scholarly journals Simple Sensitive Spectrophotometric Determination of Vanadium in Biological and Environmental Samples

2006 ◽  
Vol 3 (4) ◽  
pp. 286-297 ◽  
Author(s):  
B. Krishna Priya ◽  
P. Subrahmanyam ◽  
J. Dilip Kumar ◽  
P. Chiranjeevi

Novel, rapid, highly sensitive and selective spectrophotometric method for the determination of traces of vanadium (V) in environmental and biological samples, pharmaceutical and steel samples was studied. The method is based on oxidation of 2,4- dinitro phenyl hydrazine(2,4-DNPH) by vanadium (V) followed by coupling reaction withN-(1-naphthalene-1-yl)ethane-1,2-diamine-dihydrochloride (NEDA) in acidic medium to give red colored derivative or on oxidation of 4-Amino Pyridine by vanadium (V) followed by coupling reaction with NEDA in basic medium to give pink colored derivative. The red colored derivative having an λmax495 nm which is stable for 8 days and the pink colored derivative with 525 nm is stable for more than 7 days at 350C. Beer's law is obeyed for vanadium (V) in the concentration range of 0.02 - 3.5 μg mL–1(red derivative) and 0.03 – 4.5 μg mL–1(pink derivative) at the wave length of maximum absorption. The optimum reaction conditions and other analytical parameters were investigated to enhance the sensitivity of the present method. The detailed study of various interferences made the method more selective. The proposed method was successfully applied to the analysis of vanadium in natural water samples, plant material, soil samples, synthetic mixtures, pharmaceutical samples and biological samples. The results obtained were agreed with the reported methods at the 95 % confidence level. The performance of proposed method was evaluated in terms of Student'st-test and Variance ratiof-test which indicates the significance of proposed method over reported method.

2007 ◽  
Vol 4 (4) ◽  
pp. 496-501 ◽  
Author(s):  
M. Vamsi Krishna ◽  
D. Gowri Sankar

Simple, rapid and sensitive spectrophotometric procedures were developed for the analysis of Alfuzosin hydrochloride (AFZ) in pure form as well as in pharmaceutical formulations. The methods are based on the reaction of AFZ with nitrite in acid medium to form diazonium ion, which is coupled with ethoxyethylenemaleic ester (Method A) or ethylcyanoacetate (Method B) or acetyl acetone (method C) in basic medium to form azo dyes, showing absorption maxima at 440, 465 and 490 nm respectively. Beer’s law is obeyed in the concentration of 4-20 μg/mL of AFZ for methods A, B and 3-15 μg/mL of AFZ for method C. The molar absorptivity and sandell’s sensitivity of AFZ- ethoxyethylenemaleic ester, AFZ- ethylcyanoacetate and AFZ-acetyl acetone are1.90 × 104, 0.022; 1.93 × 104, 0.021 and 2.67 × 104L mole-1cm-1, 0.015 μg cm-2respectively. The optimum reaction conditions and other analytical parameters were evaluated. The methods were successfully applied to the determination of AFZ in pharmaceutical formulations.


2006 ◽  
Vol 4 (4) ◽  
pp. 708-722 ◽  
Author(s):  
Akram El-Didamony ◽  
Alaa Amin ◽  
Ahmed Ghoneim ◽  
Ayman Telebany

AbstractFour simple, accurate, sensitive and economical procedures (A–D) for the estimation of gentamicin sulphate and vancomycin hydrochloride, both in pure form and in pharmaceutical formulations have been developed. The methods are based on the oxidation of the studied drugs by a known excess of potassium permanganate in sulphuric acid medium and subsequent determination of unreacted oxidant by reacting it with amaranth dye (method A), acid orange II (method B), indigocarmine (method C) and methylene blue (method D), in the same acid medium at a suitable λmax=521, 485, 610 and 664 nm, respectively. The reacted oxidant corresponds to the drug content. Regression analysis of Beer-Lambert plots showed good correlations in the concentration ranges 4–8, 3–8, 4–9 and 5–9 µg ml−1 with gentamicin and 4–8, 1.5–4, 1.5–4 and 3.5–5.5 µg ml−1 with vancomycin for methods A, B, C, and D, respectively. The molar absorptivity, sandell sensitivity, detection and quantification limits were calculated. The stoichiometric ratios for the cited drugs were studied. The optimum reaction conditions and other analytical parameters were evaluated. The influence of the substance commonly employed as excipients with these drugs were studied. The proposed methods were applied to the determination of these drugs in pharmaceutical formulations. The results have demonstrated that the methods are equally accurate and reproducible as the official methods.


2018 ◽  
Vol 142 ◽  
pp. 01002
Author(s):  
Xiaodong Shao

Spoolable reinforced plastic line pipe will be widely used in the exploitation of acid gas and oil wells. End-fitting is a mechanical device that forms the transition from the spoolable reinforced plastic line pipe to the connector. It was well known that nickel was an important element in the end-fitting. In this paper, a novel spectrophotometric method was described for determination of nickel in the end-fitting of spoolable reinforced plastic line pipe. The method was based on the color reaction between nickel and dimethylglyoxime, which was favored in an alkaline medium, producing a red compound in the presence of ammonium persulfate as an oxidant. Under the optimum reaction conditions the absorption value was proportional to the concentration of nickel in the range of 0.080~0.50% (R2 = 0.9999), and the relative standard deviation was less than 3.0% (n=5). The proposed method was applied successfully to determine nickel in end-fitting of spoolable reinforced plastic line pipe.


2021 ◽  
Vol 18 (39) ◽  
pp. 14-32
Author(s):  
Hind Sadiq Al-WARD ◽  
Mouayed Qassssim AL-ABACHI ◽  
Mohammed Rifaat AHMED

Background: Tetracycline is one of the most important antibiotics. It is used to treat many different bacterial infections. It is often used in treating severe acne, or sexually transmitted diseases such as syphilis, gonorrhea, or chlamydia. In some cases, tetracycline is used when penicillin or another antibiotic cannot be used to treat serious infections such as the ones caused by Bacillus anthracis, Listeria, Clostridium, Actinomyces. Aim: synthesized a new novel reagent used to determine TCH spectrophotometrically by using diazonium and coupling reaction. Methods: Four new substituted procaine derivatives were prepared by simple organic methods using aniline derivatives. A spectrophotometric approach was established for the micro-determination of TCH. The stoichiometry was investigated using mole ratio and continuous variation methods, and the stability constant was also estimated. The ΔG, ΔH, and ΔS were determined as thermodynamic parameters for evaluating the effect of temperature on the reaction. Results: Substituted procaine derivatives were prepared, and o-hydroxy procaine seems to be the best reagent used to determine TCH by diazotization and coupling reaction. The result was a yellow water-soluble dye with a maximum absorbance of 380 nm. The reaction conditions were studied and optimized. Beers law was obeyed over a concentration range (2.5–50) μg.mL-1 for TCH. The molar absorptivity was (14.4669.103) L.mol-1.cm-1, and the detection limit was (0.5052) μg.mL-1. The stoichiometry of the formed product was found 1:1 (o-hydroxyprocaine: TCH). The stability constant indicated that the product formed was stable, and the thermodynamic parameters showed that the diazonium salt reaction was preferred to occur at a low temperature. Conclusions: a simple, accurate, and fast method was developed to determine TCH in pure form and pharmaceuticals by coupling the TCH with a newly synthesized procaine derivative reagent (o-hydroxy procaine) in a basic medium.


2002 ◽  
Vol 2 (2) ◽  
pp. 64-66 ◽  
Author(s):  
Justus M. Onguso . ◽  
Esther M. Kahangi . ◽  
Douglas W. Ndiritu . ◽  
Fusao Mizutani .

2019 ◽  
Vol 79 (6) ◽  
pp. 1092-1101 ◽  
Author(s):  
Krishnendu Kumar Pobi ◽  
Biplab Mondal ◽  
Sumanta Nayek ◽  
Apurba K. Patra ◽  
Rajnarayan Saha

Abstract The present study is focused on the removal of Hg2+, Cd2+ and Pb2+ ions from aqueous solution using a tridentate chelating agent, 2-pyridyl-N-(2′-methylthiophenyl) methyleneimine (PMTPM); and applicability of such removal from industrial wastewater using PMTPM is also investigated. The results showed that the metal ions removal efficiency using PMTPM was in the order of Hg2+(99.46%) > Cd2+(95.42%) > Pb2+(94.54%) under optimum reaction conditions (L:M2+ = 3:1, pH = 9, time = 24 h, temp. = 30 °C). Formed chelated complexes such as [Hg(PMTPM)Cl2] (1), [Cd(PMTPM)Cl2] (2) and [Pb(PMTPM)Cl2] (3) were characterized by numerous spectroscopic tools and X-ray structure determination of a representative complex of Hg2+. In the X-ray structure of [Hg(PMTPM)Cl2], 1, the Hg2+ adopted a distorted tetrahedral coordination geometry surrounding two N donors of PMTPM and two chloride ions. A similar coordination geometry surrounding the respective metal centres in 2 and 3 was established. The thermogravimetric analysis (TGA) revealed a stability order of [Cd(PMTPM)Cl2] > [Hg(PMTPM)Cl2] > [Pb(PMTPM)Cl2]. Further the comparative metal leaching behaviour of these chelate complexes exhibited higher stability in alkaline solution than in acidic. Moreover, PMTPM was applied in real mixed industrial wastewater with alkaline pH, and adequate removals of toxic metals were achieved.


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