scholarly journals Spectrophotometric Determination of Trace Concentrations of Copper in Waters Using the Chromogenic Reagent 4-Amino-3-Mercapto-6-[2-(2-Thienyl)Vinyl]-1,2,4-Triazin-5(4H)-One: Synthesis, Characterization, and Analytical Applications

2020 ◽  
Vol 10 (11) ◽  
pp. 3895 ◽  
Author(s):  
Salman. S. Alharthi ◽  
Hamed. M. Al-Saidi

A simple, selective, and inexpensive spectrophotometric method is described in the present study for estimation of trace concentrations of Cu2+ in water based on its reaction with chromogenic reagent namely 4-amino-3-mercapto-6-[2-(2-thienyl)vinyl]-1,2,4-triazin-5(4H)-one (AMT). The reaction between copper(II) ions and AMT reagent gives [Cu(L)(NO3)(H2O)2]•H2O complex, where L represents AMT molecule with NH group. The formed complex exhibits a sharp, and well-defined peak at λmax = 434 nm with a molar absorptivity (ε) of 1.90 × 104 L mol−1 cm−1, and Sandell’s factor of 0.003 μg mL−2. Absorbance of the [Cu(L)(NO3)(H2O)2]•H2O follows Beer’s law over a 0.7–25 μg mL−1 range with a detection limit of 0.011 μg mL−1. Validation of the submitted method was established by estimating Cu2+ in certified reference materials and actual sea and tap water samples. The results are compared with data obtained from copper concentration measurements using ICP-OES. The chemical structure of the Cu(II)-AMT complex was fully characterized by FT-IR, SEM, EDX, TGA, and ESR techniques.

2013 ◽  
Vol 11 (01) ◽  
pp. 20-22
Author(s):  
Esraa R. Abbas ◽  
Salih H. Kadhim ◽  
Muneer A. Abbas AL-Da,amy

A new chromogenic reagent 4-((imidazole-2-yl)diazenyl)-N-(pyrimidin-2-yl)benzenesulfonamide was synthesized by the reaction between imidazole and Sulphadiazine as azo reagent and used as new spectrophotometric method with highly sensitive to determined Nickel (II). The reagent reacts with nickel(II) in aqueous solution at pH= 7 to form dark- brown colored complex. The reagent and its complex were identified by Fourier transform infrared (FT-IR), Uv-visible,1HNMR, and 13CNMR spectroscopies and investigate the formula and charge of the prepared complex by molar ratio and molar conductivity measurements. The complex shows λmax at 486 nm with a molar absorptivity 0.3299 x 104 L.mo1-1.cm-1 and Sandell’s sensitivity 0.0177μg.cm-2.Beer’s law is obeyed in the concentration range (0.5-7.6μg.mL-1) of Ni (II) with excellent linearity depicted by correlation coefficient value of 0.9995 with a detection limit of 0.1927μg.ml-1. Recovery and relative error values of precision and accuracy of method were found to be R.S.D.% = 0.39221, Re=98.7% and Erel = -1.3% . The nature of the complex showed that (M:L) ratio was 1:2. This method was applied for the determination of Ni(II) in alloy due to Sensitive, accurate, and rapid spectrophotometric method. The results obtained were compared with the flame atomic absorption spectrometry method, and results are in conformity.


1986 ◽  
Vol 40 (7) ◽  
pp. 1068-1069 ◽  
Author(s):  
M. S. Akhter ◽  
A. R. Chughtai ◽  
D. M. Smith

2012 ◽  
Vol 260-261 ◽  
pp. 593-597
Author(s):  
Veronika Sassmanová ◽  
Zuzana Poláčková ◽  
Jaroslav Frantík ◽  
Stanislav Honus ◽  
Dagmar Juchelková

The article deals with the identification of a chemical structure of pyrolysis liquid occurring by the thermal degradation of tyre debris within the temperature interval from 500°C to 650°C and the temperature increase steps of 50°C in individual experiments and with the use of analytical methods GC/MS, FT-IR and the elementary analysis. The measured FT-IR spectra indicate the representation of functional groups included in measured samples. They could be used for the determination of basic chemical properties. There were changes in the chemical composition monitored as well as the creation of functional groups in the pyrolysis liquid on the basis of FT-IR spectra and GS/MS outcomes.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Kumble Divya ◽  
Badiadka Narayana ◽  
Majal Sapnakumari

A new spectrophotometric method is developed for the determination of Paracetamol (PCT) and protriptyline HCl (PTP) in pure forms and in pharmaceutical formulations. The experiment involves the use of 3-chloro-7-hydroxy-4-methyl-2H-chromen-2-one as a novel chromogenic reagent for the determination of PCT and PTP. The method is based on the formation of charge transfer complex between the drugs and chromogenic reagent. Beer's law is obeyed in the concentration ranges 10.00–60.00 µg mL−1 for PCT at 545 nm and 40.00–160.00 µg mL−1 for PTP at 468 nm. The molar absorptivity, Sandell, sensitivity, and limit of detection and quantification are also calculated. The method has been successfully applied for the determination of both PCT and PTP in pharmaceutical samples with acceptable results.


2021 ◽  
Vol 2 (3) ◽  
pp. 1-5
Author(s):  
Samuel Echioda ◽  
Adepeju Oluwabunmi Ogunieye ◽  
Salisu Salisu ◽  
Amina Abdulazeez Abdulrasheed ◽  
I. Y. Chindo ◽  
...  

A simple, sensitive, selective, and non-extractive UV-Vis spectrophotometric method for the determination of cadmium, lead, chromium, and arsenic in biological, soil and water samples using synthesized and characterized phenyl hydrazone; glutaraldehydephenyl hydrazone (GPH) as the chromogenic reagent was developed. GPH was synthesized as new chromogenic analytical reagents for the direct UV-Vis spectrophotometric determination of the selected metals of interest in a slightly acidic pH of 6.5-7.5 and 20 % dimethylformamide (DMF) solution to give stable coloured metal-ligand complexes. The reactions were instantaneous; the wavelengths of maximum absorptions were followed spectrophotometrically and noted. The reagent GPH revealed a wavelength of maximum absorption between 360.0 (Cr) to 395.0 nm for (Pb and As) at a working pH of 6.5 to 7.5 room temperature (37 °C). The reagent GPH had a molar absorptivity (L mol-1 cm-1) ranging from 2.213×104 (Pb) to 2.460×104 (As), a mole ratio of metal to ligand of 2:1, the detection limit (µg/g) ranging from 0.3432 (As) to 0.5250 (Pb) and the metal-ligand complex was stable for 0-48 hours. The reagents had a Beer’s law validity range (mg L-1) of 0.001 to 100. The Sandell’s sensitivities (µg/cm2) ranged from 0000409 (As) to 0.00499 (Pb) for APDH and 0.00406 (As) to 0.00452 (Pb) respectively. Large excess of cations and anions as possible interferences up to 15 folds were studied and do not interfere with the determination of the selected metals of interest. The developed method is highly selective for Cd, Pb, and Cr and As and was successfully used for the determination for the said elements in soil, water, and biological samples. The results of the developed methods were comparable with AAS and were found to be in good agreement. The method had very high precision and very good accuracy.


2016 ◽  
Vol 8 (4) ◽  
pp. 810-815 ◽  
Author(s):  
Juan A. V. A. Barros ◽  
Miguel Ángel Aguirre ◽  
Nikolay Kovachev ◽  
Antonio Canals ◽  
Joaquim A. Nóbrega

A new procedure for determining trace concentrations of Mo in plants, combining VA-DLLME and ICP-OES, is proposed here.


2017 ◽  
Vol 2017 ◽  
pp. 1-10 ◽  
Author(s):  
Tamara Jovanović ◽  
Đuro Koruga ◽  
Branimir Jovančićević

The FT-IR spectra of the stable C76and C84isomers of D2symmetry, isolated by the new, advanced extraction and chromatographic methods and processes, were recorded by the KBr technique, over the relevant region from 400 to 2000 cm−1, at room temperature. All the observed infrared bands are in excellent agreement with the semiempirical QCFF/PI, DFT, and TB potential calculations for these fullerenes, which is presented in this article, as the evidence of their validity. The molar absorptivityεand the integrated molar absorptivityψof their IR absorption bands were determined and reported together with the relative intensities. Excellent agreement is found between the relative intensities of the main and characteristic absorption maxima calculated fromελand from theψλvalues in adequate integration ranges. These results are significant for the identification and quantitative determination of the C76-D2and C84-D2:22 fullerenes, either in natural resources on Earth and in space or in artificially synthesized and biomaterials, electronic, optical, and biomedical devices, sensors, polymers, optical limiters, solar cells, organic field effect transistors, special lenses, diagnostic and therapeutic agents, pharmaceutical substances in biomedical engineering, and so forth.


2006 ◽  
Vol 3 (3) ◽  
pp. 146-153
Author(s):  
Padmarajaiah Nagaraja ◽  
Jainara S. Prakash ◽  
Besagarahally L. Bhaskara

A simple, rapid and sensitive spectrophotometric method has been developed for the trace determination of nitrite using Dapsone and α-Naphthol. The proposed method is based on the diazotization of Dapsone followed by coupling with α-Naphthol in sodium hydroxide medium to give an intense pink coloured azo dye. The dye shows absorption maximum at 540 nm. The molar absorptivity and Sandell’s sensitivity being 5.749 × 104l mol-1cm-1and 0.24 ng cm-3respectively. Tolerance limit for interfering ions and complexing agents were reported. Other analytical parameters and applications of the method for analysis of tap water, lake water, and industrial effluents have been investigated.


2021 ◽  
Vol 40 (1) ◽  
pp. 108-126
Author(s):  
Jumana W. Ammar ◽  
Zainab A. Khan ◽  
Marwa N. Ghazi ◽  
Naser A. Naser

Abstract A modern development discusses the synthesis and validity of simple, sensitive, and versatile spectrophotometric methods for Bi(III) and Al(III) determination in pharmaceutical formulations have been conducted. In the present paper, 4-(4 acetamidophenylazo) pyrogallol has been synthesized as a new organic compound, 4-APAP, by coupling pyrogallol in a regulated pH medium with diazotized p-aminoacetanilide. 4-APAP was identified by methods of FT-IR, 1H-NMR, 13C-NMR, and thermal analysis (thermogravimetry and differential scanning calorimetry). Solvatochromic activity was also studied in solvents with different polarities. The Kamlet and Taft linear solvation energy relationship was used to correlate shifts in UV-Visible spectra of 4-APAP with Kamlet-Taft parameters (α, β, and π*). The optimum assay conditions showed linearity from 0.3–13 to 0.5–11 μg·mL−1 for Bi(III) and Al(III), respectively. Molar absorptivity values were 3.365 × 104 and 0.356 × 104 L·mol−1·cm−1 for Bi(III) and Al(III), with similar Sandell's sensitivity measures of 0.006 and 0.008 μg·cm−2. Detection limits and quantification limits were 0.013 and 0.043 μg·mL−1 for Bi(III), respectively, and 0.018 and 0.059 μg·mL−1 for Al(III) with the relative standard deviation for determination of both metal ions using 4-APAP probe being <2.0%. The validity, accuracy, and efficiency of the approaches were demonstrated by the determination of Bi(III) and Al(III) in different formulations.


2019 ◽  
Author(s):  
Chem Int ◽  
Pranab Kumar Tarafder

The surfactant sensitized bottle-green complex (1:2:1) formed of cobalt-thiocyanate-cetyltrimethylammonium bromide is suitably extracted into an organic solvent, ethylacetate, at a pH range, 6-8 and the absorption measurements were carried out at 630 nm (ƛmax). The Beer’s law is obeyed in the range from 0.05 to 10 μg per mL. The molar absorptivity and Sandell’s sensitivity of the present system were found to be 2.2 x 103 L.mol-1cm-1 and 0.026 μg cm-2, respectively. No other element forms complex of similar colour with thiocyanate at this pH range. The method was applied to a number of samples like rock, soil, sediment, polymetallic nodules etc., as well as Certified Reference Materials and the values were found highly satisfactory. The interference of Fe3+ which formed a reddish complex at acidic pH (&lt;7) was eliminated when the complex was extracted at pH 8.0. The method is highly useful for the determination of cobalt in geological samples having its concentration from μg/mL to percentage level. As the method has been made highly selective for spectrophotometric determination of cobalt, it might be applied to almost all types of geological sample of diverse matrices.


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