Sequential Chemical Extraction Research Articles

Potassium Reserves in the Clay Fraction of a Tropical Soil Fertilized for Three Decades

AbstractHighly weathered soils of the humid tropics generally provide a poor mineral reserve of potassium (K), but evidence has been found which indicates that even in such soils non-exchangeable forms of K can be made plant available and this warrants further investigation. The objective of this study was, therefore, to determine the extent to which K can be released from poorly available reserves over a long period of time. The focus was on an Oxisol in southern Brazil cultivated for 32 years with a rotation of soybeans (Glycine max L.), maize (Zea mays L.), wheat (Triticum aestivum L.), and oats (Avena strigosa L.) with and without K fertilization. Mineral sources of K were identified by X-ray diffraction and by sequential chemical extraction from the clay fraction. The amounts of K-bearing mineral species and the amounts of total and plant-available K were quantified, then the effects of the long-term K-fertilization regime on these values were evaluated. The clay fraction was dominated by hematite, gibbsite, and phyllosilicates such as kaolinite. These minerals were unaffected by the K deprivation in the cropping systems, but in the clay fraction the absence of K fertilization for 32 years reduced the structural order of the 2:1 phyllosilicates associated with K reserves. This effect was most prominent in the root zone of the soil. Deprivation of K for more than three decades decreased the crystallinity of 2:1 phyllosilicates, which could be better evaluated from XRD patterns after the removal of kaolinite and Fe (oxyhydr)oxides. The K-free cultivation reduced the amounts of total soil K by increasing the depletion of K from pools that typically are poorly accessible to plants.

Mercury fractionation in tropical soils: A critical point of view

Problems related to specificity and re-precipitation of metals in sequential chemical extractions can impair their routine use. In order to test the efficiency of a sequential chemical procedure, model compounds composed by soil components commonly found in tropical soils such as goethite, Al-goethite, ferrihydrite, hematite, bauxite, and humic acid were incubated with either Hg(NO3)2 or HgSO4 and submitted to chemical extraction. The procedure aims to assess: (i) water soluble Hg; (ii) bioaccessible Hg at pH near human stomach; (iii) Hg associated with organic matter; (iv) reduced Hg; (v) Hg associated with Fe, Al, and Mn oxides; and, (vi) residual Hg. This procedure was also tested via single and sequential extractions using the surface and subsurface samples of two tropical soils, i.e., a Rhodic Acrudox and a Typic Hapludox, with and without lime application. Soil samples were submitted to an adsorption experiment with HgCl2 and a high adsorption percentage was observed. The majority of Hg at both single and sequential procedure was extracted by an acetic acid solution (pH = 2). Liming, soil depth, and soil type were not determinative on Hg extractability. The sequential extraction applied showed a lack specificity of Hg fractions, confirmed by the model components.

Chemical Speciation and Stability of Uranium in Unconventional Shales: Impact of Hydraulic Fracture Fluid.

Uranium and other radionuclides are prominent in many unconventional oil/gas shales and is a potential contaminant in flowback/produced waters due to the large volumes/types of chemicals injected into the subsurface during stimulation. To understand the stability of U before and after stimulation, a geochemical study of U speciation was carried out on three shales (Marcellus, Green River, and Barnett). Two types of samples for each shale were subjected to sequential chemical extractions: unreacted and shale-reacted with a synthetic hydraulic fracture fluid. A significant proportion of the total U (20-57%) was released from these three shales after reaction with fracture fluid, indicating that U is readily leachable. The total U released exceeds labile water-soluble and exchangeable fractions in unreacted samples, indicating that fluids leach more recalcitrant phases in the shale. Radiographic analysis of unreacted Marcellus shale thin sections shows U associated with detrital quartz and the clay matrix in the shale. Detrital zircon and TiO2 identified by an electron microprobe could account for the hot spots. This study shows that significant proportions of U in three shales are mobile upon stimulation. In addition, the extent of mobilization of U depends on the U species in these rocks.

Arsenic immobilization by in-situ iron coating for managed aquifer rehabilitation

A long-lasting challenge in eliminating the worldwide impact of geogenic arsenic (As)-contaminated groundwater is the development of efficient, in-situ treatment technologies that are applicable in decentralized and rural areas. Here we present a managed aquifer rehabilitation (MAR) approach based on the in-situ creation of Fe-oxide scavengers for remediating As-contaminated groundwater. The Fe-oxide coatings on sediment surfaces were generated via periodic injection of Fe2+ and ClO− solutions into an As-affected sandy aquifer at the Datong Basin, northern China for 25 days. This treatment prompted the buildup of weakly alkaline/circumneutral and oxidizing conditions to enhance As(III) oxidation in the target aquifer. Dissolved As concentrations decreased from the initial average 78.0 to 9.8 μg/L over the 25-d amendment. Sediment imaging by scanning electron microscope-X-ray energy dispersive spectroscopy confirms the deposition of Fe-rich precipitates on sediment surfaces with the simultaneous retention of As, and high density electrical tomography suggests the occurrence of such a process throughout the target zone. Further X-ray diffraction analysis and sequential chemical extraction reveal that the neo-formed Fe minerals comprised both poorly crystalline (e.g., ferrihydrite) and better crystalline (e.g., goethite) Fe oxides. The process-based reactive-transport modeling for the variations of As species in the treated groundwater supports that the new Fe-oxide minerals, most probably goethite, acted as efficient removers of aqueous As. The low As level of ∼10 μg/L was maintained during the following 215-d monitoring, demonstrating the long effectiveness of the MAR approach. This study highlights the feasibility of As immobilization by manipulating in-situ Fe-oxide coating on sandy sediments at the pilot scale. The MAR technology may be applicable for As-affected aquifers with controlled oxidizing conditions in the Datong Basin and likely other high-As regions with similar hydrogeochemical settings.

Assessment of iron-based and calcium-phosphate nanomaterials for immobilisation of potentially toxic elements in soils from a shooting range berm

Shooting range facilities in military areas have been indicated as a hotspot of land degradation with high contents of Potentially Toxic Elements (PTEs). Currently, based on the new nanomaterials with specific characteristics, nanoremediation technologies are used to immobilise and to reduce the availability of PTEs in field and laboratory conditions. In this study, the effects of nano-hydroxyapatite and/or hematite on PTEs immobilisation (As, Cd, Cu, Pb, Sb and Zn) in military shooting range soils were assessed through the measure of available and leachable forms with three single-extractions: calcium chloride (0.01M CaCl2), low molecular weight organic acids (10 mM LMWOAs) and toxicity characteristic leaching procedure (TCLP). A sequential chemical extraction was used to determine the distribution of the PTEs in the different geochemical phases of the soils before and after the nanomaterial treatments. Results showed that the availability of PTEs decreased, especially for Pb (40–95%) and Zn (50–99%) after nanomaterial treatments. When both nanomaterial (hydroxyapatite + hematite) were combined, the immobilisation rate improved. However, when each nanomaterial was added individually to the soils, some elements, such as, Cu or Sb, showed a slight increment of their mobilisation. The sequential chemical extraction showed that the highest percentage of PTEs were mainly in the residual fraction before and after adding nanomaterials, being even higher in soils after the nanomaterial treatments. Likewise, the mobile fractions decreased after the treatment with nanomaterials. Our findings suggest that nanoremediation techniques improve the soil conditions, but they should be used carefully to avoid mobilisation of non-target PTEs or unexpected potentially impacts for soil biota.

Chemical availability versus bioavailability of potentially toxic elements in mining and quarry soils

Abandoned mining and quarry areas are sources of potentially toxic elements (PTEs), through lixiviates or transfer processes of bioavailable fractions from mining wastes and tailings. In this study, earthworms (Eisenia fetida Savigny, 1826) were exposed for 28 days to two mining soils from a lead/zinc mine and two quarry soils from an old serpentine quarry. Despite their pseudo total metal contents, a previous characterization of these soils pointed out for a low chemical availability of PTEs. Therefore, a multibiomarker approach was used and the response of E. fetida to soils was assessed through the analysis of neurotoxic, oxidative stress, energy metabolism and DNA damage biomarkers (acetylcholinesterase, catalase, glutathione-s-transferase, lactate dehydrogenase, lipid peroxidation and DNA strand breaks). Metal bioaccumulation was also assessed to evaluate bioavailability and organism’s exposure. Results showed that high contents of PTEs were recorded in the whole body of earthworms exposed to lead/zinc mine. However, the bioaccumulation factors for worms exposed to soils from both sampling sites were <1 due to the high PTEs contents in soils. Earthworms exposed to both types of soils displayed neurotoxic and energy metabolism effects. However, significant levels of oxidative stress and DNA damage were recorded only for earthworms exposed to lead/zinc mine soils. This study demonstrated that despite the low availability of PTEs showed by previous sequential chemical extractions, the results obtained from the direct toxicity assessment performed in this study, highlight the importance of a multibiomarker approach using soil organisms to provide a better evaluation of soils pollution.

Sequential chemical extraction and mineralogical bonding of metals from Styrian soils

Geogenic metal contaminations in soils are intensely discussed in waste management, as the recyclability of excavated soil is regulated by limit values for pseudo-total contents in Austria. However, the use of pseudo-total contents overestimates the release of some contaminants such as metals into the environment. Sequential extraction provides an empiric tool to better assess the mobility of metals and predicts their bonding type in individual fractions, but the relation between the obtained fractions and the exact mineralogical bonding is often unclear. Electron microprobe analyses provide detailed mineralogical insights, but do not yield direct information about the mobility of elements. A combination of both methods has been used a few times in soil sciences in general, but never to Styrian soils. Thus, six geogenic contaminated Styrian soils and one compost soil were investigated by a method combination of sequential chemical extraction and electron microprobe analyses. Sequential extraction suggested that Cr in five substrates and As and Ni in one substrate each are bound in stable crystalline minerals, whereas Pb in four samples and Cu in two samples are adsorbed to iron and manganese hydroxides. Elemental mappings obtained by electron microprobe analyses confirmed sequential chemical extraction results and specified that Cu and Pb are bound to manganese (hydr)oxides, As to Fe–Cu–Sb–S compounds, Cr to spinels and Ni to olivine. In summary, the current study gives new information about the mobility and mineralogy of metals in six Styrian soils which is relevant for their possible recycling despite exceeded limit values for pseudo-total content.

Stabilization of heavy metals in MSWI fly ash with a novel dithiocarboxylate-functionalized polyaminoamide dendrimer

A novel heavy metal chelating agent, dithiocarboxylate-functionalized polyaminoamide dendrimer (PAMAM-0G-DTC), was evaluated for the stabilization of heavy metals from municipal solids waste incineration (MSWI) fly ash. PAMAM-0G-DTC achieved overall stabilization performance at a lower dosage (3% w/w) and a wider pH range (2–13) compared to conventional chelating agents such as sodium dimethyl dithiocarbamate (SDD) and dithiocarboxylate-functionalized tetraethylenepentamine (TEPA-DTC). The leaching toxicity of Pb and Cd in the MSWI fly ash by PAMAM-0G-DTC stabilization met the landfill requirements but could not be achieved by SDD and TEPA-DTC even at a 10 wt% concentration. Sequential chemical extraction of fly ash before and after stabilization shows that PAMAM-0G-DTC can be combined with active heavy metals in water-soluble, interchangeable, and carbonate states to form more stable heavy metals in organic and residual states. Mechanistic studies show that multiple PAMAM-0G-DTC molecules can combine with multiple heavy metals to form three-dimensional network-like super-molecular compounds with an infinite extension of space size. This makes the heavy metals more stable and embedded in the network-like super-molecular structure, thus minimizing the potential risk of leaching. Overall, by forming more geochemically stable phases, the treatment of fly ash with PAMAM-0G-DTC has a strong ability to reduce the toxic leaching of heavy metals at a lower dosage and suppress the risk of secondary pollution in a landfill at a wide range of pH values (2–13).

Geochemistry of phosphorus release along transect of sediments from a tributary backwater zone in the Three Gorges Reservoir

As an important phosphorus (P) source in water, sediment P release can influence water quality in the tributary backwater zone of “river-type” reservoir. Chemical sequential extraction and diffusive gradients in thin films technique (DGT) were applied to study sediment P mobility in the Daning River backwater zone (DNB) in the Three Gorges Reservoir (TGR). Influenced by the TGR backwater intrusion, both of water P forms and sediment P forms in the DNB zone exhibited increased spatial distributions from upper reach to lower reach. Sediment particles in the upper, middle, lower reaches were mainly derived from the settled particles (with high Ca contents) carried by the Daning River outflow, the former and sedimentary dead algal, the settled particles carried by the TGR backwater, respectively. According to P adsorption/desorption experiment results and concentration gradients of DGT-labile P at the sediment-overlying interface (SWI), sediments in the DNB zone acted as P source for overlying water during the sampling period. In the lower reach of the DNB zone and the adjacent TGR mainstream, iron oxides reduction in the anoxic or anaerobic sediments drove the synchronous release of labile P and Fe(II). Whereas, algal decomposition directly produced labile P and S(-II) in the top 0 to −10 mm sediment layer in the middle reach, and then the downward increases of labile P and Fe(II) in the depth of −30 to −80 mm were caused by iron oxides reduction. In the upper reach, the released labile P in sediments might be re-trapped by precipitating with Ca(II) or being adsorbed onto the newly formed iron oxides near the SWI. Sediment P release in DNB zone had a limited influence on water quality, but the influence would be significant in the future time after the external P source is reduced efficiently.

Characterization and recovery of rare earth elements and other critical metals (Co, Cr, Li, Mn, Sr, and V) from the calcination products of a coal refuse sample

The impacts of calcination on the leaching recovery of rare earth elements (REEs) and other critical metals from a Baker seam coal refuse material were investigated in this study. Acid leaching test results showed that leaching recovery of the REEs, especially the light REEs, was increased significantly from around 24% to 80–90% after calcination under 600–750 °C for two hours. By considering the major element leaching kinetics and the mineralogical changes of the dominant minerals caused by calcination, two mechanisms were proposed for the improved leaching performance: (1) decomposition of difficult-to-dissolve REE-bearing minerals into soluble forms; and (2) liberation of REE-bearing minerals encapsulated in clays after calcination due to the dehydration and disintegration of the layered clay structure. Sequential chemical extraction tests showed that a significant fraction (around 75%) of the REEs in the raw material were present in an insoluble form. After calcination under proper temperatures (600–800 °C), the majority of the insoluble light REEs (LREEs) were converted into soluble forms. Changes in the modes of occurrence of the LREEs and phosphorous based on leaching rate and sequential leaching correlated well as a function of the calcination temperature. This finding in addition to SEM-EDX results tends to indicate the potential that the LREEs occur primarily as rare earth phosphates such as monazite in the untreated coal refuse material. The acid leaching and sequential chemical extraction results show that co-extraction of REEs and other critical metals such as Co, Mn, and Li is possible using a calcination-acid leaching procedure.

Calcium species evolution mechanism during coal pyrolysis and char gasification in H2O/CO2

The release mechanism of Ca during coal pyrolysis and char gasification in H2O, CO2 and their mixtures was studied. Sequential chemical extraction was used to determine the modes of occurrence of Ca in coal and char. The released Ca from coal pyrolysis and char gasification were captured and analyzed by activated carbon adsorption and X-ray photoelectron spectroscopy (XPS). Model compounds CaS and CaSO4 were adopted to further reveal the released form of Ca under different atmospheres. The results indicate that Ca in coal is mainly released as CaCl2 during the pyrolysis process, and the possible migration mechanism of Ca during pyrolysis was proposed. Ca in coal is mainly released in the form of CaCl2, CaCO3, and CaSO4 during the gasification, and Ca is released as CaCl2 under all conditions. In addition, Ca will be released as CaCO3 under CO2 atmosphere, as CaSO4 under H2O and H2O/CO2 atmospheres at 800 °C and 900 °C, released as CaSO4 under all conditions at 1000 °C. This is closely related to the formation of CaO2 intermediates during the gasification process.

Quantifying Uncertainties in Sequential Chemical Extraction of Soil Phosphorus Using XANES Spectroscopy.

Sequential chemical extraction has been widely used to study soil phosphorus (P) dynamics and inform nutrient management, but its efficacy for assigning P into biologically meaningful pools remains unknown. Here, we evaluated the accuracy of the modified Hedley extraction scheme using P K-edge X-ray absorption near-edge structure (XANES) spectroscopy for nine carbonate-free soil samples with diverse chemical and mineralogical properties resulting from different degrees of soil development. For most samples, the extraction markedly overestimated the pool size of calcium-bound P (Ca-P, extracted by 1 M HCl) due to (1) P redistribution during the alkaline extractions (0.5 M NaHCO3 and then 0.1 M NaOH), creating new Ca-P via formation of Ca phosphates between NaOH-desorbed phosphate and exchangeable Ca2+ and/or (2) dissolution of poorly crystalline Fe and Al oxides by 1 M HCl, releasing P occluded by these oxides into solution. The first mechanism may occur in soils rich in well-crystallized minerals and exchangeable Ca2+ regardless of the presence or absence of CaCO3, whereas the second mechanism likely operates in soils rich in poorly crystalline Fe and Al minerals. The overestimation of Ca-P simultaneously caused underestimation of the pools extracted by the alkaline solutions. Our findings identify key edaphic parameters that remarkably influenced the extractions, which will strengthen our understanding of soil P dynamics using this widely accepted procedure.

Elucidation of soil phosphorus speciation in mid-Atlantic soils using synchrotron-based microspectroscopic techniques.

Phosphorus deficiency and excess are concomitant problems in agricultural soils of the mid-Atlantic region. A fundamental understanding of soil P speciation is essential to assess P fate and transport in these soils. Current methods for soil P speciation often rely on sequential chemical extractions, which can introduce artifacts during analysis. To overcome limitations of current methods, this study evaluated synchrotron-based micro-focused X-ray fluorescence (µ-XRF) and X-ray absorption near-edge spectroscopy (µ-XANES) techniques to assess soil P speciation in agricultural soils collected from the mid-Atlantic region of the United States. Three soils with varying chemical and physical properties were analyzed with µ-XRF maps collected at high (12,000eV) and tender (2240eV) energies to evaluate colocation of P with Fe, Al, Ca, and Si in soil samples, and µ-XANES spectra were collected at the P K-edge for P hotspots. Combined µ-XRF and µ-XANES analysis was useful for identifying Ca phosphate, Fe phosphate, Al-sorbed P, and Fe-sorbed P species in heterogeneous soil samples. X-ray fluorescence maps were valuable to distinguish Al-oxide sorbed P from Fe-oxide sorbed P species. A low signal-to-noise ratio often limited µ-XANES data collection in regions with diffuse, low concentrations of P. Therefore, some P species may not have been detected during analysis. Even with varying degrees of self-absorption and signal-to-noise ratios in µ-XANES spectra, important inferences regarding P speciation in mid-Atlantic soils were made. This study highlights the potential of µ-XANES analysis for use in environmental and agricultural sciences to provide insights into P fate and transport in soils.

Mercury Speciation of Flue Gas Desulphurization By-Products in Coal-Fired Power Plants in China

The aim of this study was to develop and examine the morphology and distribution of mercury (Hg) in flue gas desulfurization (FGD) by-product. Mercury in the coal of coal-fired power plants is concentrated in the by-products of desulfurization process, and it is widely used as an additive in cement, building materials and other industries. Due to the different stability of various forms of mercury in the environment, subsequent use of products containing desulfurization by-product additives will continue to be released into the environment, endangering human health. Therefore, it is very necessary to study the form and distribution of mercury in the by-products of desulfurization in coal-fired power plants to provide a theoretical basis for subsequent harmless treatment. For content and morphology of mercury analysis, 1 sample of dry FGD ash and 6 samples of wet FGD gypsum were analyzed. The total 7 samples were extracted using a modification of sequential chemical extractions (SCE) method, which was employed for the partitioning Hg into four fractions: water soluble, acid soluble, H2O2 soluble, and residual. The Hg analysis was done with United States Environmental Protection Agency (USEPA) method 7471B. Comparing with the wet FGD gypsums of coal-fired boilers, the total Hg content in the dry FGD by-product was as high as 1.22 mg/kg, while the total Hg content in the FGD gypsum is 0.23 - 0.74 mg/kg, which was 2 times over the wet FGD gypsum. The concentration of water soluble Hg in the dry FGD by-product was the highest amount (0.72 mg/kg), accounting for 59.02% of the total mercury. While residual Hg content was 0.16 mg/kg, only about 13.11% of the total mercury. Mercury content in FGD gypsum was expressed in the form of ρ (residual Hg) > ρ (H2O2 soluble Hg) > ρ (water soluble Hg) > ρ (acid soluble Hg). The morphology and distribution of mercury in FGD by-products is supposed to be analyzed before utilization, and the impact of mercury on the environment should be considered.

The comparative research of leaching tests and the sequential chemical extraction based on the environmental risk assessment by a selected type of waste

The comparative research of leaching tests and the sequential chemical extraction based on the environmental risk assessment by a selected type of waste

Extraction and fractionation of subproteome from root tips of Hyoscyamus albus

Identification and quantification of different metabolites under stress, especially protein, is a vital way to understand plant adaptation mechanism. We established an efficient protein extraction method from the tiny amount (100 mg) of root tips of non-model medicinal plant Hyoscyamus albus, using bead-beating cell disruption, TRIzol extraction, and sequential chemical protein solubilization. H. albus is very well known for biosynthesized of different secondary metabolites like hyoscyamine, tropane alkaloids and scopolamine. Our method is rational for sample preparation even in small-scale proteomics of recalcitrant tissue and allows proficient, reproducible and impurity-free protein extraction. This method allows high-quality 2DE in mini-gel format (25 µg of protein/gel) for hydrophilic and hydrophobic sub-proteomes and is compatible to high-sensitive matrix-assisted laser/desorption ionization quadrupole ion trap time-of-flight (MALDI-QIT-TOF) mass spectrometry (MS). A protocol using TRIzol is more effective and reproducible to sequential chemical extraction of both hydrophilic and hydrophobic membrane proteins. We also demonstrated cell disrupted together with dithiothreitol (DTT) and polyvinylpolypyrrolidone (PVPP) is more useful to prevent polymerization of the phenolic compound than commonly used added DTT and PVPP with TRIzol reagent. Despite the unavailability of genomic sequence database, the efficacy of the protocol was also confirmed by MS/MS ion searches.&#x0D; &#x0D; J Bangladesh Agril Univ 17(4): 430–436, 2019

The assessment and remediation of mercury contaminated sites: A review of current approaches

Remediation of mercury (Hg) contaminated sites has long relied on traditional approaches, such as removal and containment/capping. Here we review contemporary practices in the assessment and remediation of industrial-scale Hg contaminated sites and discuss recent advances. Significant improvements have been made in site assessment, including the use of XRF to rapidly identify the spatial extent of contamination, Hg stable isotope fractionation to identify sources and transformation processes, and solid-phase characterization (XAFS) to evaluate Hg forms. The understanding of Hg bioavailability for methylation has been improved by methods such as sequential chemical extractions and porewater measurements, including the use of diffuse gradient in thin-film (DGT) samplers. These approaches have shown varying success in identifying bioavailable Hg fractions and further study and field applications are needed. The downstream accumulation of methylmercury (MeHg) in biota is a concern at many contaminated sites. Identifying the variables limiting/controlling MeHg production—such as bioavailable inorganic Hg, organic carbon, and/or terminal electron acceptors (e.g. sulfate, iron) is critical. Mercury can be released from contaminated sites to the air and water, both of which are influenced by meteorological and hydrological conditions. Mercury mobilized from contaminated sites is predominantly bound to particles, highly correlated with total sediment solids (TSS), and elevated during stormflow. Remediation techniques to address Hg contamination can include the removal or containment of Hg contaminated materials, the application of amendments to reduce mobility and bioavailability, landscape/waterbody manipulations to reduce MeHg production, and food web manipulations through stocking or extirpation to reduce MeHg accumulated in desired species. These approaches often rely on knowledge of the Hg forms/speciation at the site, and utilize physical, chemical, thermal and biological methods to achieve remediation goals. Overall, the complexity of Hg cycling allows many different opportunities to reduce/mitigate impacts, which creates flexibility in determining suitable and logistically feasible remedies.

Mercury Speciation in Contaminated Soils from Old Mining Activities in Mexico Using a Chemical Selective Extraction

Amalgamation was heavily used in mining since 1557 in Spanish Colonies. In Mexico and other parts of Latin-America,this process generated tailings which were left aside in the mine backyards. In the valley of Zacatecas, tailings were carried out of the mines due to the run-off from the mountains and contaminated most of the Zacatecan Valley which most important economic activity is agricultural (crop and livestock raising). The main concern in this area is the high level of total mercury found in previous studies. So far, various research studies have been conducted in Mexico toidentify the contamination by total mercury in contaminated soils. However, research has not been developed to determine the available fraction by an analysis of the chemical species present in contaminated sites, which represent a risk to human health and the environment. The aim of this study is to develop a mercury sequential chemical extraction methodology with appropriate conditions for identifying: 1) water-soluble fraction, 2) elemental fraction, 3) interchangeable fraction, 4) strongly bound fraction, 5) organic fraction, 6) fraction as sulphides and 7) residual fraction. With this, it might be determined if the mercury species present in mining soils in the state of Zacatecas, Mexico represent a potential risk because of its mobility in the different environmental compartments. Results show that chemical species in the towns of Osiris and La Zacatecana (HgS and amalgamated mercury) have high stability and low mobility.&#x0D; &#x0D; , Soil contamination, Mining wastes,Chemical selective extraction

Evaluation of the Extraction Efficiency of Heavy Metals (Pb, Cd, Cu) in Soil–Bayberry System

ABSTRACT This study focused on the efficiency of three chemical extractions (two single procedures, using EDTA or CaCl2 as a reactant, and a sequential chemical extraction) for selected metals (Pb, Cd, Cu) in real agricultural soils, which are different from most researchers using artificial deployment of contaminated soil. The total concentration of metals in soils is frequently insufficient to ascertain environmental risk. Soil washing based on chemical extraction with inorganic and organic acids, bases, surfactants, chelating agents, and redox agents has been widely applied to estimate the mobility of metals. Our results clearly showed that the applied sequential extraction procedure is less aggressive than EDTA for the studied elements. For estimation of metal mobility in real agricultural soils, EDTA leaching is better adapted for Cu, whereas the sequential extraction procedure is better suited for Pb. Different extractants should be used to assess the environmental risk of different soils, rather than to unify the established methods. The validation of the practicability of the method should be based on actual soil rather than artificial deployment of contaminated soil.

Sequential extraction for heavy metal distribution of bottom ash from fluidized bed co-combusted phosphorus-rich sludge under the agglomeration/defluidization process.

Agglomeration that occurs during municipal sewage sludge (MSS) fluidized bed co-combustion might affect heavy metal distribution and the transformation of bottom ash. A study on the mobility and speciation of heavy metals that accompanies agglomeration behavior and phosphorus addition should be examined during MSS co-combustion. Meanwhile, the aim of this study was to evaluate the total content and speciation of heavy metals during the MSS fluidized bed co-combustion by the chemical sequential extraction procedure (SEP). The risk assessment code (RAC) and individual contamination factor (ICF) are calculated to evaluate the mobility of heavy metals and their environmental risks in agglomerates. Moreover, identification of agglomerates is established by both characterization (scanning electron microscopy/energy-dispersive spectroscopy, X-ray photoelectron spectroscopy) and thermodynamic simulation (HSC chemistry software). The experimental results indicated that P and Na would form the lower melting-point compounds such as NaPO3 and Na2O in the bottom ash, which promoted agglomeration during MSS fluidized bed co-combustion. According to the simulation, Na and P have a stronger affinity than Si and Cr, and this reaction is not only influenced by particle agglomeration, but also by heavy metal distribution during modified MSS co-combustion. Nevertheless, the results of ICFs and RACs obtained from the SEP indicated that for heavy metals trapped in agglomerates, a weaker binding such as physical covering by eutectics might be considered as the dominant reaction compared with chemical binding to form a metal complex.