any of the samples, inorganic tin being the only species detected. The reliability of the procedure was checked by analyzing the total tin content of the samples by electrothermal atomic absorption spectrometry and by speciation of tin in a certified reference material, mussel tissue (CRM 477). The method can be used for environmental monitoring of organotins contaminated samples.

Chromatography, Liquid↗
PubMed2004

Trace metal speciation and contamination in an intertidal estuary.

An analysis of the geochemical distribution of selected trace metals among various geochemical phases of the sediments in the Tees estuary was carried out using a sequential extraction technique and Differential Stripping Voltammetry. The sediments of the estuary are mainly organic rich clay silts and metal concentrations exceed those in the water column. Speciation results show that contamination of the estuary is mainly from anthropogenic sources. Pb and Zn are associated with the reducible, residual and oxidisable fractions. The speciation pattern of Cd was similar to those of lead and zinc. However there were also some exchangeable and bound to carbonate fractions although these were less significant. Cu is largely associated with the oxidisable and residual fractions, with insignificant bound to carbonate, exchangeable and reducible fractions. The most bioavailable forms of the metals are the free inorganic ions. Total metal concentrations in the estuary display a downward trend since the 1970s.

Adsorption↗
PubMed2004

Speciation and mass-balance of mercury from pulverized coal fired power plants burning western Canadian subbituminous coals.

This report summarizes the results of a study carried out on six pulverized coal-fired power plants in western Canada burning subbituminous coal for the mass-balance and speciation of mercury. The main objectives of this study were to: determine the total gaseous mercury (TGM) emitted from stacks of power plants using the Ontario Hydro method; identify the speciation of emitted mercury such as metallic (Hg(0)) and gaseous elemental (GEM) mercury; and perform mass-balance calculations of mercury for milled-coal, bottom ash, electrostatic precipitators (ESP) fly ash and stack-emitted mercury based on three tests. Sampling of mercury was carried out using the Ontario Hydro method and mercury was determined using the USEPA method 7473 by cold vapor atomic absorption (CVAAS). The sample collection efficiencies confirmed that both oxidized and the elemental mercury had been successfully sampled at all power plants. The total gaseous mercury emitted (TGM) is 6.95-15.66 g h(-1) and is mostly in gaseous elemental mercury (GEM, Hg(0)) form. The gaseous elemental mercury is emitted at a rate of 6.59-12.62 g h(-1). Reactive gaseous mercury (RGM, Hg(2+)) is emitted at a rate of 0.34-3.68 g h(-1). The rate of emission of particulate mercury (Hg(p)) is low and is in the range 0.005-0.076 g h(-1). The range of mass-balances for each power plant is more similar to the variability in measured mercury emissions, than to the coal and ash analyses or process data. The mass-balance calculations for the six power plants, performed on results of the three tests at each power plant, are between 86% and 123%, which is acceptable and within the range 70-130%. The variation in mass-balance of mercury for the six power plants is mostly related to the variability of coal feed rate.

Air Pollutants↗
PubMed2005

A systematic investigation of aluminium ion speciation at high temperature. Part 1. Solution studies.

Speciation diagrams of aluminium ions in aqueous solution (0.2 M) at high temperature (90 degrees C) have been obtained from 48 h time-resolved multi-batch titration experiments monitored by 27Al NMR spectroscopy, potentiometry and dynamic light scattering. The quantitative speciation patterns and kinetic data obtained offer a dynamic picture of the distribution of soluble and insoluble Al species as a function of hydrolysis ratio h(h=[OH-]/[Al3+]) over a very broad range of conditions (-1.0 < or =h < or = 4.0). Monomeric, small oligomeric, tridecameric (the 'Al13-mer') and the recently characterised 30-meric aluminium species (the 'Al30-mer') as well as aluminium hydroxide have been identified and quantified. The Al13-mer species dominates over a relatively broad range of hydrolysis ratios (1.5 < or =h< or = 2.7) during the first 6 h of experiment, but are gradually replaced by Al30-mers at longer reaction times. Kinetic profiles indicate that the formation of the Al30-mer is limited by the disappearance of the Al13 species at mildly acidic conditions. The estimated rate constants of both hydrolytic processes show good internal correlation at h> or = 1.5. The effect of local perturbations leading to the formation of aluminium hydroxide below the electroneutrality point (h= 3.0) has been estimated quantitatively.

Journal Article↗
PubMed2005

Speciation of dissolved iron(II) and iron(III) in environmental water samples by gallic acid-modified nanometer-sized alumina micro-column separation and ICP-MS determination.

A method has been developed for the speciation of trace dissolved Fe(II) and Fe(III) in water by coupling gallic acid (GA) modified nanometer-sized alumina micro-column separation with inductively coupled plasma mass spectrometry (ICP-MS). The separation of Fe(II) and Fe(III) was achieved based on the obvious difference in reaction kinetics between Fe(II) and Fe(III) with GA. Fe(III) was selectively retained on the micro-column at pH 5.5-6.5, while Fe(II) could not be retained by the micro-column at the whole tested pH range of 1.0-6.5, and passed through the micro-column. The Fe(II) can be determined by ICP-MS directly without preconcentration/separation procedure, while Fe(III) retained on the micro-column was then eluted with 1.0 mL of 1 mol L(-1) HCl and determined by ICP-MS. The parameters affecting the separation of Fe(II) and Fe(III) were investigated systematically and the optimum separation conditions were established. Under the optimized conditions, the detection limits of 0.48 microg L(-1) and 0.24 microg L(-1) with relative standard deviation of 5.6% and 4.3%(C= 5 microg L(-1), n= 7) for Fe(II) and Fe(III) were found, respectively. No obvious effect on the speciation of Fe(II) and Fe(III) was found with the change of the ratio of Fe(II) and Fe(III) from 0 ratio 10 to 10 ratio 0. The proposed method was applied for the determination of trace Fe(II) and Fe(III) in environmental water and the recoveries for spiked samples were found to be in the range of 97-105%.

Fresh Water↗