A sensitive spectrophotometric method for the determination of arsenic in environmental samples

We developed a cost-effective and sensitive spectrophotometric method for the determination of arsenic at trace level using a new reagent, leuco malachite green. Here we show that, arsenic reacts with potassium iodate in acidic conditions to liberate iodine, and the liberated iodine selectively oxidizes leuco malachite green to malachite green dye. We studied the Beer’s law at 617 nm, which showed linearity over the concentration range 0.09–0.9 μg ml⁻¹ of arsenic. We show that the molar absorptivity, Sandell’s sensitivity and detection limit of the method are 6.1 × 10⁴ l mol⁻¹ cm⁻¹, 0.0012 μg cm⁻² and 0.025 μg ml⁻¹, respectively. We applied the developed method for the determination of arsenic in environmental samples.     

Biosorption of hexavalent chromium and malachite green from aqueous effluents,using Cladophora sp.

Biosorption potential of green macroalgae Cladophora sp., (GAC) for the removal of hexavalent chromium (Cr(VI)) and malachite green (MG) from aqueous medium was investigated. Optimal conditions for biosorption experiments were determined as a function of initial pH, GAC dosage, temperature and initial concentration of Cr(VI) and MG. The biosorption equilibrium data were fitted with the isotherm models of Langmuir, Freundlich, Kiselev, Frumkin and Jovanovic, while the experimental data were analysed using the kinetic models such as pseudo-first-order, pseudo-second-order, Ritchie's and intraparticle diffusion. The Langmuir maximum biosorption capacity was calculated as 100.00?mg/g (Cr(VI)) and 142.85?mg/g (MG). The biosorption kinetic data showed better agreement with the pseudo-second-order kinetic model. The thermodynamic parameters indicated spontaneous and endothermic nature of the biosorption process for Cr(VI) removal, whereas exothermic in the case of MG removal. Furthermore, the biosorption efficiencies of the GAC reusability were found significant up to five cycles and tested using 0.1, 0.5 and 1.0?M HCl, respectively. The results of the present study indicated that GAC is a suitable biosorbent for the sequestration of Cr(VI) and MG from aqueous solutions.     

A fast and reliable method for quantitative determination of total mercury in vegetables

A cloud-point extraction (CPE) process using the nonionic surfactant, polyethylene glycol tert octylphenyl ether (Triton X-114) was employed for determination of Hg(II) ions in aqueous solutions. The method is based on the ion-pairing reaction of Hg(II) with Pyronin B (PyrB⁺) in the presence of excess iodide at pH 6.0 and extraction of the complex formed. The chemical variables affecting CPE efficiency were studied, and the analytical characteristics of the method were obtained. The calibration curves were linear in the range of 1–40 μg L^?1 with the detection limits of 0.35 and 0.30 μg L^?1 at 556 and 521 nm. Selectivity was also tested. The coefficients of variation of the method are 2.4% and 5.2% for five replicate measurements of mercury at levels of 10 and 25 μg L^?1, respectively. The results obtained for two certified reference samples were in a good agreement with the certified values. The method was applied to the determination of total mercury in vegetable samples.     

孔雀绿染料的微生物脱色研究

从印染废水处理池的活性污泥中分离到五株对孔雀绿染料有脱色能力的细菌,其中编号为３＃的菌株人苍白杆菌（Ｏｃｈｒｏｂａｃｔｒｕｍ ａｎｔｈｒｏｐｉ）的脱色能力较强。对３＃菌株的脱色反应条件进行初步研究表明,３＃细菌的脱色反应的ｐＨ为５－１１,最佳范围ｐＨ６－７;温度１０－３０℃,最佳温度３０℃;有氧气民政部下的脱色效果较缺氧情况下好;在最佳条件下该菌对孔雀绿染料的脱色作用较强,处理４、１２、２４ｈ后,     

酞菁锌改性介孔分子筛催化降解孔雀石绿

以介孔分子筛MCM-41为载体,采用浸渍法将1,4,8,11,15,18,22,25-八环戊氧基酞菁锌(α-CyOPcZn)负载到分子筛上得到了一种新型的催化剂CyOPcZn/MCM-41.并通过氮气吸附、红外光谱扫描及电镜扫描对催化剂的结构进行表征.考察了该催化剂的用量、H2O2浓度对孔雀石绿降解作用的影响.实验结果表明,在模拟可见光照射下,当催化剂用量0.6 g.L-1、H2O2浓度为0.1 mmol.L-1时,60 min后使0.1 mmol.L-1的孔雀石绿水溶液的脱色率达到98.6%,并呈现出一级反应的动力学特征,速率常数k为0.0891 min-1.催化剂重复使用3次后,脱色率可达96%以上.     

Preparation of magnetic nanocomposite beads and optimizing the conditions for effective removal of U(VI) from aqueous solutions

Magnetic ion-imprinted polymers (IIPs) were prepared by precipitate polymerization and leached with HCl to remove uranium. Their ability to remove hexavalent uranium from wastewater effluents was studied. Batch adsorption studies to determine the optimum conditions of U(VI) removal were conducted at different levels of sample pH, sorbent amount, agitation time, and initial uranium concentration. It was observed that, under optimum conditions (i.e. pH 4, adsorbent amount of 50 mg, 45 min agitation time, and initial U(VI) concentration of 2 mg L^?1), the maximum removal of U(VI) cations was >98% and 80% for the magnetic IIP and the corresponding magnetic non-imprinted polymers (NIP), respectively. Langmuir and Freundlich isotherms were used to describe the adsorption of U(VI) onto magnetic IIP and NIP. The adsorption capacity of U(VI) was determined to be 1.06 and 0.85 mg g^?1 for the two isotherms, respectively. The order of selectivity was found to be U(VI) > Fe(III) > Pb(II). For six cycles of regeneration and reuse, the magnetic polymers maintained their stabilities with only a 4% loss in the extraction efficiency. The average extraction efficiencies of the magnetic polymers for the spiked acid mine drainage and sewage wastewater effluents were 71% and 58% for the magnetic IIP and NIP, respectively. From powder X-ray diffraction analysis, application of the Scherrer equation yielded magnetic nanoparticles of an average mean diameter of 11.9 nm. Thermo-gravimetric analysis revealed that the HCl-leached magnetic polymers had a magnetite residual weight of 5%.     

Cloud point extraction of trace cyanide from environmental waters for indirect flame atomic absorption spectrometric determination

A method has been developed for indirect determination of cyanide in environmental waters based on cloud point extraction (CPE), preconcentration and determination by flame atomic absorption spectrometry (FAAS). The method was based on reduction of Cu(II) to Cu(I) in the presence of cyanide and complexation of the produced Cu(I)(CN)₂^? with gallocyanin (GC⁺) as an ion-pairing reagent at pH 4.0, followed by its extraction into polyethyleneglycol mono-p-nonylphenylether (Ponpe 7.5). Selectivity was improved with the use of suitable masking agents. Various factors influencing separation and preconcentration of cyanide have been investigated, and conditions were optimized, allowing determination of cyanide in the range of up to 1.2 mg L^?1 with a detection limit of 0.00045 mg L^?1. The method has been applied to the determination of cyanide in environmental waters, the results being in agreement with those obtained by a reference method.     

Ligand-less in situ surfactant-based solid phase extraction for preconcentration of silver from natural water samples prior to its determination by atomic absorption spectroscopy

A simple and rapid ligand-less in situ surfactant-based solid phase extraction method for preconcentration of silver from water samples is developed. In this method, a cationic surfactant containing a proper alkyl group (n-dodecyltrimethylammonium bromide) is dissolved in the aqueous sample and then a proper ion-pairing agent (ClO₄^?) is added. Due to the interaction between surfactant and ion-pairing agent, solid particles are formed and used for adsorption of silver carbonate. After centrifugation, the sediment is dissolved in 2.0 mL 1 M HNO₃ in ethanol and then aspirated directly into the flame atomic absorption spectrometer. Variables affecting the extraction efficiencies such as pH, concentrations of surfactant and CO₃^2?, ion pair concentration, and extraction time, are optimized. Under such conditions, the calibration curve is linear from 3 to 700 μg L^?1. Detection limit is 1.1 μg L^?1 with an enrichment factor of 37. The relative standard deviation for eight replicate measurements of 100 μg L^?1 is 2.1%. The method has been applied for the determination of silver in water samples.     

A sensitive method for selective determination of vanadium species by dispersive liquid–liquid microextraction (DLLME) with spectrophotometric detection

A simple, fast, and low-cost analytical procedure was developed for trace-level determination of inorganic vanadium species by dispersive liquid–liquid microextraction in combination with spectrophotometry. Vanadium in pentavalent form, V(V), was quantitatively extracted into organic phase as 4-(2-pyridylazo)-recorcinol (PAR) complex in the presence of N-cetyl-N,N,N-trimethyl ammonium bromide (CTAB) as counter-ion. Vanadium (IV) was masked with 1,2-diaminocyclohexanetetraacetic acid to allow speciation analysis. Total vanadium was determined after oxidation of V(IV) to V(V). The main factors affecting preconcentration and spectrophotometric detection of vanadium species such as pH, concentration of PAR and CTAB, the type and volume of the extraction, and disperser solvents were optimized. The limit of detection and enhancement factor obtained under optimum conditions were found to be 0.06 μg L^?1 and 98, respectively. Relative standard deviations for V(IV) and V(V) at 3.0 μg L^?1 were less than 2.4%. The presented procedure was applied to environmental water samples for selective determination of vanadium species. Moreover, the method was applied to determination of vanadium in edible salt samples, due to its applicability in high-NaCl-containing solutions. The validity of proposed method was proven by spike recovery experiments and also independent analysis by inductively coupled plasma mass spectrometry.     

Degradation of biopolymeric pigments in distillery spentwash by electrocoagulation using copper anodes: statistical and canonical analysis

The electrocoagulation studies of distillery spentwash using copper anodes were utilized to demonstrate the usefulness of Box–Behnken experimental design of response surface analysis to derive a statistical model and the optimum parameters for color removal. The current intensity (1.5 A), dilution (10%) and time of electrolysis (5 h) had been found to be the optimum conditions for maximum 77.11% color removal. The actual color removal at optimized conditions was found to be 78.26%, which is to the predicted response using response surface methodology. The energy consumption and current efficiency were determined from reduction in chemical oxygen demand.     

Determination of cobalt by air-assisted liquid–liquid microextraction

Abstract

A rapid and selective technique for extraction, preconcentration and determination of trace amounts of cobalt in water and pharmaceutical samples by air-assisted liquid–liquid microextraction combined with flame atomic absorption spectrometry is proposed. 1-Nitroso-2-naphthol is used as a complexing agent and 1-octanol as an extraction solvent. Parameters relevant for analytical effectivity, i.e. pH of sample solution, concentration of complexing agent, volume of extraction solvent, and number of extraction cycles are optimized using a Box–Behnken design. At optimum conditions, a dynamic linear range of 5–600?µg L^?1 is obtained, with a limit of detection of 1.2?µg L^?1. The method is used for determination of Co(II) in environmental water and pharmaceutical samples.     

Room temperature aqueous Paal–Knorr pyrrole synthesis catalyzed by aluminum tris(dodecyl sulfate)trihydrate

This article reports a novel procedure to prepare pyrroles using a modification of the Paal–Knorr reaction. Water is a safe solvent meeting environmental considerations, but most organic substrates are not soluble in water. A possible solution to improve the solubility of substrates is the use of surface-active reagents that can form micelles. For instance, combined Lewis acid–surfactant catalyst acts both as a Lewis acid to activate the substrate molecules and as a surfactant to form emulsions in water. Here, we prepared and used aluminum tris(dodecyl sulfate)trihydrate to condense various amines to 2,5-hexadione at room temperature. The sole solid pyrrole was separated by a simple filtration. Our findings thus show a novel and improved modification of the Paal–Knorr reaction in terms of mild reaction conditions and clean reaction profiles, using a simple workup procedure and improved yields with excellent chemo-selectivity.     

乳状液膜法萃取氨基酸的研究

本文以ＴＯＭＡＣ为载体，ＥＣＡ４３６０Ｊ为表面活性剂，内外相Ｃｌ＾－浓度梯度为推动力，研究了Ｌ－苯丙氨酸在乳状液膜体系中的传输，并对影响液膜萃取的各种因素进行了系统的阐述，确定了此体系的最佳膜相组成的实验条件，实现了Ｌ－苯丙氨酸的提取和浓缩。     

A Biosurfactant-Enhanced Soil Flushing for the Removal of Phenanthrene and Diesel in Sand

In order to examine the potential of biosurfactants in soil remediation, and to investigate the effects of several operating conditions, such as flow rate, biosurfactant concentration and surfactant type, biosurfactant-enhanced soil flushing was conducted. In the biosurfactant-enhanced soil flushing process, the removal efficiency increased as the flow rate decreased. Rhamnolipid showed no effect on the removal efficiency of phenanthrene and diesel from sand in the concentration range 0.3-0.5%. However, rhamnolipid showed higher efficiencies for the removal of phenanthrene and diesel from sand than Tween 80. Based on total recovery, following an equivalent pore volume flush, it was more difficult to remove diesel than phenanthrene. In order to obtain the specific removal efficiency, more pore volumes of surfactant solution may be required in field applications. Under optimum conditions, the biosurfactant removed as much as 70% of the phenanthrene and 60% of the diesel in the sand. These results indicate that the use of biosurfactants in the flushing process is favorable, not only with respect to the environment, but also on removal efficiencies.     

A preliminary assessment of levels of antifouling booster biocides in harbours and marinas of the island of Gran Canaria, using SPE-HPLC

An analytical procedure was developed to allow for the study of the levels of concentration of biocides in the various different ports on the island of Gran Canaria, The Canary Islands. The analytes studied were extracted from water samples using solid-phase extraction and then determined by high-performance liquid chromatography using a diode array detector. The relative standard deviations of the developed procedure were under 12%. Recoveries over 85% and limits of detection between 0.007 and 0.4 μg/L were obtained for all the analytes. The method was applied to the analysis of sea water samples from the ports and marinas on the island of Gran Canaria.     

Uptake and depuration of cesium in the green mussel Perna viridis

 The accumulation and depuration of Cs in the green mussels (Perna viridis) commonly found in the subtropical and tropical waters were studied under the laboratory conditions using radiotracer techniques. Following an initial rapid sorption onto the mussel's tissues, uptake of Cs exhibited linear patterns over a short exposure time (8 h) at different ambient Cs concentrations. The concentration factor was independent of ambient Cs concentration. The calculated uptake rate and initial sorption constant of Cs were directly proportional to the ambient Cs concentration. The calculated uptake rate constant from the dissolved phase in the mussels was as low as 0.026 l g⁻¹ d⁻¹. Uptake rates of Cs in the mussels were inversely related to the ambient salinity. Uptake increased about twofold when the salinity was reduced from 33 to 15 ppt. The effect of salinity on Cs uptake was primarily due to the change in ambient K⁺ concentration. The uptake rate decreased in a power function with increasing tissue dry weight of the mussels, although the initial sorption was not related to the mussel's body size. The efflux rate constant of Cs in the mussels was 0.15 to 0.18 d⁻¹, and was the highest recorded to date among different metals in marine bivalves. The efflux rate constant also decreased in a power function with increasing tissue dry weight of mussels. A simple kinetic model predicted that the bioconcentration factor of Cs in the green mussels was 145, which was higher than measurements taken in their temperate counterparts. The bioconcentration factor also decreased in a power function with increasing tissue dry weight of mussels. Received: 27 October 1999 / Accepted: 16 June 2000     

Removal of arsenic in tailings by soil flushing and the remediation process monitoring

In order to investigate the optimum conditions for the application of soil flushing of arsenic, a batch test was carried out using EDTA at various concentration and pH levels. Based on the optimum condition derived from the batch test, a column test was conducted to examine the feasibility of the soil-flushing technology under field-equivalent conditions. In this column test, a low flushing solution flow rate showed a significantly higher As removal efficiency (71.6%) than a high flow rate (56.3%). TCLP (toxicity characteristic leaching procedure) and a seed germination test were carried out to monitor the toxicity both during and after the treatment. The finally treated tailings were shown to be significantly remediated, having a reduced toxicity by both the TCLP and seed germination tests.     

Removal of arsenic in tailings by soil flushing and the remediation process monitoring

In order to investigate the optimum conditions for the application of soil flushing of arsenic, a batch test was carried out using EDTA at various concentration and pH levels. Based on the optimum condition derived from the batch test, a column test was conducted to examine the feasibility of the soil-flushing technology under field-equivalent conditions. In this column test, a low flushing solution flow rate showed a significantly higher As removal efficiency (71.6%) than a high flow rate (56.3%). TCLP (toxicity characteristic leaching procedure) and a seed germination test were carried out to monitor the toxicity both during and after the treatment. The finally treated tailings were shown to be significantly remediated, having a reduced toxicity by both the TCLP and seed germination tests.     

乳化液膜法提取苯酚的动力学研究

研究了以双丁二烯亚胺－煤油作膜相,ＮａＯＨ溶液为内水相的乳化液膜提取苯的动力学特性,测定了膜相与内外水相组成,搅拌速度,温度对提取速率的影响,得出了提取速率规律。     

As(III) adsorption onto Fe-impregnated food waste biochar: experimental investigation,modeling, and optimization using response surface methodology

Biochar derived from food waste was modified with Fe to enhance its adsorption capacity for As(III), which is the most toxic form of As. The synthesis of Fe-impregnated food waste biochar (Fe-FWB) was optimized using response surface methodology (RSM), and the pyrolysis time (1.0, 2.5, and 4.0 h), temperature (300, 450, and 600 °C), and Fe concentration (0.1, 0.3, and 0.5 M) were set as independent variables. The pyrolysis temperature and Fe concentration significantly influenced the As(III) removal, but the effect of pyrolysis time was insignificant. The optimum conditions for the synthesis of Fe-FWB were 1 h and 300 °C with a 0.42-M Fe concentration. Both physical and chemical properties of the optimized Fe-FWB were studied. They were also used for kinetic, equilibrium, thermodynamic, pH, and competing anion studies. Kinetic adsorption experiments demonstrated that the pseudo-second-order model had a superior fit for As(III) adsorption than the pseudo-first-order model. The maximum adsorption capacity derived from the Langmuir model was 119.5 mg/g, which surpassed that of other adsorbents published in the literature. Maximum As(III) adsorption occurred at an elevated pH in the range from 3 to 11 owing to the presence of As(III) as H₂AsO₃^? above a pH of 9.2. A slight reduction in As(III) adsorption was observed in the existence of bicarbonate, hydrogen phosphate, nitrate, and sulfate even at a high concentration of 10 mM. This study demonstrates that aqueous solutions can be treated using Fe-FWB, which is an affordable and readily available resource for As(III) removal.