SPECTROPHOTOMETRIC DETERMINATION OF Cu(II) AND Ni(II) USING 4 PHENYL-3-THIOSEMICARBAZONE OF 2-HYDROXY-4-n- PROPOXY-5-BROMOACETOPHENONE (HnPBAPT) AS ANALYTICAL REAGENT (original) (raw)
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2013
Trace amount of Copper(II) has determined by spectrophotometric technique using 1-(2-pyridylazo)- 2-naphthal (PAN), as a new spectrophotometric reagent which is insoluble in water. PAN reacts in highly acidic solution at pH 2.40 to 2.50 with Cu(II) to give a pink chelate which has an absorption maximum (λmax.) at 550nm. The reaction is instantaneous and absorbance remains stable for over 48hrs. The average molar absorption co- efficient (e) was found to be 2.05×10 4 L mol -1 cm -1 and Sandell sensitivity is 3.23×10 −4 μg cm −2 . Linear calibration graphs were obtained for 0.1-4.0 μgL -1 of Cu(II) and RSD (%) is 1.16. The stoichiometric composition of the chelate is 1:2 (Cu:PAN). Large excess of over 50 cations, anions, and some common complexing agents (e.g. oxalate, phosphate, tartarate, thio-urea) do not interfere in the determination. The method was successfully used in the determination of Cu(II) in Several Standard Reference Materials as well as in some environmental and indust...
Egyptian Journal of Chemistry, 2020
2-(4-biphenyl)imidazo[1,2-]pyrimidine-3-hydrazone (BIPH) is synthesized and used as a new complexation analytical reagent in quantitative determination of copper ions, a yellowish green complex is resulted from this reaction. At the beginning, the reaction conditions were optimized at 430 nm which is the maximum wave length () of the complex. The linear concentration range is 0.05-500ppm and the limit of detection is 0.122 ppm. To test validity of this determination method, it was applied on samples with different matrix, and copper ion concentrations such as life samples of urine, tap water, wastewater and industrial samples of 4%copper alloy and 99%copper alloy. Standard addition method is also used to avoid matrix effect on analytical results. In application of suggested method, the values of relative error were (-4.536)-2.071% and values of recoveries were 95.46-102.07%. The high stability constant of resulted complex (K=0.25×10 8), and the simplicity in procedure of complex preparation, both provided us a motivation to prepare complex, and to study some of its characteristics by performing the identified analyses such as FTIR, UV-Visible spectroscopy, SEM+EDX, conductance measurement, reflectance percent R% to enrich the proposed structure of complex.
Ecological Processes, 2015
Introduction: The copper content in natural waters usually range from 0.2 to 30 μg/L. The higher concentrations are habitually found in industrial effluents and other contaminated waters. Methods: This work develops the spectrophotometric method of determination of copper (II) microgram amounts with a new reagent-sodium salt of 4-phenylsemicarbazone 1,2-naphthoquinone-4-sulfonic acid (L), used as a ligand for a new coordination compound of copper (II). The complex formation is accompanied by color change, allowing use of this property for quantitative determination of copper (II) ions in various objects such as: alloys, superconducting ceramics and tap water. The determination of copper (II) ions has been carried out by voltammetric and spectrophotometric methods. Results: The complex of composition CuL is stable within the pH range from 5.74 to 6.51. Its stability constant is logβ = 4.53. The molar absorption coefficient of the complex has been found. Both methods give the same concentration of about 0.0400 mg/L of copper (II) in tap water, ceramics, and alloys. The detection limit of the spectrophotometric determination of copper (II) ions in the presence of the main metal ions in tap water is 0.012 mg/mL. Conclusions: The advantages of this method are the simplicity of the synthesis of reagent, its ease of recrystallization from water-ethanol solution, and stability in the crystalline state.
Spectrophotometric and Fluorometric Studies of cobalt(II), zinc(II), nickel(II), iron(II) and copper(II) of Pyruvic acid 4-phenyl-3-thiosemicarbazone, 2018
The reagent pyruvic acid 4-phenyl-3-thiosemicarbazone (PAPTSC) was prepared by simple condensation reaction between pyruvic acid and 4-phenyl-3-thiosemicarbazide and characterized by Fourier transform-infra red (FT-IR), Ultraviolet-visible (Uvvis)spectroscopy, mass spectrometry and thermal analysis. The reactions of the reagent towards cobalt(II),zinc(II), nickel(II), iron(II)and copper(II) were examined spectrophotometrically and spectrofluorometrically. Experimental conditions were optimized in terms of reaction time, solution stability, pH and concentration of reagent per determination for maximum absorbance. Factors affecting fluorescence intensities were also optimized. Linear calibration range obeying Beer's law was within 5-25µg/mL with molar absorptivity 0.119-0.171×10 4 L.mol-1 .cm-1 and fluorescence intensities of emission were within 666-724 nm with excitation within 332-361 nm respectively. The highly stable complexes once formed did not show any change in absorbance up to 24 hours. The method was u sed for the determination of copper from different copper wires and iron and zinc from pharmaceutical preparations.
Rasayan journal of Chemistry, 2018
The simultaneous spectrophotometric method is described for the determination of Cu(II) and Co(II) by 5bromosalicylaldehyde thiosemicarbazone (5-BSAT) using partial least squares regression method. The ligand reacts with two ions to form greenish yellow and brown colored [Cu(II)-5-BSAT] and [Co(II)-(5-BSAT)2] complexes, respectively. The absorption peaks of these complexes were found overlapping at λmax of 378 nm and 381 nm, respectively. Formation of all of these complexes was complete within 20 min at pH 5.0. The linear ranges were 4.0×10-6 M-9.6×10-6 M for Cu(II) and 8.0×10-6 M-8.0×10-5 M for Co(II) with molar absorptivity, ε of 1.09×10 4 L.mol −1 .cm −1 and 1.42×10 4 L.mol −1 .cm −1 , respectively. Partial least squares (PLS) regression method is proposed for the simultaneous determination of these ions with the spectrophotometric absorbance data between wavelengths 370 and 446 nm at an interval of 4 nm. A training set was generated and its accuracy was tested in a test set. The test set garnered a root mean square error (RMSE) of 0.192 for copper and 0.489 for cobalt. The relatively small RMSE suggests only a small difference between predicted versus measured concentrations, demonstrating the accuracy of our model. The proposed method is successfully employed in the analysis of water sample for determining concentrations of copper and cobalt.
The new organic reagent 2-[Benzo thiazolyl azo]-4,5-diphenyl imidazole was prepared and used as complexing agent for separation and spectrophotometric determination of Cu 2+ ion in some samples include plants, soil, water and human blood serum. Initially determined all factors effect on extraction method and the results show optimum pH was (pH ex =9), optimum concentration was 40μg/5mLCu 2+ and optimum shaking time was (15min.), as well stoichiometry study appears the complex structure was 1:1 Cu 2+ : BTADPI. Interferences effect of cations were studied. Synergism effect shows MIBK gave increasing in distribution ratio (D). Organic solvent effect appears there is no any linear relation between dielectric constant for organic solvent used and distribution ration (D). Thermodynamically found the reaction was Endothermic reaction, with ΔH ex = 0.0131 KJ.mole-1 ,ΔG ex =-54.20 KJ.mole-1 ,ΔS ex = 167.84 J.mole-1 .Beer's law was obeyed over the concentration 1-30μg/5mL, and ε=922.90 Lmol-1 .cm-1 ,with detection limit 1.7×10-5 and Sandell's sensitivity 6.8× 10-7 gcm-2 .
Spectrochimica Acta Part A-molecular and Biomolecular Spectroscopy, 2011
A simple and selective spectrophotometric method was developed for the determination of copper(II) with 1-(2 ,4 -dinitro aminophenyl)-4,4,6-trimethyl-1,4-dihydropyrimidine-2-thiol [2 ,4 -dinitro APTPT] as a chromogenic reagent. The procedure was based on the synergistic extraction of copper(II) with 2 ,4 -dinitro APTPT in the presence of 0.5 mol L −1 pyridine to give green colored ternary complex of a molar ratio 1:2:2 (M:L:Py) in the pH range 8.7-10.5. It exhibits a maximum absorption of colored complex at 445 nm and 645 nm in chloroform against the reagent blank. Beer's law was followed in the concentration range 10-80 g mL −1 of copper(II) and optimum range of 20-70 g mL −1 the metal as evaluated from Ringbom's plot. The molar absorptivity and Sandell's sensitivity of copper(II)-2 ,4 -dinitro APTPT-pyridine complex in chloroform are 0.87 × 10 3 L mol −1 cm −1 and 0.072 g cm −2 , respectively. The interfering effects of various cations and anions were also studied, and use of suitable masking agents enhances the selectivity of the method. The proposed method is rapid, reproducible and successfully applied for the determination of copper(II) in binary and synthetic mixtures, alloys, pharmaceutical formulations, environmental and fertilizer samples. Comparison of the results with those obtained using an atomic absorption spectrophotometer also tested the validity of the method.