Solid phase extraction of trace amounts of cadmium(II) ions in water and food samples using iron magnetite nanoparticles modified by sodium dodecyl sulfate and 2-mercaptobenzothiazole.

A new, simple and rapid method for solid phase extraction and preconcentration of trace amounts of cadmium ions using 2-mercaptobenzothiazole/sodium dodecyl sulfate immobilized on magnetite nanoparticles (MBT-SDS-MNPs) was proposed. The method is based on the extraction of cadmium ions via complexation with MBT immobilized on SDS-coated MNPs and their determination by flame atomic absorption spectrometry. The effects of different parameters - pH; eluent type, concentration and volume; amounts of salt and adsorbent; contact time and interfering ions - on the adsorption of cadmium ions were studied. Under optimized conditions, the calibration curve was linear in the range of 10-5,000 µg L-1. Detection limit and relative standard deviation of the proposed method were 0.009 µg L-1 and 2.2%, respectively. The adsorption data were analyzed by Langmuir and Freundlich isotherm models and a maximum adsorption amount of 24.80 mg g-1, a Langmuir adsorption equilibrium constant (b) of 4.62 and Freundlich constants Kf and n of 6.075 mg1-1/n L1/n g-1 and 2.391, respectively, were obtained. Finally, this adsorbent was successfully used for extraction of cadmium from water and food samples.

Synthesis and application of ion-imprinted polymer nanoparticles for the extraction and preconcentration of mercury in water and food samples employing cold vapor atomic absorption spectrometry.

We describe a nanosized Hg(II)-imprinted polymer that was prepared from methacrylic acid as functional monomer, ethyleneglycol dimethacrylate as cross-linker, 2,2'-azobisisobutyronitrile (AIBN) as radical initiator, 2, 2'-di pyrydyl amine as a specific ligand, and Hg (II) as the template ions by precipitation polymerization method in methanol as the progeny solvent. Batch adsorption experiments were carried out as a function of pH, Hg (II) imprinted polymer amount, adsorption and desorption time, volume, and concentration of eluent. The synthesized polymer particles were characterized physically and morphologically by using infrared spectroscopy, thermogravimetric analysis, X-ray diffraction, and scanning electron microscopic techniques. The maximum adsorption capacity of the ion-imprinted and non-imprinted sorbent was 27.96 and 7.89 mg g(-1), respectively. Under optimal conditions, the detection limit for mercury was 0.01 µg L(-1) and the relative standard deviation was 3.2 % (n = 6) at the 1.00 µg L(-1). The procedure was applied to determination of mercury in fish and water samples with satisfactory results.

Synthesis and application of ion-imprinted polymer nanoparticles for the extraction and preconcentration of copper ions in environmental water samples.

Novel Cu(II) ion-imprinted polymers (Cu-IIP) nanoparticles were prepared by using Cu(II) ion-thiosemicarbazide complex as the template molecule and methacrylic acid, ethylene glycol dimethacrylate (EGDMA), and 2,2'azobisisobutyronitrile (AIBN) as the functional monomer, cross-linker, and the radical initiator, respectively. The synthesized polymer nanoparticles were characterized by using infrared spectroscopy (IR), thermo gravimetric analysis (TGA), X-ray diffraction (XRD), and scanning electron microscopic (SEM) techniques. Some parameters such as pH, weight of the polymer, adsorption time, elution time, eluent type, and eluent volume which affect the extraction efficiency of the polymer were studied. In the proposed method, the maximum sorbent capacity of the ion-imprinted polymer was calculated to be 38.8 mg g(-1). The preconcentration factor, relative standard deviation, and limit of detection of the method were found to be 80, 1.7%, and 0.003 µg mL(-1), respectively. The prepared ion-imprinted polymer nanoparticles have an increased selectivity toward Cu(II) ions over a range of competing metal ions with the same charge and similar ionic radius. The method was applied to the determination of ultra trace levels of Cu2+ in environmental water samples with satisfactory results.

Synthesis and application of ion-imprinted polymer nanoparticles for the determination of nickel ions.

Novel Ni(II) ion-imprinted polymers (Ni-IIP) nanoparticles were prepared by using Ni(II) ion-1,5-diphenyl carbazide (DPC) complex as the template molecule and methacrylic acid, ethylene glycol dimethacrylate (EGDMA) and 2,2'-azobisisobutyronitrile (AIBN) as the functional monomer, cross-linker and the radical initiator, respectively. The synthesized polymer particles were characterized physically and morphologically by using infrared spectroscopy (IR), thermo gravimetric analysis (TGA), X-ray diffraction (XRD) and scanning electron microscopic (SEM) techniques. Some parameters such as pH, weight of the polymer, adsorption time, elution time, eluent type and eluent volume which affects the efficiency of the polymer were studied. The preconcentration factor, relative standard deviation, and limit of detection of the method were found to be 100, 1.9%, and 0.002 µg mL(-1), respectively. The prepared ion-imprinted polymer particles have an increased selectivity toward Ni(II) ions over a range of competing metal ions with the same charge and similar ionic radius. The method was applied to the determination of nickel in tomato and some water samples.

Synthesis and application of ion-imprinted polymer nanoparticles for the extraction and preconcentration of zinc ions.

A new Zinc (II) ion-imprinted polymer (IIPs) nanoparticles was synthesised for the separation and recovery of trace Zn (II) ion from food and water sample. Zn (II) IIP was prepared by copolymerisation of methyl methacrylate (monomer) and ethylene glycol dimethacrylate (cross-linker) in the presence of Zn (II)-N,N'-o-phenylene bis (salicylideneimine) ternary complex wherein Zn (II) ion is the imprint ion and is used to form the imprinted polymer. Moreover, control polymer (NIP) particles were similarly prepared without the zinc (II) ions. The unleached and leached IIP particles were characterised by X-ray diffraction, Fourier transform infra-red spectroscopy and scanning electron microscopy. The preconcentration of Zn(2+) from aqueous solution was studied during rebinding with the leached IIP particles as a function of pH, the weight of the polymer material, the uptake and desorption times, the aqueous phase and the desorption volumes. Flame atomic absorption spectrometry was employed for determination of zinc in aqueous solution.

Determination of tramadol by dispersive liquid-liquid microextraction combined with GC-MS.

Dispersive liquid-liquid microextraction (DLLME) coupled with gas chromatography-mass spectrometry (GC-MS) has been developed for preconcentration and determination of tramadol, ((±)-cis-2-[(dimethylamino)methyl]-1-(3-methoxyphenyl)cyclohexanol-HCl), in aqueous and biological samples (urine, blood). DLLME is a simple, rapid and efficient method for determination of drugs in aqueous samples. Efficient factors on the DLLME process has defined and optimized for extraction of tramadol including type of extraction and disperser solvents and their volumes, pH of donor phase, time of extraction and ionic strength of donor phase. Based on the results of this study, under optimal conditions and by using 2-nitro phenol as internal standard, tramadol was determined by GC-MS, and the figures of merit of this work were evaluated. The enrichment factor, relative recovery and limit of detection were obtained 420, 99.2% and 0.08 µg L(-1), respectively. The linear range was between 0.26 and 220.00 µg L(-1) (R(2) = 0.9970). The relative standard deviation for 50.00 µg L(-1) of tramadol in aqueous samples by using 2-nitro phenol as IS was 3.6% (n = 7). Finally, the performance of DLLME was evaluated for analysis of tramadol in urine and blood.

A novel kinetic spectrophotometric method for the determination of ultra trace amount of cyanide.

A kinetic spectrophotometric method is described for the determination of trace levels of cyanide based on its catalytic effect on the oxidation of Janus green by ammonium peroxodisulfate in nitric acid media. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of the Janus green at 612 nm after 4 min. The effect of reaction variables on the reaction sensitivity was investigated. Under the optimized conditions, a calibration graph from 10.0 to 500.0 ng/ml of cyanide with a detection limit of 7.0 ng/m was obtained. The proposed method is simple, sensitive and inexpensive and it was applied to directly the determination of cyanide in drinking and ground waters with the satisfactory results.

Determination of thiourea in fruit juice by a kinetic spectrophotometric method.

A catalytic kinetic method is described for determination of trace levels of thiourea based on its catalytic effect on the oxidation of Janus green (JG) by potassium iodate in hydrochloric acid media. The reaction was monitored by measuring the decrease in absorbance of the dye at 610 nm after 25 min. The effect of some factors on the reaction speed was investigated. The developed method allowed the determination of thiourea in range of 0.01-12.00 mg L(-1) with good precision, accuracy and the detection limit was 0.008 mg L(-1). Most of foreign species do not interfere with the determination. The method was found to be sensitive, selective and was applied to the determination of thiourea in fruit juices and orange peel.

A kinetic method for the determination of thiourea by its catalytic effect in micellar media.

A highly sensitive, selective and simple kinetic method was developed for the determination of trace levels of thiourea based on its catalytic effect on the oxidation of janus green in phosphoric acid media and presence of Triton X-100 surfactant without any separation and pre-concentration steps. The reaction was monitored spectrophotometrically by tracing the formation of the green-colored oxidized product of janus green at 617 nm within 15 min of mixing the reagents. The effect of some factors on the reaction speed was investigated. Following the recommended procedure, thiourea could be determined with linear calibration graph in 0.03-10.00 microg/ml range. The detection limit of the proposed method is 0.02 microg/ml. Most of foreign species do not interfere with the determination. The high sensitivity and selectivity of the proposed method allowed its successful application to fruit juice and industrial waste water.