A New Chelating Reagent: Its Synthesis/Characterization and Application for the Determination of Cd(II) and Ni(II) in Various Food and Make-Up Product Samples by FAAS Using Simultaneous Microextraction Sampling

A new and simple dispersive liquid liquid simultaneous microextraction procedure was developed for the rapid separation and simultaneous extraction/preconcentration of Cd(II) and Ni(II) at ultratrace amounts. Microextraction of the analytes was carried out in the presence of 2-methyl-5-[(Z)-pyridin-4-yldiazenyl]quinolin-8-ol as the chelating reagent. Chloroform and ethanol were used as the extraction and dispersive solvents. Various parameters that influence the microextraction procedure's efficiency such as pH, centrifugation rate and time, reagent concentration, and sampling volume on the recovery of analytes were examined. The calibration curves were linear in the range of 0.01-1.25 and 0.075-5 mg/L with LODs of 0.25 and 0.84 mu g/L, and with a preconcentration factor of 94, for Cd(II) and Ni(II), respectively. Precision was >1.0%. The accuracy of the method was confirmed by analyzing the Certified Standard Reference Material (CWW-TMD: Certified wastewater-Trace metals, wastewater). The results show that the dispersive liquid liquid simultaneous microextraction pretreatment is a sensitive, rapid, simple, green, and safe method for the separation/preconcentration of cadmium and nickel

A new procedure for determination of nickel in some fake jewelry and cosmetics samples after dispersive liquid-liquid microextraction by FAAS

A new, simple and cheap dispersive liquid-liquid microextraction (DLLME) procedure was optimized for the preconcentration of trace amounts of Ni(II) as a prior step to its determination by flame atomic absorption spectrometry (FAAS). It is based on the microextraction of nickel, where appropriate amounts of the extraction solvent (CHCl3), disperser solvent (ethanol) and chelating agent, name 5-[(Z)-isoxazol-3-yl-diazenyl]-2-methyl-quinolin-8-ol (MMD), were firstly synthesized/characterized and used. Various parameters that affect the extraction procedure such as pH, centrifugation rate and time, the chelating agent (MMD) concentration and sampling volume on the recovery of Ni(II) were investigated. The preconcentration of a 20 ml sample solution was thus enhanced by a factor of 80. The resulting calibration graph was linear in the range of 0.24-10 mg L-1 with a correlation coefficient of 0.9998. The limit of detection (3 s/b) obtained under optimal conditions was 1.00 mu g L-1. The relative standard deviation for certified reference material determinations was 1.2%. The accuracy of the method was verified by the determination of Ni(II) in the certified reference material of wastewater (Waste water CWW TMD). The proposed procedure was successfully applied to the determination of Ni(II) in some fake jewelry and cosmetics samples

Application of a new functionalized magnetic graphane oxide for aluminum determination at trace levels in honey samples by the zetasizer system

Heavy metals in honey are of interest not only for quality control, but also as an environmental indicator. In the present work, we developed a new selective and rapid magnetic dispersive solid-phase extraction (MDSPE) method for the separation/determination of Al(III) in honey samples by the zetasizer system. The synthesis of a new nanocomposite comprised of aminosilanized magnetic graphane oxide (GO/Fe3O4/APS)-coated 2-hydroxy-5-methyl-1,3-benzene-dicarboxaldehyde (HB) (GO/Fe3O4/APS@HB) is synthesized and characterized in for the first time the present work. The parameters influential on the determination of Al(III) including the pH of the sample, sorption time, amount of nanocomposite, eluent type, concentration, volume, and elution time, were investigated and optimized. These magnetic nanocomposites carrying Al(III) could be easily separated from honey samples simply by applying an external magnetic field; no filtration/centrifugation was necessary. Moreover, GO/Fe3O4/APS@HB demonstrates selectivity toward Al(III). Under the optimum conditions, the detection limits (DL) of the method for Al(III) was found to be (3 s) 0.13 mu g L--1,L- the preconcentration factor was calculated as 65, and the relative standard deviation was obtained as <= 2% for n = 11. The method was performed for the determination of Al(III) in some honey samples. The proposed techniques show satisfactory sensitivity, selectivity, detection limits and standard deviation for Al(III) determination in a honey sample. The method is suitable for the analysis of honey samples, which are challenging to analyze using other spectroscopy techniques

Grafting of glutathione to magnetic graphene oxide and application for the determination of As(III)/(V) in food samples via a zeta potential analyzer

A new selective method based on magnetic dispersive solid-phase extraction (MDSPE) and a zetasizer system is proposed for the determination of As(III)/As(V) species in some water and food samples. In the developed procedure, the crucial issue is that a novel adsorbent was synthesized and characterized by grafting L-glutathione (reduced) (GSH) onto a magnetic graphene oxide surface (GO/Fe3O4@GSH) and was also applied in quantitative adsorption of As(III)/As(V) ions. Moreover, GO/Fe3O4@GSH demonstrates selectivity towards As(III) in the presence of As(V). The best determination and speciation conditions were achieved by testing different nanocomposite quantities, the pH of the sample, type of desorption solution, sample and desorption solution volumes, and the effect of interfering ions. Due to features of the GO/Fe3O4@GSH nanocomposite such as a wrinkled structure and excellent dispersibility in water, GO/Fe3O4@GSH seems to be ideal for the fast and simple preconcentration/determination of As(III)/As(V) using methodology based on MDSPE and zetasizer measurement. As(III) was quantitatively recovered with the nanocomposite at concentrations between 0.5 and 1.5 mol L-1 of HNO3, while As(V) was not quantitatively recovered at any pH. The detection limit of the method was 0.1 mu g L-1 while the relative standard deviation was 1.0% for 0.5 mg L-1 As(III). The developed method was applied successfully for the determination of As(III) in some water and tea samples, and standard reference material samples with satisfactory results. Moreover, GO/Fe3O4@GSH can be applied for arsenic speciation due to its selectivity towards arsenite

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 mu g 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 (r(2)) 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

Synthesis of novel proponohydrazides and their hydrolysis reactions

4-(4-Methoxybenzoyl)-5-(4-methoxyphenyl)-2,3-furandione 1 reacted with N-aryl substituted phenyl-hydrazones 3a-h via the p,p'-dimethoxydibenzoylketene intermediate 2 giving the proponohydrazide derivatives 5a-h. In addition, compounds 5a-h were converted into corresponding pyrazolone derivatives 7i,j by the reactions of hydrolysis in acidic solution. The structures of these new synthesized compounds were determined by C-13 NMR, H-1 NMR and IR spectroscopic data and elemental analysis