Ultra-trace determination of cadmium in water and food samples by a thin-film microextraction using a supported liquid membrane combined with smartphone-based colorimetric detection.

A mixture of n-octanol and dithizone was introduced as an effective and novel extraction agent in a thin-film microextraction technique for the pre-concentration of cadmium ions. The extraction agent was immobilized on small pieces of porous polypropylene flat membrane as a supported liquid membrane. The analyte extraction was performed by immersing the modified film in the sample solution, and via a complex formation between the immobilized dithizone on the film and cadmium ions. After the thin-film microextraction process, the colored cadmium-dithizone complex was directly measured by a smartphone colorimetric analysis. Under optimized conditions, the linear dynamic range, the limit of detection, and the limit of quantification were 0.5-300.0, 0.1, and 0.4 µg L-1, respectively. The developed technique was successfully employed to quantify cadmium ions in water and food samples. The high relative recovery values (95.0-103.0%) along with relative standard deviations of less than 2.5% were obtained for the spiked samples.

A chemiluminescence biosensor based on the peroxidase-like property of molybdenum disulfide/zirconium metal-organic framework nanocomposite for diazinon monitoring.

BACKGROUND: Organophosphorus pesticides are widely used in agriculture owing to their high effectiveness as insecticides. Among these, diazinon is a common environmental contaminant that acts as an acetylcholinesterase (AChE) enzyme inhibitor. As the current methods are too expensive and time-consuming for routine analysis of diazinon, its trace monitoring by rapid and sensitive methods is critical to protect the environment and human health. RESULTS: A biosensor was introduced for the indirect detection of diazinon using a molybdenum disulfide/zirconium metal-organic framework (MoS2@MIP-202(Zr)) nanocomposite. The probe is based on the peroxidase mimic of the prepared nanocomposite on NaHCO3-H2O2 chemiluminescence system as well as the inhibitory effect of diazinon on the enzymatic activity of AChE. The chemiluminescence signal is gradually decreased with an increase in diazinon concentration, and there is a linear relationship between the analytical signal and diazinon concentration. Under the optimum conditions, the calibration plot is linear in the concentration range of 0.5-300.0 nmol L-1. The limit of detection and quantification limit of the method are 0.12 and 0.40 nmol L-1, respectively. The inter-day and intra-day relative standard deviations (% RSD n = 5, diazinon concentration; 100 nmol L-1) are 3.66 and 1.35%, respectively. The method was used for diazinon detection in real water samples, and the high relative recovery values for the spiked samples along with satisfactory results of a certified reference material analysis confirmed that the method is accurate and free from the matrix effect. SIGNIFICANCE AND NOVELTY: A nano-probe based on the peroxidase-like property of MoS2@MIP-202(Zr) nanocomposite was developed for the first time for indirect detection of residue levels of diazinon in water samples. The high stability of the nanocomposite makes it a good alternative for natural peroxidase enzymes such as horseradish peroxidase with low stability.

Fluorescence resonance energy transfer between carbon quantum dots and silver nanoparticles: Application to mercuric ion sensing.

Fluorescence resonance energy transfer (FRET) process as a practical and competitive sensing strategy was utilized between carbon quantum dots (C-dots) and silver nanoparticles (Ag NPs) for the determination of mercuric ions. The novel synthesized C-dots with the quantum yield of 84% acted as the donor and Ag NPs operated as the acceptor in the FRET process leading to the fluorescence quenching of the C-dots. In the presence of Hg(II) ions, the FRET-quenched fluorescence emission of the C-dots-Ag NPs system was recovered owing to oxidation of Ag NPs by Hg(II) ions, so that the turn-on fluorescence intensity was directly proportional to the Hg(II) ion concentration. Accordingly, combination of the FRET system with the redox reaction was firstly utilized to construct an innovative turn-off/on fluorescent sensor for the quantification of Hg(II) ion. The calibration plot was linear in the concentration range 0.5-500.0 nmol L-1 with a determination coefficient (R2) of 0.9965. The limit of detection and limit of quantification were 0.10 and 0.35 nmol L-1, respectively, according to the IUPAC definition. The method was applied for the determination of Hg(II) ion in lake water, wastewater and tea samples, and the proper relative recoveries (98.0-104.0%) were obtained for the spiked samples. The method has high potential to diagnose trace values of mercuric ions in real samples with high sensitivity and repeatability.

A simple magnetic solid-phase extraction method based on magnetite/graphene oxide nanocomposite for pre-concentration and determination of melamine by high-performance liquid chromatography.

In this study, a clean and simple magnetic solid-phase extraction (MSPE) procedure using magnetite/graphene oxide nanocomposite as an adsorbent was developed for melamine separation and preconcentration from water and dairy products. After synthesis and characterization of the adsorbent, adsorption isotherms and kinetic studies of the adsorption were carried out. The analyte quantification was performed by reversed phase high-performance liquid chromatography after elution of the preconcentrated analytes from the adsorbent surface. Several factors affecting the extraction/preconcentration procedure such as pH, adsorbent amount, extraction time, sample volume, type, and volume of eluent were investigated. The optimizing of some important parameters was assessed by employing a response surface method. The constructed calibration curve in the optimized conditions is linear in the working range of 0.10-100 µg L-1 with a correlation coefficient of 0.9999. The detection limit, limit of quantification, and enrichment factor are 0.03 µg L-1, 0.10 µg L-1, and 500, respectively. The melamine relative recoveries from different real samples are between 97.20 and 103.10% with relative standard deviations of 1.07-4.98%.

Preconcentration of mercury(II) using a magnetite@carbon/dithizone nanocomposite, and its quantification by anodic stripping voltammetry.

A new adsorbent is described that consists of a magnetite@carbon/dithizone nanocomposite. It was characterized using energy-dispersive X-ray spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction, and field emission scanning electron microscopy. The magnetic sorbent is shown to be a viable material for the preconcentration of mercury(II) before its quantification by differential pulse anodic stripping voltammetry. The effects of pH value, eluent, adsorbent amount, sample volume, and adsorption/desorption time were optimized. The calibration plot extends from 0.25 to 30 ng.mL-1, and the detection limit is 27 pg.mL-1. The preconcentration factor and intra-day and inter-day relative standard deviations are 100, 3.8, and 4.5%, respectively, for six measurements at 5 ng.mL-1 concentrations of mercury(II). The method was validated by the analysis of the certified reference material NIST SRM 1566b, and successfully applied to the preconcentration and quantification of mercury(II) in industrial wastewaters and spiked water samples. Graphical abstractSchematic representation of magnetic solid-phase extraction of mercury(II) ion by dithizone-modified Fe3O4@C nanocomposite (Fe3O4@C/Dz NC) before its quantification by anodic stripping voltammetry (ASV).

A turn-on/off fluorescent sensor based on nano-structured Mg-Al layered double hydroxide intercalated with salicylic acid for monitoring of ferric ion in human serum samples.

The present work aimed to provide a novel chemosensor for ferric ion detection in human serum samples using nano-structured Mg-Al layered double hydroxide intercalated with salicylic acid (Mg-Al LDH-SA) as a sensitive fluorescence probe. The Mg-Al LDH-SA nanomaterial was synthesized and characterized via Fourier transform infrared spectroscopy, X-ray diffraction analysis, field emission scanning electron microscopy, dynamic light scattering and energy dispersive spectroscopy. The synthesized nanomaterial was applied to determine ferric ions by measuring the fluorescence intensity of Mg-Al LDH-SA sol solution at λem = 404 nm with excitation at λex = 287 nm. In the presence of ferric ions, the fluorescence intensity decreases owing to the formation of a stable complex between ferric ions and salicylic acid. Several important parameters affecting the analytical signal were studied and optimized. Under optimum conditions, the calibration graph was linear in the concentration range of 0.07-100 µmol L-1 with a corresponding detection limit of 26 nmol L-1. The intra- and inter-day relative standard deviations (n = 6 and ferric ion concentration; 50 µmol L-1) were 3.4% and 4.5%, respectively. The method was successfully employed to assess ferric ion in several human serum samples with relative recovery values between 98.7 and 104.6% for the spiked samples.

Preconcentration of morphine and codeine using a magnetite/reduced graphene oxide/silver nano-composite and their determination by high-performance liquid chromatography.

A novel magnetic solid-phase extraction technique based on a ternary nano-composite, magnetite/reduced graphene oxide/silver, as a nano-sorbent was developed for simultaneous extraction/preconcentration and measurement of morphine and codeine in biological samples by high-performance liquid chromatography. The magnetic ternary nano-composite was synthesized and its functional groups, morphological structure, and magnetic properties were characterized by field emission scanning electron microscopy, vibrating sample magnetometer, powder X-ray diffraction, energy dispersive X-ray spectroscopy and Fourier transform infrared spectroscopy. The optimizing of the significant variables affecting the extraction process was evaluated by a response surface methodology. In the optimized conditions, the constructed calibration curves for morphine and codeine are linear in the range of 0.01-10 µg L-1 with correlation coefficients of 0.9983 and 0.9976, respectively. The detection limit and enrichment factor for morphine and codeine are 1.8 ng L-1, 1000 and 2.1 ng L-1, 1000, respectively. The presented technique was employed for the monitoring of morphine and codeine in numerous blood and urine samples with relative recoveries between 97.0 and 102.5%, and relative standard deviations of 1.02-5.10% for the spiked samples.

Air-assisted liquid-liquid extraction coupled with dispersive liquid-liquid microextraction and a drying step for extraction and preconcentration of some phthalate esters from edible oils prior to their determination by GC.

In this work, a new, cheap, simple, fast, and low organic solvent consuming procedure is proposed for isolation, enrichment, and gas chromatographic determination of some phthalate esters in edible oils. The method is based on a combination of air-assisted liquid-liquid extraction and dispersive liquid-liquid microextraction followed by a drying step under N2 gas. Several experimental parameters affecting both extraction and preconcentration steps were investigated and optimized. Under the optimum conditions for the proposed method, wide linear ranges (0.05-800 µg/L) and low detection limits (0.007-0.023 µg/L) were observed. The ranges of enrichment factors and extraction recoveries were 68-340 and 14-68%, respectively. Eventually, the target analytes were successfully determined in different edible oils using the proposed method.

Preconcentration of Pb(II) by using Mg(II)-doped NiFe2O4 nanoparticles as a magnetic solid phase extraction agent.

Magnesium(II)-doped nickel ferrite (Mg-NiFe2O4) nanoparticles are introduced as a new adsorbent for magnetic solid phase extraction of lead(II) ions from aqueous solutions. The structure and morphology of the adsorbent was characterized by FTIR, X-ray diffraction and scanning electron microscopy. The effects of pH value, amount of adsorbent, type, concentration and volume of the eluent and adsorption/desorption time on the extraction efficiency were studied. Following elution with hydrochloric acid, Pb(II) ions were quantified by flame atomic absorption spectrometry. Under optimized conditions, the calibration graph is linear in the 0.5-125 ng mL-1 Pb(II) ion concentration range. Other figures of merit include (a) a 0.2 ng mL-1 limit of detection, (b) an enrichment factor of 200, (c) an intra-day relative standard deviation (for n = 6 at 50 ng mL-1) of 1.6%, and (d) an inter-day precision of 3.8%. The method was validated by the analysis of the certified reference material, NIST SRM 1566b. It was successfully applied to the determination of Pb(II) ion in spiked water samples, industrial wastewater and acidic lead battery waters. Graphical abstract Schematic of the synthesis of Mg(II)-doped NiFeO4 nanoparticles and their application as a magnetic sorbent for solid-phase extraction of a Pb(II) ions prior to determination by flame atomic absorption spectrometry (FAAS).

Utilizing of Ag@AgCl@graphene oxide@Fe3O4 nanocomposite as a magnetic plasmonic nanophotocatalyst in light-initiated H2O2 generation and chemiluminescence detection of nitrite.

A simple and sensitive chemiluminescence (CL) procedure was developed for the quantification of nitrite in aqueous solutions. The method is based on light-initiated generation of H2O2 by a magnetic Ag@AgCl@Graphene oxide nanocomposite and its subsequent redox reaction with nitrite ion in acidic medium. During the carbonate-catalyzed decomposition of produced peroxynitrite and energy transferring to uranine, a CL emission was observed at λ=534n m. Several factors affecting the CL intensity were investigated and optimized. Under optimum conditions, the CL intensity was directly proportional to the nitrite concentration in the range of 5-200 ng mL(-1). The limit of detection and relative standard deviation (for n=5; at a nitrite concentration of 70 ng mL(-1)) were 1.15 ng mL(-1) and 2.57%, respectively. The method was successfully applied to determine nitrite in food stuffs with recoveries in the range of 95.0-103.0% for the spiked samples. The accuracy of the method was evaluated by comparing the results with those obtained by analyzing the samples using a standard method.

CoFe2O4 nano-particles functionalized with 8-hydroxyquinoline for dispersive solid-phase micro-extraction and direct fluorometric monitoring of aluminum in human serum and water samples.

A simple dispersive solid-phase micro-extraction method based on CoFe2O4 nano-particles (NPs) functionalized with 8-hydroxyquinoline (8-HQ) with the aid of sodium dodecyl sulfate (SDS) was developed for separation of Al(III) ions from aqueous solutions. Al(III) ions are separated at pH 7 via complex formation with 8-HQ using the functionalized CoFe2O4 nano-particles sol solution as a dispersed solid-phase extractor. The separated analyte is directly quantified by a spectrofluorometric method at 370nm excitation and 506nm emission wavelengths. A comparison of the fluorescence of Al(III)-8-HQ complex in bulk solution and that of Al(III) ion interacted with 8-HQ/SDS/CoFe2O4 NPs revealed a nearly 5-fold improvement in intensity. The experimental factors influencing the separation and in situ monitoring of the analyte were optimized. Under these conditions, the calibration graph was linear in the range of 0.1-300ngmL(-1) with a correlation coefficient of 0.9986. The limit of detection and limit of quantification were 0.03ngmL(-1) and 0.10ngmL(-1), respectively. The inter-day and intra-day relative standard deviations for six replicate determinations of 150ngmL(-1) Al(III) ion were 2.8% and 1.7%, respectively. The method was successfully applied to direct determine Al(III) ion in various human serum and water samples.

Magnetic solid phase extraction of gemfibrozil from human serum and pharmaceutical wastewater samples utilizing a ß-cyclodextrin grafted graphene oxide-magnetite nano-hybrid.

A magnetic solid phase extraction method based on ß-cyclodextrin (ß-CD) grafted graphene oxide (GO)/magnetite (Fe3O4) nano-hybrid as an innovative adsorbent was developed for the separation and pre-concentration of gemfibrozil prior to its determination by spectrofluorometry. The as-prepared ß-CD/GO/Fe3O4 nano-hybrid possesses the magnetism property of Fe3O4 nano-particles that makes it easily manipulated by an external magnetic field. On the other hand, the surface modification of GO by ß-CD leads to selective separation of the target analyte from sample matrices. The structure and morphology of the synthesized adsorbent were characterized using powder X-ray diffraction, Fourier transform infrared spectroscopy, and field emission scanning electron microscopy. The experimental factors affecting the extraction/pre-concentration and determination of the analyte were investigated and optimized. Under the optimized experimental conditions, the calibration graph was linear in the range between 10 and 5000 pg mL(-1) with a correlation coefficient of 0.9989. The limit of detection and enrichment factor for gemfibrozil were 3 pg mL(-1) and 100, respectively. The maximum sorption capacity of the adsorbent for gemfibrozil was 49.8 mg g(-1). The method was successfully applied to monitoring gemfibrozil in human serum and pharmaceutical wastewaters samples with recoveries in the range of 96.0-104.0% for the spiked samples.

Speciation of As(III)/As(V) in water samples by a magnetic solid phase extraction based on Fe3O4/Mg-Al layered double hydroxide nano-hybrid followed by chemiluminescence detection.

A novel magnetic solid phase extraction method was developed for the speciation of As(III)/As(V) in aqueous solutions utilizing Fe3O4-doped Mg-Al layered double hydroxide (LDH) as a nano-sorbent. The method is based on the separation and pre-concentration of As(V) by Fe3O4/Mg-Al LDH nano-hybrid prior to determination by a chemiluminescence (CL) technique. The CL route involves the oxidation of luminol by vanadomolybdoarsenate heteropoly acid in a basic media. Since the existing cations cannot be adsorbed by positively charged layers of the LDH and other potentially interferent anions had no considerable effect on the CL reaction, it provides a very selective and sensitive determination approach for As(V). The determination of total arsenic and hence indirectly As(III) involve the pre-oxidation of As(III) to As(V) by a mixture of hydrogen peroxide and potassium hydroxide. Several factors affecting the extraction and determination of the analyte were investigated and optimized. Under optimum conditions, the calibration graph was linear in the range of 5.0-5000 ng L(-1). The limit of detection and enrichment factor was 2.0 ng L(-1) and 80, respectively. The method was validated by the analysis of a standard reference material (NIST SRM 1643e), and successfully applied to the speciation of arsenic in several water samples with recoveries in the range of 93.3-106.7% for the spiked samples.

Utilizing a nano-sorbent for the selective solid-phase extraction of vanillic acid prior to its determination by photoluminescence spectroscopy.

Vanillic acid (VA) is a phenolic acid, and acts as a natural antioxidant in fruits, vegetables and plants. The extraction and determination of trace levels of VA in plants is important, because stimulation of protein synthesis and activation of antioxidant enzymes occur in the presence of phenolic acids at trace levels. In this research, a photoluminescence spectroscopic method was developed for the quantification of VA in plant samples after separation and pre-concentration. Selective extraction of VA from aqueous solution was performed using a solid-phase extraction column packed with nickel-aluminum layered double hydroxide as a nano-sorbent. After elution of extracted analyte from the column using 3 mL of a 3 mol/L NaOH solution, its concentration was determined spectrofluorometrically at λ(em) = 357 nm with excitation at λ(ex) = 280 nm. The spectrofluorometry method gave a linear response for VA within the range 20.0-900.0 µg/L, with a correlation coefficient of 0.9982. The limit of detection and sorption capacity were 7.6 µg/L and 66.2 mg/g, respectively. The method was validated by comparing the obtained results with gas chromatographic data. This method was used to determine VA in Chenopodium album and Prangos asperula plants.

Trace analysis of mefenamic acid in human serum and pharmaceutical wastewater samples after pre-concentration with Ni-Al layered double hydroxide nano-particles.

In this work, the nickel-aluminum layered double hydroxide (Ni-Al LDH) with nitrate interlayer anion was synthesized and used as a solid phase extraction sorbent for the selective separation and pre-concentration of mefenamic acid prior to quantification by UV detection at λmax=286 nm. Extraction procedure is based on the adsorption of mefenamate anions on the Ni-Al(NO3-) LDH and/or their exchange with LDH interlayer NO3- anions. The effects of several parameters such as cations and interlayer anions type in LDH structure, pH, sample flow rate, elution conditions, amount of nano-sorbent and co-existing ions on the extraction were investigated and optimized. Under the optimum conditions, the calibration graph was linear within the range of 2-1000 µg/L with a correlation coefficient of 0.9995. The limit of detection and relative standard deviation were 0.6 µg/L and 0.84% (30 µg/L, n=6), respectively. The presented method was successfully applied to determine of mefenamic acid in human serum and pharmaceutical wastewater samples.

Ultratrace determination of arsenic in water samples by electrothermal atomic absorption spectrometry after pre-concentration with Mg-Al-Fe ternary layered double hydroxide nano-sorbent.

A selective solid phase extraction method, based on nano-structured Mg-Al-Fe(NO3(-)) ternary layered double hydroxide as a sorbent, is developed for the pre-concentration of ultra-trace levels of arsenic (As) prior to determination by electrothermal atomic absorption spectrometry. It is found that both As(III) and As(V) could be quantitatively retained on the sorbent within a wide pH range of 4-12. Accordingly, the presented method is applied to determination of total inorganic As in aqueous solutions. Maximum analytical signal of As is achieved when the pyrolysis and atomization temperatures are close to 900 °C and 2300 °C, respectively. Several variables affecting the extraction efficiency including pH, sample flow rate, amount of nano-sorbent, elution conditions and sample volume are optimized. Under the optimized conditions, the limit of detection (3Sb/m) and the relative standard deviation are 4.6 pg mL(-1) and 3.9%, respectively. The calibration graph is linear in the range of 15.0-650 pg mL(-1) with a correlation coefficient of 0.9979, sorption capacity and pre-concentration factor are 8.68 mg g(-1) and 300, respectively. The developed method is validated by the analysis of a standard reference material (SRM 1643e) and is successfully applied to the determination of ultra-trace amounts of As in different water samples.

D-penicillamine capped cadmium telluride quantum dots as a novel fluorometric sensor of copper(II).

D-penicillamine-capped cadmium telluride quantum dots (DPA-capped CdTe QDs) were synthesized as the new fluorescent semiconductor nanocrystal in aqueous solution. Fourier transmission infrared spectroscopy, X-ray diffraction, transmission electron microscopy, ultraviolet-visible and photoluminescence spectroscopy were used for characterization of the QDs. Based on the quenching effect of Cu(2+) ions on the fluorescence intensity of DPA-capped CdTe QDs, a new fluorometric sensor for copper(II) detection was developed that showed good linearity over the concentration range 5 × 10(-9)-3 × 10(-6) M with the detection limit 0.4 × 10(-9) M. Owing to the strong affinity of the DPA to copper(II), the sensor showed appropriate selectivity for copper(II) compared with conventional QDs. The DPA-capped CdTe QDs was successfully applied for determination of Cu(2+) concentration in river, well and tap waters with satisfactory results.

Determination of iodate in food, environmental, and biological samples after solid-phase extraction with Ni-Al-Zr ternary layered double hydroxide as a nanosorbent.

Nanostructured nickel-aluminum-zirconium ternary layered double hydroxide was successfully applied as a solid-phase extraction sorbent for the separation and pre-concentration of trace levels of iodate in food, environmental and biological samples. An indirect method was used for monitoring of the extracted iodate ions. The method is based on the reaction of the iodate with iodide in acidic solution to produce iodine, which can be spectrophotometrically monitored at 352 nm. The absorbance is directly proportional to the concentration of iodate in the sample. The effect of several parameters such as pH, sample flow rate, amount of nanosorbent, elution conditions, sample volume, and coexisting ions on the recovery was investigated. In the optimum experimental conditions, the limit of detection (3s) and enrichment factor were 0.12 µg mL(-1) and 20, respectively. The calibration graph using the preconcentration system was linear in the range of 0.2-2.8 µg mL(-1) with a correlation coefficient of 0.998. In order to validate the presented method, a certified reference material, NIST SRM 1549, was also analyzed.

Determination of selenium in serum samples of preterm newborn infants with bronchopulmonary dysplasia using a validated hydride generation system.

Bronchopulmonary dysplasia (BPD), also known as chronic lung disease, is one of the most challenging complications in premature newborn infants. Selenium plays a role in antioxidant system by protecting cell membranes and neutralizing the deleterious effects of free radicals. The aim of this study was to determine the relationship between selenium concentration and incidence of bronchopulmonary dysplasia using a validated analytical method. Umbilical cord blood and blood samples 30 days after the birth were collected from 38 preterm newborn infants with gestation age of 32 weeks or less, and the separated serums were kept at -70°C until analysis time. Selenium concentration of serum was determined using an atomic absorption spectrophotometer. The method was validated on the basis of standard validation techniques. The analytical method was linear in the range of 1 to 500 µg/L with the limit of detection of 0.4 µg/L. Samples were collected from 38 infants whose gestation age was 32 weeks or less. The blood samples were collected from the umbilical cord blood at birth in 19 cases. In 25 cases, blood samples were collected 1 month after birth. Of the 15 patients diagnosed with BPD, 10 were boys (p = 0.02). The mean serum selenium concentration was not different at birth between patients with and without BPD, but it was significantly lower at 30 days after birth in patients with BPD (38.5 ± 14.1vs. 45.4 ± 18.7 µg/L, p = 0.02). Preterm newborn infants with BPD had lower serum selenium concentrations 1 month after birth.

Ultratrace determination of cadmium by cold vapor atomic absorption spectrometry after preconcentration with a simplified cloud point extraction methodology.

A simplified micelle-mediated extraction methodology for the preconcentration of ultratrace levels of cadmium as a prior step to its determination by cold vapor atomic absorption spectrometry (CV-AAS) has been developed. The methodology is based on the cloud point extraction (CPE) of cadmium at pH 8 by using the non-ionic surfactant polyethyleneglycolmono-p-nonylphenylether (PONPE 7.5) without adding any chelating agent. Cadmium cold vapor was generated from 2ml of the extracted surfactant-rich phase by means of sodium tetrahydroborate (3%, w/v) as a reducing agent and hydrochloric acid (0.2mol l(-1)) as a carrier solution. Several important variables that affect the cloud point extraction and cold vapor cadmium generation efficiency were investigated and optimized. The preconcentration of only 50ml of solution in the presence of 0.06% (v/v) PONPE 7.5 gives an enhancement factor of 62. The calibration graph using the preconcentration system was linear in the range of 4-100ng l(-1) with a correlation coefficient of 0.9992. Detection limit (3s) obtained in the optimal conditions was 0.56ng l(-1). The relative standard deviation (R.S.D.) for six replicate determinations at 20ng l(-1) Cd level was 3.2%. The proposed method was successfully applied to the ultratrace determination of cadmium in water samples.