Evaluation of toxic metals in the industrial effluents and their segregation through peanut husk fence for pollution abatement

The industrial pollution is exponentially growing in the developing countries due to the discharge of untreated effluents from the industries in the open atmosphere. This may cause severe health hazards in the general public. To reduce this effect, it is essential to remove the toxic and heavy metals from the effluents before their disposal into the biosphere. In this context, samples of the effluents were collected from the textile/yarn, ceramics and pulp/paper industries and the concentrations of the toxic metal ions were determined using neutron activation analysis (NAA) technique. The observed concentration values of the As, Cr and Fe ions, in the unprocessed industrial effluents, were 4.91 ± 0.8, 9.67 ± 0.7 and 9.71 ± 0.8 mg/L, respectively which was well above the standard recommended limits (i.e. 1.0, 1.0 and 2.0 mg/L, respectively). In order to remove the toxic metal ions from the effluents, the samples were treated with pea nut husk fence. After this treatment, 91.5% arsenic, 81.9% chromium and 66.5% iron metal ions were successfully removed from the effluents. Then the treated effluents contained concerned toxic metal ions concentrations within the permissible limits as recommended by the national environmental quality standards (NEQS).     

Parts per trillion level determination of endocrine-disrupting chlorinated compounds in river water and wastewater effluent by stir-bar-sorptive extraction followed by gas chromatography–triple quadrupole mass spectrometry

A new analytical method using stir-bar-sorptive extraction (SBSE) followed by liquid desorption (LD) and gas chromatography with triple-quadrupole mass spectrometric detection (GC-QqQ-MS-MS) has been used for quantitative determination of 25 chlorinated endocrine-disrupting compounds (EDCs) in river water and wastewater. The experimental conditions affecting the SBSE-LD performance were studied and are discussed in detail. Results from systematic assay revealed that a 100-mL water sample, stir bars coated with 47?μL PDMS, an extraction time of 14?h (at 900?rpm), 5?% MeOH as modifier and 10?% NaCl resulted in the best analytical recovery of all the target compounds studied. Use of 1:1 ACN-MeOH as back-extraction solvent and two successive sonication steps, each for 5?min, resulted in the best performance for monitoring EDCs in water matrices. The method detection limits for most of the target compounds were very good- ≤?2?ng?L(-1) and ≤10?ng?L(-1) for river water and wastewater effluents respectively. Experimental recovery for all the compounds was >70?%, with the exception of simazine for which recovery from the matrix was 65?%. Signal enhancement observed for a few of the compounds in wastewater effluents was managed by use of matrix-matched standards and different injection liners. The method was successfully used for analysis of river water samples from Henares River (Spain) and wastewater effluent samples from wastewater-treatment plants (WWTP). Eleven of the 25 compounds studied were detected in both river water and wastewater effluents. Terbutylazine and methoxychlor were detected in almost all the river water and effluent samples; amounts varied between 37-58.5?ng?L(-1) and 15.2-46.8?ng?L(-1), respectively. This method was shown enable reliable, effective, and sensitive monitoring of chlorinated EDCs at nanogram levels in surface water and wastewater effluent.     

Inorganic by-products in waters disinfected with chlorine dioxide

The continuing diminishing sources of fresh waters has stimulated the search for unconventional water resources, such as effluents from municipal sewage treatment plants, which can be reused for purposes of irrigation in agriculture, cooling water in industry, groundwater aquifer recharge and in the long term even for drinking water. The main problem of using effluents is the presence of pathogenic bacteria and viruses that can affect human and animal health. Therefore, disinfection has been used for many years to control and reduce waterborne diseases.At the moment, most water treatment plants use sodium hypochlorite as their primary biocide. However, the toxicity of chlorinated organic compounds produced during the treatment has led to increased interest in the use of alternative agents. One possible candidate as viable substitute of free chlorine is chlorine dioxide. Before this disinfectant can be recommended for routine use, it is imperative that its safety be assessed.In this research we have investigated the presence of chlorite and chlorate in sewage disinfected with chlorine dioxide. The effect of initial concentration of biocide and contact time was evaluated using a pilot plant fed with the effluent of a municipal treatment plant. Moreover, the influence of ClO₂ generator performance was analyzed and discussed.     

Matrix effect in high‐performance liquid chromatography‐tandem mass spectrometry analysis of antibiotics in environmental water samples

This paper describes the matrix effect during the analysis of ten antibiotic compounds in water by SPE followed by HPLC‐ESI‐MS/MS. The target analytes were tetracycline, oxytetracycline (tetracyclines), sulfathiazole, sulfamethazine, sulfadiazine (sulfonamides), erythromycin‐H₂O, roxithromycine, spiramycin (macrolides), ofloxacin, and norfloxacin (quinolones). The matrix effect was examined for internal standards and the target analytes in five different water matrixes, with signal suppression being increased in the order: ultrapure water, tap water, river water, sewage effluent, and sewage influent. A combined application of the internal standards and matrix‐matched extract calibration was shown to be successful in compensating the matrix effect for the analytes. The procedural recovery of the target compounds in sewage effluents and influents was higher than in river water samples, which was further enhanced by sample acidification to pH 2. The validity of the internal standard based matrix‐matched calibration approach was verified by the standard addition method.     

Analysis of organic amines and acids for water

Conventional methods for the determination of cyanide in effluents associated with steel-making procedures are compared with a method based on a cyanide-selective electrode. For cyanide levels above 1.0 mg l^-1, the standard argentimetric titration and electrode method give similar results. At lower levels (0.1–1.0 mg l^-1 and 0.01–0.10 mg l^-1), the potentiometric method is compared with pyridine-pyrazolone and pyridine—barbituric acid colorimetric procedures; the pyrazolene method tends to give higher results than the other two methods. Synthetic standards and actual effluent samples are discussed. Problems associated with the determination of cyanide in effluents containing complex iron cyanides and sulphides are examined. Sulphide removal with lead carbonate or cadmium carbonate above pH 11 should not be done until after the distillation.     

Simultaneous determination of benzotriazoles and ultraviolet filters in ground water, effluent and biosolid samples using gas chromatography-tandem mass spectrometry

A new method using gas chromatography-tandem mass spectrometry (GC-MS/MS) was developed for the determination of four benzotriazoles, i.e. benzotriazole (BT), 5-methylbenzotriazole (5-TTri), 5-chlorobenzotriazole (CBT), 5,6-dimethylbenzotriazole (XTri), and six UV filters, i.e. benzophenone-3 (BP-3), 3-(4-methylbenzylidene)camphor (4-MBC), octyl 4-methoxycinnamate (OMC), 2-(3-t-butyl-2-hydroxy-5-methylphenyl)-5-chloro benzotriazole (UV-326), 2-(2'-hydroxy-5'-octylphenyl)-benzotriazole (UV-329), and octocrylene (OC) in ground water, effluent and biosolid samples. Solid phase extraction (SPE) and pressurized liquid extraction (PLE) were applied as the preconcentration method for water samples (ground water and effluent) and biosolid samples, respectively. The optimized method allowed us to quantify all target compounds with the method detection limits ranging from 0.29 to 11.02 ng/L, 0.5 to 14.1 ng/L and 0.33 to 8.23 ng/g in tap water, effluent and biosolid samples, respectively. The recoveries of the target analytes in tap water, effluent and biosolid samples were 70-150%, 82-127% and 81-133%, respectively. The developed analytical method was applied in the determination of these target compounds in ground water, effluent and biosolid samples collected from Bolivar sewage treatment plants in South Australia. In effluent samples, the target compounds BT, 5-TTri, CBT, XTri and BP-3 tested were detected with the maximum concentration up to 2.2 μg/L for BT. In biosolid samples, eight out of ten compounds tested were found to be present at the concentrations ranging between 18.7 ng/g (5-TTri) and 250 ng/g (4-MBC).     

Geospatial and statistical approaches to nitrate health risk and groundwater quality assessment of an alluvial aquifer in SE Nigeria for drinking and irrigation purposes

In agricultural districts, like Ogbaru in southeastern Nigeria, water supplies are under obvious threats from human activities. Therefore, continuous monitoring and assessment of water quality suitability for drinking, domestic, and irrigation purposes are encouraged to keep check of the effects of water contaminants. In this paper, several quality water assessment tools were integrated to determine the suitability of the groundwater in Ogbaru for drinking and irrigation uses and to assess the ingestion and dermal health risks of nitrate occurrence. The majority of the physicochemical parameters analyzed in this study were within their respective standard limits. However, groundwater quality index classified 52.63% of the groundwaters as excellent water and 47.37% as good water. Overall index of pollution, on the other hand, classified 84.21% as excellent water and 15.79% as acceptable water. The pH ranged from 5.4 to 6.8, indicating that the groundwater is acidic. Most irrigation water quality assessment indices (SAR, Na%, PS, KR, RCO, CAI-1 and 2) revealed that the groundwater samples are suitable for irrigation. However, magnesium hazard and permeability index grouped the majority of the water samples as unsuitable resources for irrigation uses. The nitrate health risk assessment (mean score = 1.371) indicated that children are exposed to higher non-carcinogenic health risk due to ingestion of contaminated groundwater than the other populations. It was observed that 21.05% of the groundwater samples had the highest concentrations of the analyzed chemical species. Multivariate statistical methods (hierarchical cluster analysis and factor analysis) efficiently aided the contaminant source apportionment. Based on the findings of this paper, it is advised that adequate regulatory strategies and water treatment techniques be adopted in the area to protect and sustain the groundwater quality and public health.     

Kinetic speciation of nickel in mining and municipal effluents

This study presents the results of kinetic speciation of nickel in undiluted mining and municipal effluents and effluents diluted with receiving freshwaters from the surrounding environment. The dilution ratios used for the dilution of the effluents were arbitrarily chosen, but were representative of the prevailing mining practices. The purpose of the this dilution was to mimic dilution with natural waters that result from dilution of the mining and municipal effluents with receiving freshwaters, so that this study would reveal environmental realities that are of concern to the managers and regulators of water resources. Ligand exchange kinetics using the competing ligand exchange method (CLEM) was studied using two independent techniques: graphite furnace atomic absorption spectrometry (GFAAS) with Chelex 100 resin as the competing ligand, and adsorptive cathodic stripping voltammetry (AdCSV) with dimethylglyoxime (DMG) as the competing ligand to determine the percentage of Ni metal released from Ni(II)–DOC complexes and the rate of dissociation of Ni(II)–DOC complexes. Using a sample containing a mixture of 30% Copper Cliff Mine effluent, 40% Sudbury municipal effluent and 30% Vermillion River water, both techniques gave results showing that the dilution of the effluent samples increased the percentage of nickel released from Ni(II)–DOC complexes. This increase in the release of nickel from the Ni(II)–DOC complexes may be of concern to managers and regulators of water resources. Agreement between the results of these two techniques has enhanced the validity of the competing ligand exchange method used by both techniques.     

Decolorization of Distillery Effluent Using Poly(Vinyl Chloride) and Cellulose Acetate Phthalate as Adsorbents

Decolorization of distillery effluents, using low cost polymer adsorbents, is one of the challenging areas for environmental technologists. Untreated distillery effluents are harmful to the environment, causing foul smell, spoiling fresh water sources and killing aquatic life. The color of distillery effluents have been decolorized by using polymer based adsorbents, such as poly(vinyl chloride) (PVC) and cellulose acetate phthalate (CAP), which are water insoluble, easily available, and cheap. In the present article, special emphasis is given to studies such as the effect of contact time, dosage amount, dilution, and the variation in the amount of sample on the degree of decolorization of the effluent. The decolorization of a distillery effluent was monitored by using UV/Visible spectroscopy and Fourier transform infrared spectroscopy (FTIR). From these studies, it was noticed that moderate to fair results were obtained and it was also found that CAP was a better adsorbent, compared to PVC, for decolorization of distillery effluents.     

A critical review of hazardous waste generation from textile industries and associated ecological impacts

Among many industries, the textile industry is the oldest industry of human civilization. Cloth is the second most important human need after food. Textile processing includes several steps in which wet processing is the most important. As wet processing involves an extensive amount of water and chemicals, an enormous volume of textile effluent generates during wet processing. Textile effluents is disposed of on bare land or on water bodies, which causes soil and water contamination. Improper disposal of textile effluents causes severe soil and water contamination. Textile effluents contain dyes, heavy metals, inorganic salts, surfactants, organic contaminants, oil, and grease. Textile effluents cause contamination in water bodies. The colour present in effluents hinders the photosynthesis of aquatic plants. Inorganic salts cause the degradation of water quality and soil excellence. Heavy metals enter the food chain and cause severe health impacts on human life. Various physical, chemical, bailogical and hybrid methods are used to treat textile effluents. Textile processing has been explained in brief in this study. The current research deals with different textile processing steps, various pollutants generated in textile processing and their ecotoxicity, various ecological crises associated with textile processing, and numerous treatment methods for the remediation of textile effluents.     

Multi-residue analytical method for human pharmaceuticals and synthetic hormones in river water and sewage effluents by solid-phase extraction and liquid chromatography–tandem mass spectrometry

Pollutants such as human pharmaceuticals and synthetic hormones that are not covered by environmental legislation have increasingly become important emerging aquatic contaminants. This paper reports the development of a sensitive and selective multi-residue method for simultaneous determination and quantification of 23 pharmaceuticals and synthetic hormones from different therapeutic classes in water samples. Target pharmaceuticals include anti-diabetic, antihypertensive, hypolipidemic agents, β2-adrenergic receptor agonist, antihistamine, analgesic and sex hormones. The developed method is based on solid phase extraction (SPE) followed by instrumental analysis using liquid chromatography-electrospray ionization-tandem mass spectrometry (LC–ESI-MS/MS) with 30 min total run time. River water samples (150 mL) and (sewage treatment plant) STP effluents (100 mL) adjusted to pH 2, were loaded into MCX (3 cm³, 60 mg) cartridge and eluted with four different reagents for maximum recovery. Quantification was achieved by using eight isotopically labeled internal standards (I.S.) that effectively correct for losses during sample preparation and matrix effects during LC–ESI-MS/MS analysis. Good recoveries higher than 70% were obtained for most of target analytes in all matrices. Method detection limit (MDL) ranged from 0.2 to 281 ng/L. The developed method was applied to determine the levels of target analytes in various samples, including river water and STP effluents. Among the tested emerging pollutants, chlorothiazide was found at the highest level, with concentrations reaching up to 865 ng/L in STP effluent, and 182 ng/L in river water.     

Analysis of wastewater samples by direct combination of thin-film microextraction and desorption electrospray ionization mass spectrometry

An analysis method for aqueous samples by the direct combination of C18/SCX mixed mode thin-film microextraction (TFME) and desorption electrospray ionization mass spectrometry (DESI-MS) was developed. Both techniques make analytical workflow simpler and faster, hence the combination of the two techniques enables considerably shorter analysis time compared to the traditional liquid chromatography mass spectrometry (LC-MS) approach. The method was characterized using carbamazepine and triclosan as typical examples for pharmaceuticals and personal care product (PPCP) components which draw increasing attention as wastewater-derived environmental contaminants. Both model compounds were successfully detected in real wastewater samples and their concentrations determined using external calibration with isotope labeled standards. Effects of temperature, agitation, sample volume, and exposure time were investigated in the case of spiked aqueous samples. Results were compared to those of parallel HPLC-MS determinations and good agreement was found through a three orders of magnitude wide concentration range. Serious matrix effects were observed in treated wastewater, but lower limits of detection were still found to be in the low ng L(-1) range. Using an Orbitrap mass spectrometer, the technique was found to be ideal for screening purposes and led to the detection of various different PPCP components in wastewater treatment plant effluents, including beta-blockers, nonsteroidal anti-inflammatory drugs, and UV filters.     

Evaluation of an hPXR reporter gene assay for the detection of aquatic emerging pollutants: screening of chemicals and application to water samples

Many environmental endocrine-disrupting compounds act as ligands for nuclear receptors. Among these receptors, the human pregnane X receptor (hPXR) is well described as a xenobiotic sensor to various classes of chemicals, including pharmaceuticals, pesticides, and steroids. To assess the potential use of PXR as a sensor for aquatic emerging pollutants, we employed an in vitro reporter gene assay (HG5LN-hPXR cells) to screen a panel of environmental chemicals and to assess PXR-active chemicals in (waste) water samples. Of the 57 compounds tested, 37 were active in the bioassay and 10 were identified as new PXR agonists: triazin pesticides (promethryn, terbuthryn, terbutylazine), pharmaceuticals (fenofibrate, bezafibrate, clonazepam, medazepam) and non co-planar polychlorobiphenyls (PCBs; PCB101, 138, 180). Furthermore, we detected potent PXR activity in two types of water samples: passive polar organic compounds integrative sampler (POCIS) extracts from a river moderately impacted by agricultural and urban inputs and three effluents from sewage treatment works (STW). Fractionation of POCIS samples showed the highest PXR activity in the less polar fraction, while in the effluents, PXR activity was mainly associated with the dissolved water phase. Chemical analyses quantified several PXR-active substances (i.e., alkylphenols, hormones, pharmaceuticals, pesticides, PCBs, bisphenol A) in POCIS fractions and effluent extracts. However, mass-balance calculations showed that the analyzed compounds explained only 0.03% and 1.4% of biological activity measured in POCIS and STW samples, respectively. In effluents, bisphenol A and 4-tert-octylphenol were identified as main contributors of instrumentally derived PXR activities. Finally, the PXR bioassay provided complementary information as compared to estrogenic, androgenic, and dioxin-like activity measured in these samples. This study shows the usefulness of HG5LN-hPXR cells to detect PXR-active compounds in water samples, and further investigation will be necessary to identify the detected active compounds.     

Chemical speciation of Co, Ni, Cu, and Zn in mine effluents and effects of dilution of the effluent on release of the above metals from their metal-dissolved organic carbon (DOC) complexes

The paper explores the lability of DOC complexes of Co, Ni, Cu, and Zn in the mining effluent, and investigates the effects of dilution of the effluent on the release of metals from the metal-DOC complexes. This study was done using competing ligand exchange method in conjunction with adsorptive cathodic stripping voltammetry on effluent samples from Copper Cliff Mine, Sudbury, Canada, using two samples of the effluent: one, undiluted (100%) effluent, and the other, diluted (45%) effluent. The dilution was done with tap water in order to determine the effects of dilution on the metal complexes in the effluents when they were discharged into receiving streams of freshwaters. The dilution of the effluent had a small effect on release of Cu from the Cu-DOC complexes, but had a much greater effect on the release of Zn from the Zn-DOC complexes. The release of Ni and Co from their DOC complexes decreased drastically on dilution of the effluent. The much greater release of Cu from the Cu-DOC complexes compared to the release of Ni, Co, and Zn from their DOC complexes in both the undiluted and the diluted effluent was probably due to the higher absolute concentration of Cu and the higher [Cu]/[DOC] ratio. The drastic decrease in the release of Ni and Co from the Ni- and Co-DOC complexes in the diluted (45%) effluent compared with the undiluted (100%) effluent probably resulted from strengthening of the metal-DOC bond due to the reduced screening of charges by a smaller concentration of Ca²⁺ in the diluted (45%) effluent. This work also shows that change in the ionic strength produces conformational changes in and in aggregation and precipitation of the DOC and also changes in electrostatic interactions between the metal cations and the humate polyanions.     

Analytical approach for monitoring endocrine-disrupting compounds in urban waste water treatment plants

The presence of endocrine-disrupting compounds in influent and effluent water samples from four waste water treatment plants located in Italy was studied. The estrogen-like activity of the water samples was measured using a chemiluminescent recombinant yeast assay which is based on genetically engineered yeast cells that express the human estrogen receptor. This receptor, once activated, elicits the expression of the reporter gene lac-Z and, consequently, the production of β-galactosidase, which is then measured by chemiluminescence. To control and minimize sample matrix effects, an external control based on a modified yeast strain stably expressing β-galactosidase was developed and also used in the assay. Rapid and sensitive chemiluminescent enzyme immunoassays were also developed and validated for the quantification of 17β-estradiol, estrone, and estriol in waste water samples. Results from both methods were compared with a reference high-performance liquid chromatography and electrospray ionization tandem mass spectrometry (HPLC ESI-MS-MS) method developed for the quantification of natural estrogens. The recombinant yeast assay revealed a significant estrogenic activity in the influent samples, ranging from 80 to 400 pmol/L 17β-estradiol equivalents (EEQ), which was reduced by 70–95 % in the effluent samples. The yeast assay also showed a systematic 20–30 % overestimation of estrogenic activity relative to the HPLC ESI-MS-MS method, suggesting the presence of other compounds in the samples with estrogenic activity. The chemiluminescent enzyme immunoassays showed the presence of estrogens in the influent samples (mean concentrations: 350–450 pmol/L for estrone, 5–100 pmol/L for 17β-estradiol, 25–300 pmol/L for estriol), with significantly lower concentrations detected in the respective effluent samples. The waste water treatment was able to reduce natural estrogen concentrations by 40–95 %, although a high variability was observed. The enzyme immunoassay data correlated well with data obtained by the HPLC ESI-MS-MS method. Although the recombinant yeast assay represents a useful tool for a first-level screening of estrogenic activity due to its simplicity and high analytical throughput, sample matrix effects observed in waste water of industrial origin were found to strongly affect the yeast cells response, even when properly corrected for using the external control, thereby limiting its use to urban waste water. Its integration with chemiluminescent enzyme immunoassays would improve its performance by reducing false negative results, thereby enabling its use in extensive studies monitoring for the presence of endocrine-disrupting compounds in urban treatment plant effluents.     

Simultaneous Determination of Sulfonamides, Fluoroquinolones, Macrolides and Trimethoprim in Wastewater and River Water by LC-Tandem-MS

A sensitive and highly selective method for the simultaneous determination of sulfonamides, macrolides, fluoroquinolones and trimethoprim in wastewater and river water has been developed. Samples were enriched by solid-phase extraction and analysed by reversed-phase liquid chromatography coupled to electrospray ionisation tandem mass spectrometry. Several surrogate standards were used for quantification purposes. Absolute recoveries of individual antimicrobials were between 49 and 133% with RSD between 1 and 18% in all investigated matrices. Detection limits in low ng L^?1 range were achieved. The method was successfully applied to the analysis of raw municipal wastewater, wastewater effluents and river waters.     

Evaluation of toxicity level of the polluted eco-system for an industrial city of Pakistan

The indiscriminate discharge of untreated industrial effluents and solid wastes into the open environment poses a serious threat to the ecosystem. Gujranwala is an industrial city of Pakistan wherein a large number of different industries are situated and majority of them are not equipped with proper recycling or effluent treatment plants. Unfortunately, untreated industrial effluents are locally used for the irrigation purposes which may result in higher concentrations of toxic metals in the crops and vegetables. Therefore, prime objective of the present study was to determine concentrations of toxic metals in the polluted soils, vegetables and crops grown in the vicinity of industrial areas using neutron activation analysis technique. The results obtained showed higher values of toxic metals in the studied samples. The observed highest concentration of As (0.94 ± 0.06) in spinach, Br (69 ± 9) in turnip, Co (0.83 ± 0.01) in millet, Cr (51.7 ± 4.2) in wheat, Mn (76.2 ± 7.3) in tomato, Sb (0.5 ± 0.06) in rice, Cl (31698 ± 3921) and Se (3.4 ± 0.4) in carrot. These values are higher than those reported in the literature.     

Application of dispersive liquid–liquid microextraction followed by HPLC–MS/MS for the trace determination of clotrimazole in environmental water samples

A method for the analysis of clotrimazole was developed with dispersive liquid–liquid microextraction for sample pre‐concentration and HPLC–MS/MS for analysis. A linear ion trap was used for the confirmation of clotrimazole identity in the samples. The developed method enables the analysis of clotrimazole in river water and sewage effluent from wastewater treatment plants with a LOQ of 0.7 ng/L. Environmental monitoring of clotrimazole was undertaken. Samples from river water and sewage effluents were analysed over a one‐year period. Clotrimazole was found in every tested sample with concentration range from 1 to 31 ng/L. The amount of clotrimazole in tested samples was highly dependent on sampling season. The highest results were obtained in summer and autumn.     

Tandem on-line dialysis with a double and single dialyser in flow injection dialysis — Simultaneous determination of calcium and high chloride in industrial effluents

The on-line double membrane dialyser described previously was coupled in series to a single dialyser in the manifold of a flow injection system to include the determination of samples with a high chloride content simultaneously with calcium in industrial effluents from a single sample injection. 50 μl of industrial effluent samples are injected into a carrier stream and are simultaneously dialysed in the double on-line dialyser for chloride and calcium. The dialysed chloride sample zones are further directed to a second dialyser that is incorporated in series with the first dialyser. This enables laboratories to determine samples with a very high chloride content up to 60 g/l simultaneously with calcium by using an automated tandem on-line dialysis technique. The fast and reliable fully automated two-component flow injection procedure operated at a sampling frequency of 90 samples per hour and the results obtained for chloride and calcium in industrial effluents compared well with those obtained by standard methods.     

Trace Determination of Benzalkonium Chlorides in River and Wastewater by Capillary Electrophoresis following Solid‐Phase Extraction Coupled with Salting‐Out Extraction

Trace levels analysisbenzalkonium chlorides (BAKs) in river water and wastewater treatment plants (WWTP) effluents were determined by capillary electrophoresis (CE) following solid‐phase extraction (SPE) and salting‐out extraction. Salting‐out extraction using an appropriate ratio of sodium chloride (NaCl) and acetonitrile (ACN) mixed with concentrated SPE elutant was capable of providing more than 500‐fold enhancement in detection sensitivity. The ratios of ACN and NaCl for salting‐out extraction were investigated and optimized. Matrix interference was eliminated by salting‐out extraction. Limits of quantitation of BAK homologues were achieved at 0.1 μg/L in 250 mL water samples. Recoveries of BAKs in various spiked water samples ranged from 70% to 84% with relative standard deviation (RSD) less than 9%. Trace amounts of total BAKs were detected in river water and WWTP effluent samples ranging from 27 to 145 μg/L at the first time by CE.