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PubMed2006

Speciation of antimony by preconcentration of Sb(III) and Sb(V) in water samples onto nanometer-size titanium dioxide and selective determination by flow injection-hydride generation-atomic absorption spectrometry.

A novel method for prevention of the oxidation of Sb(III) during sample pretreatment, preconcentration of Sb(III) and Sb(V) with nanometer size titanium dioxide (rutile) and speciation analysis of antimony, has been developed. Antimony(III) could be selectively determined by flow injection-hydride generation-atomic absorption spectrometry, coexisting with Sb(V). Trace Sb(III) and Sb(V) were all adsorbed onto 50 m g TiO2 from 500 ml solution at pH 3.0 within 15 min, then eluted by 10 ml of 5 mol/l HCl solution. One eluent was directly used for the analysis of Sb(III); to the other eluent was added 0.5 g KI and 0.2 g thiourea to reduce Sb(V) to Sb(III), then the mixture was used for the determination of total antimony. The antimony(V) content is the mathematical difference of the two concentrations. Detection limits (based on 3sigma of the blank determinations, n=11) of 0.05 ng/ml for Sb(III) and 0.06 ng/ml for Sb(V), were obtained.

Journal Article↗
PubMed2006

Pneumatic flow injection analysis-tandem spectrometer system for iron speciation.

A pneumatic flow injection-tandem spectrometer system, without a delivery pump was used for the speciation of iron. In this system, the suction force of a pneumatic nebulizer of a flame absorption spectrometer was used for solution delivery through the manifold. The Fe(III) and total Fe concentrations were determined using thiocyanate ion in a UV-Vis spectrometer and a FAAS, respectively. The Fe(II) was determined by the difference. The calibration curves were linear up to 18 microg mL(-1) and 25 microg mL(-1) with detection limits of 0.09 microg mL(-1) and 0.07 microg mL(-1) for Fe(III) and Fe(II), respectively. The mid-range precision and accuracy were <2.5% and +/-3% for the two species, respectively, at a sampling rate of 120 h(-1). This system was applied for the determination of Fe(III) and Fe(II) in industrial water, natural water and spiked samples.

Calibration↗
PubMed2006

Speciation of chromium in seawater by ICP-AES with dual mini-columns containing chelating resin.

A method for the preconcentration and speciation of chromium in seawater was developed. On-line preconcentration and determination were carried out by using inductively coupled plasma atomic emission spectrometry (ICP-AES) with dual mini-columns containing a chelating resin. In this system, Cr(III) was collected on the first column. The effluent containing residual chromium from the first column was collected on the second column after passing through a reduction-switching unit, in which the reducing agent was introduced, or not, for the reduction of Cr(VI) to Cr(lII). Cr(VI) was determined as the difference between the concentration of pre-reduced Cr(VI) and Cr(III) in the effluent from the first column. The detection limits for Cr(III) and Cr(VI) were 0.04 and 0.09 microg l(-1), respectively.

Chelating Agents↗
PubMedDate not supplied

Metal bioavailability and speciation in a wetland tailings repository amended with biosolids compost, wood ash, and sulfate.

Lead poisoning of waterfowl from direct ingestion of wetland mine tailings has been reported at the Coeur d'Alene River basin in Idaho. A greenhouse study was conducted to evaluate the effects of surface applications of amendments on lead bioavailability in the tailings. Treatments included sediment only, and sediment with three different surface amendments: (i) biosolids compost plus wood ash, (ii) compost + wood ash + a low SO4(2-) addition as K2SO4, and (iii) compost + wood ash + a high SO4(2-) addition. Measured variables included growth and tissue Pb, Zn, and Cd concentration of arrowhead (Sagittaria latifolia Willd.) and cattail (Typha latifolia L.) and soil pH, redox potential (Eh), pore water Pb, Pb speciation by X-ray absorption spectroscopy, and in vitro Pb bioavailability. The compost + ash amendment alleviated phytotoxicity for both plant species. Bioavailability of Pb as measured by a rapid in vitro extract decreased by 24 to 34% (over control) in the tailings directly below the amendment layer in the compost + SO4 treatments. The ratio of acid volatile sulfide (AVS) to simultaneously extracted metals (SEM) also indicated a reduction in Pb bioavailability (1:40 control, 1:20 compost, 1:8 compost + low SO4, and 1:3 compost + high SO4). Extended X-ray adsorption fine structure (EXAFS) and X-ray absorption near edge structure (XANES) spectroscopy data indicated that lead sulfide was greater after 99 d in the treatments that included additions of sulfate. These results indicated that, under reducing conditions, surface amendments of compost + wood ash (with or without sulfate) decreased the bioavailability of Pb in metal-contaminated mine tailings.

Biodegradation, Environmental↗
PubMed2005

Temporal variability in physical speciation of metals during a winter rain-on-snow event.

Particulate matter in urban rivers transports a significant fraction of pollutants, changes rapidly during storm events, and is difficult to characterize. In this study, the physical speciation of trace metals and organic C in an urban river and upstream headwaters site in Torrington, CT, were measured during a winter rain-on-snow event. In addition, a selective fractionation scheme, using membrane and tangential-flow ultrafiltration methods to separate suspended particulate matter into sand, silt, clay, and colloid fractions, was evaluated based on the appropriateness of the chosen size categories. During peak runoff at the urban river site, total-recoverable concentrations of the metals Cu and Pb increased 6- and 13-fold to 16.9 and 9.5 microg L(-1), respectively, compared with baseflow concentrations. Concentrations of Cu and Pb reached only 0.9 and 0.86 microg L(-1) at the headwaters site. For the measured storm event, the majority of metals were transported by the urban river in association with coarse silt (20-80 microm particle diam.) during peak runoff. During peak runoff at the urban site, organic C associated with the large colloid fraction (0.1-1.0 microm) increased from 5% (at baseflow) to 54% of the total C in transport, whereas dissolved organic C and that associated with smaller colloids decreased from 91.5% (at baseflow) to 41% of the total. Other elements that were monitored as part of the study were Na, K, Ca, Mg, Fe, Mn, Al, Cd, Cl-, NO3(-), and SO4(2-). The chosen fractionation scheme was useful to characterize pollutant transport during this event, but further testing should be undertaken to determine the most appropriate size range categories, and to ensure that the sizes measured are comparable to those used in other studies.

Connecticut↗
PubMedDate not supplied

Water-soluble and solid-state speciation of phosphorus in stabilized sewage sludge.

Three chemicals, ferrous sulfate (Fe-sul), calcium oxide (CaO), and aluminum sulfate (alum), were used to stabilize phosphorus (P) in fresh, anaerobically digested sewage sludge (FSS). The chemically stabilized sludge materials and biosolids compost (BSC) were compared with the FSS with respect to water-soluble phosphorus (WSP) content in its inorganic (WSP(i)) and organic (WSP(o)) forms as well as water-soluble organic carbon (DOC). Solid-state P speciation was further probed by X-ray diffraction (XRD) and scanning electron microscopy (SEM) equipped with energy-dispersive X-ray elemental spectrometry (EDXS). Water-soluble P was effectively controlled by a wide range of Fe-sul or CaO additions to the sludge (Ca to P ratio = 3.47-17.72, Fe to P ratio = 1.01-16.53), but by only a narrow range (Al to P ratio = 1.04-2.87) of alum addition. The WSP content in the BSC was also depressed, but to a lesser extent. The pH in the treated sludge ranged from 3.0 to 12.5 and served as a key factor to control P chemistry. No correlation was observed between DOC and WSP(o). No crystallized Ca-P minerals were detected in the CaO-stabilized sludge, but brushite crystallization seemed to be obtained by low addition of Fe-sul and alum. Variscite and strengite crystallization was obtained following high addition of Fe-sul or alum, as detected by XRD and SEM-EDXS. Adsorption of P by newly formed Fe-hydroxide seems to play an important role in the Fe-sul-stabilized sludge. We concluded that administration of the tested chemicals at the proper rate can effectively reduce the hazard of P release and leaching from sludge.

Adsorption↗
PubMedDate not supplied

Prediction of zinc, cadmium, lead, and copper availability to wheat in contaminated soils using chemical speciation, diffusive gradients in thin films, extraction, and isotopic dilution techniques.

To predict the availability of metals to plants, it is important to understand both solution- and solid-phase processes in the soil, including the kinetics of metal release from its binding agent (ligand and/or particle). The present study examined the speciation and availability of Zn, Cd, Pb, and Cu in a range of well-equilibrated metal-contaminated soils from diverse sources using several techniques as a basis for predicting metal uptake by plants. Wheat (Triticum aestivum L.) was grown in 13 metal-contaminated soils and metal tissue concentrations (Zn, Cd, Pb, and Cu) in plant shoots were compared with total soil metal concentrations, total soluble metal, and free metal activities (pM2+) in soil pore waters, 0.01 M CaCl2-extractable metal concentrations, E values measured by isotope dilution, and effective metal concentrations, C(E), measured by diffusive gradients in thin films (DGT). In the DGT technique, ions are dynamically removed by their diffusion through a gel to a binding resin, while E values represent the isotopically exchangeable (labile) metal pools. Free metal activities (Zn2+, Cd2+, and Pb2+) in soil pore waters were determined using a Donnan dialysis technique. Plant Zn and Cd concentrations were highly related to C(E), while relationships for Zn and Cd with respect to the other measures of metals in the soils were generally lower, except for CaCl2-extractable Cd. These results suggest that the kinetically labile solid-phase pool of metal, which is included in the DGT measurement, played an important role in Zn and Cd uptake by wheat along with the labile metal in soil solution. Plant Pb concentrations were highly related to both soil pore water concentrations and C(E), indicating that supply from the solid phase may not be so important for Pb. Predictions of Cu uptake by wheat from these soils by the various measures of Cu were generally poor, except surprisingly for total Cu.

Biological Availability↗
PubMedDate not supplied

Phosphorus speciation in broiler litter and turkey manure produced from modified diets.

Modifying poultry diets by reducing mineral P supplementation and/or adding phytase may change the chemical composition of P in manures and affect the mobility of P in manure-amended soils. We studied the speciation of P in manures produced by broiler chickens and turkeys from either normal diets, or diets with reduced amounts of non-phytate phosphorus (NPP) and/or phytase, using a combination of chemical fractionation and synchrotron X-ray absorption near edge structure (XANES) spectroscopy. All broiler litters were rich in dicalcium phosphate (65-76%), followed by aqueous phosphate (13-18%), and phytic acid (7-20%); however, no hydroxylapatite was observed. Similarly, normal turkey manure had 77% of P as dicalcium phosphate and had no hydroxylapatite, while turkey manure from diets that had reduced NPP and phytase contained equal proportions of dicalcium phosphate (33-45%) and hydroxylapatite (35-39%). This is attributed to the higher total Ca to P ratio (>2) in modified turkey manures that resulted in transformation of more soluble (dicalcium phosphate) to less soluble P compounds (hydroxylapatite). Chemical fractionation showed that H2O-extractable P was the predominant form in broiler litter (56-77%), whereas aqueous phosphate determined with XANES was <18% indicating that H2O probably dissolved mineral forms of P (e.g., dicalcium phosphate). Results show that HCl extraction primarily removed phytic acid from broiler litters and normal turkey manure, while it removed a mixture of hydroxylapatite and phytic acid from modified turkey manures. The combination of chemical fractionation and XANES provided information about the nature of P in these manures, which may help to devise best management practices for manure use.

Animal Feed↗
PubMed2001

Biogeography of Asterias: North Atlantic climate change and speciation.

Fossil evidence suggests that the seastar genus Asterias arrived in the North Atlantic during the trans-Arctic interchange around 3.5 Ma. Previous genetic and morphological studies of the two species found in the Atlantic today suggested two possible scenarios for the speciation of A. rubens and A. forbesi. Through phylogenetic and population genetic analysis of data from a portion of the cytochrome oxidase I mitochondrial gene and a fragment of the ribosomal internal transcribed spacer region, I show that the formation of the Labrador Current 3.0 Ma was probably responsible for the initial vicariance of North Atlantic Asterias populations. Subsequent adaptive evolution in A. forbesi was then possible in isolation from the European species A. rubens. The contact zone between these two species formed recently, possibly due to a Holocene founding event of A. rubens in New England and the Canadian Maritimes.

Animals↗
PubMedDate not supplied

Advances in instrumental methods for the measurement and speciation of trace metals.

Progress in understanding the role of trace metals in biology has been largely dependent on the development of sensitive, accurate and precise analytical methods. Atomic spectroscopic techniques, particularly atomic absorption, have made the greatest contribution. Key to the success of such analytical techniques has been the simplification of sample processing so that contamination is minimized. Electrothermal atomization has allowed sensitivity limits to be lowered sufficiently so that even ultra-trace metals can be detected. More recently, mass spectrometric detection of metal ions has added to the repertoire of available instrumentation, particularly with the use of inductively coupled plasma to introduce ions into the mass analyzer. These analyzers are suitable for multielement analysis. More conventional mass spectrometric analysis of metal chelates offer an alternate solution but require considerable specimen preparation time. Intracellular localization of trace metals necessitates complex specimen processing prior to analysis on instruments that are highly sophisticated and expensive. Metal speciation is a rapidly growing area of trace metal research, with the major advances coming from coupling of the separation process, such as capillary electrophoresis or high performance liquid chromatography, with the analytical instrument for metal detection. Inductively coupled plasma-mass spectrometry has proved to be an excellent choice for such detection purposes. Refinement of these methods as well as more widely available instruments for microanalysis will add greatly to continued advances in our knowledge of the role of trace metals in biology and medicine.

Animals↗
PubMed1999

Broad-sense sexual selection, sex gene pool evolution, and speciation.

Studies of sexual selection have traditionally focused on explaining the extreme sexual dimorphism in male secondary sexual traits and elaborate mating behaviors displayed by males during courtship. In recent years, two aspects of sexual selection have received considerable attention in the literature: an extension of the sexual selection concept to other traits (i.e., postcopulatory behaviors, external and internal genital morphology, gametes, molecules), and alternative mechanistic explanations of the sexual selection process (i.e., coevolutionary runaway, good-genes, sexual conflicts). This article focuses on the need for an extension of sexual selection as a mechanism of change for courtship and (or) mating male characters (i.e., narrow-sense sexual selection) to all components of sexuality not necessarily related to courtship or mating (i.e., broad-sense sexual selection). We bring together evidence from a wide variety of organisms to show that sex-related genes evolve at a fast rate, and discuss the potential role of broad-sense sexual selection as an alternative to models that limit speciation to strict demographic conditions or treat it simply as an epiphenomenon of adaptive evolution.

Animals↗
PubMedDate not supplied

[Speciation of bioactive Al(III) and VO(IV) complexes in biological systems].

The speciation of the toxic Al(III) and the beneficial VO(IV) in various biofluids and tissues is discussed in order to describe the solution state of these metal ions in the organism. The possibility and the importance of ternary complex formation with relevant biomolecules is emphasised. The importance of the biospeciation of Al(III) ion in its transport and involvement in neurological disorders, and of insulin mimetic VO(IV) complexes is discussed.

Aluminum↗
PubMed2001

Distribution, speciation, and bioavailability of lanthanides in the Rhine-Meuse estuary, The Netherlands.

Changing environmental conditions may influence the fate and bioavailability of lanthanides (part of the rare earth elements [Ln]) in estuaries. The aim of this study was to quantify the variation in estuarine lanthanide solid/water distribution, speciation, and bioaccumulation. The latter was studied in the amphipod Corophium volutator under field and laboratory conditions. Calculations with the chemical equilibrium model MINEQL+ indicate that dissolved lanthanides are complexed mainly to carbonates and dissolved organic matter. In the water phase, the relative abundance of the free ion, LnCO3, and humic complexes decreases from lanthanum to lutetium, whereas the relative abundance of Ln(CO3)2 increases. Cerium and europium anomalies were found in the water. Europium anomalies were also found in some biota. The biota sediment accumulation factors (BSAFs) decreased across the series from lanthanum to lutetium. Regression analysis revealed that alkalinity correlated negatively with lanthanide uptake. This suggests that increasing complexation reduced bioavailability under the prevailing conditions. The BSAFs did not depend on salinity or pH, which may simplify sediment-quality criteria for fresh versus saline waters. Field BSAFs were significantly lower than laboratory values for the same sediments, which is explained by adaptation of the organisms to lanthanides.

Animals↗
PubMed2001

Linking ecological impact to metal concentrations and speciation: a microcosm experiment using a salt marsh meiofaunal community.

Microcosm experiments addressed the impact of a mixture of Cu, Cr, Cd, Pb, and Hg at three concentrations after 36 h, 12 d, and 30 d on a meiofauna-dominated salt marsh community. In addition to analyzing effects on meiofaunal abundances, the study quantified the sediment metal concentrations of all five metals and pore-water concentrations, speciation, and ligand complexation of Cu. Abundances of deposit feeders such as the polychaete Streblospio benedicti, gastropods, and bivalves were impacted at lower metal concentrations than the mainly algal-feeding copepods, ostracods, and nematodes. We suggest that this might be due to bulk ingestion of metal-contaminated sediments resulting in relatively higher metal exposure in the deposit feeders than in the other, nondeposit feeding taxa. Copepod and ostracod abundances decreased only in the highest metal treatment, where levels of inorganic Cu ([Cu']) in pore waters were similar to levels associated with both acute and subacute toxicity in published in vivo toxicity studies of marine copepods. The higher metal treatments yielded disproportionately higher pore-water [Cu] compared with sediment [Cu], suggesting saturation of sediment-associated ligands with increased additions of Cu. Similarly, the higher metal treatments appeared to reach saturation of the organic Cu ligands, with the excess pore-water [Cu] present in the more toxic, inorganic species of Cu. Acid-volatile sulfide (AVS) concentrations at sediment horizons inhabited by meiofauna were low and AVS was not considered a significant metal ligand at these depths. Since meiofauna are predominantly associated with oxic surface sediments, it is doubtful that AVS is a major factor controlling availability of free metal for exposure to these taxa.

Animals↗
PubMedDate not supplied

Protonation and complex formation of 5-sulfosalicylate in NaCl, CaCl2 and MgCl2 aqueous media. Speciation in synthetic seawater.

The binding capacity of 5-sulfosalicylic acid (ssa) towards cationic macro-components of natural waters has been investigated in different ionic media (NaCl, MgCl2 and CaCl2 aqueous solutions) and in the ionic strength range 0 < or = I < or = 1 mol dm-3. In order to contribute to the speciation of this multi-sites ligand, measurements have been carried out also in a synthetic seawater (SSWE) containing the major components of seawater (Na+, K+, Ca2+, Mg2+, Cl- and SO4(2-)). Measurements have been performed by potentiometry ([H+]-glass electrode), at t = 25 degrees C. A critical analysis on the experimental and literature data is also given.

Benzenesulfonates↗
PubMedDate not supplied

Interaction of alkyltin(IV) compounds with ligands of interest in the speciation of natural fluids: carboxylate and hydroxycarboxylate complexes of monomethyltin(IV) trichloride.

The formation and stability of some carboxylate and hydroxycarboxylate (acetate, 1,2,3-propanetricarboxylate, 1,2,3,4-butanetetracarboxylate, malate and citrate) complexes of monomethyltin trichloride was studied potentiometrically at 25 degrees C and at different ionic strengths in NaNO3 aqueous solution. The following quite stable species are formed in the different systems (M = CH3Sn3+): ML(OH)+, ML2(OH)0, ML(OH)2(0) and M2L(OH)5(0) for acetate; MLH+, ML0, ML(OH)- and ML(OH)2(2-) for propanetricarboxylate; MLH2+, MLH0, ML-, ML(OH)2- and ML(OH)2(3-) for butanetetracarboxylate; ML(OH)0, ML(OH)2- and ML(OH)3(2-) for malate; ML0, ML(OH)-, ML(OH)2(2-) and ML(OH)3(3-) for citrate. Hydroxycarboxylate complexes are significantly stronger than simple carboxylate ones and this is likely to be due to the interaction of the -OH group in citrate and malate with monomethyltin(IV), whose strength was also quantified. It was found that the stability of these complexes can be roughly expressed by the simple relationship log K = a zeta, where zeta is the product of the charges of reactants and log K is the equilibrium constant. For simple carboxylic ligands we have a = 1.8 +/- 0.4 and, for hydroxycarboxylic ligands, a = 3.7 +/- 0.9. Other useful empirical relationships are reported. Moreover, hydroxycarboxylic complexes also play a prominent role in the speciation of monomethyltin(IV) under the pH conditions of interest for natural fluids.

Carboxylic Acids↗
PubMed2002

Measuring metal and phosphorus speciation in P-rich anaerobic digesters.

High concentrations of soluble orthophosphate, magnesium and potassium are released during anaerobic digestion of biological phosphorus removal (BPR) sludge. This research was undertaken to investigate the effects of phosphorus enrichment on digester performance, metal and phosphorus speciation. High concentrations of soluble PO4-P (> 250 mg/l) were found to have a retarding effect on anaerobic digestion, reducing the rate of volatile solids digestion and methane production in comparison to control digesters. This was found to be reversible after a period of time, which was related to the amount of PO4-P added to the digesters, higher concentrations of PO4-P requiring more time for digester recovery. Addition of magnesium and potassium to the digesters, together with PO4-P, reduced the inhibitory effect of phosphorus enrichment but these digesters still showed lower rates of volatile solids digestion and methane production in comparison to the control digesters. Phosphorus enrichment resulted in extensive precipitation of calcium, magnesium and manganese, markedly reducing the soluble and easily available fractions of these metals. Other trace metals such as copper, zinc, chromium, nickel and cobalt actually showed increased levels of solubility as a result of phosphorus enrichment. This was thought to be caused by high levels of soluble organic carbon in the phosphorus-rich anaerobic digesters, which acted as organic ligands for metal complexation.

Bacteria, Anaerobic↗