Cloud point extraction and determination of Nickel (II) ions complex in real samples using New azo reagent
DOI:
https://doi.org/10.6084/rjas.v1i2.304Keywords:
Cloud point extraction, Azo preparation identification, thermodynamic treatment, purification Ni 2Abstract
New azo reagent(2-[Ceffodoxime azo]-4-Nitro -2-Phenol) ( CefAN) preparation by coupled reaction. The reagent was diagnosed by spectral methods using infrared (FTIR) and (UV. –Vis.) as an identification using( HNMR) spectrum and (C.H.N).This reagent use to determination nickel (II) ion as a pair ion complex that extracted and estimated according to the cloud point extraction(CPE) technique in enrichment layer ,after adjusting the optimal conditions and factors affected in efficiency extraction processes .The ion pare complex of nickel(II) is estimated according to the spectral method at λmax =401 nm. The optimization of complexation and extraction conditions by (CPE) investigated as well as optimum pH =10, critical concentration of TX-100 was 0.2mL, heating time=80C˚. Thermodynamic parameters of CPE for extraction process of the ion-pair association complex in Triton X-100 were also considered ΔH = 129.107264KJ ,ΔG=-56.4845 KJ and ΔS =525.75552J That referred endothermic reaction, withLimit of Detection (LOD=5.044µg mL-1) and Limit of Quantitation (LOQ=50.044 µg mL-1) ,Molar absorptivity (Ɛ= 3888.4L.mol-1.cm-1).The Stiochoimetry study to determination complex stricture that ratios of metal: reagent obtained are (1:1). Under the optimized conditions of a 10 mL sample gave preconcentration and enrichment factors are(50 and 10.1055) respectively withSandell's sensitivity(1.4854 x10-6µg cm-2/0.001A.U). The calibration curve linear in the range of 1-8ppm with a correlation coefficient of 0.9972. The relative standard deviation for replicate determinations at (30) µg 10mL−1 level is58.63%. The proposed method applied for the determination of nickel in fish, vegetables, plant leaves and water which gave satisfactory results.
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