Preparative isolation and characterization of heavy metal complexes from acid mine drainage and surface wastewater

A preparative method was developed to sample dissolved organic carbon (DOC) and heavy metals (Ni, Mn) from polluted surface waters. Main focus was set on the preparative production of freeze‐dried samples mainly composed of organic ligands from heavy metal complexes. First characterizations were done in the aqueous phase. Finally, freeze‐dried samples provide stable organic matter for multiple characterizations. Acid mine drainage of the former mining area of Ronneburg (Germany) hold elevated concentrations of heavy metals and low concentrations of DOC. Municipal wastewater, passing the spoil pile, held elevated concentrations of DOC and low concentrations of heavy metals. Dissolved components smaller than 0.45 μm and larger than 1 nm were concentrated by nanofiltration. Organic heavy metal complexes were isolated from this solution by size‐exclusion chromatography (SEC). Different size classes of molecules were collected from the column effluent, depending on their elution time, and were characterized by UV spectroscopy, ICP‐OES, and DOC measurements. All samples held organic heavy metal compounds with different retention times. The organic heavy metal complexes in acid mine drainage had higher retention times than complexes from municipal wastewater. Most interestingly, we found different affinities of heavy metals to different size classes of DOC. This affinity of the heavy metals differs with size and origin of the DOC.     

Study of Metal Distribution in Raw and Screened Swine Manure

The growth of industrial swine production over the last few years has led to a growth in concern over effluents generated by the activity. Several elements, mainly toxic metals, can be present in swine wastewater and can have a serious environmental impact. It is important, therefore, to know the metal concentration before the discharge of wastewater. In this work the temporal metal distribution in swine manure and its potential reduction using coarse (2 mm) and fine (<0.45 μm) liquid‐solid separation techniques were investigated. In order to do this, different swine manure sample preparation methods for Al, Ba, Cd, Co, Cr, Cu, Fe, Mg, Mn, Ni, Pb, Sr and Zn determination by Inductively Coupled Plasma Optical Emission Spectrometry (ICP OES) were tested. The acid mixtures used to digest the manure sample significantly affected the metal recovery. Good analyte recoveries were observed with nitric acid/hydrogen peroxide mixtures or nitric acid/perchloric acid mixtures. Sulfuric acid/hydrogen peroxide mixtures produced inconsistent results and poor recoveries, mainly for Ba and Pb. It was observed that metal concentrations in swine manure varied greatly with time, up to one order of magnitude, due to changes in swine production such as feed and animal numbers. Metals concentrations observed in the raw wastewater exceeded Brazilian limits for discharge into water bodies and recommendations for agricultural use. Results obtained from the liquid‐solid separation study showed that metals in the raw swine manure were not removed with coarse screening. However, the major fraction of metals were removed by filtration (0.45 μm), with the exception of Na, K and Sr. Thus, the use of liquid‐solid separation techniques that capture the fine solid fractions (and associated metals) from raw manure can have a favorable impact on the environment and contribute to swine production wastewater treatment.     

Development of Bench‐Scale Bio‐Packed Column for Wastewater Treatment from Optical Emission Spectrometry

An eco‐friendly and inexpensive technique for wastewater treatment originated from inductively coupled plasma‐optical emission spectrometry (ICP‐OES) is presented within this paper. The proposed process comprised of loading waste crab shells in packed column for adsorption of heavy metal ions, followed by desorption using 0.01 M HCl. An exhaustive physical and chemical characterization of ICP‐OES wastewater revealed the complex nature of effluent, including the presence of 15 different metals and metalloid under strong acidic condition (pH 1.3). Based on the preliminary batch experiments, it was identified that solution pH played a major role in metal sequestration by crab shell with pH 3.5 identified as optimum pH. Rapid metal biosorption kinetics along with complete desorption and subsequent reuse for three cycles was possible with crab shell‐based treatment process. Continuous flow‐through column experiments confirmed the high performance of crab shell towards multiple metal ions with the column able to operate for 22 h at a flow rate of 10 mL/min before outlet concentration of arsenic reached 0.25 times of its inlet concentration. Other metal ions such as Cu, Cd, Co, Cr, Pb, Ni, Zn, Mn, Al, and Fe were only in trace levels in the treated water until 22 h. The performance of the treatment process was compared with trade effluent discharge standards, and the process flow diagram along with cost analysis was suggested.     

Alkaline Degradation of Dissolved Organic Matter

The degradation of dissolved organic matter (DOM) was studied in alkaline solution. The products were characterised using UV/vis spectroscopy, size‐exclusion chromatography (SEC), and by the analysis of low‐molecular‐weight organic acids (LMWOA). The degradation experiments were performed with water from a brown water lake or its isolated fulvic acid fraction and sodium hydroxide at different reaction times and temperatures. Depending on the wavelength and the reaction time, the UV/vis absorbance between 230 nm and 600 nm increased or decreased. The behaviour of model compounds during reactions in alkaline media was compared to the UV/vis spectroscopic behaviour of DOM. The release of LMWOA was described by kinetic data and compared to the data of model reactions. Evidence was given for the carboxylic esters playing a significant role in the release of LMWOA only during the beginning of the alkaline degradation. The results gained by SEC with on‐line UV and DOC detection showed that the average size of DOM was decreasing, and that a major part of the degradation products consisted of low‐molecular‐weight mono‐ and dicarboxylic acids.     

Use of the Anion‐Exchange Resin Amberlite IRA‐93 for the Separation of Arsenite and Arsenate in Aqueous Samples

The method described uses the separation of As(III) and As(V) species in aqueous samples by means of the anion‐exchange resin Amberlite IRA‐93. The samples were acidified using acetic acid and passed through a glass column filled with pre‐treated Amberlite IRA‐93 resin. As(III) was poorly adsorbed on the anionic exchanger material, whereas As(V) was retained. The arsenic concentration was measured in the column effluent by graphite furnace AAS (GF‐AAS). The retained As(V) was eluted from the column using 1 M NaOH. Prior to the determination of the As(V) concentration in the NaOH eluate, the eluate was passed through a glass column filled with a cation‐exchange resin (Amberlite 200) to remove sodium ions and minimize the Na⁺ interference with the AAS determination. After calibration the method was applied to the separation of As(III) and As(V) species in two aqueous extracts of arsenic contaminated soils. The results were compared with those obtained from an on‐line separation and determination of As(III) and As(V) in the aqueous soil extracts using a state of the art HPLC‐ICP‐MS system.     

Provenance of long‐travelled dust determined with ultra‐trace‐element composition: a pilot study with samples from New Zealand glaciers

We report high‐precision inductively coupled plasma mass spectrometric (ICP‐MS) compositional data for 39 trace elements in a variety of dust deposits, trapped sediments and surface samples from New Zealand and Australia. Dusts collected from the surface of alpine glaciers in the Southern Alps, New Zealand, believed to have undergone long‐distance atmospheric transport from Australia, are recognizable on account of their overabundances of Pb and Cu with respect to typical upper crustal values. Long‐travelled dust from Australia therefore scavenges these and other metals (e.g. Zn, Sb and Cd) from the atmosphere during transport and deposition. Hence, due to anthropogenic pollution, long‐travelled Australian dusts can be recognized by elevated metal contents. The relative abundance of 25 other elements that are not affected by atmospheric pollution, mineral sorting (Zr and Hf) and weathering[sol ]solubility (alkali and earth alkali elements) reflects the geochemistry of the dust source sediment. As a result, we are able to establish the provenance of dust using ultra‐trace‐element chemistry at regional scale. Comparison of long‐travelled dust chemistry with potential Australian sources shows that fits of variable quality are obtained. We propose that the best fitting potential source chemistry most likely represents the major dust source area. A binary mixing model is used to demonstrate that admixture of small quantities of local dust provides an even better fitting dust chemistry for the long‐travelled dusts. Copyright © 2005 John Wiley & Sons, Ltd.     

Fractionation of Ni,Cr and Cu from Soil by Sequential Extraction Procedure and Determination by Inductively Coupled Plasma Optical Emission Spectrometry

Five‐step sequential extractions were employed to fractionation of Ni, Cr and Cu in soil polluted by anthropogenic activities and determine the mobility of the metals. Twelve samples were collected on an agricultural area that was located near an airport and intercity roads in Elazig‐Turkey. Exchangeable, organically bounded, carbonate bounded, adsorbed species on Fe and Mn oxides and residual species (except silicates) of Ni, Cr and Cu were extracted into solution by using CaCl₂, Na₄P₂O₇, Na₂EDTA, NH₂OH–HCl and HNO₃–H₂O₂, respectively. Mobile metal concentrations in fractions and total recoverable in soils were determined by using inductively coupled plasma‐optical emission spectrometry (ICP‐OES). Total recoverable Ni, Cr and Cu concentrations were in the range of 40–119, 45–126 and 23–72 mg kg^?1, respectively. It was observed that total concentrations of metals in some of the samples were higher than the permitted values. The sum of the mobile percentages of metals was found to be lower than 50%. The Ni, Cr and Cu percentages for exchangeable species are in the ranges of 0.18–1.64, 0.03–0.59 and 0.42–2.53%, respectively.     

Organically Bound Nutrients in Dissolved Organic Matter Fractions in Seepage and Pore Water of Weakly Developed Forest Soils

Previous field and laboratory studies showed that organically bound nutrients can contribute largely to the export of N, P, and S from soil into aquatic systems. One possible determinant for the losses of dissolved organic nutrients leaving the soil environment could be their distribution between dissolved organic matter (DOM) fractions of different mobility in soil. To elucidate the potential influence of DOM fractions under varying flow conditions on the vertical translocation of organically bound nutrients, we determined the concentrations and fluxes of dissolved organic C (DOC) and nutrients (DON, DOP, DOS) in soil water under a Scots pine (Pinus sylvestris L.) and a European beech (Fagus sylvatica L.) forest. We sampled seepage water from the organic forest floor layer and the mineral subsoil using zero‐tension lysimeters and soil pore water using tension lysimeters and suction cups. DOM in soil water was fractionated into hydrophilic and hydrophobic compounds by XAD‐8 at pH 2. We found that the organic forest floor layers were large sources for DOC, DON, DOP, and DOS. The dissolved organic nutrients were mainly concentrated in the hydrophilic DOM fraction which proved to be more mobile in mineral soil pore water than the hydrophobic one. Consequently, the concentrations and fluxes of dissolved organic nutrients decreased less with depth than those of DOC. Concentrations as well as fluxes in subsoil pore water of DOC and dissolved organic nutrients in the studied weakly developed soils were high as compared with literature data on deeply developed forest soils. Under conditions of rapid water flow through the strongly structured mineral soil at the beech site, almost no retention of DOM took place and thus the influence of the distribution of organically bound nutrients between the DOM fractions on the export of DON, DOP, and DOS was negligible.     

Metals in Sediments of the Upper Laguna Madre

The Laguna Madre system is the largest hypersaline coastal basin in the United States. Surface sediments from 22 Upper Laguna Madre (ULM) sites were analyzed for grain size and metals (Cd, Cu, Ba, Cr, Mn, Ni, Pb, V, Zn, Fe, and Al) to assess the extent of contamination in the area. Sediments were found to consist mainly of sand texture. Clay and silts were minor constituents (<10%) of the sediments. Anomalies in metal concentrations were found at some sites and were related to probable sources, i.e., recreational and industrial activities. Concentrations of metals were normalized to grain size, Al, and Fe to distinguish natural and anthropogenic sources. Most metals showed positive correlations (p < 0.001) with Fe and Al, suggesting a natural variability of metal concentrations in sediments. Concentrations of metals, except Cd and Pb, at most sites were found to be below threshold concentrations thought to produce toxic effects in marine and estuarine organisms.     

Dissolved and particulate trace metals in meltwater from the Rhône glacier

Glacial meltwater and sediment at the source of the River Rhône have been analyzed to determine: 1. the partitioning of Al, Cd, Co, Cu, Cr. Fe, Mn, Ni, Pb and Zn between the water and particulate phase. 2. the particle size ranges which affect the dissolved trace metal ion composition of the meltwater and 3. the availability (potential release) of the ten trace metal ions from the sediment. Greater than 80% of the total Cd, Cu, Mn, Ni and Zn were found to be in operationally-defined (0.4 μm) dissolved forms. Fe and Al in the meltwater are primarily associated with particles in the size range 0.4–8 μm, while Cd. Cu, Mn, Ni and Zn occur with particles smaller than 0.1 μm. For the sediment, Cu, Ni and Pb were significantly present as exchangeable forms; only Cu, Ni, Pb and Zn were determined as organicallybound forms.     

Coupling of a Column System with ICP‐MS for the Characterisation of Colloid‐mediated Metal(loid) Transport in Porous Media

In this work a coupling method for the characterisation of colloid‐mediated transport of the metal(loid) species in porous media was developed. For this transport experiments quartz sand was used as column packing material and the synthetic three‐layer clay mineral laponite as model colloid. The determination of colloids was conducted by means of UV detection. The quantification of the metal(loid) ions was carried out in two different ways: (1) The fractions collected at the column outlet were analysed with an inductively coupled plasma mass spectrometer (ICP‐MS) (offline measurements); (2) the column system was directly coupled with ICP‐MS (online measurements). In the column experiments the influence of laponite colloids on the transport of Cu, Pb, Zn, Pt and As species was investigated. In the offline experiments as a consequence of dilution during sample preparation no metal(loid) species at the column outlet could be found. Unlike this the breakthrough of all metal(loid)s could be detected under the same experimental column conditions in the coupling experiments. This coupling technique offers the online detection of the metal species and colloidal particles with high resolution even at low concentrations and without any time‐consuming preparation. The coupling experiments have shown that the laponite particles accelerate the transport of the cationic metals. For anionic metal(loid) species no influence of laponite on their transport behaviour was found.     

泥炭沼泽不同植物群落中地表糙度变化及其影响机制

对藏南沉错CCl孔216个沉积物样品进行了15种金属元素含量的测试,研究金属元素含量的分布特征,以及与粒度参数的变化关系．结果显示：金属元素的分布特征可分为三组,K、Na、Mg、Al、Ti、Ba、Cu、Zn、Fe、Pb、Cr、V等12种元素具有较为相似的变化趋势;Ca和Sr变化趋势相同;而Mn与其他任何一种元素都不相似．元素分布与粒度参数的相关分析结果表明,Ca、Ti、Pb的变化与沉积物粒度没有明显的关系;K、Na、Al、Ba、Cu、Fe、Cr、V等8种元素与沉积物粘土含量（〈4um）呈正相关关系;Mg、Zn、Mn与粉砂含量（4—63μm）呈正相关关系;而Sr与砂含量（〉63gm）呈正相关关系本研究中大部分元素的粒度效应与其他湖泊、海洋等水体沉积物中元素的粒度效应具有一致的结果．与本岩芯已有的过去1400年来的环境重建资料对比可以发现,在不同的环境变化阶段,元素组合特征都与湖区环境状况具有较好的对应性．其中大部分元素的含量变化受物源条件即流域风化侵蚀程度的影响,而Ca含量不受沉积物粒度变化影响,且与沉积物中碳酸盐含量、Sr／Ba具有很好的相关性,说明其变化受物源条件影响小,而主要与湖水理化性质、蒸发强度以及湖泊沉积过程有关．     

Determination of Cu,Fe, and Ni in Spices after Preconcentration on Diaion‐HP 20 Resin as Their Zincon Complexes

In this work, a new separation–preconcentration method was developed for the determination of trace amounts of Cu(II), Ni(II), and Fe(III) by flame atomic absorption spectrometry (FAAS). Analytes were complexed by using zincon (2‐[2‐[alpha(2‐hydroxy‐5‐sulfophenylazo) benzylidene] hydrazino] benzoic acid sodium salt). The analyte ions were quantitatively adsorbed on a Diaion HP‐20 resin at pH 5. The retained metal ions on the resin were eluted by acetone. The analytical parameters such as pH of the sample, eluent type and volume, sample volume, and flow rates of the solution and the eluent were investigated. The influences of concomitant ions on the recoveries of the analytes were also examined. The instrumental detection limits for the analytes after application of the presented solid‐phase extraction procedure were in the range of 0.72–1.41 µg/L. The validation of the presented procedure was checked by analyzing certified reference material of SRM1515 Apple Leaves. The procedure was performed by analyzing some spice samples.     

Preparation and evaluation of polyaluminum chloride sulfate (PACS) as a coagulant to remove natural organic matter from water

A series of polyaluminum chloride sulfate (PACS) coagulants, which have different SO₄^2–/Al³⁺ and OH/Al (γ) mole ratio, has been successfully developed using AlCl₃·6H₂O, Al₂(SO₄)₃·18H₂O and Na₂CO₃ as raw materials. The coagulation performance of PACS for removing natural organic matter (NOM) from surface water was evaluated, and the effect of SO₄^2–/Al³⁺ mole ratio and γ value in coagulants PACS on DOC and UV₂₅₄ removal was determined. Furthermore, the influence of pH and dosage of the selected PACS with a SO₄^2–/Al³⁺ ratio of 0.0664 and a γ value of 2.0, which achieved the best coagulation performance for the removal of DOC and UV₂₅₄ of all PACS coagulants, on the removal of DOC and UV₂₅₄ and residual aluminum concentration in treated water was investigated. The results were compared with the ones of polyaluminum chloride (PAC) with γ value of 2.0. The experimental data show that the performance of PACS as a coagulant was highly dependent on SO₄^2–/Al³⁺ mole ratio and γ value. Both for the selected PACS and for PAC, the best DOC and UV₂₅₄ removal results were obtained in the range of pH from 5.0 to 8.2 and at the coagulation dose of 5.0 mg/L as Al. Under the optimum coagulation conditions, the selected PACS gave higher DOC and UV₂₅₄ removal efficiencies, and lower residual aluminum concentrations in the treated water than PAC. The maximum removal of DOC and UV₂₅₄ for PACS was approximately 88.0% and 93.0%, respectively. At the optimum coagulant dose and pH 6.5, the concentration of residual aluminum in treated water by both selected PACS and PAC can comply with the regulated limits. The major mechanisms of NOM removal by PACS and PAC coagulation involve complexation‐charge‐neutralization‐precipitation.     

Assessment of Metal Pollution in Water and Surface Sediments of the Seyhan River,Turkey, Using Different Indexes

The aim of this study was to assess the level of heavy metals (Al, Cd, Cr, Cu, Fe, Mn, Ni, Pb, and Zn) contamination and enrichment in the surface sediments of the Seyhan River, which is the receiving water body of both treated and untreated municipal and industrial effluents as well as agricultural drainage waters generated within Adana, Turkey. Sediment and water samples were taken from six previously determined stations covering the downstream of the Seyhan dam during both wet and dry seasons and the samples were then analyzed for the heavy metals of concern. When both dry and wet seasons were considered, metal concentrations varied significantly within a broad range with Al, 7210–33 967 mg kg^?1 dw; Cr, 46–122 mg kg^?1 dw; Cu, 6–57 mg kg^?1 dw; Fe, 10 294–26 556 mg kg^?1 dw; Mn, 144–638 mg kg^?1 dw; Ni, 82–215 mg kg^?1 dw; Pb, 11–75 mg kg^?1 dw; Zn, 34–146 mg kg^?1 dw in the sediments while Cd was at non‐detectable levels for all stations. For both seasons combined, the enrichment factor (EF) and the geo‐accumulation index (I_geo) for the sediments in terms of the specified metals ranged from 0.56 to 10.36 and ?2.92 to 1.56, respectively, throughout the lower Seyhan River. The sediment quality guidelines (SQG) of US‐EPA suggested the sediments of the Seyhan River demonstrated “unpolluted to moderate pollution” of Cu, Pb, and Zn, “moderate to very strong pollution” of Cr and Ni. The water quality data, on the other hand, indicated very low levels of these metals suggesting that the metal content in the surface sediments were most probably originating from fine sediments transported along the river route instead of water/wastewater discharges with high metal content.     

Ageing of Dissolved Halogenated Humic Substances and the Microbiological Influence on this Process

The distribution of halogens in various fractions of humic substances (HS), separated by their molecular weight, was found to be different for the different halogens. This was demonstrated for chlorine, bromine, and iodine in sewage and brown water samples by applying inductively coupled plasma mass spectrometry coupled with size‐exclusion chromatography. Quantification of the different fractions of iodinated humic substances was obtained by quadrupole mass spectrometry in connection with the isotope dilution technique using an ¹²⁹I‐enriched spike solution. Quantitative analysis was not possible for the corresponding chlorine and bromine species because of spectrometric interferences in the quadrupole instrument. The ageing of HS/halogen species was followed with respect to possible transformations of these species in a ground and sewage water sample up to eight weeks. Even if a distinct structural variation of the humic substance was observed with time by measuring the UV absorption, chlorine remained in the same molecular weight fraction and only a small change was found for the HS/bromine species after eight weeks. In contrast to these findings a substantial transformation of HS/iodine compounds took place, which demonstrated that the transfer probability of halogens from one to another HS fraction is increased with decreasing strength of the halogen bond to carbon. By comparing the results of an original sewage water sample with a filtered one and with another one which was enriched by microorganisms cultivated from the same original sample, a strong microbiological influence on the transformation of HS/iodine species was found. A quantitative balance of the corresponding HS/iodine fractions was calculated for an ageing period of eight weeks showing that iodine was preferably transferred to newly formed UV active HS substances of high molecular weight. In total, no iodine was released from the humic substances.     

Selective Separation and Preconcentration of Fe(III) and Zn(II) Ions by Solvent Extraction Using a New Triketone Reagent

A simple, rapid, and accurate method was developed for separation and preconcentration of trace levels of iron(III) and zinc(II) ions in environmental samples. Methyl‐2‐(4‐methoxy‐benzoyl)‐3‐(4‐methoxyphenyl)‐3‐oxopropanoylcarbamate (MMPC) has been proposed as a new complexing agent for Fe(III) and Zn(II) ions using solvent extraction prior to their determination by flame atomic absorption spectrometry (FAAS). Fe(III) and Zn(II) ions can be selectively separated from Fe(II), Pb(II), Co(II), Cu(II), Mn(II), Cr(III), Ni(II), Cd(II), Ag(I), Au(III), Pd(II), Cr(VI), and Al(III) ions in the solution by using the MMPC reagent. The analytical parameters such as pH, sample volume, shaking time, amount of MMPC reagent, volume of methyl isobutyl ketone (MIBK), effect of ionic strength, and type of back extractant were investigated. The recovery values for Fe(III) and Zn(II) ions were greater than 95% and the detection limits for Fe(III) and Zn(II) ions were 0.26 and 0.32 µg L^?1, respectively. The precision of the method as the relative standard deviation changed between 1.8 and 2.1%. Calibration curves have a determination coefficient (r²) of at least 0.997 or higher. The preconcentration factor was found to be 100. Accuracy of the method was checked by analyzing of a certified reference material and spiked samples. The developed method was applied to several matrices such as water, hair, and food samples.     

Quantitative Separation of As(III) and As(V) from a Synthetic Water Solution Using Ion Exchange Columns in the Presence of Fe and Mn Ions

The quantitative separation of As(III) from a water sample containing As(III) and As(V) in the presence of Fe and Mn in an ion exchange resin (AG1 X8) column for the speciation of arsenic is described. Individual and combined effects of Fe and Mn on the separation of As(III) from the solution have been studied separately. In absence of Fe and Mn, the ratio between the As(T) concentration in the eluent and the As(III) concentration in the original sample has been found to be 0.9717 under optimum process conditions. The presence of Fe(II) in the water sample increased the As(T) concentration in the eluent whereas Mn(II) decreased it. Combined effects of Fe and Mn on the percentage increment in the eluent arsenic concentration have been expressed by additive and interactive models. The interactive model has been developed by a statistical software with a 95 % confidence level. In most of the cases the error on the determination of the As(III) concentration had a minimum when using the interactive model.     

Transport and retention of Escherichia coli in a mixture of quartz,Al‐coated and Fe‐coated sands

Transport and retention of Escherichia coli through the mixture of quartz, Al‐coated and Fe‐coated sands was examined using column experiments to investigate the effect of geochemical heterogeneity on bacteria transport. The first set of the experiments was performed in quartz, Al‐coated and Fe‐coated sand mixtures (coated sand: 0, 5, 10, 25, 50, 100%) to examine the influence of positively‐charged sand grains on bacteria transport. The second experiments were carried out to observe the impact of pH (range 6·74–8·21) on bacteria transport in the mixture of quartz 50% and Fe‐coated sand 50%. The third experiments were conducted to analyse the effect of ionic strength (0, 50, 100, 200 mM) on bacteria transport in the mixture of quartz 50% and Al‐coated sand 50%. The first experiments show that bacterial mass recoveries were in the range of 3·6–43·4%, decreasing nonlinearly as the content of Al‐ and Fe‐coated sands increased. In the second experiments, the bacterial mass recoveries were in the range of 35·5–79·2%, increasing linearly as the solution pH increased. In the third experiments, the mass recovery was 3·4% at 0 mM. As the ionic strength increased to 50mM, the mass recovery decreased to 0%. When the ionic strength increased further to 100 and 200 mM, no bacterial mass was recovered as in the case of 50 mM. It indicates that in the mixed medium of quartz 50% and Al‐coated sand 50% both positive (increment of bacterial adhesion) and negative (decrement) effects of ionic strength may be counterbalanced, minimizing the impact of ionic strength on the bacterial adhesion. This study helps to understand the role of metal oxides and solution chemistry in the transport of bacteria in geochemically heterogeneous media Copyright © 2008 John Wiley & Sons, Ltd.     

Coprecipitation with Cu(II)‐4‐(2‐Pyridylazo)‐resorcinol for Separation and Preconcentration of Fe(III) and Ni(II) in Water and Food Samples

The coprecipitation method is widely used for the preconcentration of trace metal ions prior to their determination by flame atomic absorption spectrometry (FAAS). A simple and sensitive method based on coprecipitation of Fe(III) and Ni(II) ions with Cu(II)‐4‐(2‐pyridylazo)‐resorcinol was developed. The analytical parameters including pH, amount of copper (II), amount of reagent, sample volume, etc., were examined. It was found that the metal ions studied were quantitatively coprecipitated in the pH range of 5.0–6.5. The detection limits (DL) (n = 10, 3s/b) were found to be 0.68 µg L^?1 for Fe(III) and 0.43 µg L^?1 for Ni(II) and the relative standard deviations (RSD) were ≤4.0%. The proposed method was validated by the analysis of three certified reference materials (TMDA 54.4 fortified lake water, SRM 1568a rice flour, and GBW07605 tea) and recovery tests. The method was successfully applied to sea water, lake water, and various food samples.