Spectrophotometric Methods for the Determination of Ketoconazole ...

African Journals Online (AJOL)

Spectrophotometric Methods for the Determination of Ketoconazole in Pharmaceutical Dosage Forms. ... Tropical Journal of Pharmaceutical Research ... Methods: The first method (A) was based on the oxidation of the studied drug by a known excess of cerium (IV) as an oxidizing agent and subsequent determination of ...

Sensitive kinetic spectrophotometric determination of captopril and ethamsylate in pharmaceutical preparations and biological fluids.

Science.gov (United States)

El-Shabrawy, Y; El-Enany, N; Salem, K

2004-10-01

A highly sensitive kinetic spectrophotometric method was developed for the determination of captopril (CPL) and ethamsylate (ESL) in pharmaceutical preparations and biological fluids. The method is based on a catalytic acceleration of the reaction between sodium azide and iodine in an aqueous solution. Concentration range of 0.1-1.5 microg ml(-1) for CPL and 0.3-3 microg ml(-1) for ESL was determined by measuring the decrease in the absorbance of iodine at 348 nm by a fixed time method. The decrease in absorbance after 5 min was markedly correlated to the concentration. The relative standard deviations obtained were 1.30 and 1.87 for CPL and ESL, respectively, in pure forms. Correlation coefficients were 0.9997 and 0.9999 for CPL and ESL, respectively. The detection limits were determined as (S/N = 3) were 20 ng ml(-1) for CPL and 50 ng ml(-1) for ESL. The proposed procedure was successively applied for the determination of both drugs in pharmaceutical preparations and in biological fluids.

Development of Ultraviolet Spectrophotometric Method for Analysis ...

African Journals Online (AJOL)

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Method for Analysis of Lornoxicam in Solid Dosage. Forms. Sunit Kumar Sahoo ... testing. Mean recovery was 100.82 % for tablets. Low values of % RSD indicate .... Saharty E, Refaat YS, Khateeb ME. Stability-. Indicating. Spectrophotometric.

A Sensitive Validated Spectrophotometric Method for the Determination of Flucloxacillin Sodium

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R. Singh Gujral

2009-01-01

Full Text Available A simple and sensitive spectrophotometric method has been proposed for the determination of flucloxacillin sodium. The determination method is based on charge transfer complexation reaction of the drug with iodine in methanol-dichloromethane medium. The absorbance was measured at 362 nm against the reagent blank. Under optimized experimental conditions, Beer's law is obeyed in the concentration ranges 1-9 μg/mL for flucloxacillin. The method was validated for specificity, linearity, precision, accuracy. The degree of linearity of the calibration curves, the percent recoveries, limit of detection and quantitation for the spectrophotometric method were determined. No interferences could be observed from the additives commonly present in the pharmaceutical formulations. The method was successfully applied for in vitro determination of human urine samples with low RSD value. This is simple, specific, accurate and sensitive spectrophotometric method.

Multicomponent kinetic spectrophotometric determination of pefloxacin and norfloxacin in pharmaceutical preparations and human plasma samples with the aid of chemometrics

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Ni, Yongnian; Wang, Yong; Kokot, Serge

2008-10-01

A spectrophotometric method for the simultaneous determination of the important pharmaceuticals, pefloxacin and its structurally similar metabolite, norfloxacin, is described for the first time. The analysis is based on the monitoring of a kinetic spectrophotometric reaction of the two analytes with potassium permanganate as the oxidant. The measurement of the reaction process followed the absorbance decrease of potassium permanganate at 526 nm, and the accompanying increase of the product, potassium manganate, at 608 nm. It was essential to use multivariate calibrations to overcome severe spectral overlaps and similarities in reaction kinetics. Calibration curves for the individual analytes showed linear relationships over the concentration ranges of 1.0-11.5 mg L -1 at 526 and 608 nm for pefloxacin, and 0.15-1.8 mg L -1 at 526 and 608 nm for norfloxacin. Various multivariate calibration models were applied, at the two analytical wavelengths, for the simultaneous prediction of the two analytes including classical least squares (CLS), principal component regression (PCR), partial least squares (PLS), radial basis function-artificial neural network (RBF-ANN) and principal component-radial basis function-artificial neural network (PC-RBF-ANN). PLS and PC-RBF-ANN calibrations with the data collected at 526 nm, were the preferred methods—%RPE T ˜ 5, and LODs for pefloxacin and norfloxacin of 0.36 and 0.06 mg L -1, respectively. Then, the proposed method was applied successfully for the simultaneous determination of pefloxacin and norfloxacin present in pharmaceutical and human plasma samples. The results compared well with those from the alternative analysis by HPLC.

Validation of different spectrophotometric methods for determination of vildagliptin and metformin in binary mixture

Science.gov (United States)

Abdel-Ghany, Maha F.; Abdel-Aziz, Omar; Ayad, Miriam F.; Tadros, Mariam M.

New, simple, specific, accurate, precise and reproducible spectrophotometric methods have been developed and subsequently validated for determination of vildagliptin (VLG) and metformin (MET) in binary mixture. Zero order spectrophotometric method was the first method used for determination of MET in the range of 2-12 μg mL-1 by measuring the absorbance at 237.6 nm. The second method was derivative spectrophotometric technique; utilized for determination of MET at 247.4 nm, in the range of 1-12 μg mL-1. Derivative ratio spectrophotometric method was the third technique; used for determination of VLG in the range of 4-24 μg mL-1 at 265.8 nm. Fourth and fifth methods adopted for determination of VLG in the range of 4-24 μg mL-1; were ratio subtraction and mean centering spectrophotometric methods, respectively. All the results were statistically compared with the reported methods, using one-way analysis of variance (ANOVA). The developed methods were satisfactorily applied to analysis of the investigated drugs and proved to be specific and accurate for quality control of them in pharmaceutical dosage forms.

Development of an indirect spectrophotometric method for ...

African Journals Online (AJOL)

A simple and rapid indirect spectrophotometric method for determination of ... of the colored product was measured at 405 nm and pH 3 against a reagent blank. ... The limit of detection and quantification were found to be 0.20±0.03 and ...

Kinetic Spectrophotometric Determination of Trace Amounts of Sulfide

Energy Technology Data Exchange (ETDEWEB)

Barzegar, Mohsen [Tarbiat Modarres University, Tehran (Iran, Islamic Republic of); Jabbari, Ali [K. N. Toosi University, Tehran (Iran, Islamic Republic of); Esmaeili, Majid [Razi University, Kermanshah (Iran, Islamic Republic of)

2003-09-15

A method for the determination of trace amount of sulfide based on the addition reaction of sulfide with methyl green at pH 7.5 and 25 .deg. C is described. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of the dyestuff at 637 nm by the initial rate and fixed time method. The calibration graph is linear in the range 30-1200 ppb. The theoretical limit of detection was 0.014 ppm. Seven replicate analysis of a sample solution containing 0.70 ppm sulfide gave a relative standard deviation of 1.5%. The interfering effects of various ions on sulfide determination have been reported and procedures for removal of interference have been described. The proposed method was applied successfully to the determination of sulfide in tap and wastewater samples.

Kinetic Spectrophotometric Determination of Trace Amounts of Sulfide

International Nuclear Information System (INIS)

Barzegar, Mohsen; Jabbari, Ali; Esmaeili, Majid

2003-01-01

A method for the determination of trace amount of sulfide based on the addition reaction of sulfide with methyl green at pH 7.5 and 25 .deg. C is described. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of the dyestuff at 637 nm by the initial rate and fixed time method. The calibration graph is linear in the range 30-1200 ppb. The theoretical limit of detection was 0.014 ppm. Seven replicate analysis of a sample solution containing 0.70 ppm sulfide gave a relative standard deviation of 1.5%. The interfering effects of various ions on sulfide determination have been reported and procedures for removal of interference have been described. The proposed method was applied successfully to the determination of sulfide in tap and wastewater samples

A highly sensitive kinetic spectrophotometric method for the determination of ascorbic Acid in pharmaceutical samples.

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Shishehbore, Masoud Reza; Aghamiri, Zahra

2014-01-01

In this study, a new reaction system for quantitative determination of ascorbic acid was introduced. The developed method is based on inhibitory effect of ascorbic acid on the Orange G-bromate system. The change in absorbance was followed spectrophotometrically at 478 nm. The dependence of sensitivity on the reaction variables including reagents concentration, temperature and time was investigated. Under optimum experimental conditions, calibration curve was linear over the range 0.7 - 33.5 μg mL(-1) of ascorbic acid including two linear segments and the relative standard deviations (n = 6) for 5.0 and 20.0 μg mL(-1) of ascorbic acid were 1.08 and 1.02%, respectively. The limit of detection was 0.21 μg mL(-) (1) of ascorbic acid. The effect of diverse species was also investigated. The developed method was successfully applied for the determination of ascorbic acid in pharmaceutical samples. The results were in a good agreement with those of reference method.

Thionine-Bromate as a New Reaction System for Kinetic Spectrophotometric Determination of Hydrazine in Cooling Tower Water Samples

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Masoud Reza Shishehbore

2013-01-01

Full Text Available A simple, selective, and inexpensive kinetic method was developed for the determination of hydrazine based on its inhibitory effect on the thionine-bromate system in sulfuric acid media. The reaction was monitored spectrophotometrically at 601 nm by a fixed time method. The effect of different parameters such as concentration of reactants, ionic strength, temperature, and time on the rate of reaction was investigated, and the optimum conditions were obtained. Under optimum conditions, the calibration curve was linear in the concentration range from 0.8–23.0 μg mL−1 of hydrazine, and the detection limit of the method was 0.22 μg mL−1. The relative standard deviation for five replicate determinations of 1.0 μg mL−1 of hydrazine was 0.74%. The potential of interfering effect of foreign species on the hydrazine determination was studied. The proposed method was successfully applied for the determination of hydrazine in different water samples.

SHORT COMMUNICATION CATALYTIC KINETIC ...

African Journals Online (AJOL)

IV) catalyzes the discoloring reaction of DBS-arsenazo oxidized by potassium bromate, a new catalytic kinetic spectrophotometric method for the determination of trace titanium (IV) was developed. The linear range of the determination of ...

NEW SPECTROPHOTOMETRIC METHOD WITH KMnO 4 FOR ...

African Journals Online (AJOL)

The new method, an instrument-based and simple experimental procedure involves the reaction of the hypochlorite with arsenious oxide (As2O3) (pH 6.5) followed by the coupled reaction of residual As2O3 with permanganate at acidic pH. A titration procedure is described and spectrophotometric method is designed using ...

A Spectrophotometric Method for the Determination of Ramipril in ...

African Journals Online (AJOL)

A Spectrophotometric Method for the Determination of Ramipril in Solid Dosage Forms. ... Tropical Journal of Pharmaceutical Research ... Methods: UV spectrophotometry was used to develop and validate a simple method for the assay of ramipril in solid dosage form at λmax of 210 nm, as per International Conference on ...

Development of a Spectrophotometric Method for Monitoring Angiotensin-Converting Enzyme in Dairy Products

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Julijana Tomovska*, S. Presilski, N. Gjorgievski, N. Tomovska1, M. S. Qureshi2 and N. P. Bozinovska3

2013-01-01

Full Text Available The angiotensin-converting enzyme (ACE regulates the levels of blood pressure through generation of angiotensin-II from angiotensin-I. It is of great importance to have a reliable and yet simple method for a quantitative determination ACE inhibitory peptides in whey of milk products. A rapid, simple, sensitive and accurate spectrophotometric kinetic method has been developed for determination of ACE inhibitory peptides, using competitive inhibition. Samples of dairy product from the market were used for the determination of ACE inhibitory peptides in whey. Holmquist’s kinetic method was used for determining ACE inhibitory activity in blood serum and Ronca-Testoni method was used for the determination of ACE inhibitory activity in whey. Enzymatic inhibition activity was determined using 0.8 mmol/L FAPGG (N-[3-(Furyl –Acryloyl]-L-Phenylalanyl Glycyl Glycyne as the substrate in 50 mmol/L Tris buffer at pH 8.2 at 37°C and a standard serum containing ACE. First, a solution of whey was mixed in a 1 to 10 ratio with serum (elevation containing high ACE activity. The enzymatic activity was determined by monitoring the decrease in absorbance at 340 nm as result of hydrolysis of the substrate. The concentration of ACE inhibitory peptides was determined from a standard curve of inhibitor concentration versus percent of ACE inhibition. The study suggests that the method possesses good reproducibility and accuracy. The linear range enabled determination of high enzymatic activity of ACE and all ACE inhibitory peptides from dairy products act as competitive inhibitors.

Kinetic spectrophotometric determination of Bi(III based on its catalytic effect on the oxidation of phenylfluorone by hydrogen peroxide

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SOFIJA M. RANČIĆ

2009-08-01

Full Text Available A new reaction was suggested and a new kinetic method was elaborated for determination of Bi(III in solution, based on its catalytic effect on the oxidation of phenyl-fluorone (PF by hydrogen peroxide in ammonia buffer. By application of spectrophotometric technique, a limit of quantification (LQ of 128 ng cm-3 was reached, and the limit of detection (LD of 37 ng cm-3 was obtained, where LQ was defined as the ratio signal:noise = 10:1 and LD was defined as signal 3:1 against the blank. The RSD value was found to be in the range 2.8–4.8 % for the investigated concentration range of Bi(III. The influence of some ions upon the reaction rate was tested. The method was confirmed by determining Bi(III in a stomach ulcer drug (“Bicit HP”, Hemofarm A.D.. The obtained results were compared to those obtained by AAS and good agreement of results was obtained.

Extraction-spectrophotometric method for silicon determination in high-purity substances. 1. Silicon determination in tellurium

Energy Technology Data Exchange (ETDEWEB)

Shaburova, V P; Yudelevich, I G [AN SSSR, Novosibirsk (USSR). Inst. Neorganicheskoj Khimii

1989-01-01

The extraction-spectrophotometric method for silicon determination in tellurium based on extraction isolation of the base by tributyl phosphate from hydrochloride solutions and with addition of HNO/sub 3/ and spectrophotometric silicon determination using malachite green is developed. The method permits to determine 2x10/sup -1/-3x10/sup -4/ % Si.

Determination of Modafinil in Tablet Formulation Using Three New Validated Spectrophotometric Methods

International Nuclear Information System (INIS)

Basniwal, P.K.; Jain, D.; Basniwal, P.K.

2014-01-01

In this study, three new UV spectrophotometric methods viz. linear regression equation (LRE), standard absorptivity (SA) and first order derivative (FOD) method were developed and validated for determination of modafinil in tablet form. The Beer-Lamberts law was obeyed as linear in the range of 10-50 μg/ mL and all the methods were validated for linearity, accuracy, precision and robustness. These methods were successfully applied for assay of modafinil drug content in tablets in the range of 100.20 - 100.42 %, 100.11 - 100.58 % and 100.25 - 100.34 %, respectively with acceptable standard deviation (less than two) for all the methods. The validated spectrophotometric methods may be successfully applied for assay, dissolution studies, bio-equivalence studies as well as routine analysis in pharmaceutical industries. (author)

Role of Ru(IlI) as an inhibitor in oxidation of lactose by (Cu(bipy)2)2+ in alkaline medium: spectrophotometric and kinetic studies

International Nuclear Information System (INIS)

Singh, Ashok Kumar; Singh, Manjula; Srivastava, Jaya; Rahmani, Shahla

2013-01-01

Kinetics of oxidation of lactose by (Cu(bipy) 2 ) 2+ in alkaline medium using Ru(III) as an inhibitor has been studied spectrophotometrically at 40 °C. The studies show that the rate of the reaction is zero order with respect to (Cu(bipy) 2 ) 2+ and first order with respect to (lactose). The order of reaction is found to be two at low concentrations of OH - (from 1.48×10 5 to 3.47×10 5 M) and less than two at its high concentrations (from 4.27×10 5 to 6.31×10 5 M). There is a substantial decrease in the pseudo-zero order rate constant with increase in the concentration of Ru(III) chloride, indicating the role of Ru(III) chloride as an inhibitor. Decrease in the rate with increase in dielectric constant of the medium is observed, while ionic strength of the medium and bipyridyl concentration has no influence on the rate. Based on kinetic data and spectrophotometric evidences, a suitable mechanism is proposed for the studied reaction. (author)

Validated UV-Spectrophotometric Methods for Determination of Gemifloxacin Mesylate in Pharmaceutical Tablet Dosage Forms

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R. Rote Ambadas

2010-01-01

Full Text Available Two simple, economic and accurate UV spectrophotometric methods have been developed for determination of gemifloxacin mesylate in pharmaceutical tablet formulation. The first UV-spectrophotometric method depends upon the measurement of absorption at the wavelength 263.8 nm. In second area under curve method the wavelength range for detection was selected from 268.5-258.5 nm. Beer’s law was obeyed in the range of 2 to 12 μgmL-1 for both the methods. The proposed methods was validated statistically and applied successfully to determination of gemifloxacin mesylate in pharmaceutical formulation.

Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

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Sonia T. Hassib

2011-12-01

Full Text Available Simple, accurate and precise reversed-phase liquid chromatographic (LC and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS and trimethoprim (TMP in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9:acetonitrile:water (25:100:50, v/v/v at a flow rate of 1.6 ml min−1 with UV detection at 210 nm for ERS and 280 nm for TMP. Besides, two spectrophotometric methods were applied after reaction with perchloric acid (12 M which gives a colored product with ERS. Then, the spectral interference between the colored product of ERS and TMP was resolved by either ratio spectra derivative spectrophotometry in the first spectrophotometric method or chemometric techniques, namely classical least-squares (CLS, principal component regression (PCR and partial least-squares regression (PLS in the second spectrophotometric method. The results were statistically compared using one-way analysis of variance (ANOVA. The methods developed were satisfactorily applied to the analysis of the pharmaceutical preparation containing the two drugs and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

Spectrophotometric methods for determining noble metals

International Nuclear Information System (INIS)

Gur'eva, R.F.; Savvin, S.B.

2002-01-01

The main trends of the development of spectrophotometric methods for determining noble metals (NMs) including ruthenium are considered. One of these trends is the synthesis and study of new, highly sensitive and selective organic reagents for determining NMs in solutions and solid phase. Another trend is the search for and developing of new methodological approaches (techniques) and color reactions, including those that involve modified and immobilized reagents. The third trend includes the improvement of equipment and automation. It is shown that the present-day spectrophotometry can provide the determination of NMs in samples with concentrations from several to 10 -4 % (photometry and differential photometry) and down to 10 -7 % (test and sorption-spectroscopic methods based on photometry and diffuse-reflectance spectroscopy, including the use of chromaticity functions) [ru

Development and Application of Ligand-Exchange Reaction Method ...

African Journals Online (AJOL)

Purpose: This paper presents an improved kinetic-spectrophotometric procedure for determining clonazepam (CZP) in pharmaceutical formulations and human serum. Methods: The method is based on ligand-exchange reaction. The reaction was followed spectrophotometrically by measuring the rate of change of ...

Simultaneous Spectrophotometric Determination of Valsartan and ...

African Journals Online (AJOL)

Purpose: To develop a direct, simple and extraction-free spectrophotometric method for the simultaneous estimation of valsartan and ezetimibe in pharmaceuticals. Methods: A spectrophotometric method for the determination of valsartan and ezetimibe was developed using acidic dyes, namely, bromophenol blue (BPB) ...

UV Spectrophotometric Method for Determination of Cinitapride in Pure and its Solid Dosage Form

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B. Thangabalan

2009-01-01

Full Text Available A new, rapid, precise, accurate and sensitive analytical method was developed for the UV spectrophotometric assay of cinitapride (CTP. The drug obeyed the Beer's law and showed good correlation. It showed absorption maxima at 260 nm in methanol. The linearity was observed between 5-40 µg mL-1. The results of analysis were validated by recovery studies. The recovery was more than 99%. The proposed method is the only method available for spectrophotometric determination of the drug. It is simple, precise, sensitive and reproducible and can be used for the routine quality control testing of the marketed formulations.

Spectrophotometric method for the determination of thorium in UO2 pellets

International Nuclear Information System (INIS)

Acosta L, E.

1995-04-01

This report presents a procedure with the description of the spectrophotometric method for the determination of the thorium element in uranium products including powders and pellets of uranium dioxide. Quantities can be determined starting from 1 ppm. (Author)

Spectrophotometric methods for the determination of ampicillin by potassium permanganate and 1-chloro-2,4-dinitrobenzene in pharmaceutical preparations

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Aftab Aslam Parwaz Khan

2015-03-01

Full Text Available Two simple and sensitive kinetic methods for the determination of ampicillin (AMP are described. The first method is based on kinetic investigation of the oxidation reaction of the drug with alkaline potassium permanganate at room temperature for a fixed time of 25 min. The absorbance of the colored manganate ions is measured at 610 nm. The second method is based on the reaction of AMP with 1-chloro-2,4-dinitrobenzene (CDNB in the presence of 0.1 mol L−1 sodium bicarbonate. Spectrophotometric measurement was achieved by recording the absorbance at 490 nm for a fixed time of 60 min. All variables affecting the development of the color were investigated and the conditions were optimized. Plots of absorbance against concentration in both procedures were rectilinear over the ranges 5–30 and 50–260 μg mL−1, with mean recoveries 99.80 and 99.91, respectively. The proposed methods were successfully applied for the determination of AMP in bulk powder and in capsule dosage form. The determination of AMP by the fixed concentration method is feasible with the calibration equations obtained, but the fixed time method proves to be more applicable.

Spectrophotometric Analysis of Caffeine

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Showkat Ahmad Bhawani

2015-01-01

Full Text Available The nature of caffeine reveals that it is a bitter white crystalline alkaloid. It is a common ingredient in a variety of drinks (soft and energy drinks and is also used in combination with various medicines. In order to maintain the optimum level of caffeine, various spectrophotometric methods have been developed. The monitoring of caffeine is very important aspect because of its consumption in higher doses that can lead to various physiological disorders. This paper incorporates various spectrophotometric methods used in the analysis of caffeine in various environmental samples such as pharmaceuticals, soft and energy drinks, tea, and coffee. A range of spectrophotometric methodologies including chemometric techniques and derivatization of spectra have been used to analyse the caffeine.

Estimation of citicoline sodium in tablets by difference spectrophotometric method

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Sagar Suman Panda

2013-01-01

Full Text Available Aim: The present work deals with development and validation of a novel, precise, and accurate spectrophotometric method for the estimation of citicoline sodium (CTS in tablets. This spectrophotometric method is based on the principle that CTS shows two different forms that differs in the absorption spectra in basic and acidic medium. Materials and Methods: The present work was being carried out on Shimadzu 1800 Double Beam UV-visible spectrophotometer. Difference spectra were generated using 10 mm quartz cells over the range of 200-400 nm. Solvents used were 0.1 M NaOH and 0.1 M HCl. Results: The maxima and minima in the difference spectra of CTS were found to be 239 nm and 283 nm, respectively. Amplitude was calculated from the maxima and minima of spectrum. The drug follows linearity in the range of 1-50 μ/ml (R 2 = 0.999. The average % recovery from the tablet formulation was found to be 98.47%. The method was validated as per International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use: ICH Q2(R1 Validation of Analytical Procedures: Text and Methodology guidelines. Conclusion: This method is simple and inexpensive. Hence it can be applied for determination of the drug in pharmaceutical dosage forms.

Different Spectrophotometric and Chromatographic Methods for Determination of Mepivacaine and Its Toxic Impurity.

Science.gov (United States)

Abdelwahab, Nada S; Fared, Nehal F; Elagawany, Mohamed; Abdelmomen, Esraa H

2017-09-01

Stability-indicating spectrophotometric, TLC-densitometric, and ultra-performance LC (UPLC) methods were developed for the determination of mepivacaine HCl (MEP) in the presence of its toxic impurity, 2,6-dimethylanaline (DMA). Different spectrophotometric methods were developed for the determination of MEP and DMA. In a dual-wavelength method combined with direct spectrophotometric measurement, the absorbance difference between 221.4 and 240 nm was used for MEP measurements, whereas the absorbance at 283 nm was used for measuring DMA in the binary mixture. In the second-derivative method, amplitudes at 272.2 and 232.6 nm were recorded and used for the determination of MEP and DMA, respectively. The developed TLC-densitometric method depended on chromatographic separation using silica gel 60 F254 TLC plates as a stationary phase and methanol-water-acetic acid (9 + 1 + 0.1, v/v/v) as a developing system, with UV scanning at 230 nm. The developed UPLC method depended on separation using a C18 column (250 × 4.6 mm id, 5 μm particle size) as a stationary phase and acetonitrile-water (40 + 60, v/v; pH 4 with phosphoric acid) as a mobile phase at a flow rate of 0.4 mL/min, with UV detection at 215 nm. The chromatographic run time was approximately 1 min. The proposed methods were validated with respect to International Conference on Harmonization guidelines regarding precision, accuracy, ruggedness, robustness, and specificity.

REVIEW ARTICLE: Spectrophotometric applications of digital signal processing

Science.gov (United States)

Morawski, Roman Z.

2006-09-01

Spectrophotometry is more and more often the method of choice not only in analysis of (bio)chemical substances, but also in the identification of physical properties of various objects and their classification. The applications of spectrophotometry include such diversified tasks as monitoring of optical telecommunications links, assessment of eating quality of food, forensic classification of papers, biometric identification of individuals, detection of insect infestation of seeds and classification of textiles. In all those applications, large numbers of data, generated by spectrophotometers, are processed by various digital means in order to extract measurement information. The main objective of this paper is to review the state-of-the-art methodology for digital signal processing (DSP) when applied to data provided by spectrophotometric transducers and spectrophotometers. First, a general methodology of DSP applications in spectrophotometry, based on DSP-oriented models of spectrophotometric data, is outlined. Then, the most important classes of DSP methods for processing spectrophotometric data—the methods for DSP-aided calibration of spectrophotometric instrumentation, the methods for the estimation of spectra on the basis of spectrophotometric data, the methods for the estimation of spectrum-related measurands on the basis of spectrophotometric data—are presented. Finally, the methods for preprocessing and postprocessing of spectrophotometric data are overviewed. Throughout the review, the applications of DSP are illustrated with numerous examples related to broadly understood spectrophotometry.

Spectrophotometric Determination of Ezetimibe

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P. Baby Sudha Lakshmi

2010-01-01

Full Text Available Two simple, sensitive, selective and accurate spectro-photometric methods (Method A and Method B for the determination of eztimibe in bulk drug and pharmaceutical formulations (tablets have been described. Method A and B are based on the redox/complex formation reaction of drug with 1,10-phenanthroline and hexacyano-ferrate(III in presence of ferric chloride to form coloured chromogens exhibiting λmax at 510 and 740 nm respectively. The results of analysis for the two methods have been validated statistically and by recovery studies. The results are compared with those obtained using UV spectrophotometric method in alcohol at 231.7 nm.

Compatible validated spectrofluorimetric and spectrophotometric methods for determination of vildagliptin and saxagliptin by factorial design experiments

Science.gov (United States)

Abdel-Aziz, Omar; Ayad, Miriam F.; Tadros, Mariam M.

2015-04-01

Simple, selective and reproducible spectrofluorimetric and spectrophotometric methods have been developed for the determination of vildagliptin and saxagliptin in bulk and their pharmaceutical dosage forms. The first proposed spectrofluorimetric method is based on the dansylation reaction of the amino group of vildagliptin with dansyl chloride to form a highly fluorescent product. The formed product was measured spectrofluorimetrically at 455 nm after excitation at 345 nm. Beer's law was obeyed in a concentration range of 100-600 μg ml-1. The second proposed spectrophotometric method is based on the charge transfer complex of saxagliptin with tetrachloro-1,4-benzoquinone (p-chloranil). The formed charge transfer complex was measured spectrophotometrically at 530 nm. Beer's law was obeyed in a concentration range of 100-850 μg ml-1. The third proposed spectrophotometric method is based on the condensation reaction of the primary amino group of saxagliptin with formaldehyde and acetyl acetone to form a yellow colored product known as Hantzsch reaction, measured at 342.5 nm. Beer's law was obeyed in a concentration range of 50-300 μg ml-1. All the variables were studied to optimize the reactions' conditions using factorial design. The developed methods were validated and proved to be specific and accurate for quality control of vildagliptin and saxagliptin in their pharmaceutical dosage forms.

Comparison of spectrophotometric and radioisotopic methods for the assay of Rubisco in ozone-treated plants

International Nuclear Information System (INIS)

Reid, C.D.; Tissue, D.T.; Fiscus, E.L.; Strain, B.R.

1997-01-01

Radioisotopic and spectrophotometric assays for ribulose-1,5-bisphosphate carboxylase/oxygenase (Rubisco) initial and final activities and Rubisco content were compared in plants chronically exposed to ozone (O 3 ) in a greenhouse and the field. In a greenhouse experiment, Glycine max was treated in exposure chambers with either charcoal-filtered air (CF air) or 100 nl O 3 l -1 for 6 h daily during vegetative growth. Samples were collected after 7 days of exposure. In a field experiment, G. max was treated in open-top chambers with either CF air or non-filtered air with O 3 added at 1.5 times ambient O 3 for 12 h daily. Average daily O 3 concentrations were 21 and 92 nl l -1 in the CF and O 3 treatments, respectively. Samples were collected during vegetative and reproductive growth. Both assays generally yielded comparable Rubisco initial and final activities for greenhouse-grown plants regardless of the O 3 treatment. However for field-grown plants, Rubisco initial and final activities average 15 and 23% lower when assayed by the spectrophotometric rather than the radioisotopic method. For Rubisco content estimated by the spectrophotometric method, lower values for the regression of Rubisco activity vs concentration of carboxyarabinitol-1.5-bisphosphate were observed in O 3- than in CF-treated plants. Both assays yielded comparable Rubisco contents in the greenhouse and in the field although the variation was larger with the spectrophotometric method in field-grown plants. Growth conditions, field vs greenhouse, were more critical to the spectrophotometric assay performance than the O 3 treatments for measurement of Rubisco activity and content. (au) 40 refs

A COMPARISON OF A SPECTROPHOTOMETRIC (QUERCETIN) METHOD AND AN ATOMIC-ABSORPTION METHOD FOR DETERMINATION OF TIN IN FOOD

DEFF Research Database (Denmark)

Engberg, Å

1973-01-01

Procedures for the determination of tin in food, which involve a spectrophotometric method (with the quercetin-tin complex) and an atomic-absorption method, are described. The precision of the complete methods and of the individual analytical steps required is evaluated, and the parameters...

Kinetics of the H 2O 2-dependent ligninase-catalyzed oxidation of veratryl alcohol in the presence of cationic surfactant studied by spectrophotometric technique

Science.gov (United States)

Liu, Airong; Huang, Xirong; Song, Shaofang; Wang, Dan; Lu, Xuemei; Qu, Yinbo; Gao, Peiji

2003-09-01

The kinetics of ligninase-catalyzed oxidation of veratryl alcohol (VA) by H 2O 2 in the aqueous medium containing cationic surfactant cetyltrimethylammonium bromide (CTAB) has been investigated using spectrophotometric technique. Steady-state kinetic studies at different concentrations of CTAB indicate that the reaction follows a ping pong mechanism and the mechanism always holds but the kinetic parameters vary with CTAB concentrations. CTAB is a weak inhibitor for ligninase; it lowers the maximum initial velocity. CTAB also causes the Michaelis constant of H 2O 2 to decrease dramatically and that of VA to increase markedly. Based on the changes in kinetic parameters of the enzyme-catalyzed reaction at different CTAB concentrations (lower than, near to and larger than its critical micelle concentration) and the effects of the CTAB monomer and the micelles on the spectra of VA and its corresponding aldehyde, a conclusion could be made that modification of the enzymatic protein by the surfactant monomer should be responsible for the above-mentioned results.

Determination of tartrazine in beverage samples by stopped-flow analysis and three-way multivariate calibration of non-linear kinetic-spectrophotometric data.

Science.gov (United States)

Schenone, Agustina V; Culzoni, María J; Marsili, Nilda R; Goicoechea, Héctor C

2013-06-01

The performance of MCR-ALS was studied in the modeling of non-linear kinetic-spectrophotometric data acquired by a stopped-flow system for the quantitation of tartrazine in the presence of brilliant blue and sunset yellow FCF as possible interferents. In the present work, MCR-ALS and U-PCA/RBL were firstly applied to remove the contribution of unexpected components not included in the calibration set. Secondly, a polynomial function was used to model the non-linear data obtained by the implementation of the algorithms. MCR-ALS was the only strategy that allowed the determination of tartrazine in test samples accurately. Therefore, it was applied for the analysis of tartrazine in beverage samples with minimum sample preparation and short analysis time. The proposed method was validated by comparison with a chromatographic procedure published in the literature. Mean recovery values between 98% and 100% and relative errors of prediction values between 4% and 9% were indicative of the good performance of the method. Copyright © 2012 Elsevier Ltd. All rights reserved.

Batch and flow-injection methods for the spectrophotometric determination of olanzapine

Energy Technology Data Exchange (ETDEWEB)

Jasinska, A.; Nalewajko, E

2004-04-22

An indirect batch spectrophotometric and direct flow-injection (FI) visible spectrophotometric methods have been developed for the determination of the novel anti-psychotic drug olanzapine (OLA). The batch method is based on the oxidation of olanzapine by a known excess of potassium hexacyanoferrate(III) in the presence of the mixture of sulphuric and phosphoric acids (1:1 (v/v)). The absorbance of unreacted oxidant is measured at 425 nm. The absorbance decreases linearly with increasing concentration of the assayed drug. The FI method with detection at 540 nm is based on the direct oxidation of olanzapine one of two oxidants, cerium(IV) sulphate or potassium hexacyanoferrate(III) in acidic medium. The calibration graph were linear over the range of 2.5-40 {mu}g ml{sup -1} in the batch method and 0.05-300 and 0.5-250 {mu}g ml{sup -1} in the FI methods, used cerium (IV) sulphate and potassium hexacyanoferrate (III) respectively. Both FI methods gave similar results in terms of precision and accuracy. The relative standard deviation (R.S.D.), was <1%. The accuracy, obtained from recovery experiments, was 97.9-99.4%. The batch method gave slightly higher R.S.D. values (up to 2.3%) and lower values of accuracy (the recovery was between 96.5 and 96.6%). The methods developed were applied to the determination of olanzapine in a pharmaceutical product.

Spectrophotometric determination of chlorthalidone in pharmaceutical formulations using different order derivative methods

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Narmeen S. Abdullah

2017-05-01

Full Text Available Simple, repaid and accurate zero-, first- and second-order derivative spectrophotometric methods have been developed for determination of chlorthalidone (CLT in commercially available tablets. Normal spectrophotometric scan (zero order shows maximum absorbance at 276 nm in methanol solution and a good linearity in the range of 10.0–75.0 μg/mL. Linear relations using first (D1 and second (D2 order derivative methods were obtained at 278 and 288 nm for D1 and 286 and 292 nm for D2.The calibration curves were constructed in the range of 1.0–25.0 μg/mL for D1 (R = 0.998 and D2 (R = 0.999. Different analytical validations were determined (accuracy, precision, specificity, recovery, stability and robustness to demonstrate its suitability for routine quality control labs. All the developed methods were successfully applied to a tablet formulation and the results were compared statistically with each other and with those obtained by the HPLC reference method.

Development and Application of Kinetic Spectrophotometric Method ...

African Journals Online (AJOL)

ISSN: 1596-5996 (print); 1596-9827 (electronic) ... Methods: The method is based on oxidation reaction of MNZ by hydrogen peroxide ... optimum operating conditions for reagent concentrations and temperature were ... 1-yl) ethanol] is an amebicide, antiprotozoal and .... The dependence of reaction rate on concentration of.

Analysis of Protein by Spectrophotometric and Computer Colour Based Intensity Method from Stem of Pea (Pisum sativum at Different Stages

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Afsheen Mushtaque Shah

2010-12-01

Full Text Available In this study proteins were analyzed from pea plants at three different growth stages of stem by spectrophotometric i.e Lowry and Bradford quantitative methods and computer colour intensity based method. Though Spectrophotometric methods are regarded as classical methods, we report an alternate computer based method which gave comparable results. Computer software was developed the for protein analysis which is easier, time and money saving method as compared to the classical methods.

Development and validation of spectrophotometric method for assay determination and in vitro dissolution studies of sofosbuvir tablets

International Nuclear Information System (INIS)

Zaman, B.; Hassan, W.; Noreen, H.

2017-01-01

In vitro dissolution of sofosbuvir 400 mg tablets dosage form was performed, using USP dissolution apparatus type-II (paddle type), at 75rpm ± 4 %, and 900mL ± 1%, 0.05 M phosphate buffer pH 6.8 ± 0.05 equilibrated at 37.0 ± 0.5ºC as dissolution medium. Percentage of dissolved sofosbuvir as a function of time was determined using the straight line equation and linear regression using zero order and first order ANOVA based kinetics model. Comparative dissolution studies on two different generic brands A and B was performed comparing the drug release profile with innovator brand Sovaldi 400 mg tablets. The comparison of dissolution profiles was evaluated using model independent approach. The values of similarity factor f2 were (4 and 3) and the difference factor f1 were (64 and 50) for both generic products A and B respectively. A simple and precise spectrophotometric method was developed for estimation of sofosbuvir in dissolution medium based on spectrophotometric detection at wavelength 262 nm. The specific absorbance (A = 1%) of sofosbuvir was 178.5 ± 4% and Beer’s law was obeyed in the concentration ranges 4µg mL−1 to 48µg mL−1. The method was validated appropriately for accuracy, precision, linearity, and specificity, according the guidelines of United State Pharmacopoeia and International Conference on Harmonization. The calibration curve was linear with correlation coefficient (r > 0.9999) and there was no spectral interference from excipients present in the tablets dosage form. This method is precise, rapid and specific for determination of sofosbuvir in tablets dosage form and successfully applied for assay determination and in vitro dissolution studies. (author)

New Spectrophotometric and Conductometric Methods for Macrolide Antibiotics Determination in Pure and Pharmaceutical Dosage Forms Using Rose Bengal

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Rania A. Sayed

2013-01-01

Full Text Available Two Simple, accurate, precise, and rapid spectrophotometric and conductometric methods were developed for the estimation of erythromycin thiocyanate (I, clarithromycin (II, and azithromycin dihydrate (III in both pure and pharmaceutical dosage forms. The spectrophotometric procedure depends on the reaction of rose bengal and copper with the cited drugs to form stable ternary complexes which are extractable with methylene chloride, and the absorbances were measured at 558, 557, and 560 nm for (I, (II, and (III, respectively. The conductometric method depends on the formation of an ion-pair complex between the studied drug and rose bengal. For the spectrophotometric method, Beer's law was obeyed. The correlation coefficient ( for the studied drugs was found to be 0.9999. The molar absorptivity (, Sandell’s sensitivity, limit of detection (LOD, and limit of quantification (LOQ were also calculated. The proposed methods were successfully applied for the determination of certain pharmaceutical dosage forms containing the studied drugs

Semi-empirical spectrophotometric (SESp) method for the indirect determination of the ratio of cationic micellar binding constants of counterions X⁻ and Br⁻(K(X)/K(Br)).

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Khan, Mohammad Niyaz; Yusof, Nor Saadah Mohd; Razak, Norazizah Abdul

2013-01-01

The semi-empirical spectrophotometric (SESp) method, for the indirect determination of ion exchange constants (K(X)(Br)) of ion exchange processes occurring between counterions (X⁻ and Br⁻) at the cationic micellar surface, is described in this article. The method uses an anionic spectrophotometric probe molecule, N-(2-methoxyphenyl)phthalamate ion (1⁻), which measures the effects of varying concentrations of inert inorganic or organic salt (Na(v)X, v = 1, 2) on absorbance, (A(ob)) at 310 nm, of samples containing constant concentrations of 1⁻, NaOH and cationic micelles. The observed data fit satisfactorily to an empirical equation which gives the values of two empirical constants. These empirical constants lead to the determination of K(X)(Br) (= K(X)/K(Br) with K(X) and K(Br) representing cationic micellar binding constants of counterions X and Br⁻). This method gives values of K(X)(Br) for both moderately hydrophobic and hydrophilic X⁻. The values of K(X)(Br), obtained by using this method, are comparable with the corresponding values of K(X)(Br), obtained by the use of semi-empirical kinetic (SEK) method, for different moderately hydrophobic X. The values of K(X)(Br) for X = Cl⁻ and 2,6-Cl₂C6H₃CO₂⁻, obtained by the use of SESp and SEK methods, are similar to those obtained by the use of other different conventional methods.

Spectrophotometric Investigations of Macrolide Antibiotics: A Brief Review

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Mrudul R. Keskar

2015-01-01

Full Text Available Macrolides, one of the most commonly used class of antibiotics, are a group of drugs produced by Streptomyces species. They belong to the polyketide class of natural products. Their activity is due to the presence of a large macrolide lactone ring with deoxy sugar moieties. They are protein synthesis inhibitors and broad-spectrum antibiotics, active against both gram-positive and gram-negative bacteria. Different analytical techniques have been reported for the determination of macrolides such as chromatographic methods, flow injection methods, spectrofluorometric methods, spectrophotometric methods, and capillary electrophoresis methods. Among these methods, spectrophotometric methods are sensitive and cost effective for the analysis of various antibiotics in pharmaceutical formulations as well as biological samples. This article reviews different spectrophotometric methods for the determination of macrolide antibiotics.

Purohit's spectrophotometric method for determination of stability constants of complexes using Job's curves

International Nuclear Information System (INIS)

Purohit, D.N.; Goswami, A.K.; Chauhan, R.S.; Ressalan, S.

1999-01-01

A spectrophotometric method for determination of stability constants making use of Job's curves has been developed. Using this method stability constants of Zn(II), Cd(II), Mo(VI) and V(V) complexes of hydroxytriazenes have been determined. For the sake of comparison, values of the stability constants were also determined using Harvey and Manning's method. The values of the stability constants developed by two methods compare well. This new method has been named as Purohit's method. (author)

Determination of the acidity constants of neutral red and bromocresol green by solution scanometric method and comparison with spectrophotometric results

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Ardeshir Shokrollahi

2016-03-01

The method is based on scanning cells containing the indicator solution with a scanner, and analyzing the color of each cell with a software written in visual basic (VB 6 media to red, green and blue values. The cells were made by making holes in the Plexiglas® sheet. Also, the acidity constants of the neutral red and bromocresol green indicators were studied with spectrophotometrically. HypSpec program has been applied for the estimation of pKa values based on spectrophotometric data. The agreement between obtained pKa values by solution scanometric, spectrophotometric method and values reported in the literature demonstrates the utility of the method here used. Also the HySS 2009 program was applied for drawing of the corresponding distribution diagrams.

Kinetic determination of As(III in solution

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TODOR G. PECEV

2003-10-01

Full Text Available A new reaction is suggested and a new kinetic method is elaborated for the As(III traces determination in solution, on the basis of their catalyzing effect on komplexon III (EDTA oxidation by KMnO4 in a strong acid solution (H2SO4. Using a spectrophotometric technique, a sensitivity of 72 ng/cm3 As(III was achieved. The relative error of method varies from 5.5 to 13.9 % for As(III concentration range from 83 to 140 ng/cm3. Appropriate kinetic equations are formulated and the influence of some other ions, including the As(V, upon the reaction rate is tested.

Spectrophotometric Methods for Simultaneous Determination of Oxytetracycline HCl and Flunixin Meglumine in Their Veterinary Pharmaceutical Formulation

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Hanan A. Merey

2017-01-01

Full Text Available Four precise, accurate, selective, and sensitive UV-spectrophotometric methods were developed and validated for the simultaneous determination of a binary mixture of Oxytetracycline HCl (OXY and Flunixin Meglumine (FLU. The first method, dual wavelength (DW, depends on measuring the difference in absorbance (ΔA 273.4–327 nm for the determination of OXY where FLU is zero while FLU is determined at ΔA 251.7–275.7 nm. The second method, first-derivative spectrophotometric method (1D, depends on measuring the peak amplitude of the first derivative selectively at 377 and 266.7 nm for the determination of OXY and FLU, respectively. The third method, ratio difference method, depends on the difference in amplitudes of the ratio spectra at ΔP 286.5–324.8 nm and ΔP 249.6–286.3 nm for the determination of OXY and FLU, respectively. The fourth method, first derivative of ratio spectra method (1DD, depends on measuring the amplitude peak to peak of the first derivative of ratio spectra at 296.7 to 369 nm and 259.1 to 304.7 nm for the determination of OXY and FLU, respectively. Different factors affecting the applied spectrophotometric methods were studied. The proposed methods were validated according to ICH guidelines. Satisfactory results were obtained for determination of both drugs in laboratory prepared mixture and pharmaceutical dosage form. The developed methods are compared favourably with the official ones.

Spectrophotometric Methods for the Assay of Fluvoxamine Using Chromogenic Reagents

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V. Annapurna

2010-01-01

Full Text Available Simple, accurate and reproducible UV-Visible spectrophotometric methods were established for the assay of FXA based on the oxidative coupling and condensation reactions. Condensation and coupling of the FXA with Ninhydrin-Ascorbic acid is proposed in method A. Method B includes complexation of FXA with cobalt thiocyanate. The ligating property of FXA with sodium nitro prusside is incorporated in method C. The optical characteristics such as Beers law limits, molar absorptivity and Sandell’s sensitivity for the methods (A-C are given. Regression analysis using the method of least squares was made to evaluate the slope(b, intercept(a and correlation coefficient (r and standard error of estimation (Se for each system. Determination of FXA in bulk form and in pharmaceutical formulations were also incorporated.

Automated spectrophotometric bicarbonate analysis in duodenal juice compared to the back titration method.

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Erchinger, Friedemann; Engjom, Trond; Gudbrandsen, Oddrun Anita; Tjora, Erling; Gilja, Odd H; Dimcevski, Georg

2016-01-01

We have recently evaluated a short endoscopic secretin test for exocrine pancreatic function. Bicarbonate concentration in duodenal juice is an important parameter in this test. Measurement of bicarbonate by back titration as the gold standard method is time consuming, expensive and technically difficult, thus a simplified method is warranted. We aimed to evaluate an automated spectrophotometric method in samples spanning the effective range of bicarbonate concentrations in duodenal juice. We also evaluated if freezing of samples before analyses would affect its results. Patients routinely examined with short endoscopic secretin test suspected to have decreased pancreatic function of various reasons were included. Bicarbonate in duodenal juice was quantified by back titration and automatic spectrophotometry. Both fresh and thawed samples were analysed spectrophotometrically. 177 samples from 71 patients were analysed. Correlation coefficient of all measurements was r = 0.98 (p titration gold standard. This is a major simplification of direct pancreas function testing, and allows a wider distribution of bicarbonate testing in duodenal juice. Extreme values for Bicarbonate concentration achieved by the autoanalyser method have to be interpreted with caution. Copyright © 2016 IAP and EPC. Published by Elsevier India Pvt Ltd. All rights reserved.

New kinetic-spectrophotometric method for monitoring the concentration of iodine in river and city water samples.

Science.gov (United States)

Farmany, A; Khosravi, A; Abbasi, S; Cheraghi, J; Hushmandfar, R; Sobhanardakani, S; Noorizadeh, H; Mortazavi, S S

2013-01-01

A new kinetic method has been developed for the determination of iodine in water samples. The method is based on the catalytic effect of I(-) with the oxidation of Indigo Carmine (IC) by KBrO(3) in the sulfuric acid medium. The optimum conditions obtained are 0.16 M sulfuric acid, 1 × 10(-3) M of IC, 1 × 10(-2) M KBrO(3), reaction temperature of 35°C, and reaction time of 80 s at 612 nm. Under the optimized conditions, the method allowed the quantification of I(-) in a range of 12-375 ng/mL with a detection limit of 0.46 ng/mL. The method was applied to the determination of iodine in river and city water samples with the satisfactorily results.

Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples.

Science.gov (United States)

Fukushima, Romualdo S; Hatfield, Ronald D

2004-06-16

Present analytical methods to quantify lignin in herbaceous plants are not totally satisfactory. A spectrophotometric method, acetyl bromide soluble lignin (ABSL), has been employed to determine lignin concentration in a range of plant materials. In this work, lignin extracted with acidic dioxane was used to develop standard curves and to calculate the derived linear regression equation (slope equals absorptivity value or extinction coefficient) for determining the lignin concentration of respective cell wall samples. This procedure yielded lignin values that were different from those obtained with Klason lignin, acid detergent acid insoluble lignin, or permanganate lignin procedures. Correlations with in vitro dry matter or cell wall digestibility of samples were highest with data from the spectrophotometric technique. The ABSL method employing as standard lignin extracted with acidic dioxane has the potential to be employed as an analytical method to determine lignin concentration in a range of forage materials. It may be useful in developing a quick and easy method to predict in vitro digestibility on the basis of the total lignin content of a sample.

Computation of geometric representation of novel spectrophotometric methods used for the analysis of minor components in pharmaceutical preparations.

Science.gov (United States)

Lotfy, Hayam M; Saleh, Sarah S; Hassan, Nagiba Y; Salem, Hesham

2015-01-01

Novel spectrophotometric methods were applied for the determination of the minor component tetryzoline HCl (TZH) in its ternary mixture with ofloxacin (OFX) and prednisolone acetate (PA) in the ratio of (1:5:7.5), and in its binary mixture with sodium cromoglicate (SCG) in the ratio of (1:80). The novel spectrophotometric methods determined the minor component (TZH) successfully in the two selected mixtures by computing the geometrical relationship of either standard addition or subtraction. The novel spectrophotometric methods are: geometrical amplitude modulation (GAM), geometrical induced amplitude modulation (GIAM), ratio H-point standard addition method (RHPSAM) and compensated area under the curve (CAUC). The proposed methods were successfully applied for the determination of the minor component TZH below its concentration range. The methods were validated as per ICH guidelines where accuracy, repeatability, inter-day precision and robustness were found to be within the acceptable limits. The results obtained from the proposed methods were statistically compared with official ones where no significant difference was observed. No difference was observed between the obtained results when compared to the reported HPLC method, which proved that the developed methods could be alternative to HPLC techniques in quality control laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

Validated spectrophotometric methods for determination of Alendronate sodium in tablets through nucleophilic aromatic substitution reactions

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Walash Mohamed I

2012-04-01

Full Text Available Abstract Background Alendronate (ALD is a member of the bisphosphonate family which is used for the treatment of osteoporosis, bone metastasis, Paget's disease, hypocalcaemia associated with malignancy and other conditions that feature bone fragility. ALD is a non-chromophoric compound so its determination by conventional spectrophotometric methods is not possible. So two derivatization reactions were proposed for determination of ALD through the reaction with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl and 2,4-dinitrofluorobenzene (DNFB as chromogenic derivatizing reagents. Results Three simple and sensitive spectrophotometric methods are described for the determination of ALD. Method I is based on the reaction of ALD with NBD-Cl. Method II involved heat-catalyzed derivatization of ALD with DNFB, while, Method III is based on micellar-catalyzed reaction of the studied drug with DNFB at room temperature. The reactions products were measured at 472, 378 and 374 nm, for methods I, II and III, respectively. Beer's law was obeyed over the concentration ranges of 1.0-20.0, 4.0-40.0 and 1.5-30.0 μg/mL with lower limits of detection of 0.09, 1.06 and 0.06 μg/mL for Methods I, II and III, respectively. The proposed methods were applied for quantitation of the studied drug in its pure form with mean percentage recoveries of 100.47 ± 1.12, 100.17 ± 1.21 and 99.23 ± 1.26 for Methods I, II and III, respectively. Moreover the proposed methods were successfully applied for determination of ALD in different tablets. Proposals of the reactions pathways have been postulated. Conclusion The proposed spectrophotometric methods provided sensitive, specific and inexpensive analytical procedures for determination of the non-chromophoric drug alendronate either per se or in its tablet dosage forms without interference from common excipients. Graphical abstract

Extractive Spectrophotometric Methods for the Determination of Etoricoxib in Tablets

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Kamal Shah

2009-01-01

Full Text Available Two simple, rapid, sensitive, precise and economic spectrophotometric methods have been developed for the estimation of etoricoxib in tablet formulation. During the course of study, it was observed that acidic solution of the drug formed colored ion-association complexes with Bromocresol Green (BCG and Bromocresol Purple (BCP which were soluble in chloroform. This property of the drug was followed for the development of colorimetric methods for analysis of drug. The complex of etoricoxib with BCG and BCP showed λmax at 416 nm and 408 nm respectively. These methods were validated statistically. Recovery studies gave satisfactory results indicating that none of common additives and excipients interfere the assay method. The proposed methods are found to be simple, accurate and reproducible that was successfully applied for the analysis of tablet formulation.

Estimation of very low concentrations of Ruthenium by spectrophotometric method using barbituric acid as complexing agent

International Nuclear Information System (INIS)

Ramakrishna Reddy, S.; Srinivasan, R.; Mallika, C.; Kamachi Mudali, U.; Natarajan, R.

2012-01-01

Spectrophotometric method employing numerous chromogenic reagents like thiourea, 1,10-phenanthroline, thiocyanate and tropolone is reported in the literature for the estimation of very low concentrations of Ru. A sensitive spectrophotometric method has been developed for the determination of ruthenium in the concentration range 1.5 to 6.5 ppm in the present work. This method is based on the reaction of ruthenium with barbituric acid to produce ruthenium(ll)tris-violurate, (Ru(H 2 Va) 3 ) -1 complex which gives a stable deep-red coloured solution. The maximum absorption of the complex is at 491 nm due to the inverted t 2g → Π(L-L ligand) electron - transfer transition. The molar absorptivity of the coloured species is 9,851 dm 3 mol -1 cm -1

Comparison of gravimetric and spectrophotometric methods for the determination of O/U ratios in uranium oxides

International Nuclear Information System (INIS)

Esteban, Adolfo; Eppis, Maria Rosa

2004-01-01

One important parameter to specify in nuclear fuels is the oxygen-metal ratio; many tests were described in literature to determine it. Possibly, gravimetric methods are the most used and usually a good precision was obtained analysing sintered materials. However, the humidity sorbed in the samples and impurities affect these methods, especially in powders. On the other hand, the spectrophotometric methods determine oxygen-uranium ratio by measuring the absorbances of different ionic species in phosphoric acid. This technique is simply and is not affected by humidity and impurities. Owing to discrepancy in the results between both methods, it was carried out in our laboratory, a study on various gravimetric and spectrophotometric methods. Several assays and analysis were performed comparing test procedures, trying to obtain better precision and accuracy. This work presents the results obtained and the recommend procedure to use with sintered and unsintered materials

Development and Validation of Spectrophotometric Methods for the Determination of Rasagiline in Pharmaceutical Preparations

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Serife Evrim Kepekci Tekkeli

2013-01-01

Full Text Available This study presents three simple, rapid, and accurate spectrophotometric methods for the determination of Rasagiline (RSG in pharmaceutical preparations. The determination procedures depend on the reaction of RSG with chloranilic acid for method A, tetrachloro-1,4-benzoquinone for method B, and 7,7,8,8-tetracyanoquinodimethane for method C. The colored products were quantitated spectrophotometrically at 524, 535, and 843 nm for methods A, B, and C, respectively. Different variables affecting the reaction were optimized. Linearity ranges of the methods with good correlation coefficients (0.9988–0.9996 were observed as 25–300 µg mL−1, 25–350 µg mL−1, and 50–500 µg mL−1 for methods A, B, and C, respectively. The formation of products takes place through different mechanisms. The sites of interaction were confirmed by elemental analysis using IR and 1H-NMR spectroscopy. The validation of the methods was carried out in terms of specificity, linearity, accuracy, precision, robustness, limit of detection, and limit of quantitation. No interference was observed from concomitants usually present in dosage forms. The methods were applied successfully to the determination of RSG in pharmaceutical preparations.

Quantization of buspirone hydrochloride in pure and pharmaceutical formulation by spectrophotometric method

International Nuclear Information System (INIS)

Kazi, A.A.; Mumtaz, A.; Sabri, M.U.

2008-01-01

A simple and sensitive method is described for the determination of bus pirone hydrochloride in bulk drug and in formulations employing spectrophotometric technique. The method is based on the interaction orbuspirone hydrochloride with ammonium molybdate in acidic media and the absorbance is measured at 700 nm. Beer's Law is obeyed in the range of 5 macro g to 350 micro g/ml and RSD is 0.96% for buspirone hydrochloride. Analytical data for the determination of pure compound is presented along with the application of the proposed method for the analysis of pharmaceutical formulation. (author)

Validated univariate and multivariate spectrophotometric methods for the determination of pharmaceuticals mixture in complex wastewater

Science.gov (United States)

Riad, Safaa M.; Salem, Hesham; Elbalkiny, Heba T.; Khattab, Fatma I.

2015-04-01

Five, accurate, precise, and sensitive univariate and multivariate spectrophotometric methods were developed for the simultaneous determination of a ternary mixture containing Trimethoprim (TMP), Sulphamethoxazole (SMZ) and Oxytetracycline (OTC) in waste water samples collected from different cites either production wastewater or livestock wastewater after their solid phase extraction using OASIS HLB cartridges. In univariate methods OTC was determined at its λmax 355.7 nm (0D), while (TMP) and (SMZ) were determined by three different univariate methods. Method (A) is based on successive spectrophotometric resolution technique (SSRT). The technique starts with the ratio subtraction method followed by ratio difference method for determination of TMP and SMZ. Method (B) is successive derivative ratio technique (SDR). Method (C) is mean centering of the ratio spectra (MCR). The developed multivariate methods are principle component regression (PCR) and partial least squares (PLS). The specificity of the developed methods is investigated by analyzing laboratory prepared mixtures containing different ratios of the three drugs. The obtained results are statistically compared with those obtained by the official methods, showing no significant difference with respect to accuracy and precision at p = 0.05.

Simultaneous determination of the brand new two-drug combination for the treatment of hepatitis C: Sofosbuvir/ledipasvir using smart spectrophotometric methods manipulating ratio spectra

Science.gov (United States)

Eissa, Maya S.

2017-08-01

In this work, various sensitive and selective spectrophotometric methods were first introduced for the simultaneous determination of sofosbuvir and ledipasvir in their binary mixture without preliminary separation. Ledipasvir was determined simply by zero-order spectrophotometric method at its λmax = 333.0 nm in a linear range of 2.5-30.0 μg/ml without any interference of sofosbuvir even in low or high concentrations and with mean percentage recovery of 100.05 ± 0.632. Sofosbuvir can be quantitatively estimated by one of the following smart spectrophotometric methods based on ratio spectra developed for the resolution of the overlapped spectra of their binary mixture; ratio difference spectrophotometric method (RD) by computing the difference between the amplitudes of sofosbuvir ratio spectra at 228 nm and 270 nm, first derivative (DD1) of ratio spectra by measuring the sum of amplitude of trough and peak at 265 nm and 277 nm, respectively, ratio subtraction (RS) spectrophotometric method in which sofosbuvir can be successfully determined at its λmax = 261.0 nm and mean centering (MC) of ratio spectra by measuring the mean centering values at 270 nm. All of the above mentioned spectrophotometric methods can estimate sofosbuvir in a linear range of 7.5-90.0 μg/ml with mean percentage recoveries of 100.57 ± 0.810, 99.92 ± 0.759, 99.51 ± 0.475 and 100.75 ± 0.672, respectively. These methods were successfully applied to the analysis of their combined dosage form and bulk powder. The adopted methods were also validated as per ICH guidelines and statistically compared to an in-house HPLC method.

Spectrophotometric determination of nitrite by its catalytic effect on the oxidation of congo red with bromate

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Zenovia Moldovan

2012-08-01

Full Text Available A novel simple, sensitive and rapid kinetic-spectrophotometric method for the determination of trace amounts of nitrite is proposed. The method is based on its catalytic effect on the oxidation of congo red (CR by potassium bromate in acidic solution. The oxidation reaction is monitored spectrophotometrically by measuring the decrease in the absorbance of CR at a suitable λmax = 570 nm for the first 10–40 s from the start of the reaction. Under the optimum experimental conditions (sulfuric acid, 0.3 M; CR, 0.75Χ10-4 M; potassium bromate, 5Χ10-4 M and 25 oC, nitrite can be determined in the range of 0.015–0.75 µg mL−1 with the detection limit of 0.006 µg mL−1. The relative standard deviation of five replicate determination of 0.25 µg mL−1 nitrite was 2.5%. The proposed method was applied satisfactorily to the determination of nitrite in spiked drinking water samples.DOI: http://dx.doi.org/10.4314/bcse.v26i2.1

Determination of niobium in rocks by an isotope dilution spectrophotometric method

Science.gov (United States)

Greenland, L.P.; Campbell, E.Y.

1970-01-01

Rocks and minerals are fused with sodium peroxide in the presence of carrierfree 95Nb. The fusion cake is leached with water and the precipitate dissolved in hydrofluoric-sulfuric acid mixture. Niobium is extracted into methyl isobutyl ketone and further purified by ion exchange. The amount of niobium is determined spectrophotometrically with 4-(2-pyridylazo)-resorcinol, and the chemical yield of the separations determined by counting 95Nb. This procedure is faster and less sensitive to interferences than previously proposed methods for determining niobium in rocks.The high purity of the separated niobium makes the method applicable to nearly all matrices. ?? 1970.

The analysis of impurities in the diuranate-determination of phosphate by phosphomolybdate blue spectrophotometric method

International Nuclear Information System (INIS)

Sun Haobo

2014-01-01

Phosphomolybdenum blue spectrophotometric method was used for determination of phosphate in the diuranate. Diuranate was dissolved in nitric acid solution, in which formed a soluble heteropolyacid complex (namely phosphomolybdenum yellow) due to interaction of phosphate and ammonium molybdate. Then phosphomolybdenum yellow was reduced to phosphomolybdenum blue with Bismuth nitrate as catalyst. Colour intensity at 700 nm is in proportion to the content of phosphate determined by spectrophotometric method. This experiment presents good linearity at the range of 30 μg to 245 μg phosphate, and the relative standard deviation of the experimental result is 2.4%, and the recovery rate is from 95% to 105%. The determination result of phosphate content will not be effected under conditions of 4 mg of SiO 2 , 6 mg of Fe, 400 mg of Cl - and 4.5 mg of Ge in the solution. (author)

Reaction of uranium (IV) with xenon difluoride by chemiluminescence, spectrophotometric, and spectrofluorimetric methods

Energy Technology Data Exchange (ETDEWEB)

Mamykin, A.V.; Kazakov, V.P.

1988-07-01

A study is made of the kinetics of the chemiluminescent reaction of oxidation of uranium (IV) by xenon difluoride in 1M HClO/sub 4/ U/sup 4 +/ + XeF/sub 2/ ..-->.. UO/sub 2//sup 2 +/ = h/eta/. The optical density D and the intensity of the photoluminescence of the solution I/sub PL/ were measured in parallel with recording of the luminescence intensity I/sub CL/. I/sub CL/ attains a maximum value some time after the beginning of the reaction, after which it decays exponentially. On the kinetic curves of the time dependence of D and I/sub PL/ an induction period is observed, the extent of which depends on concentrations of reagents and temperature of the solution. The maximum of I/sub CL/ coincides with the end of the induction period if the measurements are carried out under identical conditions. The rate of the reaction after the induction period is described by a first order equation in U/sup (IV)/. The rate constants of the reaction, obtained by chemiluminescence, spectrophotometric, and spectrofluorimetric methods, have close values 2.0 +- 0.4, 1.8 +- 0.3, and 2.1 +- 0.3 sec/sup /minus/1/ x 10/sup 2/, respectively. On the basis of the results obtained, we conclude that the stages of formation of UO/sub 2//sup 2 +/ and of chemiluminescence coincide, i.e., formation of the excited state (UD/sub 2//sup 2 +/) and of chemiluminescence coincide, i.e., formation of the excited state (UD/sub 2//sup 2 +/)* takes place during the reaction. It is proposed and experimentally verified that the reaction passes through an intermediate stage of formation of uranyl ion UO/sub 2//sup +/.

Spectrophotometric method of the determination of gold (III) by using imipramine hydrochloride and promethazine hydrochloride

International Nuclear Information System (INIS)

Dembinski, B.; Kurzawa, M.; Szydlowska-Czerniak, A.

2003-01-01

Imipramine hydrochloride (IPM.HCl) and promethazine hydrochloride (PMT-HCl) were used for the spectrophotometric determination of gold (III) in the aqueous solution. The halides complexes of gold (III) created a coloured coupling with the studied drugs which were extractable in chloroform. These new compounds were characterized by IR,UV-VIS spectra and thermal and elemental analysis. Rapid and sensitive spectrophotometric method for the determination of gold (III) in the aqueous solution is described. The absorbance was found to be linear function of the gold (III) concentration in the range from 0.2 to 20 x10/sup -1/ mg. The ratio of complex (AuX/sub 4/) to the organic cation from drug in the obtained compounds was determined as 1:1. The method was satisfactorily applied to the analysis of gold (III). A great advantage of the proposed method is that the trace amounts of gold (III) can also be examined. (author)

Kinetic spectrophotometric determination of ethamsylate in dosage forms.

Science.gov (United States)

El-Enany, Nahed; Belal, Fathalla; Rizk, Mohamed

2007-01-01

A simple and sensitive kinetic method has been developed for the determination of ethamsylate (ESL) in its pharmaceutical preparations. The method is based upon oxidation of ESL with 3-methyl-2-benzothiazolinone hydrazone hydrochloride in presence of cerium (IV) ammonium sulfate at room temperature for 20 min. The absorbance of the reaction product is measured at 514 nm. The absorbance-concentration plot was rectilinear over the range of 4-30 microg/mL (r = 0.9999). The lower detection limit was 0.267 microl/mL (9.110 x 10(-6) M) and the lower quantitation limit was 0.808 microg/mL. The different experimental parameters affecting the development and stability of the reaction product were studied and optimized. The proposed method was applied to the determination of ESL in formulations, and the results obtained were in good agreement with those obtained using a reference method. The proposed method was also used for the in vitro detection of ESL in spiked human plasma at its therapeutic concentration level.

Differential spectrophotometric determination of plutonium

International Nuclear Information System (INIS)

Lecat, J.

1980-01-01

Differential spectrophotometric method is used for determination of plutonium reduced to oxydation state III+ by ascorbic acid, at 560 nm. Concentration of solutions is 4 g/l and accuracy of the method is better than 0,3% [fr

Determination of dissociation constants for coordination compounds of Cr(III) and Co(III) using potentiometric and spectrophotometric methods

International Nuclear Information System (INIS)

Chylewska, A.; Jacewicz, D.; Zarzeczanska, D.; Chmurzynski, L.

2008-01-01

The acid-base properties of analogous complex ions of chromium(III) and cobalt(III) in aqueous solution have been studied. The equilibrium constants for all metal complexes were determined by using potentiometric and spectrophotometric titration methods. First, dissociation constants for the studied complexes of Cr(III) and Co(III) were determined by means of the potentiometric titration method and using the STOICHIO computer programme. Then, pH-spectrophotometric titrations were performed and the OriginPro 7.5 computer programme was used to calculate the same constants. The measurements using both methods were carried out under the same conditions of temperature, T = 298.15 K, and over the same pH range 2.00-10.00, respectively. It turned out that the two methods used enabled us to obtain acidity constants in very good agreement

Determination of dissociation constants for coordination compounds of Cr(III) and Co(III) using potentiometric and spectrophotometric methods

Energy Technology Data Exchange (ETDEWEB)

Chylewska, A.; Jacewicz, D.; Zarzeczanska, D. [Department of Chemistry, University of Gdansk, Sobieskiego 18/19, 80-952 Gdansk (Poland); Chmurzynski, L. [Department of Chemistry, University of Gdansk, Sobieskiego 18/19, 80-952 Gdansk (Poland)], E-mail: lech@chem.univ.gda.pl

2008-08-15

The acid-base properties of analogous complex ions of chromium(III) and cobalt(III) in aqueous solution have been studied. The equilibrium constants for all metal complexes were determined by using potentiometric and spectrophotometric titration methods. First, dissociation constants for the studied complexes of Cr(III) and Co(III) were determined by means of the potentiometric titration method and using the STOICHIO computer programme. Then, pH-spectrophotometric titrations were performed and the OriginPro 7.5 computer programme was used to calculate the same constants. The measurements using both methods were carried out under the same conditions of temperature, T = 298.15 K, and over the same pH range 2.00-10.00, respectively. It turned out that the two methods used enabled us to obtain acidity constants in very good agreement.

Acceptability criteria for linear dependence in validating UV-spectrophotometric methods of quantitative determination in forensic and toxicological analysis

Directory of Open Access Journals (Sweden)

L. Yu. Klimenko

2014-08-01

Full Text Available Introduction. This article is the result of authors’ research in the field of development of the approaches to validation of quantitative determination methods for purposes of forensic and toxicological analysis and devoted to the problem of acceptability criteria formation for validation parameter «linearity/calibration model». The aim of research. The purpose of this paper is to analyse the present approaches to acceptability estimation of the calibration model chosen for method description according to the requirements of the international guidances, to form the own approaches to acceptability estimation of the linear dependence when carrying out the validation of UV-spectrophotometric methods of quantitative determination for forensic and toxicological analysis. Materials and methods. UV-spectrophotometric method of doxylamine quantitative determination in blood. Results. The approaches to acceptability estimation of calibration models when carrying out the validation of bioanalytical methods is stated in international papers, namely «Guidance for Industry: Bioanalytical method validation» (U.S. FDA, 2001, «Standard Practices for Method Validation in Forensic Toxicology» (SWGTOX, 2012, «Guidance for the Validation of Analytical Methodology and Calibration of Equipment used for Testing of Illicit Drugs in Seized Materials and Biological Specimens» (UNODC, 2009 and «Guideline on validation of bioanalytical methods» (ЕМА, 2011 have been analysed. It has been suggested to be guided by domestic developments in the field of validation of analysis methods for medicines and, particularly, by the approaches to validation methods in the variant of the calibration curve method for forming the acceptability criteria of the obtained linear dependences when carrying out the validation of UV-spectrophotometric methods of quantitative determination for forensic and toxicological analysis. The choice of the method of calibration curve is

Spectrophotometric determination of eflornithine hydrochloride ...

African Journals Online (AJOL)

Purpose: To develop and validate a spectrophotometric method for the quantitative determination of eflornithine hydrochloride as a pure compound and in pharmaceutical formulations. Methods: The method involved the reaction of the target compound with vanillin reagent at specific pH 5.6 to produce a green reddish color ...

Spectrophotometric Determination of Eflornithine Hydrochloride ...

African Journals Online (AJOL)

Purpose: To develop and validate a spectrophotometric method for the quantitative determination of eflornithine hydrochloride as a pure compound and in pharmaceutical formulations. Methods: The method involved the reaction of the target compound with vanillin reagent at specific pH. 5.6 to produce a green reddish color ...

SPECTROPHOTOMETRIC METHOD FOR SIMULTANEOUS ESTIMATION OF TOLPERISONE HYDROCHLORIDE AND DICLOFENAC SODIUM IN SYNTHETIC MIXTURE

OpenAIRE

Patel Satish A; Hariyani Kaushik P

2012-01-01

The present manuscript describes simple, sensitive, rapid, accurate, precise and economical spectrophotometric method for the simultaneous determination of Diclofenac sodium and Tolperisone hydrochloride in bulk and synthetic mixture. The method is based on the simultaneous equations for analysis of both the drugs using methanol as solvent. Diclofenac sodium has absorbance maxima at 281 nm and Tolperisone hydrochloride has absorbance maxima at 255 nm in methanol. The linearity was obtained in...

SPECTROPHOTOMETRIC METHOD FOR SIMULTANEOUS ESTIMATION OF EPERISONE HYDROCHLORIDE AND DICLOFENAC SODIUM IN SYNTHETIC MIXTURE

OpenAIRE

Patel Paresh U; Patel Sejal K; Patel Umang J

2012-01-01

The present manuscript describes simple, sensitive, rapid, accurate, precise and economical spectrophotometric method for the simultaneous determination of diclofenac sodium and Eperisone hydrochloride in bulk and synthetic mixture. The method is based on the simultaneous equations for analysis of both the drugs using methanol as solvent. Diclofenac sodium has absorbance maxima at 281 nm and Eperisone hydrochloride has absorbance maxima at 255 nm in methanol. The linearity was obtained in the...

Validation of HPLC and UV spectrophotometric methods for the determination of meropenem in pharmaceutical dosage form.

Science.gov (United States)

Mendez, Andreas S L; Steppe, Martin; Schapoval, Elfrides E S

2003-12-04

A high-performance liquid chromatographic method and a UV spectrophotometric method for the quantitative determination of meropenem, a highly active carbapenem antibiotic, in powder for injection were developed in present work. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by reversed-phase technique on an RP-18 column with a mobile phase composed of 30 mM monobasic phosphate buffer and acetonitrile (90:10; v/v), adjusted to pH 3.0 with orthophosphoric acid. The UV spectrophotometric method was performed at 298 nm. The samples were prepared in water and the stability of meropenem in aqueous solution at 4 and 25 degrees C was studied. The results were satisfactory with good stability after 24 h at 4 degrees C. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and can be used for the reliable quantitation of meropenem in pharmaceutical dosage form.

A novel method for spectrophotometric determination of pregabalin in pure form and in capsules

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Gaur Prateek

2011-10-01

Full Text Available Abstract Background Pregabalin, a γ-amino-n-butyric acid derivative, is an antiepileptic drug not yet official in any pharmacopeia and development of analytical procedures for this drug in bulk/formulation forms is a necessity. We herein, report a new, simple, extraction free, cost effective, sensitive and reproducible spectrophotometric method for the determination of the pregabalin. Results Pregabalin, as a primary amine was reacted with ninhydrin in phosphate buffer pH 7.4 to form blue violet colored chromogen which could be measured spectrophotometrically at λmax 402.6 nm. The method was validated with respect to linearity, accuracy, precision and robustness. The method showed linearity in a wide concentration range of 50-1000 μg mL-1 with good correlation coefficient (0.992. The limits of assays detection was found to be 6.0 μg mL-1 and quantitation limit was 20.0 μg mL-1. The suggested method was applied to the determination of the drug in capsules. No interference could be observed from the additives in the capsules. The percentage recovery was found to be 100.43 ± 1.24. Conclusion The developed method was successfully validated and applied to the determination of pregabalin in bulk and pharmaceutical formulations without any interference from common excipients. Hence, this method can be potentially useful for routine laboratory analysis of pregabalin.

Development of Vanadometric System for Spectrophotometric ...

African Journals Online (AJOL)

rugged, and compares well with some complex methods for assay of timolol maleate in ... 3-[[4-(4-morpholinyl)-1, 2, 5-thiadiazol-3-yl] oxy]- ... preparation methods, costly reagents, expertise ..... chemical characterization, UV spectrophotometric.

Method development for arsenic analysis by modification in spectrophotometric technique

Directory of Open Access Journals (Sweden)

M. A. Tahir

2012-01-01

Full Text Available Arsenic is a non-metallic constituent, present naturally in groundwater due to some minerals and rocks. Arsenic is not geologically uncommon and occurs in natural water as arsenate and arsenite. Additionally, arsenic may occur from industrial discharges or insecticide application. World Health Organization (WHO and Pakistan Standard Quality Control Authority have recommended a permissible limit of 10 ppb for arsenic in drinking water. Arsenic at lower concentrations can be determined in water by using high tech instruments like the Atomic Absorption Spectrometer (hydride generation. Because arsenic concentration at low limits of 1 ppb can not be determined easily with simple spectrophotometric technique, the spectrophotometric technique using silver diethyldithiocarbamate was modified to achieve better results, up to the extent of 1 ppb arsenic concentration.

Artificial neural networks study of the catalytic reduction of resazurin: stopped-flow injection kinetic-spectrophotometric determination of Cu(II) and Ni(II)

International Nuclear Information System (INIS)

Magni, Diana M.; Olivieri, Alejandro C.; Bonivardi, Adrian L.

2005-01-01

An artificial neural network (ANN) procedure was used in the development of a catalytic spectrophotometric method for the determination of Cu(II) and Ni(II) employing a stopped-flow injection system. The method is based on the catalytic action of these ions on the reduction of resazurin by sulfide. ANNs trained by back-propagation of errors allowed us to model the systems in a concentration range of 0.5-6 and 1-15 mg l -1 for Cu(II) and Ni(II), respectively, with a low relative error of prediction (REP) for each cation: REP Cu(II) = 0.85% and REP Ni(II) = 0.79%. The standard deviations of the repeatability (s r ) and of the within-laboratory reproducibility (s w ) were measured using standard solutions of Cu(II) and Ni(II) equal to 2.75 and 3.5 mg l -1 , respectively: s r [Cu(II)] = 0.039 mg l -1 , s r [Ni(II)] = 0.044 mg l -1 , s w [Ni(II)] = 0.045 mg l -1 and s w [Ni(II)] = 0.050 mg l -1 . The ANNs-kinetic method has been applied to the determination of Cu(II) and Ni(II) in electroplating solutions and provided satisfactory results as compared with flame atomic absorption spectrophotometry method. The effect of resazurin, NaOH and Na 2 S concentrations and the reaction temperature on the analytical sensitivity is discussed

Stopped-flow injection spectrophotometric method for determination of chlorate in soil

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Jaroon Jakmunee

2008-06-01

Full Text Available A stopped-flow injection (FI spectrophotometric procedure based on iodometric reaction for the determination of chlorate has been developed. Standard/sample was injected into a stream of potassium iodide solution and then merged with a stream of hydrochloric acid solution to produce triiodide. By stopping the flow while the sample zone is being in a mixing coil, a slow reaction of chlorate with iodide in acidic medium was promoted to proceed with minimal dispersion of the triiodide product zone. When the flow started again, a concentrated product zone was pushed into a flow cell and a signal profile due to light absorption of the product was recorded. Employing a lab-built semi-automatic stopped-FI analyser, the analysis can be performed with higher degree of automation and low chemical consumption. Linear calibration graph in the range of 5-50 mg ClO3- L-1 was obtained, with detection limit of 1.4 mg ClO3- L-1. Relative standard deviation of 2.2% (30 mg ClO3- L-1, n=10 and sample throughput of about 20 h-1 were achieved. The system was applied to soil samples and validated by batch spectrophotometric and standard titrimetric methods.

Verification of spectrophotometric method for nitrate analysis in water samples

Science.gov (United States)

Kurniawati, Puji; Gusrianti, Reny; Dwisiwi, Bledug Bernanti; Purbaningtias, Tri Esti; Wiyantoko, Bayu

2017-12-01

The aim of this research was to verify the spectrophotometric method to analyze nitrate in water samples using APHA 2012 Section 4500 NO3-B method. The verification parameters used were: linearity, method detection limit, level of quantitation, level of linearity, accuracy and precision. Linearity was obtained by using 0 to 50 mg/L nitrate standard solution and the correlation coefficient of standard calibration linear regression equation was 0.9981. The method detection limit (MDL) was defined as 0,1294 mg/L and limit of quantitation (LOQ) was 0,4117 mg/L. The result of a level of linearity (LOL) was 50 mg/L and nitrate concentration 10 to 50 mg/L was linear with a level of confidence was 99%. The accuracy was determined through recovery value was 109.1907%. The precision value was observed using % relative standard deviation (%RSD) from repeatability and its result was 1.0886%. The tested performance criteria showed that the methodology was verified under the laboratory conditions.

DETERMINATION OF PROTOPINE IN FUMARIA DENSIFLORA DC. BY TLC- DENSITOMETRIC AND SPECTROPHOTOMETRIC METHOD

OpenAIRE

FAFAL, Tuğçe; ÖNÜR, Mustafa Ali

2007-01-01

The isoquinoline alkaloid protopine in Fumaria densiflora DC. (Fumariaceae) was quantitatively determined by TLC-densitometry and spectrophotometry. In TLC-densitometry two different solvent systems as toluene : chloroform : methanol : % 25 ammonium hydroxide (5:3:1:1) and cyclohexane : diethylamine (9:1) were used and protopine was detected as 0.351 and 0.352 % respectively. The content of protopine in Fumaria densiflora DC. was estimated as 0.366 % in spectrophotometric method. The quantita...

Measurement of Capsaicinoids in Chiltepin Hot Pepper: A Comparison Study between Spectrophotometric Method and High Performance Liquid Chromatography Analysis

Directory of Open Access Journals (Sweden)

Alberto González-Zamora

2015-01-01

Full Text Available Direct spectrophotometric determination of capsaicinoids content in Chiltepin pepper was investigated as a possible alternative to HPLC analysis. Capsaicinoids were extracted from Chiltepin in red ripe and green fruit with acetonitrile and evaluated quantitatively using the HPLC method with capsaicin and dihydrocapsaicin standards. Three samples of different treatment were analyzed for their capsaicinoids content successfully by these methods. HPLC-DAD revealed that capsaicin, dihydrocapsaicin, and nordihydrocapsaicin comprised up to 98% of total capsaicinoids detected. The absorbance of the diluted samples was read on a spectrophotometer at 215–300 nm and monitored at 280 nm. We report herein the comparison between traditional UV assays and HPLC-DAD methods for the determination of the molar absorptivity coefficient of capsaicin (ε280=3,410 and ε280=3,720 M−1 cm−1 and dihydrocapsaicin (ε280=4,175 and ε280=4,350 M−1 cm−1, respectively. Statistical comparisons were performed using the regression analyses (ordinary linear regression and Deming regression and Bland-Altman analysis. Comparative data for pungency was determined spectrophotometrically and by HPLC on samples ranging from 29.55 to 129 mg/g with a correlation of 0.91. These results indicate that the two methods significantly agree. The described spectrophotometric method can be routinely used for total capsaicinoids analysis and quality control in agricultural and pharmaceutical analysis.

New potentiometric and spectrophotometric methods for the determination of dextromethorphan in pharmaceutical preparations.

Science.gov (United States)

Elmosallamy, Mohamed A F; Amin, Alaa S

2014-01-01

New, simple and convenient potentiometric and spectrophotometric methods are described for the determination of dextromethorphan hydrobromide (DXM) in pharmaceutical preparations. The potentiometric technique is based on developing a potentiometric sensor incorporating the dextromethorphan tetrakis(p-chlorophenyl)borate ion-pair complex as an electroactive species in a plasticized PVC matrix membrane with o-nitophenyl octyl ether or dioctyl phthalate. The sensor shows a rapid near Nernstian response of over 1 × 10(-5) - 1 × 10(-2) mol L(-1) dextromethorphan in the pH range of 3.0 - 9.0. The detection limit is 2 × 10(-6) mol L(-1) DXM and the response time is instantaneous (2 s). The proposed spectrophotometric technique involves the reaction of DXM with eriochrom black T (EBT) to form an ion-associate complex. Solvent extraction is used to improve the selectivity of the method. The optimal extraction and reaction conditions have been studied, and the analytical characteristics of the method have been obtained. Linearity is obeyed in the range of 7.37 - 73.7 × 10(-5) mol L(-1) DXM, and the detection limit of the method is 1.29 × 10(-5) mol L(-1). The relative standard deviation (RSD) and relative error for six replicate measurements of 3.685 × 10(-4) mol L(-1) are 0.672 and 0.855%, respectively. The interference effect of some excepients has also been tested. The drug contents in pharmaceutical preparations were successfully determined by the proposed methods by applying the standard-addition technique.

Spectrophotometric and spectrofluorimetric methods for determination of certain biologically active phenolic drugs in their bulk powders and different pharmaceutical formulations

Science.gov (United States)

Omar, Mahmoud A.; Badr El-Din, Kalid M.; Salem, Hesham; Abdelmageed, Osama H.

2018-03-01

Two simple and sensitive spectrophotometric and spectrofluorimetric methods for the determination of terbutaline sulfate, fenoterol hydrobromide, etilefrine hydrochloride, isoxsuprine hydrochloride, ethamsylate, doxycycline hyclate have been developed. Both methods were based on the oxidation of the cited drugs with cerium (IV) in acid medium. The spectrophotometric method was based on measurement of the absorbance difference (ΔA), which represents the excess cerium (IV), at 317 nm for each drug. On the other hand, the spectrofluorimetric method was based on measurement of the fluorescent of the produced cerium (III) at emission wavelength 354 nm (λexcitation = 255 nm) for the concentrations studied for each drug. For both methods, the variables affecting the reactions were carefully investigated and the conditions were optimized. Linear relationships were found between either ΔA or the fluorescent of the produced cerium (III) values and the concentration of the studied drugs in a general concentration range of 2.0-24.0 μg mL- 1, 20.0-24.0 ng mL- 1 with good correlation coefficients in the following range 0.9990-0.9999, 0.9990-0.9993 for spectrophotometric and spectrofluorimetric methods respectively. The limits of detection and quantitation of spectrophotometric method were found in general concentration range 0.190-0.787 and 0.634-2.624 μg mL- 1respectively. For spectrofluorimetric method, the limits of detection and quantitation were found in general concentration range 4.77-9.52 and 15.91-31.74 ng mL- 1 respectively. The stoichiometry of the reaction was determined, and the reactions pathways were postulated. The analytical performance of the methods, in terms of accuracy and precision, were statistically validated and the results obtained were satisfactory. The methods have been successfully applied to the determination of the cited drugs in their commercial pharmaceutical formulations. Statistical comparison of the results with the reference methods

Development of microwave assisted spectrophotometric method for the determination of glucose

Science.gov (United States)

Ali, Asif; Hussain, Zahid; Arain, Muhammad Balal; Shah, Nasrullah; Khan, Khalid Mohammad; Gulab, Hussain; Zada, Amir

2016-01-01

A spectrophotometric method was developed based on the microwave assisted synthesis of Maillard product. Various conditions of the reaction were optimized by varying the relative concentration of the reagents, operating temperature and volume of solutions used in the reaction in the microwave synthesizer. The absorbance of the microwave synthesized Maillard product was measured in the range of 360-740 nm using UV-Visible spectrophotometer. Based on the maximum absorbance, 370 nm was selected as the optimum wave length for further studies. The LOD and LOQ of glucose was found 3.08 μg mL- 1 and 9.33 μg mL- 1 with standard deviation of ± 0.05. The developed method was also applicable to urine sample.

Optimization, Validation and Application of Spectrophotometric ...

African Journals Online (AJOL)

... 3Research Center of Food and Drug Evaluation, Wuhan University, Wuhan 430071, ... Methods: Spectrophotometric HMG-CoA reductase detection in male Wistar ... protein expression in various regulatory ... reagents were analytical grade.

Spectrophotometric determination of uranium using quercetin

International Nuclear Information System (INIS)

Barros, A.R.

1972-10-01

A spectrophotometric method for quantitative determination of uranium, using a flavone (quercetin) as complexing agent, is described. The method is based on the reaction between uranyl ion and alcoholic solution of quercetin with a complex formation of intense yellow color. (M.C.L.) [pt

Titanium Analysis of Ilmenite Bangka by Spectrophotometric Method Using Perhidrol

International Nuclear Information System (INIS)

Rusydi-S

2004-01-01

Determination of titanium by spectrofotometric method using perhydrol has been done. The purpose of experiment is to find out the condition of titanium analysis of ilmenite by spectrophotometric method. The experiment parameter e c. analysis condition include the Ti-perhydrol complex spectrum, acidity of complex, perhydrol concentration, linearity, influence of anion, limit detection, interfere elements, application of the method using 40 SRM Standard and analysis for ilmenite samples. Result of experiments are spectrum of Ti-perhydrol complex at 410 nm, acidity of complex is the H 2 SO 4 2 M, perhydrol concentration is 0,24 %, the curve calibration is linier at 1-80 ppm, anion of PO 4 , NO 3 , Cl, CO 3 not be influence until 2000 ppm, limit detection is 0,30 ppm and Mo, V is interfere. The method which was aplicated to 40 SRM standard, shown that the content of Ti is 1580 ppm while the standard is 1600 ppm, and the content of Ti from ilmenite high grade samples is 31,46 % and low grade is 13,55 %. (author)

Separation and spectrophotometric determination of elements

International Nuclear Information System (INIS)

Marczenko, Z.

1986-01-01

This book is a useful text intended as a reference for the laboratory that is either involved in spectrophotometric analysis or requires separations prior to analysis by any method. It attempts to cover a diverse series of topics in fewer than 700 pages. Part I of the book covers general topics such as separation schemes (solvent extraction, precipitation, volatility, ion exchange), principles and instrumentation used for spectrophotometry, and color reagents in only 119 pages. Entire books have been written on each of those subjects. The author must therefore resort to extensive referencing to cover each subject adequately. Part II, Methods for Separation and Determination of Individual Elements, discusses all elements - both nonmetals and metals and major procedures for the separation and spectrophotometric determination of each element are adequately covered

Spectrophotometric measurement of calcium carbonate saturation states in seawater.

Science.gov (United States)

Easley, Regina A; Patsavas, Mark C; Byrne, Robert H; Liu, Xuewu; Feely, Richard A; Mathis, Jeremy T

2013-02-05

Measurements of ocean pH and carbonate ion concentrations in the North Pacific and Arctic Oceans were used to determine calcium carbonate saturation states (Ω(CaCO(3))) from spectrophotometric methods alone. Total carbonate ion concentrations, [CO(3)(2-)](T), were for the first time at sea directly measured using Pb(II) UV absorbance spectra. The basis of the method is given by the following: [formula see text] where (CO(3))β(1) is the PbCO(3)(0) formation constant, e(i) are molar absorptivity ratios, and R = (250)A/(234)A (ratio of absorbances measured at 250 and 234 nm). On the basis of shipboard and laboratory Pb(II) data and complementary carbon-system measurements, the experimental parameters were determined to be (25 °C) the following: [formula see text]. The resulting mean difference between the shipboard spectrophotometric and conventional determinations of [CO(3)(2-)](T) was ±2.03 μmol kg(-1). The shipboard analytical precision of the Pb(II) method was ∼1.71 μmol kg(-1) (2.28%). Spectrophotometric [CO(3)(2-)](T) and pH(T) were then combined to calculate Ω(CaCO(3)). For the case of aragonite, 95% of the spectrophotometric aragonite saturation states (Ω(Aspec)) were within ±0.06 of the conventionally calculated values (Ω(Acalc)) when 0.5 ≤ Ω(A) ≤ 2.0. When Ω(A) > 2.0, 95% of the Ω(Aspec) values were within ±0.18 of Ω(Acalc). Our shipboard experience indicates that spectrophotometric determinations of [CO(3)(2-)](T) and Ω(CaCO(3)) are straightforward, fast, and precise. The method yields high-quality measurements of two important, rapidly changing aspects of ocean chemistry and offers capabilities suitable for long-term automated in situ monitoring.

Extractive spectrophotometric determination of molybdenum using p-chloroisonitroso acetophenone hydrazone

International Nuclear Information System (INIS)

Lokhande, R.S.; Agashe, A.P.; Hundiwale, D.G.

2001-01-01

Separation technique like solvent extraction can be advantageously employed for the determination of metals at low concentration in micrograms using spectrophotometric methods. Hydrazoxine has been used for the extraction and spectrophotometric determination of metals at trace level as well as for the studies of transition metals in complex form. In the present paper, solvent extraction technique has been used to develop methods for the separation and spectrophotometric determination of Mo(VI) with p-chloroisonitroso acetophenone hydrazone was extracted into chloroform from aqueous solution in the pH range 8 to 8.5. The absorption maxima was also tried for the extracted species and Beer's law was also studied for its applicability. In this, interference from the foreign ion has also been examined. (author)

Extractive Spectrophotometric Determination of Omeprazole in ...

African Journals Online (AJOL)

Erah

Abstract. Purpose: To develop a simple, rapid and selective method for the extractive spectrophotometric determination of .... The colour intensity of the organic layer had shown a very .... considerable attention for quantitative analyses of many ...

Thermo-Kinetic Investigation of Comparative Ligand Effect on Cysteine Iron Redox Reaction

OpenAIRE

Rizvi, Masood Ahmad; Teshima, Norio; Maqsood, Syed Raashid; Akhoon, Showket Ahmad; Peerzada, Ghulam Mustafa

2015-01-01

Transition metal ions in their free state bring unwanted biological oxidations generating oxidative stress. The ligand modulated redox potential can be indispensable in prevention of such oxidative stress by blocking the redundant bio-redox reactions. In this study we investigated the comparative ligand effect on the thermo-kinetic aspects of biologically important cysteine iron (III) redox reaction using spectrophotometric and potentiometric methods. The results were corroborated...

Spectrophotometric Determination of Cilostazol in Tablet Dosage Form

African Journals Online (AJOL)

Erah

Purpose: To develop simple, rapid and selective spectrophotometric methods for ... Conclusion: These validated methods may be useful for routine analysis of cilostazol ... Keywords: Cilostazol tablets, UV spectrophotometry, Linear regression ...

Kinetics of neptunim(6) reduction by hydroxylamine in chloric acid solutions

International Nuclear Information System (INIS)

Shilov, V.P.; Stepanova, E.S.; Krot, N.N.

1975-01-01

Stoichiometry and kinetics of neptunium (6) reaction with hydroxylamine is studied by spectrophotometric method at the ionic strength equal to unity and at 20-30 deg C. The reaction obeys the equation: -d[Np(6)]/dt = k 0 [Np(6)][NH 3 OH + ]/[H + ]sup(0.74), where k 0 = 2.6 M -1 min -1 at 25 deg C. Possible mechanism of the process includes two steps

Spectrophotometric determination of fluoride with alizarin complexone

Energy Technology Data Exchange (ETDEWEB)

Marczenko, Z; Lenarczyk, L [Politechnika Warszawska (Poland)

1976-01-01

The modification of direct spectrophotometric method of fluoride determination by alizarin complexone has been developed. It was shown that the lanthanum alizarin complexone chelate is more convenient than that of cerium (3). The influence of acetone, dioxane and dimethyl sulphoxide in water solution on the increase of sensitivity of the method and the rate of colour reaction has been determined. The optimal pH ranges for the reaction with lanthanum and cerium (3) have been estimated. Some amines having a large molecule are useful for extraction of blue fluoride complex with isobutanol. Dioctylamine was applied in a new extraction spectrophotometric procedure of fluoride determination. Conditions in reagent have been established. Both variants of the method have been applied to the fluoride determination in several chemicals. The obtained results show a good precision and accuracy.

Second derivative spectrophotometric determination of ...

African Journals Online (AJOL)

Hemn

2013-11-13

Nov 13, 2013 ... olanzapine in pharmaceutical formulation.Int.J.ChemTech. Res.2(1):756-761. Stanisz B, Paszun S, Lesniak M (2009). Validation of UV derivative spectrophotometric method for determination of benazepril hydrochloride in tablets and evaluation of its stability.ActaPoloniaePharmaceutica-Drug Research.

Spectrophotometric evaluation of surface morphology dependent catalytic activity of biosynthesized silver and gold nanoparticles using UV–vis spectra: A comparative kinetic study

Energy Technology Data Exchange (ETDEWEB)

Ankamwar, Balaprasad, E-mail: bankamwar@yahoo.com [Bio-inspired Materials Research Laboratory, Department of Chemistry, Savitribai Phule Pune University, Ganeshkhind, Pune 411007 (India); Kamble, Vaishali; Sur, Ujjal Kumar [Bio-inspired Materials Research Laboratory, Department of Chemistry, Savitribai Phule Pune University, Ganeshkhind, Pune 411007 (India); Santra, Chittaranjan [Department of Chemistry, Netaji Nagar Day College, Regent Park, Kolkata 700092 (India)

2016-03-15

Graphical abstract: - Highlights: • The biosynthesized silver nanoparticles were stable for 6 months and used as effective SERS active substrate. • They are effective catalyst in the chemical reduction of 4-nitrophenol to 4-aminophenol. • Comparative catalytic efficiency of both silver and gold nanoparticles was studied spectrophotometrically. • Our results demonstrate surface morphology dependent catalytic activity of both nanoparticles. - Abstract: The development of eco-friendly and cost-effective synthetic protocol for the preparation of nanomaterials, especially metal nanoparticles is an emerging area of research in nanotechnology. These metal nanoparticles, especially silver can play a crucial role in various catalytic reactions. The biosynthesized silver nanoparticles described here was very stable up to 6 months and can be further exploited as an effective catalyst in the chemical reduction of 4-nitrophenol to 4-aminophenol. The silver nanoparticles were utilized as an efficient surface-enhanced Raman scattering (SERS) active substrate using Rhodamine 6G as Raman probe molecule. We have also carried out systematic comparative studies on the catalytic efficiency of both silver and gold nanoparticles using UV–vis spectra to monitor the above reaction spectrophotometrically. We find that the reaction follows pseudo-first order kinetics and the catalytic activity can be explained by a simple model based on Langmuir–Hinshelwood mechanism for heterogeneous catalysis. We also find that silver nanoparticles are more efficient as a catalyst compare to gold nanoparticles in the reduction of 4-nitrophenol to 4-aminophenol, which can be explained by the morphology of the nanoparticles as determined by transmission electron microscopy.

Spectrophotometric evaluation of surface morphology dependent catalytic activity of biosynthesized silver and gold nanoparticles using UV–vis spectra: A comparative kinetic study

International Nuclear Information System (INIS)

Ankamwar, Balaprasad; Kamble, Vaishali; Sur, Ujjal Kumar; Santra, Chittaranjan

2016-01-01

Graphical abstract: - Highlights: • The biosynthesized silver nanoparticles were stable for 6 months and used as effective SERS active substrate. • They are effective catalyst in the chemical reduction of 4-nitrophenol to 4-aminophenol. • Comparative catalytic efficiency of both silver and gold nanoparticles was studied spectrophotometrically. • Our results demonstrate surface morphology dependent catalytic activity of both nanoparticles. - Abstract: The development of eco-friendly and cost-effective synthetic protocol for the preparation of nanomaterials, especially metal nanoparticles is an emerging area of research in nanotechnology. These metal nanoparticles, especially silver can play a crucial role in various catalytic reactions. The biosynthesized silver nanoparticles described here was very stable up to 6 months and can be further exploited as an effective catalyst in the chemical reduction of 4-nitrophenol to 4-aminophenol. The silver nanoparticles were utilized as an efficient surface-enhanced Raman scattering (SERS) active substrate using Rhodamine 6G as Raman probe molecule. We have also carried out systematic comparative studies on the catalytic efficiency of both silver and gold nanoparticles using UV–vis spectra to monitor the above reaction spectrophotometrically. We find that the reaction follows pseudo-first order kinetics and the catalytic activity can be explained by a simple model based on Langmuir–Hinshelwood mechanism for heterogeneous catalysis. We also find that silver nanoparticles are more efficient as a catalyst compare to gold nanoparticles in the reduction of 4-nitrophenol to 4-aminophenol, which can be explained by the morphology of the nanoparticles as determined by transmission electron microscopy.

The catalytic kinetic method for the determination of trace formaldehyde (FA) base on a bromate-eosin Y system

Science.gov (United States)

Tang, Yufang; Chen, Hao; Weng, Chao; Tang, Xiaohui; Zhang, Miaoling; Yang, Qiongqiong; Hu, Tao; Cai, Changqun

A new simple and highly sensitive catalytic kinetic method for the determination of trace amount of FA in food sample has been established. The method was based on the catalytic effect of FA on the oxidation of eosin Y by potassium bromate in present of phosphoric acid. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of eosin Y at 518 nm. Under the optimized experimental conditions, the developed method allowed the determination of FA in the range of 0.03-0.6 μg mL-1 with a good precision, and the limit of detection was down to 0.00988 μg mL-1. The relative standard deviation of five replicate measurements for the determination of FA in concentration 0.12 μg mL-1 was 1.8%. The proposed method was successfully applied to the determination of FA in food directly and satisfactory results were obtained.

Validation of a spectrophotometric method for quantification of carboxyhemoglobin.

Science.gov (United States)

Luchini, Paulo D; Leyton, Jaime F; Strombech, Maria de Lourdes C; Ponce, Julio C; Jesus, Maria das Graças S; Leyton, Vilma

2009-10-01

The measurement of carboxyhemoglobin (COHb) levels in blood is a valuable procedure to confirm exposure to carbon monoxide (CO) either for forensic or occupational matters. A previously described method using spectrophotometric readings at 420 and 432 nm after reduction of oxyhemoglobin (O(2)Hb) and methemoglobin with sodium hydrosulfite solution leads to an exponential curve. This curve, used with pre-established factors, serves well for lower concentrations (1-7%) or for high concentrations (> 20%) but very rarely for both. The authors have observed that small variations on the previously described factors F1, F2, and F3, obtained from readings for 100% COHb and 100% O(2)Hb, turn into significant changes in COHb% results and propose that these factors should be determined every time COHb is measured by reading CO and O(2) saturated samples. This practice leads to an increase in accuracy and precision.

The kinetics of hydrolysis of acetylsalicylic acid (Aspirin) in different ...

African Journals Online (AJOL)

The kinetics of hydrolysis of Acetylsalicylic acid (Aspirin) to salicylic acid was followed by the direct spectrophotometric measurement of the amount of salicylic acid produced with time. Salicylic acid was complexed with ferric ion giving a characteristic purple colour (λlm 523nm). The kinetics of hydrolysis was found to follow ...

Development and Validation of Eco-Friendly Liquid Chromatographic and Spectrophotometric Methods for Simultaneous Determination of Coformulated Drugs: Phenylephrine Hydrochloride and Prednisolone Acetate.

Science.gov (United States)

Mostafa, Nadia M; Elsayed, Ghada M; Hassan, Nagiba Y; El Mously, Dina A

2017-11-01

Five simple, sensitive, and eco-friendly LC and UV spectrophotometric methods have been developed for the simultaneous determination of phenylephrine hydrochloride (PHE) and prednisolone acetate (PRD) in their combined dosage form. The first method was reversed-phase (RP) LC using methanol-water-heptane-1-sulfonic acid sodium salt (75 + 25 + 0.1, v/v/w) as a mobile phase. Separation was achieved using an XSelect HSS reversed-phase C18 analytical column (250 × 4.6 mm, 5µm). The flow rate was 1.0 mL/min and UV detection was done at 230 nm. Quantification was achieved over the concentration ranges of 5-50 µg/mL for PHE and 2-90 µg/mL for PRD. Four spectrophotometric methods were proposed, namely dual wavelength, first derivative of ratio spectra, ratio difference, and mean-centering of ratio spectra. Linearity was observed in the concentration ranges of 10-120 and 5-35 µg/mL for PHE and PRD, respectively, for the spectrophotometric methods. Green solvents were used in the proposed methods because they play a vital role in the analytical methods' influence on the environment. The suggested methods were validated regarding linearity, accuracy, and precision according to the International Conference on Harmonization guidelines, with satisfactory results. These methods could be used as harmless substitutes for routine analysis of the mentioned drugs, with no interference from excipients.

Oxidation kinetics of crystal violet by potassium permanganate in acidic medium

Science.gov (United States)

Khan, Sameera Razi; Ashfaq, Maria; Mubashir; Masood, Summyia

2016-05-01

The oxidation kinetics of crystal violet (a triphenylmethane dye) by potassium permanganate was focused in an acidic medium by the spectrophotometric method at 584 nm. The oxidation reaction of crystal violet by potassium permanganate is carried out in an acidic medium at different temperatures ranging within 298-318 K. The kinetic study was carried out to investigate the effect of the concentration, ionic strength and temperature. The reaction followed first order kinetics with respect to potassium permanganate and crystal violet and the overall rate of the reaction was found to be second order. Thermodynamic activation parameters like the activation energy ( E a), enthalpy change (Δ H*), free energy change (Δ G*), and entropy change (Δ S*) have also been evaluated.

SIMULTANEOUS SPECTROPHOTOMETRIC DETERMINATION OF MONTELUKAST SODIUM AND BAMBUTEROL HYDROCHLORIDE IN TABLETS

OpenAIRE

Patel Satish A; Patel Dhara J; Patel Natavarlal J.

2011-01-01

The present manuscript describe simple, sensitive, rapid, accurate, precise and economical first derivative spectrophotometric method for the simultaneous determination of montelukast sodium and bambuterol hydrochloride in combined tablet dosage form. The derivative spectrophotometric method was based on the determination of both the drugs at their respective zero crossing point (ZCP). The first order derivative spectra was obtained in chloroform and the determinations were made at 241 nm (ZC...

A new innovative spectrophotometric method for the simultaneous determination of sofosbuvir and ledipasvir

Science.gov (United States)

Mansour, Fotouh R.

2018-01-01

A new innovative spectrophotometric method is developed to determine the concentration ratios in binary mixtures by determining the zero crossing point in the first derivative of the gross curve. This relationship can be applied if the part of the UV spectrum of substance Y, that intersects with the overlaid spectra of substance X is straight. By plotting the intersection wavelength against the concentration ratio (Cx/Cy), a straight line was obtained with a co-efficient of determination equals 0.9999. As an application, simultaneous determination of sofosbuvir and ledipasvir in their binary mixtures was performed using two methods; a direct UV spectrophotometric method for determination of ledipasvir at 333 nm, and the new "wavelength-intersection ratio" method for determination of sofosbuvir. In the wavelength-intersection ratio method, different mixtures of sofosbuvir and ledipasvir containing different concentration ratios were prepared; the zero crossing point of the first derivative curve in the range 285 to 295 nm were determined for each mixture. An absorbance shift in the intersection was obtained with the change in the concentration ratio (sofosbuvir/ledipasvir). When the concentration ratio was plotted against the intersection wavelength, a straight line was obtained with a coefficient of determination of 0.9992. The direct method was linear in the range 3 to 18 μg/mL while the wavelength-intersection ratio method was linear in the range 11-110 μg/mL. The limits of detection were determined and found to be 0.5 and 3 μg/mL for ledipasvir and sofosbuvir, respectively. The accuracy and repeatability of the two methods were tested. The mean %recovery was found to be 100.19% and 100.75% for ledipasvir and sofosbuvir, respectively. The relative standard deviation was 0.57 for ledipasvir and 1.79 for sofosbuvir. The intermediate precision was also checked, the coefficients of variation for sofosbuvir and ledipasvir measurements between days did not exceed 1.88%.

Liquid chromatographic and spectrophotometric methods for the determination of erythromycin stearate and trimethoprim in tablets

OpenAIRE

Hassib, Sonia T.; Farag, Awatef E.; Elkady, Ehab F.

2011-01-01

Simple, accurate and precise reversed-phase liquid chromatographic (LC) and spectrophotometric methods have been developed and validated for the determination of erythromycin stearate (ERS) and trimethoprim (TMP) in mixture. In LC method, chromatographic separation was achieved on a Symmetry® Waters C18 column (150 × 4.6 mm, 5 μm) based on isocratic elution using a mobile phase consisting of potassium dihydrogen phosphate buffer pH (9):acetonitrile:water (25:100:50, v/v/v) at a flow rate of 1...

New development of spectrophotometric analysis of thorium

International Nuclear Information System (INIS)

Yang Xiangzhen

1992-01-01

This review covers new development of spectrophotometric determination of thorium since 1980's. The methods include general spectrophotometry, double wavelength spectrophotometry, catalytic spectrophotometry, total differential spectrophotometry, derivative spectrophotometry and fluorescent spectrophotometry, etc

Spectrophotometric and Spectrofluorimetric Methods for the Determination of Dothiepin Hydrochloride in its Pure and Dosage Forms using Eosin

Science.gov (United States)

Walash, M. I.; Belal, F.; El-Enany, N.; Elmansi, H.

2010-01-01

Spectrophotometric and spectrofluorimetric methods were developed for the determination of dothiepin hydrochloride (DOP) in different dosage forms. The spectrophotometric method (Method I) is based on formation of a binary complex with eosin at 540 nm in acetate buffer of pH3.7. The absorbance-concentration plot is rectilinear over the range 1–10 μg/mL with LOD of 0.18 μg/mL and LOQ of 0.54 μg/mL. The spectroflurimetric method (Method II) is based on the quantitative quenching effect of Dothiepin on the native fluorescence of eosin at the same pH. The quenching of the fluorescence of eosin was measured at 543 nm after excitation at 304 nm. The fluorescence-concentration plot is rectilinear over the range 0.3–8 μg/ mL with LOD of 0.11 μg/mL and LOQ of 0.34 μg/mL. The proposed methods were successfully applied to the analysis of commercial tablets and capsules containing the drug. Statistical comparison of the results with those of the reference method revealed good agreement and proved that there were no significant differences in the accuracy and precision between the two methods respectively. PMID:23675210

Second derivative spectrophotometric determination of ...

African Journals Online (AJOL)

A new, simple, rapid, wide applicable range and reliable second derivative spectrophotometric method has been developed for determination of cyclophosphamide (CP) in bulk and pharmaceutical dosage forms. Calibration graph is linear in the concentration range of 25 - 200 μg/ml of CP with 10 μg/ml of detection limit and ...

Azeotropic mixture used for development and validation of Lornoxicam in bulk and its tablet dosage form by spectrophotometric method

Directory of Open Access Journals (Sweden)

Prajesh Prajapati

2012-08-01

Full Text Available A novel, safe, economic and sensitive method of spectrophotometric estimation has been developed using Azeoptropic mixture (water:methanol: 60:40, v/v for the quantitative determination of Lornoxicam, a practically water-insoluble drug. Hence, Lornoxicam stock solution was prepared in Azeoptropic mixture. Lornoxicam showed maximum absorbance at 383 nm. Beer's law was obeyed in the concentration range 4–24 μg/mL with regression coefficient of 0.999. The method was validated in terms of linearity (R2=0.999, precision (CV for intra-day and inter-day was 0.28–0.68 and 0.12–0.92, respectively, accuracy (98.03–100.59% w/w and specificity. This method is simple, precise, accurate, sensitive and reproducible and can be used for the routine quality control testing of the marketed formulations. Keywords: Analgesic, Chlortenoxicam, Lornoxicam, Oxicam, Spectrophotometric, Azeotropic mixture

Spectrophotometric Determination of Nitrate in Vegetables Using ...

African Journals Online (AJOL)

DR. MIKE HORSFALL

ABSTRACT: A rapid and sensitive spectrophotometric method for the determination of nitrate in vegetables is described. The method is based on the measurement of the absorbance of yellow sodium nitrophenoxide formed via the reaction of phenol with the vegetable-based nitrate in presence of sulphuric acid.

Spectrophotometric Determination of Trimipramine in Tablet Dosage ...

African Journals Online (AJOL)

Purpose: To develop and validate simple, rapid and sensitive spectrophotometric procedures for determination of trimipramine in tablet dosage form. Methods: The methods were based on the interaction of trimipramine as n-electron donor with the ο-acceptor, iodine and various π-acceptors, namely: chloranil (CH), ...

Determination of total antioxidant capacity by a new spectrophotometric method based on Ce(IV) reducing capacity measurement.

Science.gov (United States)

Ozyurt, Dilek; Demirata, Birsen; Apak, Resat

2007-02-28

Dietary antioxidants widely found in fruits and vegetables may serve the task of reducing oxidative damage in humans induced by free radicals and reactive oxygen species under 'oxidative stress' conditions. The aim of this work is to develop a simple, low-cost, sensitive, and diversely applicable indirect spectrophotometric method for the determination of total antioxidant capacity of several plants. The method is based on the oxidation of antioxidants with cerium(IV) sulfate in dilute sulfuric acid at room temperature. The Ce(IV) reducing capacity of the sample is measured under carefully adjusted conditions of oxidant concentration and pH such that only antioxidants and not other organic compounds would be oxidized. The spectrophotometric determination of the remaining Ce(IV) was performed after completion of reaction with antioxidants. Quercetin and gallic acid were used as standards for flavonoids and phenolic acids, respectively, and results of antioxidant measurements were reported as trolox equivalents. The developed procedure was successfully applied to the assay of total antioxidant capacity due to simple compounds such as trolox, quercetin, gallic acid, ascorbic acid, catechin, naringin, naringenin, caffeic acid, chlorogenic acid, ferulic acid, and p-coumaric acid, and due to phenolic acids and flavonoids in the arieal parts of nettle (Urtica Dioica L.). Blank correction of significantly absorbing plant extracts at 320nm could be made with the aid of spectrophotometric titration. Plant selection was made in respect to high antioxidant content, and extraction was made with water. The proposed method was reproducible, and the trolox equivalent antioxidant capacities (TEAC coefficients) of the tested antioxidant compounds were correlated to those found by reference methods such as ABTS and CUPRAC. Since the TEAC coefficients found with the proposed method of naringin-naringenin and rutin-catechin pairs were close to each other, this Ce(IV)-based assay

Determination of cyanide by a highly sensitive indirect spectrophotometric method.

Science.gov (United States)

Blanco, M; Maspoch, S

1984-01-01

Complexation of Pd(2+) with cyanide inhibits the extraction of the palladium complex of 5-phenylazo-8-aminoquinoline. This effect is used for the indirect spectrophotometric determination of cyanide at the mug level. Cyanide in industrial waste water and in sea-water is determined after distillation as HCN from the sample and collection in sodium hydroxide solution.

Determination of phenol in locally grown fruits and vegetable by spectrophotometric method

International Nuclear Information System (INIS)

Iqbal, M.; Khan, F.A.; Farooqui, Z.H.; Ifrahim, A.F.K.

2005-01-01

Spectrophotometric method for the determination of phenol in the sample of locally grown fruits apple, pear, sweet orange and vegetable radish of Quetta, Hyderabad and Nawabshah are described juices from these fruits and vegetable were squeezed, filtered and decolorized with charcoal. The antipyrine dye formed by reaction between phenol and 4-aminoantipyrine was analyzed. The calibration graphs were prepared in the range of 0.5 to 4 ppm of phenol. Phenol in apple, pear and sweet orange was found to be in the range of 1-1.2 ppm and in radish was found to be 0.5 ppm. Possible source of organic pollutant were pointed out and were discussed. Limits of detection of the method was investigated and was found to be 0.2 mu g/ml

Oxidation of L-cystine by chromium(VI) - a kinetic study | Kumar ...

African Journals Online (AJOL)

The kinetics of the title reaction was studied spectrophotometrically in HClO4 medium at 380 nm. The data suggested that the order with respect to cystine is fractional, whereas chromium(VI) follows first order kinetics. The reaction was second order in [H+]. Cysteic acid was found to be the main product of oxidation.

Development of a new spectrophotometric method to determine the total aromatic contents in kerosene

International Nuclear Information System (INIS)

Harfoush, A.; shlewit, H.

1996-12-01

This developed spectrophotometric method is helpful to determine and control the total aromatic contents in kerosene, during the treatment process of kerosene with conc. H sup 2 SO sup 4 and P sup 2 O sup 5 to remove aromatics, which have negative effect on the solvent extraction coefficient KD of uranium from the Syrian phosphoric acid, where kerosene is used as diluent. this method is rapid according to others, and simply, using the standard curve prepared by the separated aromatics from the Syrian kerosene, A =f (C) at 272 nm, we can calculate the aromatic contents in the known samples. (author). 24 Refs., 5 Figs

A study of selective spectrophotometric methods for simultaneous determination of Itopride hydrochloride and Rabeprazole sodium binary mixture: Resolving sever overlapping spectra

Science.gov (United States)

Mohamed, Heba M.

2015-02-01

Itopride hydrochloride (IT) and Rabeprazole sodium (RB) are co-formulated together for the treatment of gastro-esophageal reflux disease. Three simple, specific and accurate spectrophotometric methods were applied and validated for simultaneous determination of Itopride hydrochloride (IT) and Rabeprazole sodium (RB) namely; constant center (CC), ratio difference (RD) and mean centering of ratio spectra (MCR) spectrophotometric methods. Linear correlations were obtained in range of 10-110 μg/μL for Itopride hydrochloride and 4-44 μg/mL for Rabeprazole sodium. No preliminary separation steps were required prior the analysis of the two drugs using the proposed methods. Specificity was investigated by analyzing the synthetic mixtures containing the two cited drugs and their capsules dosage form. The obtained results were statistically compared with those obtained by the reported method, no significant difference was obtained with respect to accuracy and precision. The three methods were validated in accordance with ICH guidelines and can be used for quality control laboratories for IT and RB.

Spectrophotometric estimation of ethamsylate and mefenamic acid from a binary mixture by dual wavelength and simultaneous equation methods

OpenAIRE

Goyal Anju; Singhvi I

2008-01-01

Two simple, accurate, economical and reproducible spectrophotometric methods for simultaneous estimation of two-component drug mixture of ethamsylate and mefenamic acid in combined tablet dosage form have been developed. The first developed method involves formation and solving of simultaneous equation using 287.6 nm and 313.2 nm as two wavelengths. Second developed method is based on two wavelength calculation. Two wavelengths selected for estimation of ethamsylate were 274.4 nm and 301.2 nm...

Kinetic equation solution by inverse kinetic method

International Nuclear Information System (INIS)

Salas, G.

1983-01-01

We propose a computer program (CAMU) which permits to solve the inverse kinetic equation. The CAMU code is written in HPL language for a HP 982 A microcomputer with a peripheral interface HP 9876 A ''thermal graphic printer''. The CAMU code solves the inverse kinetic equation by taking as data entry the output of the ionization chambers and integrating the equation with the help of the Simpson method. With this program we calculate the evolution of the reactivity in time for a given disturbance

Development and Validation of a UV Spectrophotometric and a RP-HPLC Methods for Moexipril Hydrochloride in Pure Form and Pharmaceutical Dosage Form

International Nuclear Information System (INIS)

Mastiholimath, V.S.; Gupte, P.P.; Mannur, V.S.

2012-01-01

A simple and reliable UV spectrophotometric and high-performance liquid chromatography (HPLC) methods were developed and validated for Moexipril hydrochloride in pure form and pharmaceutical dosage form. The RP-HPLC method was developed on agilant eclipse C 18 , (150 mm x 4.6 mm, 5 μm) with a mobile phase gradient system of 60 % (methanol:acetonitrile (70:30 % v/v)) : 40 % 20 mM ammonium acetate buffer pH 4.5 (v/v) and UV spectrophotometric method was developed in phosphate buffer pH 6.8. The effluent was monitored by SPD-M20A, prominence PDA detector at 210 nm. Calibration curve was linear over the concentration range of 10-35 μg/ml and 1-9 μg/ml for RP-HPLC and UV with a regression coefficient of 0.999. For RP-HPLC method Inter-day and intra-day precision % RSD values were found to be 1.00078 % and 1.49408 % respectively. For UV method 0.73386 % to 1.44111 % for inter day 0.453864 to 1.15542 intra-day precision. Recovery of Moexipril hydrochloride was found to be in the range of 99.8538 % to 101.5614 % and 100.5297586 % to 100.6431587 % for UV and RP-HPLC respectively. The limits of detection (LOD) and quantification (LOQ) for HPLC were 0.98969 and 2.99907 μg/ml, respectively. The developed RP-HPLC and UV spectrophotometric method was successfully applied for the quantitative determination of Moexipril hydrochloride in pharmaceutical dosage. (author)

Spectrophotometric Determination of Cilostazol in Tablet Dosage Form

African Journals Online (AJOL)

Purpose: To develop simple, rapid and selective spectrophotometric methods for the determination of cilostazol in tablet dosage form. Methods: Cilostazol was dissolved in 50 % methanol and its absorbance was scanned by ultraviolet (UV) spectrophotometry. Both linear regression equation and standard absorptivity were ...

Titrimetric and Spectrophotometric Determination of Metaprolol tartrate in Pharmaceuticals Using N-Bromosuccinimide

OpenAIRE

K. Basavaiah; B. C. Somashekar

2007-01-01

One titrimetric and two spectrophotometric methods are presented for the assay of metaprolol tartrate (MPT) in bulk drug and in tablets. The methods employ N-bromosuccinimide (NBS) as the oxidimetric reagent and two dyes, methyl orange and indigo carmine as spectrophotometric reagents. In titrimetry, an acidified solution of MPT is treated with a known excess amount of NBS and after a definite time, the unreacted oxidant is determined by iodometric back titration. Spectrophotometry involve...

Derivative spectrophotometric method for simultaneous determination of clindamycin phosphate and tretinoin in pharmaceutical dosage forms.

Science.gov (United States)

Barazandeh Tehrani, Maliheh; Namadchian, Melika; Fadaye Vatan, Sedigheh; Souri, Effat

2013-04-10

A derivative spectrophotometric method was proposed for the simultaneous determination of clindamycin and tretinoin in pharmaceutical dosage forms. The measurement was achieved using the first and second derivative signals of clindamycin at (1D) 251 nm and (2D) 239 nm and tretinoin at (1D) 364 nm and (2D) 387 nm.The proposed method showed excellent linearity at both first and second derivative order in the range of 60-1200 and 1.25-25 μg/ml for clindamycin phosphate and tretinoin respectively. The within-day and between-day precision and accuracy was in acceptable range (CVpharmaceutical dosage form.

Spectrophotometric determination of proteins associated with ...

African Journals Online (AJOL)

Twenty six Aeromonas isolates from fishes, poultry and humans in Zaria were quantified for total soluble proteins (enzymes) profiles in January, 2007 by spectrophotometric (Biuret) method. Isolates were grown on Brain Heart Infusion (BHI) broth, they were incubated at 370C and centrifuged at 1,000 g/dl using harous ...

Salicylate-spectrophotometric determination of inorganic monochloramine

International Nuclear Information System (INIS)

Tao Hui; Chen Zhonglin; Li Xing; Yang Yanling; Li Guibai

2008-01-01

On the basis of classical Berthelot reaction, a simple salicylate-spectrophotometric method was developed for quantitative determination of inorganic monochloramine in water samples. With the catalysis of disodium pentacyanonitrosylferrate(III), inorganic monochloramine reacts with salicylate in equimolar to produce indophenol compound which has an intense absorption at 703 nm. Parameters that influence method performance, such as pH, dosage of salicylate and nitroprussiate and reaction time, were modified to enhance the method performance. By using this method, inorganic monochloramine can be distinguished from organic chloramines and other inorganic chlorine species, such as free chlorine, dichloramine, and trichloramine. The molar absorptivities of the final products formed by these compounds are below ±3% of inorganic monochloramine, because of the α-N in them have only one exchangeable hydrogen atom, and cannot react with salicylate to produce the indophenol compound. The upper concentrations of typical ions that do not interfere with the inorganic monochloramine determination are also tested to be much higher than that mostly encountered in actual water treatment. Case study demonstrates that the results obtained from this method are lower than DPD-titrimetric method because the organic chloramines formed by chlorination of organic nitrogenous compounds give no response in the newly established method. And the result measured by salicylate-spectrophotometric method is coincident with theoretical calculation

Validated Spectrophotometric Methods for Simultaneous Determination of Food Colorants and Sweeteners

Directory of Open Access Journals (Sweden)

Fatma Turak

2013-01-01

Full Text Available Two simple spectrophotometric methods have been proposed for simultaneous determination of two colorants (Indigotin and Brilliant Blue and two sweeteners (Acesulfame-K and Aspartame in synthetic mixtures and chewing gums without any prior separation or purification. The first method, derivative spectrophotometry (ZCDS, is based on recording the first derivative curves (for Indigotin, Brillant Blue, and Acesulfame-K and third-derivative curve (for Aspartame and determining each component using the zero-crossing technique. The other method, ratio derivative spectrophotometry (RDS, depends on application ratio spectra of first- and third-derivative spectrophotometry to resolve the interference due to spectral overlapping. Both colorants and sweeteners showed good linearity, with regression coefficients of 0.9992–0.9999. The LOD and LOQ values ranged from 0.05 to 0.33 μgmL−1 and from 0.06 to 0.47 μgmL−1, respectively. The intraday and interday precision tests produced good RSD% values (<0.81%; recoveries ranged from 99.78% to 100.67% for all two methods. The accuracy and precision of the methods have been determined, and the methods have been validated by analyzing synthetic mixtures containing colorants and sweeteners. Two methods were applied for the above combination, and satisfactory results were obtained. The results obtained by applying the ZCDS method were statistically compared with those obtained by the RDS method.

Spectrophotometric and Refractometric Determination of Total Protein in Avian Plasma

Directory of Open Access Journals (Sweden)

Rodica Căpriță

2013-10-01

Full Text Available The aim of this study was to compare the total protein values obtained in heparin plasma of chickens by a spectrophotometric technique (biuret method, and the values obtained on the same day in the same samples by refractometry. The results obtained by refractometry (average value 2.638±0.153g% were higher than those obtained by the spectrophotometric method (average value 2.441±0.181g%. There was a low correlation (r = 0.6709 between the total protein values, determined with both methods. Protein is the major determinant of plasma refractive index, but glucose contributes too. The refractometric method is not recommended in chickens for the determination of total protein, because avian blood glucose concentration averages about twice than in mammalian blood.

Flow injection methods for the determination of a-tocopherol with spectrophotometric detection

International Nuclear Information System (INIS)

Rishi, L.; Waseem, A.; Yaqoob, M.; Nabi, A.; Jadoon, S.

2011-01-01

The present paper describes flow injection procedures for a-tocopherol determination in pharmaceuticals and infant milk powder based on spectrophotometric detection. These two procedures are based on the reduction of iron(III) to iron(II) and of Mo(Vi) to Mo(V) by a-tocopherol and subsequent formation of iron(II)-o-phenanthroline, and phospho molybdenum complexes which were monitored at 510 and 695 nm respectively. Calibration graphs were linear over the concentration range of 0.21-43 mu g/mL for iron(III) and 0.25-10 mu g/mL for Mo(Vi) reduction methods respectively. The limits of detection (3s) of 0.05 and 0.1 mu g/mL with sample throughput of 30 and 50/h respectively were obtained. The relative standard deviations of 1.2- 3.8% (n = 4) was achieved in the concentration range studied. The developed methods were applied to pharmaceuticals and infant milk powders and the results obtained were compared with official method and no significant difference between these methods was observed at 95% confidence level. (author)

Innovative spectrophotometric methods for simultaneous estimation of the novel two-drug combination: Sacubitril/Valsartan through two manipulation approaches and a comparative statistical study

Science.gov (United States)

Eissa, Maya S.; Abou Al Alamein, Amal M.

2018-03-01

Different innovative spectrophotometric methods were introduced for the first time for simultaneous quantification of sacubitril/valsartan in their binary mixture and in their combined dosage form without prior separation through two manipulation approaches. These approaches were developed and based either on two wavelength selection in zero-order absorption spectra namely; dual wavelength method (DWL) at 226 nm and 275 nm for valsartan, induced dual wavelength method (IDW) at 226 nm and 254 nm for sacubitril and advanced absorbance subtraction (AAS) based on their iso-absorptive point at 246 nm (λiso) and 261 nm (sacubitril shows equal absorbance values at the two selected wavelengths) or on ratio spectra using their normalized spectra namely; ratio difference spectrophotometric method (RD) at 225 nm and 264 nm for both of them in their ratio spectra, first derivative of ratio spectra (DR1) at 232 nm for valsartan and 239 nm for sacubitril and mean centering of ratio spectra (MCR) at 260 nm for both of them. Both sacubitril and valsartan showed linearity upon application of these methods in the range of 2.5-25.0 μg/mL. The developed spectrophotmetric methods were successfully applied to the analysis of their combined tablet dosage form ENTRESTO™. The adopted spectrophotometric methods were also validated according to ICH guidelines. The results obtained from the proposed methods were statistically compared to a reported HPLC method using Student t-test, F-test and a comparative study was also developed with one-way ANOVA, showing no statistical difference in accordance to precision and accuracy.

[Spectrophotometric and HPLC evaluation of ceftazidime stability].

Science.gov (United States)

Palade, B; Cioroiu, B; Lazăr, Doina; Corciovă, Andreia; Lazăr, M I

2010-01-01

In this paper we followed up the stability of ceftazidime, raw material used in drug industry. Matherials and methods: We used three spectrophotometric methods based on ceftazidime property to form complexes with p-chloranilic acid (ac. p-CA), 3-methylbenzothiazolin-2-on hydrazone (MBTH) and N-(1-naphtil) etilendiamine (NEDA) and a chromatographic method (HPLC). Our results revealed that the substances analyzed maintained minimum content allowable.

Using Spectrophotometric Titrations To Characterize Humic Acid Reactivity at Environmental Concentrations

International Nuclear Information System (INIS)

Janot, N.; Benedetti, M. F.; Janot, N.; Reiller, P. E.; Korshin, G. V.

2010-01-01

Potentiometric titration is a common method to characterize dissolved organic matter (DOM) reactivity. Because of the sensitivity of pH electrodes, it is necessary to work with very high DOM (≥1 g/L) concentrations that are unrealistic compared to those found in natural waters (0. 1 to 100 mg/L). To obtain proton binding data for concentrations closer to environmental values, spectroscopic titration methodology is a viable alternative to traditional potentiometric titrations. Spectrophotometric titrations and UV visible spectra of a diluted solution of purified Aldrich humic acid (5 mg(DOC)/L) are used to estimate changes in proton binding moieties as function of pH and ionic strength after calculation of differential absorbance spectra variations. After electrostatic correction of spectrophotometric data, there is a linear operational correlation between spectrophotometric and potentiometric data which can be used as a transfer function between the two properties. Spectrophotometric titrations are then used to determine the changes of humic acid protonation after adsorption onto alpha-alumina. (authors)

Using Spectrophotometric Titrations To Characterize Humic Acid Reactivity at Environmental Concentrations

Energy Technology Data Exchange (ETDEWEB)

Janot, N.; Benedetti, M. F. [Univ Paris Diderot, Lab Geochim Eaux, UMR CNRS 7154, IPGP, F-75025 Paris 13 (France); Janot, N.; Reiller, P. E. [CE Saclay, CEA DEN DANS DPC SECR, Lab Speciat Radionucleides and Mol, F-91191 Gif Sur Yvette (France); Korshin, G. V. [Univ Washington, Dept Civil and Environm Engn, Seattle, WA 98195 (United States)

2010-07-01

Potentiometric titration is a common method to characterize dissolved organic matter (DOM) reactivity. Because of the sensitivity of pH electrodes, it is necessary to work with very high DOM ({>=}1 g/L) concentrations that are unrealistic compared to those found in natural waters (0. 1 to 100 mg/L). To obtain proton binding data for concentrations closer to environmental values, spectroscopic titration methodology is a viable alternative to traditional potentiometric titrations. Spectrophotometric titrations and UV visible spectra of a diluted solution of purified Aldrich humic acid (5 mg(DOC)/L) are used to estimate changes in proton binding moieties as function of pH and ionic strength after calculation of differential absorbance spectra variations. After electrostatic correction of spectrophotometric data, there is a linear operational correlation between spectrophotometric and potentiometric data which can be used as a transfer function between the two properties. Spectrophotometric titrations are then used to determine the changes of humic acid protonation after adsorption onto alpha-alumina. (authors)

Kinetic Evaluation of Naphthalene Removal using Acid - Modified ...

African Journals Online (AJOL)

Kinetic evaluation of naphthalene onto acid – modified and unmodified bentonite clay mineral was investigated by means of the effects of concentration, contact time and pH. The amount of naphthalene adsorbed was determined spectrophotometrically. The optimum pH value and equilibrium contact time for the adsorption ...

Spectrophotometric determination of pizotefin maleate in pure form ...

African Journals Online (AJOL)

Two simple, quick and sensitive methods were described for the spectrophotometric determination of pizotefin maleate (PZT) either in pure form or pharmaceutical form (tablets). The methods were based on the reaction of pizotefin maleate as 'n' electron donor with chloranilic acid (p-CLA) and 7,7,8 ...

Analytical method development and validation of spectrofluorimetric and spectrophotometric determination of some antimicrobial drugs in their pharmaceuticals

Science.gov (United States)

Ibrahim, F.; Wahba, M. E. K.; Magdy, G.

2018-01-01

In this study, three novel, sensitive, simple and validated spectrophotometric and spectrofluorimetric methods have been proposed for estimation of some important antimicrobial drugs. The first two methods have been proposed for estimation of two important third-generation cephalosporin antibiotics namely, cefixime and cefdinir. Both methods were based on condensation of the primary amino group of the studied drugs with acetyl acetone and formaldehyde in acidic medium. The resulting products were measured by spectrophotometric (Method I) and spectrofluorimetric (Method II) tools. Regarding method I, the absorbance was measured at 315 nm and 403 nm with linearity ranges of 5.0-140.0 and 10.0-100.0 μg/mL for cefixime and cefdinir, respectively. Meanwhile in method II, the produced fluorophore was measured at λem 488 nm or 491 nm after excitation at λex 410 nm with linearity ranges of 0.20-10.0 and 0.20-36.0 μg/mL for cefixime and cefdinir, respectively. On the other hand, method III was devoted to estimate nifuroxazide spectrofluorimetrically depending on formation of highly fluorescent product upon reduction of the studied drug with Zinc powder in acidic medium. Measurement of the fluorescent product was carried out at λem 335 nm following excitation at λex 255 nm with linearity range of 0.05 to 1.6 μg/mL. The developed methods were subjected to detailed validation procedure, moreover they were used for the estimation of the concerned drugs in their pharmaceuticals. It was found that there is a good agreement between the obtained results and those obtained by the reported methods.

Spectrophotometric and Voltammetric Studies on the Interaction of ...

African Journals Online (AJOL)

0.84V(vs. SCE) also changed correspondingly without change of the peak potential, which also indicated that the binding reaction had taken place. Under the selected conditions a new spectrophotometric analytical method was established for ...

Application of spectrophotometric, densitometric, and HPLC techniques as stability indicating methods for determination of Zaleplon in pharmaceutical preparations

Science.gov (United States)

Metwally, Fadia H.; Abdelkawy, M.; Abdelwahab, Nada S.

2007-12-01

Spectrophotometric, spectrodensitometric and HPLC are stability indicating methods described for determination of Zaleplon in pure and dosage forms. As Zaleplon is easily degradable, the proposed techniques in this manuscript are adopted for its determination in presence of its alkaline degradation product, namely N-[4-(3-cyano-pyrazolo[1,5a]pyridin-7-yl)-phenyl]- N-ethyl-acetamide. These approaches are successfully applied to quantify Zaleplon using the information included in the absorption spectra of appropriate solutions. The second derivative (D 2) spectrophotometric method, allows determination of Zaleplon without interference of its degradate at 235.2 nm using 0.01N HCl as a solvent with obedience to Beer's law over a concentration range of 1-10 μg ml -1 with mean percentage recovery 100.24 ± 0.86%. The first derivative of the ratio spectra ( 1DD) based on the simultaneous use of ( 1DD) and measurement at 241.8 nm using the same solvent and over the same concentration range as (D 2) spectrophotometric method, with mean percentage recovery 99.9 ± 1.07%. The spectrodensitometric analysis allows the separation and quantitation of Zaleplon from its degradate on silica gel plates using chloroform:acetone:ammonia solution (9:1:0.2 by volume) as a mobile phase. This method depends on quantitave densitometric evaluation of thin layer chromatogram of Zaleplon at 338 nm over a concentration range of 0.2-1 μg band -1, with mean percentage recovery 99.73 ± 1.35. Also a reversed-phase liquid chromatographic method using 5-C8 (22 cm × 4.6 mm i.d. 5 μm particle size) column was described and validated for quantitation of Zaleplon using acetonitrile:deionised water (35:65, v/v) as a mobile phase using Paracetamol as internal standard and a flow rate of 1.5 ml min -1 with UV detection of the effluent at 232 nm at ambient temperature over a concentration range of 2-20 μg ml -1 with mean percentage recovery 100.19 ± 1.15%. The insignificance difference of the proposed

Spectrophotometric and chromatographic determination of insensitive energetic materials: HNS and NTO, in the presence of sensitive nitro-explosives.

Science.gov (United States)

Can, Ziya; Uzer, Ayşem; Tekdemir, Yasemin; Erçağ, Erol; Türker, Lemi; Apak, Reşat

2012-02-15

As there are no molecular spectroscopic determination methods for the most widely used insensitive energetic materials, 2,2',4,4',6,6'-hexanitrostilbene (HNS) and 3-nitro-1,2,4-triazole-5-one (NTO), in the presence of sensitive nitro-explosives, two novel spectrophotometric methods were developed. For HNS and TNT mixtures, both analytes react with dicyclohexylamine (DCHA) forming different colored charge-transfer complexes, which can be resolved by derivative spectroscopy. The spectrophotometric method for NTO measures the 416-nm absorbance of its yellow-colored Na(+)NTO(-) salt formed with NaOH. TNT, if present, is pre-extracted into IBMK as its Meisenheimer anion forming an ion-pair with the cationic surfactant cetyl pyridinium (CP(+)) in alkaline medium, whereas the unextracted NTO is determined in the aqueous phase. The molar absorptivity (ε, L mol(-1)cm(-1)) and limit of quantification (LOQ, mg L(-1)) are as follows: for HNS, ε=2.75 × 10(4) and LOQ=0.48 (in admixture with TNT); for NTO, ε=6.83 × 10(3) and LOQ=0.73. These methods were not affected from nitramines and nitrate esters in synthetic mixtures or composite explosives. The developed methods were statistically validated against HPLC, and the existing chromatographic method was modified so as to enable NTO determination in the presence of TNT. These simple, low-cost, and versatile methods can be used in criminology, remediation/monitoring of contaminated sites, and kinetic stability modeling of munitions containing desensitized energetic materials. Copyright © 2012 Elsevier B.V. All rights reserved.

Novel Spectrophotometric Method for the Determination of Pindolol in Pharmaceutical Samples

Science.gov (United States)

Nagaraja, P.; Kumar, H. R. Arun; Bhaskara, B. L.; Kumar, S. Anil

2011-10-01

A new facile and sensitive spectrophotometric determination of Pindolol (PDL), a beta blocker drug has been developed and validated. The method was based on the reaction between pindolol and K3 [Fe(CN)6] in presence of FeCl3 to form Prussian blue. The absorbance values were recorded at 700 nm and a calibrated graph was constructed. A dynamic Beer's law range was observed in the range 0.125-2.5 μg mL-1 with a detection limit of 0.03 μg mL-1 and a quantitation limit of 0.08 μg mL-1. Various experimental parameters such as effect of solvents, stability, interference effects due to excipients etc were studied. The reproducibility of this methods were checked by six replicate determinations at 1.0 μg ml-1 PDL and the standard deviation was found to be between 0.20 and 0.42%. The results were statistically compared with those of the reference/literature method by applying Student's t-test and F-test. The sensitivity, simplicity, temperature independence and stability of the colored product are the advantages of the proposed method and it is also free from extraction steps and use of carcinogenic solvents.

Development and Validation of UV-Visible Spectrophotometric Methods for Simultaneous Estimation of Thiocolchicoside and Dexketoprofen in Bulk and Tablet Dosage Form

OpenAIRE

M. T. Harde; S. B. Jadhav; D. L. Dharam; P. D. Chaudhari

2012-01-01

Development and validation of two simple, accurate, precise and economical UV Spectrophotometric methods for simultaneous estimation of Thiocolchicoside and Dexketoprofen in bulk and in tablet dosage form. The methods employed were Method-1 Absorbance correction method and Method-2 First order derivative spectroscopic method. In method-1 Absorbance is measured at two wavelengths 370nm at which Dexketoprofen has no absorbance and 255nm at which both the drug have considerable absorbance. In me...

A Method Based on Ultrasound-assisted Solidification of Floating Drop Microextraction Technique for the Spectrophotometric Determination of Curcumin in Turmeric Powder

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Abbas Afkhami

2017-06-01

Full Text Available A method based on the ultrasound-assisted solidification of floating drop microextraction technique was developed for the spectrophotometric and spectrofluorimetric determination of curcumin in turmeric powder. In this work a small volume of an organic solvent was floated on the surface of an aqueous solution. After sonication the organic solvent is solidified and separated. The effect of extraction parameters such as type and the volume of organic solvent, temperature, salt addition and exposure time, on the extraction recovery was investigated and optimized. Finally, the method droplet was used for the determination of analyte. Under the optimum extraction conditions, a linear range of 0.006–30 μg mL-1 and a relative standard deviation (RSD of 2.72% for curcumin wasachieved. Limits of detection of 7 and 2 ng mL-1 curcumin was obtained for the spectrophotometric and spectrofluometric methods, respectively. The obtained results show that the application of this method can be successful for the analysis of curcumin in turmeric powder samples.

Stability indicating spectrophotometric and spectrodensitometric methods for the determination of diatrizoate sodium in presence of its degradation product

Science.gov (United States)

Abd El-Rahman, Mohamed K.; Riad, Safaa M.; Abdel Gawad, Sherif A.; Fawaz, Esraa M.; Shehata, Mostafa A.

2015-02-01

Three sensitive, selective, and precise stability indicating methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA), in the presence of its acidic degradation product (highly cytotoxic 3,5 diamino metabolite) and in pharmaceutical formulation were developed and validated. The first method is a first derivative (D1) spectrophotometric one, which allows the determination of DTA in the presence of its degradate at 231.2 nm (corresponding to zero crossing of the degradate) over a concentration range of 2-24 μg/mL with mean percentage recovery 99.95 ± 0.97%. The second method is the first derivative of the ratio spectra (DD1) by measuring the peak amplitude at 227 nm over the same concentration range as D1 spectrophotometric method, with mean percentage recovery 99.99 ± 1.15%. The third method is a TLC-densitometric one, where DTA was separated from its degradate on silica gel plates using chloroform:methanol:ammonium hydroxide (20:10:2 by volume) as a developing system. This method depends on quantitative densitometric evaluation of thin layer chromatogram of DTA at 238 nm over a concentration range of 4-20 μg/spot, with mean percentage recovery 99.88 ± 0.89%. The selectivity of the proposed methods was tested using laboratory-prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed.

A New Spectrophotometric Method for Determination of Selenium in Cosmetic and Pharmaceutical Preparations after Preconcentration with Cloud Point Extraction

Directory of Open Access Journals (Sweden)

Mohammad Hosein Soruraddin

2011-01-01

Full Text Available A simple, rapid, and sensitive spectrophotometric method for the determination of trace amounts of selenium (IV was described. In this method, all selenium spices reduced to selenium (IV using 6 M HCl. Cloud point extraction was applied as a preconcentration method for spectrophotometric determination of selenium (IV in aqueous solution. The proposed method is based on the complexation of Selenium (IV with dithizone at pH < 1 in micellar medium (Triton X-100. After complexation with dithizone, the analyte was quantitatively extracted to the surfactant-rich phase by centrifugation and diluted to 5 mL with methanol. Since the absorption maxima of the complex (424 nm and dithizone (434 nm overlap, hence, the corrected absorbance, Acorr, was used to overcome the problem. With regard to the preconcentration, the tested parameters were the pH of the extraction, the concentration of the surfactant, the concentration of dithizone, and equilibration temperature and time. The detection limit is 4.4 ng mL-1; the relative standard deviation for six replicate measurements is 2.18% for 50 ng mL-1 of selenium. The procedure was applied successfully to the determination of selenium in two kinds of pharmaceutical samples.

A spectrophotometric method for the determination of Hydrogen Sulphide sugar cane juice and water

International Nuclear Information System (INIS)

Mahadeviah, S.; Galil, Mansour S.; Kumar, M.S. Yogender; Suresha, M.S.; Nagendrappa, G.

2006-01-01

A sensitive spectrophotometric is developed for the determination of hydrogen sulphide in water and sugarcane juice. The method is based on the reaction of hydrogen sulphide with phospomolybdate (ammonium molybdate and phosphate) in sulphuric acid medium. The system obeys Lambert-Beer's law at 715 nm in the concentration range of 0.284-5.68 ug ml. Molar absorptivity, correlation coefficient and Sandell sensitivity values were found to be 5x10 l mol cm, 0.9995 and 0.0494 ug cm respectively. The method was employed for the determination of hydrogen sulphide in sugar cane juice and in water samples. The results obtained were reproducible with acceptable standard deviation 0.1140-0.1337 and relative standard deviation varies from 0.0797-0.6038%. For comparison, hydrogen sulphide present in sugarcane juice and water samples were also determined separately following the methylene blue official method. The results of the proposed method compare well with the official method. (author)

Extraction-spectrophotometric method for silicon determination in high-purity substances. 2. Silicon determination in cadmium

Energy Technology Data Exchange (ETDEWEB)

Yudelevich, I G; Shaburova, V P; Shamrina, L V [AN SSSR, Novosibirsk (USSR). Inst. Neorganicheskoj Khimii

1989-01-01

Cadmium extraction by tributyl phosphate and trialkylbenzylammonium chloride (TABAC) depending on acid (HCl, HI), extracting agent concentration, volume of aqueous and organic phases, number of extraction steps is investigated. On the basis of the obtained results the spectrophotometric method for silicon determination in cadmium and CdCl/sub 2/ using malachite green with preliminary extraction of the base by the TABAC from HCl solutions. The method detection limit is 3.9x10/sup -4/ % Si with respect to initial cadmium sample of 100 mg and 7.8x10/sup -5/ % with respect to 0.5 g of CdCl/sub 2/. The relative standard deviation is S/sub r/-0.07-0.13.

Application and validation of superior spectrophotometric methods for simultaneous determination of ternary mixture used for hypertension management

Science.gov (United States)

Mohamed, Heba M.; Lamie, Nesrine T.

2016-02-01

Telmisartan (TL), Hydrochlorothiazide (HZ) and Amlodipine besylate (AM) are co-formulated together for hypertension management. Three smart, specific and precise spectrophotometric methods were applied and validated for simultaneous determination of the three cited drugs. Method A is the ratio isoabsorptive point and ratio difference in subtracted spectra (RIDSS) which is based on dividing the ternary mixture of the studied drugs by the spectrum of AM to get the division spectrum, from which concentration of AM can be obtained by measuring the amplitude values in the plateau region at 360 nm. Then the amplitude value of the plateau region was subtracted from the division spectrum and HZ concentration was obtained by measuring the difference in amplitude values at 278.5 and 306 nm (corresponding to zero difference of TL) while the total concentration of HZ and TL in the mixture was measured at their isoabsorptive point in the division spectrum at 278.5 nm (Aiso). TL concentration is then obtained by subtraction. Method B; double divisor ratio spectra derivative spectrophotometry (RS-DS) and method C; mean centering of ratio spectra (MCR) spectrophotometric methods. The proposed methods did not require any initial separation steps prior the analysis of the three drugs. A comparative study was done between the three methods regarding their; simplicity, sensitivity and limitations. Specificity was investigated by analyzing the synthetic mixtures containing different ratios of the three studied drugs and their tablets dosage form. Statistical comparison of the obtained results with those found by the official methods was done, differences were non-significant in regard to accuracy and precision. The three methods were validated in accordance with ICH guidelines and can be used for quality control laboratories for TL, HZ and AM.

Development and application of spectrophotometric method for the determination of cefaclor in pharmaceutical formulations

Directory of Open Access Journals (Sweden)

Asad Raza

2009-01-01

Full Text Available A simple, fast and sensitive spectrophotometric method for the determination of cefaclor in pharmaceutical raw and dosage forms based on reaction with ninhydrin is developed, optimized and validated. The purple color (Ruhemenn's purple that resulted from the reaction was stabilized and measured at 560 nm. Beer's law is obeyed in the concentration range of 4-80 µg mL-1 with molar absorptivity of 1.42 × 10(5 L mole-1 cm-1. All variables including the reagent concentration, heating time, reaction temperature, color stability period, and cefaclor/ninhydrin ratio were studied in order to optimize the reaction conditions. No interference was observed from common pharmaceutical adjuvant. The developed method is easy to use, accurate and highly cost-effective for routine studies relative to HPLC and other techniques.

Spectrophotometric titration of zirconium in siliceous materials

International Nuclear Information System (INIS)

Sugawara, K.F.; Su, Y.-S.; Strzegowski, W.R.

1978-01-01

An accurate and selective complexometric titration procedure based upon a spectrophotometrically detected end-point has been developed for the determination of zirconium in glasses, glass-ceramics and refractories. A p-bromomandelic acid separation step for zirconium imparts excellent selectivity to the procedure. The method is particularly important for the 1 to 5% concentration range where a simple, accurate and selective method for the determination of zirconium has been lacking. (author)

Validated UV-spectrophotometric method for the evaluation of the efficacy of makeup remover.

Science.gov (United States)

Charoennit, P; Lourith, N

2012-04-01

A UV-spectrophotometric method for the analysis of makeup remover was developed and validated according to ICH guidelines. Three makeup removers for which the main ingredients consisted of vegetable oil (A), mineral oil and silicone (B) and mineral oil and water (C) were sampled in this study. Ethanol was the optimal solvent because it did not interfere with the maximum absorbance of the liquid foundation at 250 nm. The linearity was determined over a range of makeup concentrations from 0.540 to 1.412 mg mL⁻¹ (R² = 0.9977). The accuracy of this method was determined by analysing low, intermediate and high concentrations of the liquid foundation and gave 78.59-91.57% recoveries with a relative standard deviation of makeup remover efficacy. © 2011 The Authors. ICS © 2011 Society of Cosmetic Scientists and the Société Française de Cosmétologie.

A nanosilver-based spectrophotometric method for determination of malachite green in surface water samples.

Science.gov (United States)

Sahraei, R; Farmany, A; Mortazavi, S S; Noorizadeh, H

2013-07-01

A new spectrophotometric method is reported for the determination of nanomolar level of malachite green in surface water samples. The method is based on the catalytic effect of silver nanoparticles on the oxidation of malachite green by hexacyanoferrate (III) in acetate-acetic acid medium. The absorbance is measured at 610 nm with the fixed-time method. Under the optimum conditions, the linear range was 8.0 × 10(-9)-2.0 × 10(-7) mol L(-1) malachite green with a correlation coefficient of 0.996. The limit of detection (S/N = 3) was 2.0 × 10(-9) mol L(-1). Relative standard deviation for ten replicate determinations of 1.0 × 10(-8) mol L(-1) malachite green was 1.86%. The method is featured with good accuracy and reproducibility for malachite green determination in surface water samples without any pre-concentration and separation step.

Spectrophotometric and spectrofluorimetric methods for the determination of saxagliptin and vildagliptin in bulk and pharmaceutical preparations

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Marwa S. Moneeb

2013-12-01

Full Text Available New simple and sensitive spectrophotometric and spectrofluorimetric methods have been developed and validated for the determination of saxagliptin (SAX and vildagliptin (VDG in bulk and pharmaceutical preparations. The spectrophotometric methods were based on derivatization of the investigated drugs with two reagents: 1,2-naphthoquinone-4-sulfonic acid sodium salt (NQS and 4-chloro-7-nitrobenzofurazan (NBD-Cl. For further increase in the sensitivity, the D1 spectra of the reactions products were also recorded. For NQS reaction, Beer’s law was obeyed over the ranges of 5–30 and 7–45 μg mL−1 for the absorbance readings; and 3–32 and 5–50 μg mL−1 for the derivative readings of SAX and VDG, respectively. For NBD-Cl reaction, Beer’s law was obeyed over the ranges of 3–20 and 4.5–35 μg mL−1 for the absorbance readings; and 1.5–25 and 2.5–40 μg mL−1 for the derivative readings of SAX and VDG, respectively. Spectrofluorimetric methods were developed based on the fact that the derivatized investigated drugs with NBD-Cl reagent are highly fluorescent products. The fluorescence concentration plots were linear over the ranges of 0.02–0.25 and 0.03–0.37 μg mL−1 for SAX and VDG, respectively. The fluorescence measurement enabled the detection of SAX and VDG at concentrations of about 3 and 7 ng mL−1, respectively. The proposed methods have been validated and successfully applied to the determination of the investigated drugs in their pharmaceutical preparations. The results obtained were statistically compared to those obtained from reference methods.

Determination of cyanide by an indirect spectrophotometric method using 5-Br-PADAP.

Science.gov (United States)

Fu-Sheng, W; Yu-Qin, L; Fang, Y; Nai-Kui, S

1981-09-01

Complexation of Ni(2+) with cyanide inhibits its colour reaction with 5-Br-PADAP and this reaction is used in the spectrophotometric determination of cyanide at the ug level. Cyanide in industrial waste waters is determined after an initial transfer as hydrogen cyanide from the sample into sodium hydroxide solution with a stream of air.

Development and Validation of New Spectrophotometric Methods to Determine Enrofloxacin in Pharmaceuticals

Science.gov (United States)

Rajendraprasad, N.; Basavaiah, K.

2015-07-01

Four spectrophotometric methods, based on oxidation with cerium(IV), are investigated and developed to determine EFX in pure form and in dosage forms. The frst and second methods (Method A and method B) are direct, in which after the oxidation of EFX with cerium(IV) in acid medium, the absorbance of reduced and unreacted oxidant is measured at 275 and 320 nm, respectively. In the third (C) and fourth (D) methods after the reaction between EFX and oxidant is ensured to be completed the surplus oxidant is treated with either N-phenylanthranilic acid (NPA) or Alizarin Red S (ARS) dye and the absorbance of the oxidized NPA or ARS is measured at 440 or 420 nm. The methods showed good linearity over the concentration ranges of 0.5-5.0, 1.25-12.5, 10.0-100.0, and 6.0-60.0 μg/ml, for method A, B, C and D, respectively, with apparent molar absorptivity values of 4.42 × 10 4 , 8.7 × 10 3 , 9.31 × 10 2 , and 2.28 × 10 3 l/(mol· cm). The limits of detection (LOD), quantification (LOQ), and Sandell's sensitivity values and other validation results have also been reported. The proposed methods are successfully applied to determine EFX in pure form and in dosage forms.

Performance Evaluation of Monolith Based Immobilized Acetylcholinesterase Flow-Through Reactor for Copper(II Determination with Spectrophotometric Detection

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Parawee Rattanakit

2014-01-01

Full Text Available A monolith based immobilized acetylcholinesterase (AChE flow-through reactor has been developed for the determination of copper(II using flow injection spectrophotometric system. The bioreactor was prepared inside a microcapillary column by in situ polymerization of butyl methacrylate, ethylene dimethacrylate, and 2,2-dimethoxy-1,2-diphynyletane-1-one in the presence of 1-decanol, followed by vinyl azlactone functionalization and AChE immobilization. The behavior of AChE before and after being immobilized on the monolith was evaluated by kinetic parameters from Lineweaver and Burk equation. The detection was based on measuring inhibition effect on the enzymatic activity of AChE by copper(II using Ellman’s reaction with spectrophotometric detection at 410 nm. The linear range of the calibration graph was obtained over the range of 0.02–3.00 mg L−1. The detection limit, defined as 10% inhibition (I10, was found to be 0.04 mg L−1. The repeatability was 3.35 % (n=5 for 1.00 mg L−1 of copper(II. The proposed method was applied to the determination of copper(II in natural water samples with sampling rate of 4 h−1.

Thorium coprecipitation method for spectrophotometric determination of arsenic (III) and arsenic (V) in groundwaters

International Nuclear Information System (INIS)

Tamari, Yuzo; Yamamoto, Nobuki; Tsuji, Haruo; Kusaka, Yuzuru

1989-01-01

A new coprecipitation method for the spectrophotometry of arsenic (III) and arsenic (V) in groundwater has been developed. Arsenic (III) and arsenic (V) were coprecipitated with thorium (IV) hydroxide from 1000ml of groundwater at pH9. The precipitate was centrifuged and then dissolved with hydrochloric acid. Arsenic (III) was spectrophotometrically determined by the usual silver diethylditiocarbamate (Ag-DDTC) method after generating the arsenic to arsine with sodium tetrahydroborate under masking the thorium with EDTA-NaF at pH6. From another portion of the same groundwater, both arsenic (III) and arsenic (V) were determined by the Ag-DDTC method after reducing all the arsenic to arsine with sodium tetrahydroborate at pH less than 1 in the presence of the EDTA-NaF. The concentration of arsenic (V) was obtained by subtracting that of arsenic (III) from the total for arsenic. (author)

TITRIMETRIC AND SENSITIVE SPECTRO-PHOTOMETRIC METHODS FOR THE ASSAY OF QUETIAPINE FUMARATE IN PHARMACEUTICAL FORMULATIONS

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Nagaraju Rajendraprasad

2011-03-01

Full Text Available Quetiapine fumarate (QTF is a selective monoaminergic antagonist with high affinity for the serotonin Type 2 (5HT2, and dopamine type 2 (D2 receptors. Titrimetric and spectrophotometric assay of quetiapine fumarate (QTF using perchloric acid and acetic acid as reagents are described. The first method (method A is a non-aqueous titrimetric method and is based on the titration of QTF in glacial acetic acid with 0.01 M acetous perchloric acid using crystal violet as indicator. In the second method (method B, QTF has been measured in 0.1M acetic acid spectrophotometrically at a wavelength of 222 nm. The titri¬metric method was applicable over the range of 2.0–20.0 mg of QTF. The reac¬tion stoichiometry of 1:3 is obtained which served as the basis for calculation. In spectrophotometry, Beer’s law was obeyed over the concentration range of 1.25–15.0 µg mL-1. The linear regression equation of the calibration graph was A = 0.0115 + 0.0673c with a regression coefficient (r of 0.9986 (n = 7. The apparent molar absorptivity was calculated to be 4.25104 L mol-1cm-1 and the Sandell sensitivity was 0.0145 µg cm-2. The limits of detection (LOD and quantification (LOQ calculated as per the ICH guidelines were 0.07 and 0.21 µg mL-1, respectively. Accuracy and precision of the assays were determined by computing the intra-day and inter-day variations at three different levels of QTF. The intra-day and inter-day relative standard deviation (%RSD were in the range of 0.99–2.88 and 1.65–2.32%, for method A and B, respectively, with an acceptable percentage relative error (%RE < 2%. The methods were successfully applied to the determination of QTF in two different brands of tablets with good accuracy and precision and without detectable interference by excipients. The methods have demonstrated to be simple and easy to apply in routine usage and do not need any costly instrumentation. Therefore, the proposed procedures are advantageous and can be

Microwave assisted spectrophotometric method for the determination of copper using leucocrystal violet

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Sunitha B. Mathew

2007-04-01

Full Text Available A sensitive spectrophotometric method has been developed for the trace determination of copper using leucocrystal violet as chromogenic reagent. The proposed method is based on the reaction of copper(II with potassium iodide in acid medium to liberate iodine, which oxidizes leucocrystal violet to crystal violet dye having absorption maximum at 590 nm. The reaction between copper and potassium iodide is accelerated by irradiating the mixture with microwave energy for 15 s at 480 W. Beer’s law is obeyed in the concentration range 0.004 – 0.04 μg mL-1. The molar absorptivity, Sandell’s sensitivity, detection limit and quantitation limit were found to be 1.47 x 106 L mol-1 cm-1, 4.3 x 10-5 μg mL-2, 0.001 μg mL-1, 0.0043 μg mL-1, respectively. The optimum conditions and other analytical parameters were evaluated. The effect of interfering ions on the determination is described. The proposed method has been successfully applied for the determination of copper in environmental samples like tap water, agricultural run off water, plant materials and pharmaceutical samples.

Simultaneous determination of a binary mixture of pantoprazole sodium and itopride hydrochloride by four spectrophotometric methods

Science.gov (United States)

Ramadan, Nesrin K.; El-Ragehy, Nariman A.; Ragab, Mona T.; El-Zeany, Badr A.

2015-02-01

Four simple, sensitive, accurate and precise spectrophotometric methods were developed for the simultaneous determination of a binary mixture containing Pantoprazole Sodium Sesquihydrate (PAN) and Itopride Hydrochloride (ITH). Method (A) is the derivative ratio method (1DD), method (B) is the mean centering of ratio spectra method (MCR), method (C) is the ratio difference method (RD) and method (D) is the isoabsorptive point coupled with third derivative method (3D). Linear correlation was obtained in range 8-44 μg/mL for PAN by the four proposed methods, 8-40 μg/mL for ITH by methods A, B and C and 10-40 μg/mL for ITH by method D. The suggested methods were validated according to ICH guidelines. The obtained results were statistically compared with those obtained by the official and a reported method for PAN and ITH, respectively, showing no significant difference with respect to accuracy and precision.

Development and Validation of UV Spectrophotometric Method For Estimation of Dolutegravir Sodium in Tablet Dosage Form

International Nuclear Information System (INIS)

Balasaheb, B.G.

2015-01-01

A simple, rapid, precise and accurate spectrophotometric method has been developed for quantitative analysis of Dolutegravir sodium in tablet formulations. The initial stock solution of Dolutegravir sodium was prepared in methanol solvent and subsequent dilution was done in water. The standard solution of Dolutegravir sodium in water showed maximum absorption at wavelength 259.80 nm. The drug obeyed Beer-Lamberts law in the concentration range of 5-40 μg/ mL with coefficient of correlation (R"2) was 0.9992. The method was validated as per the ICH guidelines. The developed method can be adopted in routine analysis of Dolutegravir sodium in bulk or tablet dosage form and it involves relatively low cost solvents and no complex extraction techniques. (author)

Pregabalin and Tranexamic Acid Evaluation by Two Simple and Sensitive Spectrophotometric Methods

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Nawab Sher

2015-01-01

Full Text Available This paper demonstrates colorimetric visible spectrophotometric quantification methods for amino acid, namely, tranexamic acid and pregabalin. Both drugs contain the amino group, and when they are reacted with 2,4-dinitrophenol and 2,4,6-trinitrophenol, they give rise to yellow colored complexes showing absorption maximum at 418 nm and 425 nm, respectively, based on the Lewis acid base reaction. Detailed optimization process and stoichiometric studies were conducted along with investigation of thermodynamic features, that is, association constant and standard free energy changes. The method was linear over the concentration range of 0.02–200 µgmL−1 with correlation coefficient of more than 0.9990 in all of the cases. Limit of detection was in range from 0.0041 to 0.0094 µgmL−1 and limit of quantification was in the range from 0.0137 to 0.0302 µgmL−1. Excellent recovery in Placebo spiked samples indicated that there is no interference from common excipients. The analytical methods under proposal were successfully applied to determine tranexamic acid and pregabalin in commercial products. t-test and F ratio were evaluated without noticeable difference between the proposed and reference methods.

Spectrophotometric Method for the Determination of Two Coformulated Drugs with Highly Different Concentrations. Application on Vildagliptin and Metformin Hydrochloride

Science.gov (United States)

Zaazaa, H. E.; Elzanfaly, E. S.; Soudi, A. T.; Salem, M. Y.

2016-03-01

A new smart simple validated spectrophotometric method was developed for the determination of two drugs one of which is in a very low concentration compared to the other. The method is based on spiking and dilution then simple mathematical manipulation of the absorbance spectra. This method was applied for the determination of a binary mixture of vildagliptin and metformin hydrochloride in the ratio 50:850 in laboratory prepared mixtures containing both drugs in this ratio and in pharmaceutical dosage form with good recoveries. The developed method was validated according to ICH guidelines and can be used for routine quality control testing.

Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies

International Nuclear Information System (INIS)

Luca, Michele De; Ragno, Gaetano; Ioele, Giuseppina; Tauler, Romà

2014-01-01

Highlights: • A new MCR-ALS algorithm is proposed for the analysis of incomplete fused multiset. • Resolution of the data allowed the description of amiloride kinetic photodegradation. • The new MCR-ALS algorithm can be easily applied to other drugs and chemicals. - Abstract: An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid–base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described

Multivariate curve resolution of incomplete fused multiset data from chromatographic and spectrophotometric analyses for drug photostability studies

Energy Technology Data Exchange (ETDEWEB)

Luca, Michele De, E-mail: michele.deluca@unical.it [Department of Pharmacy, Health and Nutritional Sciences, University of Calabria, Via P. Bucci, Rende, CS 87036 (Italy); Ragno, Gaetano; Ioele, Giuseppina [Department of Pharmacy, Health and Nutritional Sciences, University of Calabria, Via P. Bucci, Rende, CS 87036 (Italy); Tauler, Romà [Department of Environmental Chemistry, IDAEA-CSIC, C/Jordi Girona, 18-26, Barcelona 08034 (Spain)

2014-07-21

Highlights: • A new MCR-ALS algorithm is proposed for the analysis of incomplete fused multiset. • Resolution of the data allowed the description of amiloride kinetic photodegradation. • The new MCR-ALS algorithm can be easily applied to other drugs and chemicals. - Abstract: An advanced and powerful chemometric approach is proposed for the analysis of incomplete multiset data obtained by fusion of hyphenated liquid chromatographic DAD/MS data with UV spectrophotometric data from acid–base titration and kinetic degradation experiments. Column- and row-wise augmented data blocks were combined and simultaneously processed by means of a new version of the multivariate curve resolution-alternating least squares (MCR-ALS) technique, including the simultaneous analysis of incomplete multiset data from different instrumental techniques. The proposed procedure was applied to the detailed study of the kinetic photodegradation process of the amiloride (AML) drug. All chemical species involved in the degradation and equilibrium reactions were resolved and the pH dependent kinetic pathway described.

Three different spectrophotometric methods manipulating ratio spectra for determination of binary mixture of Amlodipine and Atorvastatin

Science.gov (United States)

Darwish, Hany W.; Hassan, Said A.; Salem, Maissa Y.; El-Zeiny, Badr A.

2011-12-01

Three simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra are developed for the simultaneous determination of Amlodipine besylate (AM) and Atorvastatin calcium (AT) in tablet dosage forms. The first method is first derivative of the ratio spectra ( 1DD), the second is ratio subtraction and the third is the method of mean centering of ratio spectra. The calibration curve is linear over the concentration range of 3-40 and 8-32 μg/ml for AM and AT, respectively. These methods are tested by analyzing synthetic mixtures of the above drugs and they are applied to commercial pharmaceutical preparation of the subjected drugs. Standard deviation is <1.5 in the assay of raw materials and tablets. Methods are validated as per ICH guidelines and accuracy, precision, repeatability and robustness are found to be within the acceptable limit.

Investigation of a New Spectrophotometric Method for the analysis of carbohydrates using glucose as model

International Nuclear Information System (INIS)

Hussain, Z.; Ali, A.; Shah, N.U.; Khan, K.M.

2013-01-01

Carbohydrates are biomolecule of significant importance. Its analysis is of prime importance in the clinical investigations, delivery of medicines and quality control operations of food and fuel products. Based on its importance a novel spectrophotometric method was investigated for the trace analysis of carbohydrates using glucose as model carbohydrate. This method is based on glucosazation followed by oxidation of the glucosazone with acidified iron (III) chloride. Oxidation of the glucsazone is necessary for enhancing the color intensity and optimum conditions were investigated for the process. All the absorbance measurements were carried out using 390 nm as gamma max. The ratio of the reactants was 1: 1.5: 0.1 mole for the glucose, phenyl hydrazine and iron (III) chloride. This method was used for the analysis of carbohydrates in real samples from plants, industrial products, blood and urine using glucose as reference. (author)

Validated spectrophotometric methods for simultaneous determination of troxerutin and carbazochrome in dosage form

Science.gov (United States)

Khattab, Fatma I.; Ramadan, Nesrin K.; Hegazy, Maha A.; Al-Ghobashy, Medhat A.; Ghoniem, Nermine S.

2015-03-01

Four simple, accurate, sensitive and precise spectrophotometric methods were developed and validated for simultaneous determination of Troxerutin (TXN) and Carbazochrome (CZM) in their bulk powders, laboratory prepared mixtures and pharmaceutical dosage forms. Method A is first derivative spectrophotometry (D1) where TXN and CZM were determined at 294 and 483.5 nm, respectively. Method B is first derivative of ratio spectra (DD1) where the peak amplitude at 248 for TXN and 439 nm for CZM were used for their determination. Method C is ratio subtraction (RS); in which TXN was determined at its λmax (352 nm) in the presence of CZM which was determined by D1 at 483.5 nm. While, method D is mean centering of the ratio spectra (MCR) in which the mean centered values at 300 nm and 340.0 nm were used for the two drugs in a respective order. The two compounds were simultaneously determined in the concentration ranges of 5.00-50.00 μg mL-1 and 0.5-10.0 μg mL-1 for TXN and CZM, respectively. The methods were validated according to the ICH guidelines and the results were statistically compared to the manufacturer's method.

Highly sensitive spectrophotometric kinetic determination of vanadium by catalysis of the gallic acid-bromate reaction

International Nuclear Information System (INIS)

Fukasawa, Tsutomu; Kawakubo, Susumu; Yamanouchi, Tatsuo

1985-01-01

Conditions are described for improving the speed and sensitivity of this catalytic determination of vanadium. The reaction of 0.018 M gallic acid with 0.96 M sodium bromate at pH 3.8 and double-beam spectrophotometric measurement at 380 nm are recommended. The highest practical sensitivity at 22-30 0 C was ca. 40 pg for an absorbance change of 0.0005, 50 times better than previously. The detection limit was ca. 0.5 ng of vanadium. Reaction at 50 0 C gave even better sensitivity. (Auth.)

Determination of U and Impurities Elements in The Uranium Tetra Fluoride by Potentiometric and Atomic Absorption Spectrophotometric Methods

International Nuclear Information System (INIS)

Putro Kasino, P

1998-01-01

The determination of u and impurities contents in the Uranium tetra fluoride (UF 4 )has been carried out by potentiometric titration using modified 'Davies-Gray' and atomic absorption spectrophotometric methods. Dissolution process of the powder sample using saturated Al 2 (SO 4 ) 3 solution introduced to determine UF 4 compound content in the UF 4 sample. The uranium Content in the obtained filtrate is analyzed by potentiometric. The impurities content is determined by ato-Mic absorption spectrophotometric using ammonium oxalate powder in introducing of the sample preparation. The experiment covered the observation on influence of stirring time of UF 4 sample dissolution in respect to separate UF 4 from its impurities in determination of uranium content. Also the effects of Ammonium Oxalate added and agitating time were observed deal with the sample preparation for the determination of Impurities content.The analysis result found that UF 4 content was 96.15 ± 0.04% the relative station 0.7%. However the best impurities determination was achieved by addition of ammonium oxalate powder and 15 Minutes of agitation time at temperature of 800 0 C

Spectrophotometric estimation of ethamsylate and mefenamic Acid from a binary mixture by dual wavelength and simultaneous equation methods.

Science.gov (United States)

Goyal, Anju; Singhvi, I

2008-01-01

Two simple, accurate, economical and reproducible spectrophotometric methods for simultaneous estimation of two-component drug mixture of ethamsylate and mefenamic acid in combined tablet dosage form have been developed. The first developed method involves formation and solving of simultaneous equation using 287.6 nm and 313.2 nm as two wavelengths. Second developed method is based on two wavelength calculation. Two wavelengths selected for estimation of ethamsylate were 274.4 nm and 301.2 nm while that for mefenamic acid were 304.8 nm and 320.4 nm. Both the developed methods obey Beer's law in the concentration ranges employed for the respective methods. The results of analysis were validated statistically and by recovery studies.

Spectrophotometric method for quantitative determination of triclabendazole in bulk and pharmaceutical

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Alankar Shrivastava

2011-01-01

Full Text Available Background: Triclabendazole (TCBZ, 6-chloro-5(2-3 dichlorophenoxy-2-methyl thio-benzimidazole, an halogenated benzimidazole (BZD thiol derivative, shows high efficacy against both the immature and mature stages of Fasciola hepatica in sheep and cattle, which is a differential feature compared to other available trematodicidal drugs. As a consequence of its excellent activity against the liver fluke, it has been extensively used and this has inevitably promoted the selection of TCBZ-resistant populations, which is now a worrying problem in several areas of the world. We propose simple ultraviolet spectrophotometric method for the estimation of triclabendazole in 0.1 methanolic HCl for the estimation of the drug. Method was validated as per ICH guidelines. Materials and Methods: Spectral absorbance measurements were made on Shimadzu UV-1800 with 10 mm matched quartz cells and dilutions were made in 0.1 M methanolic HCl. Results: The LOD and LOQ of triclabendazole at 305 nm were found to be 0.068434 and 2.73×10-4 μg/ml respectively. The calibration was linear in the range of 1-10 μg/ml. Analytical parameters such as stability, selectivity, accuracy, and precision have been established for the method in Endex and Fasinex tablets and evaluated statistically to assess the application of the method. Conclusion: Method passes all parameters with in desirable limits and found to be simple, stable, sensitive, reproducible, and accurate for the routine analysis of the drug in pharmaceutical formulations and in pharmaceutical investigations involving triclabendazole.

Stopped-flow injection spectrophotometric method for determination of chlorate in soil

OpenAIRE

Jaroon Jakmunee

2008-01-01

A stopped-flow injection (FI) spectrophotometric procedure based on iodometric reaction for the determination of chlorate has been developed. Standard/sample was injected into a stream of potassium iodide solution and then merged with a stream of hydrochloric acid solution to produce triiodide. By stopping the flow while the sample zone is being in a mixing coil, a slow reaction of chlorate with iodide in acidic medium was promoted to proceed with minimal dispersion of the triiodide product z...

Spectrophotometric and theoretical studies on the determination of ...

African Journals Online (AJOL)

Purpose: To develop a simple and cost effective spectrophotometric method for the ... species exhibited absorption maxima at 410 and 479 nm for the two systems in ... etilefrine in plasma and urine in pharmacokinetic ... In this work, the interactions of ET with BCG and ... prepared where the total volume of investigated.

Validated spectrofluorimetric and spectrophotometric methods for the determination of brimonidine tartrate in ophthalmic solutions via derivatization with NBD-Cl. Application to stability study.

Science.gov (United States)

Ibrahim, F; El-Enany, N; El-Shaheny, R N; Mikhail, I E

2015-05-01

Two simple, selective and accurate methods were developed and validated for the determination of brimonidine tartrate (BT) in pure state and pharmaceutical formulations. Both methods are based on the coupling of the drug with 4-chloro-7-nitro-2,1,3-benzoxadiazole in borate buffer (pH 8.5) at 70 °C and measurement of the reaction product spectrophotometrically at 407 nm (method I) or spectrofluorimetrically at 528 nm upon excitation at 460 nm (method II). The calibration graphs were rectilinear over the concentration ranges of 1.0-16.0 and 0.1-4.0 µg/mL with lower detection limits of 0.21 and 0.03, and lower quantification limits of 0.65 and 0.09 µg/mL for methods I and II, respectively. Both methods were successfully applied to the analysis of commercial ophthalmic solution with mean recovery of 99.50 ± 1.00 and 100.13 ± 0.71%, respectively. Statistical analysis of the results obtained by the proposed methods revealed good agreement with those obtained using a comparison method. The proposed spectrofluorimetric method was extended to a stability study of BT under different ICH-outlined conditions such as alkaline, acidic, oxidative and photolytic degradation. Furthermore, the kinetics of oxidative degradation of the drug was investigated and the apparent first-order reaction rate constants, half-life times and Arrhenius equation were estimated. The proposed methods are practical and valuable for routine applications in quality control laboratories for the analysis of BT. Copyright © 2014 John Wiley & Sons, Ltd.

SPECTROPHOTOMETRIC, ATOMIC ABSORPTION AND CONDUCTOMETRIC ANALYSIS OF TRAMADOL HYDROCHLORIDE

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Sara M. Anis

2011-09-01

Full Text Available Six simple and sensitive spectroscopic and conductometric procedures (A-F were developed for the determination of tramadol hydrochloride. Methods A, B and C are based on the reaction of cobalt (II thiocyanate with tramadol to form a stable ternary complex, which could be measured by spectrophotometric (method A, atomic absorption (method B or conductometric (method C procedures. Methods D and E depend on the reaction of molybdenum thiocyanate with tramadol to form a stable ternary complex, measured by spectrophotometric means (method D or by atomic absorption procedures (method E, while method F depends on the formation of an ion pair complex between the studied drug and bromothymol blue which is extractable into methylene chloride. Tramadol hydrochloride could be assayed in the range of 80-560 and 40-–220 μg ml-1, 1-15 mg ml-1 and 2.5-22.5, 1.25-11.25 and 5-22 μg ml-1 using methods A,B,C,D,E and F, respectively. Various experimental conditions were studied. The results obtained showed good recoveries. The proposed procedures were applied successfully to the analysis of tramadol in its pharmaceutical preparations and the results were favorably comparable with the official method.

Sensitive spectrophotometric methods for determination of some organophosphorus pesticides in vegetable samples

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MAGDA A. AKL

2010-03-01

Full Text Available Three rapid, simple, reproducible and sensitive spectrophotometric methods (A, B and C are described for the determination of two organophosphorus pesticides, (malathion and dimethoate in formulations and vegetable samples. The methods A and B involve the addition of an excess of Ce4+ into sulphuric acid medium and the determination of the unreacted oxidant by decreasing the red color of chromotrope 2R (C2R at a suitable lmax = 528 nm for method A, or a decrease in the orange pink color of rhodamine 6G (Rh6G at a suitable lmax = = 525 nm. The method C is based on the oxidation of malathion or dimethoate with the slight excess of N-bromosuccinimide (NBS and the determination of unreacted oxidant by reacting it with amaranth dye (AM in hydrochloric acid medium at a suitable lmax = 520 nm. A regression analysis of Beer-Lambert plots showed a good correlation in the concentration range of 0.1-4.2 μg mL−1. The apparent molar absorptivity, Sandell sensitivity, the detection and quantification limits were calculated. For more accurate analysis, Ringbom optimum concentration ranges are 0.25-4.0 μg mL−1. The developed methods were successfully applied to the determination of malathion, and dimethoate in their formulations and environmental vegetable samples.

SHORT COMMUNICATION KINETIC SPECTROPHOTOMETRIC ...

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deviation of the method was from 1.34% to 1.78% for 11 replicate determinations. ... A sample solution was prepared by adding a suitable amount of the standard .... Under the optimum conditions, the effect of the amount of 0.2, 0.5, 0.6, 0.8,.

Extractive spectrophotometric determination of thorium

International Nuclear Information System (INIS)

Venkatesan, M.; Gopalakrishnan, V.; Ramanujam, A.; Nadkarni, M.N.

1981-01-01

An extractive spectrophotometric method has been standardized for the analysis of 0.2 to 1.6 milligrams of thorium present in nitric acid solutions. The method involves the extraction of thorium from nitric acid solutions into 0.5 M thenoyl trifluoro acetone (HTTA) in benzene and its direct estimation from the organic extract by spectrophotometry as Thoron colour complex. In this method, interference due to iron upto 5 milligrams can be suppressed by adding ascorbic acid in the ratio of 1:2 prior to HTTA extraction. Uranium(VI) does not interefere even when present in 2000 times the amount of thorium. Plutonium and cerium do not interfere at one milligram level whereas zirconium interferes in this method. The overall error variation and precision of this method has been determined to be +- 3.5%. (author)

Development and Statistical Validation of Spectrophotometric Methods for the Estimation of Nabumetone in Tablet Dosage Form

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A. R. Rote

2010-01-01

Full Text Available Three new simple, economic spectrophotometric methods were developed and validated for the estimation of nabumetone in bulk and tablet dosage form. First method includes determination of nabumetone at absorption maxima 330 nm, second method applied was area under curve for analysis of nabumetone in the wavelength range of 326-334 nm and third method was First order derivative spectra with scaling factor 4. Beer law obeyed in the concentration range of 10-30 μg/mL for all three methods. The correlation coefficients were found to be 0.9997, 0.9998 and 0.9998 by absorption maxima, area under curve and first order derivative spectra. Results of analysis were validated statistically and by performing recovery studies. The mean percent recoveries were found satisfactory for all three methods. The developed methods were also compared statistically using one way ANOVA. The proposed methods have been successfully applied for the estimation of nabumetone in bulk and pharmaceutical tablet dosage form.

New simple spectrophotometric assay of total carotenes in margarines

NARCIS (Netherlands)

Luterotti, S.; Bicanic, D.D.; Pozgaj, R.

2006-01-01

Direct and reliable spectrophotometric method for assaying total carotenes (TC) in margarines with the minimum of sample manipulation is proposed. For the first time saponification step used in determination of carotenes in margarines was omitted leading to a substantial cost saving and reduction of

Comparative study on the selectivity of various spectrophotometric techniques for the determination of binary mixture of fenbendazole and rafoxanide.

Science.gov (United States)

Saad, Ahmed S; Attia, Ali K; Alaraki, Manal S; Elzanfaly, Eman S

2015-11-05

Five different spectrophotometric methods were applied for simultaneous determination of fenbendazole and rafoxanide in their binary mixture; namely first derivative, derivative ratio, ratio difference, dual wavelength and H-point standard addition spectrophotometric methods. Different factors affecting each of the applied spectrophotometric methods were studied and the selectivity of the applied methods was compared. The applied methods were validated as per the ICH guidelines and good accuracy; specificity and precision were proven within the concentration range of 5-50 μg/mL for both drugs. Statistical analysis using one-way ANOVA proved no significant differences among the proposed methods for the determination of the two drugs. The proposed methods successfully determined both drugs in laboratory prepared and commercially available binary mixtures, and were found applicable for the routine analysis in quality control laboratories. Copyright © 2015 Elsevier B.V. All rights reserved.

Spectrophotometric activity microassay for pure and recombinant cytochrome P450-type nitric oxide reductase

CSIR Research Space (South Africa)

Garny, S

2014-02-01

Full Text Available spectrophotometric quantification of NADH [19]. Kaya et al. (2004) [19] demonstrated the linearly proportional relationship between the oxidation of NADH to NAD+, with the release of NO from NOC-5, but did not develop a kinetic assay for NOR activity using... this principle, the primary aim of this study. Nakahara et al. (1993) [10] determined the stoichiometry of NO reduction by NOR as 2:1:1 for NO:NADH:N2O. Therefore, for each NADH oxidized to NAD+, two molecules of NO are converted to N2O (refer Equation 1). 2...

Development of a Direct Spectrophotometric and Chemometric Method for Determining Food Dye Concentrations.

Science.gov (United States)

Arroz, Erin; Jordan, Michael; Dumancas, Gerard G

2017-07-01

An ultraviolet visible (UV-Vis) spectrophotometric and partial least squares (PLS) chemometric method was developed for the simultaneous determination of erythrosine B (red), Brilliant Blue, and tartrazine (yellow) dyes. A training set (n = 64) was generated using a full factorial design and its accuracy was tested in a test set (n = 13) using a Box-Behnken design. The test set garnered a root mean square error (RMSE) of 1.79 × 10 -7 for blue, 4.59 × 10 -7 for red, and 1.13 × 10 -6 for yellow dyes. The relatively small RMSE suggests only a small difference between predicted versus measured concentrations, demonstrating the accuracy of our model. The relative error of prediction (REP) for the test set were 11.73%, 19.52%, 19.38%, for blue, red, and yellow dyes, respectively. A comparable overlay between the actual candy samples and their replicated synthetic spectra were also obtained indicating the model as a potentially accurate method for determining concentrations of dyes in food samples.

Use of spectrophotometric readout method for free radical dosimetry in radiation processing including low energy electrons and bremsstrahlung

International Nuclear Information System (INIS)

Gupta, B.L.

2000-01-01

Our laboratory maintains standards for high doses in India. The glutamine powder dosimeter (spectrophotometric readout) is used for this purpose. Present studies show that 20 mg of unirradiated/irradiated glutamine dissolved in freshly prepared 10 ml of aerated aqueous acidic FX solution containing 2 x 10 -3 mol dm -3 ferrous ammonium sulphate and 10 -4 mol dm -3 xylenol orange in 0.033 mol dm -3 sulphuric acid is suitable for the dosimetry in the dose range of 0.1-100 kGy. Normally no corrections are required for the post-irradiation fading of the irradiated glutamine. The response of glutamine dosimeter is independent of irradiation temperature in the range of about 23-30 deg. C and at other temperatures, a correction is necessary. The dose intercomparison results for photon, electron and bremsstrahlung radiations show that glutamine can be used as a reference standard dosimeter. The use of flat polyethylene bags containing glutamine powder has proved very successful for electron dosimetry of wide energies. Several other amino acids like alanine, valine and threonine can also be used to cover wide range of doses using spectrophotometric readout method. (author)

The effect of the extraction techniques on the kinetics, yield and antioxidative activity of ethyl acetate extracts of Hieracium pilosella L.

OpenAIRE

Stanojević, Ljiljana P.; Stanković, Mihajlo Z.; Veljković, Vlada; Cakić, Milorad D.; Nikolić, Vesna D.; Ilić, Dušica P.

2011-01-01

The influence of three extraction techniques (Reflux maceration, Soxhlet and Tillepape extraction) on the kinetics, yield and antioxidant activity of ethyl acetate extracts of Hieracium pilosella L. was investigated. The antioxidant activity of the extracts on stable 1,1-diphenyl-2-picryl hydrazyl (DPPH) radical was determined spectrophotometrically. The total phenolic content was determined by using the Folin-Ciocalteu assay and the total flavonoids content was measured by spectrophotometric...

The Comparison Of Silicon Analysis For The Uranium Silicide Fuel Using Spectrophotometrical And Gravimetrical Methods

International Nuclear Information System (INIS)

Putro, P. K.; Suripto, A.; Putra, S.; Gunanjar

1996-01-01

The analysis of silicon content in the uranium silicide fuel spectro-photometrical and gravimetrical method have been performed. The nitrous oxide-acetylene was used in the atomic absorption spectrophotometry (AAS) on the wave length of 251.6 nm, and the mixture of ammonium hepta molybdate complexes and SnC1 2 as reductor were applied during analysis by UV-VIS spectrophotometry (UV-VIS) on the wave length of 757.5 mm. The reagent of HCLO 4 and HNO 3 were used for determining Si content by gravimetrical methods. The results of this comparison is as follows: the accuracy result is around 96.37 % + 0.24 % for the Si concentration up to 300 ppm (the AAS), is 138.60 % = 0.43 % for the Si concentration range between 0.1-1.5 ppm (UV-VIS), and is 51.13 % + 0.8 % for 1 gram of Si (gravimetry). The results also show that the lowest analytical error is obtained by AAS method

Different Spectrophotometric Methods for Simultaneous Determination of Trelagliptin and Its Acid Degradation Product

Science.gov (United States)

Hassan, Mostafa A.; Zaghary, Wafaa A.

2018-01-01

New spectrophotometric and chemometric methods were carried out for the simultaneous assay of trelagliptin (TRG) and its acid degradation product (TAD) and applied successfully as a stability indicating assay to recently approved Zafatek® tablets. TAD was monitored using TLC to ensure complete degradation. Furthermore, HPLC was used to confirm dealing with one major acid degradation product. The proposed methods were developed by manipulating zero-order, first-derivative, and ratio spectra of TRG and TAD using simultaneous equation, first-derivative, and mean-centering methods, respectively. Using Spectra Manager II and Minitab v.14 software, the absorbance at 274 nm–260.4 nm, amplitudes at 260.4 nm–274.0 nm, and mean-centered values at 287.6 nm–257.2 nm were measured against methanol as a blank for TRG and TAD, respectively. Linearity and the other validation parameters were acceptable at concentration ranges of 5–50 μg/mL and 2.5–25 μg/mL for TRG and TAD, respectively. Using one-way analysis of variance (ANOVA), the optimized methods were compared and proved to be accurate for the simultaneous assay of TRG and TAD. PMID:29629213

Spectrophotometric and Spectrofluorimetric Studies on Azilsartan Medoxomil and Chlorthalidone to be Utilized in Their Determination in Pharmaceuticals

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Walid M. Ebeid

2014-01-01

Full Text Available The recently approved angiotensin II receptor blocker, azilsartan medoxomil (AZL, was determined spectrophotometrically and spectrofluorimetrically in its combination with chlorthalidone (CLT in their combined dosage form. The UV-spectrophotometric technique depends on simultaneous measurement of the first derivative spectra for AZL and CLT at 286 and 257 nm, respectively, in methanol. The spectrofluorimetric technique depends on measurement of the fourth derivative of the synchronous spectra intensities of AZL in presence of CLT at 298 nm in methanol. The effects of different solvents on spectrophotometric and spectrofluorimetric responses were studied. For, the spectrofluorimetric study, the effect of pH and micelle-assisted fluorescence enhancement were also studied. Linearity, accuracy, and precision were found to be satisfactory over the concentration ranges of 8-50 μg mL −1 and 2-20 μg mL −1 for AZL and CLT, respectively, in the spectrophotometric method as well as 0.01-0.08 μg mL −1 for AZL in the spectrofluorimetric method. The methods were successfully applied for the determination of the studied drugs in their co-formulated tablets. The developed methods are inexpensive and simple for the quality control and routine analysis of the cited drugs in bulk and in pharmaceuticals.

Spectrophotometric Determination of Iron(II and Cobalt(II by Direct, Derivative, and Simultaneous Methods Using 2-Hydroxy-1-Naphthaldehyde-p-Hydroxybenzoichydrazone

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V. S. Anusuya Devi

2012-01-01

Full Text Available Optimized and validated spectrophotometric methods have been proposed for the determination of iron and cobalt individually and simultaneously. 2-hydroxy-1-naphthaldehyde-p-hydroxybenzoichydrazone (HNAHBH reacts with iron(II and cobalt(II to form reddish-brown and yellow-coloured [Fe(II-HNAHBH] and [Co(II-HNAHBH] complexes, respectively. The maximum absorbance of these complexes was found at 405 nm and 425 nm, respectively. For [Fe(II-HNAHBH], Beer’s law is obeyed over the concentration range of 0.055–1.373 μg mL−1 with a detection limit of 0.095 μg mL−1 and molar absorptivity ɛ, 5.6 × 104 L mol−1 cm−1. [Co(II-HNAHBH] complex obeys Beer’s law in 0.118–3.534 μg mL−1 range with a detection limit of 0.04 μg mL−1 and molar absorptivity, ɛ of 2.3 × 104 L mol−1 cm−1. Highly sensitive and selective first-, second- and third-order derivative methods are described for the determination of iron and cobalt. A simultaneous second-order derivative spectrophotometric method is proposed for the determination of these metals. All the proposed methods are successfully employed in the analysis of various biological, water, and alloy samples for the determination of iron and cobalt content.

A new method for determination of trace amount thorium-spectrophotometric determination of thorium in aqueous phase by chlorophosphonazo-mA

International Nuclear Information System (INIS)

Xia Yuanxian; Qian Hesheng

1986-01-01

In this paper the spectrophotometric method for determination of trace amount of thorium in weak acidic medium by chlorophosphonazo-mA is described. The composition of the complex was estimated to be 1:4 by slope ratio method. The apparent molar absorption of thorium at 675 nm is 9.2 x 10 4 . Beer's law is obeyed for 0-12.0 μg of thorium in 10 ml solution. The coefficient of variation for thorium is 0.88%. The method has been applied to the determination of trace amounts of thorium in the extraction process of thorium

Spectrophotometric determination of silica in water. Low range

International Nuclear Information System (INIS)

Acosta L, E.

1992-07-01

The spectrophotometric method for the determination of the silica element in water, demineralized water, raw waters, laundry waters, waters treated with ion exchange resins and sea waters is described. This method covers the determination of the silica element in the interval from 20 to 1000 μg/l on 50 ml. of base sample. These limits its can be variable if the size of the used aliquot one is changed for the final determination of the silica element. (Author)

Application of different spectrophotometric methods for simultaneous determination of elbasvir and grazoprevir in pharmaceutical preparation

Science.gov (United States)

Attia, Khalid A. M.; El-Abasawi, Nasr M.; El-Olemy, Ahmed; Abdelazim, Ahmed H.

2018-01-01

The first three UV spectrophotometric methods have been developed of simultaneous determination of two new FDA approved drugs namely; elbasvir and grazoprevir in their combined pharmaceutical dosage form. These methods include simultaneous equation, partial least squares with and without variable selection procedure (genetic algorithm). For simultaneous equation method, the absorbance values at 369 (λmax of elbasvir) and 253 nm (λmax of grazoprevir) have been selected for the formation of two simultaneous equations required for the mathematical processing and quantitative analysis of the studied drugs. Alternatively, the partial least squares with and without variable selection procedure (genetic algorithm) have been applied in the spectra analysis because the synchronous inclusion of many unreal wavelengths rather than by using a single or dual wavelength which greatly increases the precision and predictive ability of the methods. Successfully assay of the drugs in their pharmaceutical formulation has been done by the proposed methods. Statistically comparative analysis for the obtained results with the manufacturing methods has been performed. It is noteworthy to mention that there was no significant difference between the proposed methods and the manufacturing one with respect to the validation parameters.

Spectrophotometric determination of trace uranium in phosphate ore samples from kurum and uro areas, Nuba mountains, Sudan

International Nuclear Information System (INIS)

Mohamed, A. A.; Ali, A. H.; Altayeb, M. A. H.

2004-01-01

A method was proposed for the spectrophotometric determination of uranium content in phosphate ores. the method is based on the use of nitrogen (v) acid for leaching the rock, and treatment with ammonium carbonate solution, whereby uranium (Vi) is kept in solution as its carbonate complex. The ion-exchange technique was used for the recovery of uranium. Uranium was determined spectrophotometrically by measurement of the absorbance of the yellow uranium (Vi)-8-hydroxyquinolate complex at λ 425 nm. The procedure was used for the determination of trace uranium content in 30 phosphate ore samples collected from Kurun and Uro areas in Nuba mountains in Sudan. X-ray fluorescence technique was employed for the assessment of the method used. The spectrophotometric method results show a high similarity with those obtained by XRF technique. This agreement indicates that the procedure proposed here has been successfully applied for the determination of uranium in phosphate ores. (Author)

Spectrophotometric titrations: Application to the determination of some elements in uranium solutions

International Nuclear Information System (INIS)

L'Her, M.

1967-01-01

The aim of this work is the application of spectrophotometric titrations to the analysis of uranium-containing solutions. We have been led to examine the general principles involved in these titrations, and we give a brief outline of these principles. In the first part we deal therefore with spectrophotometric titrations from a general point of view, examining their fundamental principle, their practical execution as well as the various possibilities of the method. The advantage of the titration are examined, in particular that of lending itself simultaneous determination of two species. The possibility of applying these spectrophotometric titrations to the analysis of uranium-containing solutions is the subject of the second part of this report: the dosage of a few species in uranium (VI) solutions is described. To this second part is added an experimental appendix consisting of a description of the apparatus, as well as of the operational techniques used for certain titrations, in particular those involving solutions containing uranium. (author) [fr

Different spectrophotometric methods applied for the analysis of simeprevir in the presence of its oxidative degradation product: Acomparative study

Science.gov (United States)

Attia, Khalid A. M.; El-Abasawi, Nasr M.; El-Olemy, Ahmed; Serag, Ahmed

2018-02-01

Five simple spectrophotometric methods were developed for the determination of simeprevir in the presence of its oxidative degradation product namely, ratio difference, mean centering, derivative ratio using the Savitsky-Golay filters, second derivative and continuous wavelet transform. These methods are linear in the range of 2.5-40 μg/mL and validated according to the ICH guidelines. The obtained results of accuracy, repeatability and precision were found to be within the acceptable limits. The specificity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. Furthermore, these methods were statistically comparable to RP-HPLC method and good results were obtained. So, they can be used for the routine analysis of simeprevir in quality-control laboratories.

Kinetics and Mechanism of Paracetamol Oxidation by Chromium(VI in Absence and Presence of Manganese(II and Sodiumdodecyl Sulphate

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Maqsood Ahmad Malik

2007-11-01

Full Text Available The kinetics of paracetamol oxidation are first order each in [paracetamol] and [HClO4]. The kinetic study shows that the oxidation proceeds in two steps. The effects of anionic micelles of sodiumdodecyl sulphate (SDS and complexing agents (ethylenediammine tetraacetic acid (EDTA and 2,2′-bipyridyl (bpy were also studied. Fast kinetic spectrophotometric method has been described for the determination of paracetamol. The method is based on the catalytic effect of manganese(II on the oxidation of paracetamol by chromium(VI in the presence of HClO4 (= 0.23 mol dm−3. Optimum reaction time is 4 to 6 minutes at a temperature of 30∘C. The addition of manganese(II ions largely decreased the absorbance of chromium(VI at 350 nm. This reaction can be utilized for the determination of paracetamol in drugs.

A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations

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Shipra Singh

2012-01-01

Full Text Available The present study was undertaken to develop a validated, rapid, simple, and low-cost ultraviolet (UV spectrophotometric method for estimating Etoricoxib (ETX in pharmaceutical formulations. The analysis was performed on λ max 233 nm using 0.1 M HCl as blank/diluent. The proposed method was validated on International Conference on Harmonization (ICH guidelines including parameters as linearity, accuracy, precision, reproducibility, and specificity. The proposed method was also used to access the content of the ETX in two commercial brands of Indian market. Beer′s law was obeyed in concentration range of 0.1-0.5 μg/ml, and the regression equation was Y = 0.418x + 0.018. The mean accuracy values for 0.1 μg/ml and 0.2 μg/ml concentration of ETX were found to be 99.76 ± 0.52% and 99.12 ± 0.84, respectively, and relative standard deviation (RSD of interday and intraday was less than 2%. The developed method was suitable and specific to the analysis of ETX even in the presence of common excipients. The method was applied on two different marketed brands and ETX contents were 98.5 ± 0.56 and 99.33 ± 0.44, respectively, of labeled claim. The proposed method was validated as per ICH guidelines and statistically good results were obtained. This method can be employed for routine analysis of ETX in bulk and commercial formulations.

A simple Ultraviolet spectrophotometric method for the determination of etoricoxib in dosage formulations.

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S Singh

2012-01-01

Full Text Available The present study was undertaken to develop a validated, rapid, simple, and low-cost ultraviolet (UV spectrophotometric method for estimating Etoricoxib (ETX in pharmaceutical formulations. The analysis was performed on Î max 233 nm using 0.1 M HCl as blank/diluent. The proposed method was validated on International Conference on Harmonization (ICH guidelines including parameters as linearity, accuracy, precision, reproducibility, and specificity. The proposed method was also used to access the content of the ETX in two commercial brands of Indian market. Beer′s law was obeyed in concentration range of 0.1-0.5 μg/ml, and the regression equation was Y = 0.418x + 0.018. The mean accuracy values for 0.1 μg/ml and 0.2 μg/ml concentration of ETX were found to be 99.76 ± 0.52% and 99.12 ± 0.84, respectively, and relative standard deviation (RSD of interday and intraday was less than 2%. The developed method was suitable and specific to the analysis of ETX even in the presence of common excipients. The method was applied on two different marketed brands and ETX contents were 98.5 ± 0.56 and 99.33 ± 0.44, respectively, of labeled claim. The proposed method was validated as per ICH guidelines and statistically good results were obtained. This method can be employed for routine analysis of ETX in bulk and commercial formulations.

Spectrophotometric determination of dopaminergic drugs used for Parkinson's disease, cabergoline and ropinirole, in pharmaceutical preparations.

Science.gov (United States)

Onal, Armağan; Cağlar, Sena

2007-04-01

Simple and reproducible spectrophotometric methods have been developed for determination of dopaminergic drugs used for Parkinson's disease, cabergoline (CAB) and ropinirole hydrochloride (ROP), in pharmaceutical preparations. The methods are based on the reactions between the studied drug substances and ion-pair agents [methyl orange (MO), bromocresol green (BCG) and bromophenol blue (BPB)] producing yellow colored ion-pair complexes in acidic buffers, after extracting in dichloromethane, which are spectrophotometrically determined at the appropriate wavelength of ion-pair complexes. Beer's law was obeyed within the concentration range from 1.0 to 35 microg ml(-1). The developed methods were applied successfully for the determination of these drugs in tablets.

Novel and validated titrimetric method for determination of selected angiotensin-II-receptor antagonists in pharmaceutical preparations and its comparison with UV spectrophotometric determination

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Shrikant H. Patil

2012-12-01

Full Text Available A novel and simple titrimetric method for determination of commonly used angiotensin-II-receptor antagonists (ARA-IIs is developed and validated. The direct acid base titration of four ARA-IIs, namely eprosartan mesylate, irbesartan, telmisartan and valsartan, was carried out in the mixture of ethanol:water (1:1 as solvent using standardized sodium hydroxide aqueous solution as titrant, either visually using phenolphthalein as an indicator or potentiometrically using combined pH electrode. The method was found to be accurate and precise, having relative standard deviation of less than 2% for all ARA-IIs studied. Also, it was shown that the method could be successfully applied to the assay of commercial pharmaceuticals containing the above-mentioned ARA-IIs. The validity of the method was tested by the recovery studies of standard addition to pharmaceuticals and the results were found to be satisfactory. Results obtained by this method were found to be in good agreement with those obtained by UV spectrophotometric method. For UV spectrophotometric analysis ethanol was used as a solvent and wavelength of 233 nm, 246 nm, 296 nm, and 250 nm was selected for determination of eprosartan mesylate, irbesartan, telmisartan, and valsartan respectively. The proposed titrimetric method is simple, rapid, convenient and sufficiently precise for quality control purposes. Keywords: Angiotensin-II-receptor antagonists, Titrimetric assay, UV spectrophotometry, Validation

Spectrophotometric determination of procainamide hydrochloride using sodium periodate

OpenAIRE

Al-Tamrah, S.; Al-Abbad, S.

2015-01-01

A simple spectrophotometric method has been described for the determination of procainamide hydrochloride. The method is based on the oxidation of procainamide hydrochloride by sodium periodate in the presence of sulfuric acid and measurement of the absorbance of the violet color formed at 531 nm. Parameters affecting the reaction were studied and conditions were optimized. Linear calibration graph was obtained from 50 to 700 μg ml−1 of procainamide hydrochloride and the limit of detection wa...

Spectrophotometric analysis of irradiated spices

Energy Technology Data Exchange (ETDEWEB)

Josimovic, L; Cudina, I

1987-01-01

Seven different spices (thyme, cinnamon, coriander, caraway, pimento, paprika, black pepper) were treated by gamma radiation at an absorbed dose of 10 kGy, and the effect on chemical quality was determined. The effects of this dose were assessed by spectrophotometric analysis of some water-soluble constituents of spices (carbohydrates; carbonyl compounds) and on the content of water-insoluble steam-volatile oils. The colour of paprika and the content of piperine in pepper held in different packaging materials were measured in unirradiated and irradiated samples as a function of storage time. In all cases irradiation does not bring about any distinct qualitative or quantitative chemical changes based on spectrophotometric analysis of spice extracts.

Kinetic Spectrophotometric Method for the 1,4-Diionic Organophosphorus Formation in the Presence of Meldrum′s Acid: Stopped-Flow Approach

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Fatemeh Ghodsi

2016-11-01

Full Text Available The kinetics of the reaction between triphenylphosphine (TPP and dimethyl acetylenedicarboxylate (DMAD in the presence of Meldrum’s acid (MA for the generation of the 1,4-diionic organophosphorus compound has been investigated using the stopped-flow and UV-VIS spectrophotometry techniques. The first step of the reaction between TPP and DMAD for the generation of (I1 in ethanol was followed by the stopped-flow apparatus. This step was recognized as a fast step. The reaction between the intermediate (I1 and MA showed first-order kinetics, and it was followed by the UV-VIS spectrophotometry technique. The activation parameters for the slow step of the proposed mechanism were determined using two linearized forms of the Eyring equation. From the temperature, concentration and solvent studies, the activation energy (Ea = 20.16 kJ·mol−1 and the related activation parameters (ΔG‡ = 71.17 ± 0.015 kJ·mol−1, ΔS‡ = −185.49 ± 0.026 J·mol−1 and ΔH‡ =17.72 ± 0.007 kJ·mol−1 were calculated. The experimental data indicated that the reaction was zero-order in MA and second-order overall. The proposed mechanism was confirmed with the observed kinetic data obtained from the UV-VIS and stopped-flow techniques.

A discontinuous Galerkin method on kinetic flocking models

OpenAIRE

Tan, Changhui

2014-01-01

We study kinetic representations of flocking models. They arise from agent-based models for self-organized dynamics, such as Cucker-Smale and Motsch-Tadmor models. We prove flocking behavior for the kinetic descriptions of flocking systems, which indicates a concentration in velocity variable in infinite time. We propose a discontinuous Galerkin method to treat the asymptotic $\\delta$-singularity, and construct high order positive preserving scheme to solve kinetic flocking systems.

Thermo-Kinetic Investigation of Comparative Ligand Effect on Cysteine Iron Redox Reaction

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Masood Ahmad Rizvi

2015-03-01

Full Text Available Transition metal ions in their free state bring unwanted biological oxidations generating oxidative stress. The ligand modulated redox potential can be indispensable in prevention of such oxidative stress by blocking the redundant bio-redox reactions. In this study we investigated the comparative ligand effect on the thermo-kinetic aspects of biologically important cysteine iron (III redox reaction using spectrophotometric and potentiometric methods. The results were corroborated with the complexation effect on redox potential of iron(III-iron(II redox couple. The selected ligands were found to increase the rate of cysteine iron (III redox reaction in proportion to their stability of iron (II complex (EDTA < terpy < bipy < phen. A kinetic profile and the catalytic role of copper (II ions by means of redox shuttle mechanism for the cysteine iron (III redox reaction in presence of 1,10-phenanthroline (phen ligand is also reported.

Spectrophotometric determination of the sulfhydryl containing drug mesna

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Rim S. Haggag

2016-06-01

Full Text Available Four simple and sensitive spectrophotometric methods were developed for the determination of the sulfhydryl containing drug mesna (MSN. Methods I and II rely on nucleophilic aromatic substitution reactions using two UV tagging reagents namely: 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBD-Cl for method I and 2,4-dinitrofluorobenzene (DNFB for method II. Both reactions took place in alkaline buffered medium and the obtained yellowish products were measured at 414 and 332 nm for methods I and II, respectively. Methods III and IV are indirect spectrophotometric methods based on the suppressive effect of MSN on the absorption of two ternary complex systems which are composed of 1,10-phenanthroline, silver and eosin for method III and 1,10-phenanthroline, silver and bromopyrogallol red for method IV. The decrease in absorbance of the ternary complexes was measured at 547 and 635 nm for methods III and IV, respectively. All the experimental parameters affecting these reactions were carefully studied and optimized. The methods were validated as per the ICH guidelines. The methods were applicable in the linearity ranges 4–18 μg/mL for method I, 4–16 μg/mL for method II, 0.25–2.25 μg/mL for method III and 0.25–1.75 μg/mL for method IV. The proposed methods were successfully applied for the analysis of MSN in its commercial ampoules and no interference was encountered from the present excipients as indicated by the satisfactory percentage recoveries. The results obtained were in a good agreement with those obtained from a previously published method of the investigated drug.

Development of a flotation-spectrophotometric method for determination of cetylpyridinium chloride in pharmaceutical products

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Hooshang Parham

2011-01-01

Full Text Available A new simple and sensitive flotation-spectrophotometric method for the determination of cetylpyridinium chloride (CPC is reported. The method is based on the formation of an ion- associate between CPC and Orange II (OR which is floated in the interface of aqueous phase and n-hexane by vigorous shaking. The aqueous solution was discarded and the adsorbed ion associate on to the wall of a separating funnel was dissolved in a small volume of methanol solvent and its absorbance was measured at 480 nm. The apparent molar absorptivity (Ε of the ion associate was determined to be 4.12 x 10(5 L mol-1 cm-1. The calibration graph was linear in the concentration range of 15-800 ng mL-1 of CPC with a correlation coefficient of 0.9988. The limit of detection (LOD was 10.8 ng mL-1. The relative standard deviation (RSD for determination of 100 and 800 ng mL-1 of CPC was 3.47 and 2.04% (n=7, respectively. The method was successfully applied to the determination of CPC in a commercial mouth washer product.

Validation of a spectrophotometric method to determine ciprofibrate content in tablets

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Guilherme Nobre Lima do Nascimento

2011-03-01

Full Text Available Ciprofibrate is a drug indicated in cases of hypertriglyceridemia and mixed hyperlipidemia, but no monographs are available in official compendia for the analysis of this substance in tablets. The objective of this work was to develop and validate a spectrophotometric method for routine analysis of ciprofibrate in tablets. In this study, commercial and standard ciprofibrate were used, as well as placebo in absolute ethanol, analyzed by UV spectrophotometer. All tests followed the rules of Resolution RE-899, 2003. The results showed that the developed and validated method offers low cost, easy implementation, precision and accuracy, and may be included in the routine of quality control laboratories.O ciprofibrato é um fármaco indicado em casos de hipertrigliceridemia e hiperlipidemia mista, mas não há monografias em compêndios oficiais para a análise desta substância em comprimidos. O objetivo deste trabalho é desenvolver e validar um método espectrofotométrico para análise de rotina de ciprofibrato em comprimidos. Neste estudo foram empregados ciprofibrato comercial, padrão e placebo em etanol absoluto, analisadas por espectrofotometria UV. Todos os testes seguiram as regras da Resolução RE- 899, 2003. Os resultados mostraram que o método desenvolvido e validado apresenta baixo custo, fácil implementação, precisão e exatidão e pode ser incluído em rotina de laboratórios de controle de qualidade.

A New Kinetic Spectrophotometric Method for Total Polyphenols ...

African Journals Online (AJOL)

NICO

cleaned in aqueous HCl (1:1) and then thoroughly rinsed with deionized water. ... flask of 50 mL. A. 1.0 mol dm–3 solution of hydrogen peroxide (Merck) was prepared ... Some metal ions, SO2, organic acids, ethanol and phenolic compounds ...

Development and Validation of UV Spectrophotometric Method For Determination of Bisoprolol Fumarate in Bulk and Pharmaceutical Dosage Forms

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Shahinaz Mohammed

2017-10-01

Full Text Available In this study a simple, accurate and precise UV- spectrophotometric method was developed for the estimation of bisoprolol fumarate (BF in bulk and tablet dosage form. The method was based on measurement of absorbance of BF aqueous solution at 225 nm. Validation was conducted in accordance to ICH guidelines. The calibration curve was linear in the concentration range 5.0-30.0 µg/mL with correlation coefficient not less than 0.996. The limit of detection and limit of quantification were 0.22 μg/ml and 0.66 μg/ml, respectively. Intraday and intermediate precision of the developed method were reflected by the low RSD% values (1.19 and 0.854, respectively. The recovery percentage was 100.6 ± 0.6%, n=3. The proposed method was applied for the assay of BF in three different brands.

Spectrophotometric Determination of Zinc Using 7-(4-Nitrophenylazo-8-Hydroxyquinoline-5-Sulfonic Acid

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Korn Maria das Graças Andrade

1999-01-01

Full Text Available A sensitive and selective spectrophotometric method is proposed for the rapid determination of zinc(II using an 8-hydroxyquinoline derivative, 7-(4-nitrophenylazo-8-hydroxyquinoline-5-sulfonic acid (p-NIAZOXS, as a new spectrophotometric reagent. The reaction between the p-NIAZOXS and zinc(II is instantaneous at pH 9.2 (borax buffer and the absorbance remains stable for over 24 h. The method allows the determination of zinc over the range of 0.05-1.0 mug mL-1 with a molar absorptivity of 3.75x10(4 L mol-1 cm-1 and features a detection limit of 15 ng mL-1. The proposed method has been successfully applied to the determination of zinc in several pharmaceutical preparations and copper alloys. The precision (R.S.D. < 2% and the accuracy obtained were satisfactory.

Antioxidant activity profiling by spectrophotometric methods of aqueous methanolic extracts of Helichrysum stoechas subsp. rupestre and Phagnalon saxatile subsp. saxatile.

Science.gov (United States)

Haddouchi, Farah; Chaouche, Tarik Mohammed; Ksouri, Riadh; Medini, Faten; Sekkal, Fatima Zohra; Benmansour, Abdelhafid

2014-06-01

The aqueous methanolic extracts of two plants from Algeria, Helichrysum stoechas subsp. rupestre and Phagnalon saxatile subsp. saxatile, were investigated for their antioxidant activity. Total phenolics, flavonoids, and tannins were determined by spectrophotometric techniques. In vitro antioxidant and radical scavenging profiling was determined by spectrophotometric methods, through: Total antioxidant capacity, and radical scavenging effects by the DPPH and ABTS methods, reducing and chelating power, and blanching inhibition of the β-carotene. All of the extracts showed interesting antioxidant and radical scavenging activity. The highest contents in phenolics, tannins, and the highest total antioxidant capacity as gallic acid equivalents of 97.5 ± 0.33 mg GAE/g DW was obtained for the flowers of H. stoechas subsp. rupestre extract in the phosphomolybdenum assay. An extract of the leafy stems of P. saxatile subsp. saxatile revealed the highest content of flavonoids, and the highest antioxidant activity by the radical scavenging and β-carotene assays when compared with standards. The best activity was by the scavenging radical DPPH with an IC50 value of 5.65 ± 0.10 μg·mL(-1). The studied medicinal plants could provide scientific evidence for some traditional uses in the treatment of diseases related to the production of reactive oxygen species (ROS) and oxidative stress. Copyright © 2014 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

Sequential Spectrophotometric Method for the Simultaneous Determination of Amlodipine, Valsartan, and Hydrochlorothiazide in Coformulated Tablets

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Hany W. Darwish

2013-01-01

Full Text Available A new, simple and specific spectrophotometric method was developed and validated in accordance with ICH guidelines for the simultaneous estimation of Amlodipine (AML, Valsartan (VAL, and Hydrochlorothiazide (HCT in their ternary mixture. In this method three techniques were used, namely, direct spectrophotometry, ratio subtraction, and isoabsorptive point. Amlodipine (AML was first determined by direct spectrophotometry and then ratio subtraction was applied to remove the AML spectrum from the mixture spectrum. Hydrochlorothiazide (HCT could then be determined directly without interference from Valsartan (VAL which could be determined using the isoabsorptive point theory. The calibration curve is linear over the concentration ranges of 4–32, 4–44 and 6–20 μg/mL for AML, VAL, and HCT, respectively. This method was tested by analyzing synthetic mixtures of the above drugs and was successfully applied to commercial pharmaceutical preparation of the drugs, where the standard deviation is <2 in the assay of raw materials and tablets. The method was validated according to the ICH guidelines and accuracy, precision, repeatability, and robustness were found to be within the acceptable limits.

Comparison of Spectrophotometric Methods for the Determination of Copper in Sugar Cane Spirit.

Science.gov (United States)

Soares, Sarah Adriana R; Costa, Silvânio Silvério L; Araujo, Rennan Geovanny O; Teixeira, Leonardo Sena Gomes; Dantas, Alailson Falcão

2018-05-01

Three spectrophotometric methods were developed for the determination of copper (Cu) in sugar cane spirit using the chromogenic reagents neocuproine, cuprizone, and bathocuproine. Experimental conditions, such as reagent concentration, reducer concentration, pH, buffer concentration, the order of addition of reagents, and the stability of the complexes, were optimized. The work range was established from 1.0 to 10.0 µg/mL, with correlation coefficients of >0.999 for all three optimized methods. The methods were evaluated regarding accuracy by addition and recovery tests at five concentration levels, and the obtained recoveries ranged from 91 to 105% (n = 3). Precision was expressed as RSD (relative standard deviation), with values ranging from 0.01 to 0.17% (n = 10). The method using the chromogenic reagent cuprizone presented the greatest molar absorptivity, followed by bathocuproine and neocuproine. The methods were applied for the determination of Cu in sugar cane spirit, and the results were compared with a reference method by flame atomic absorption spectrometry (FAAS). Calibration curve solutions for FAAS analysis were prepared in a 40% (v/v) alcohol medium in a range of concentrations from 0.5 up to 5 µg/mL. Measurements for Cu determination were carried out at a wavelength of 324.7 nm. The concentrations obtained for Cu in sugar cane spirit samples from Brazil were between 1.99 and 12.63 µg/mL, and about 75% of the samples presented Cu concentrations above the limit established by Brazilian legislation (5.0 µg/mL or 5.0 mg/L).

EVALUATING THE ACCUMULATION TREND OF L-DOPA IN DARK-GERMINATED SEEDS AND SUSPENSION CULTURES OF Phaseolus vulgaris L. BY AN EFFICIENT UV-SPECTROPHOTOMETRIC METHOD

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Samira Rahmani-Nezhad

Full Text Available Seed germination and plant cell cultures provide an alternative mean for producing secondary metabolites. The present study is an attempt to evaluate the effect of seed dark germination and some elicitors and precursors on the production of L-DOPA in Phaseolus vulgaris L. Callus cultured on Murashige and Skoog medium supplemented with various concentrations of different plant growth regulators. L-DOPA produced was quantified by UV-spectrophotometric method. In this study, a user-friendly, quick, and economical UV-spectrophotometric method was described to determine L-DOPA content in extracts from 33 biotypes of Phaseolus vulgaris L. The method is based on the nitrosation of L-DOPA to form a yellow solution and then formation of a red solution by adding base which is measurable at 470 nm. According to our statistical studies, this method showed high efficiency and selectivity for quantitative determination of L-DOPA in herbal extracts from dried plant seeds, dark-germinated seeds and callus cultures. L-DOPA content in dark-germinated seeds and suspension cultures increased significantly to approximately several-fold compared to the control. The implication from this study is that elicitor treatment and precursor feeding of Phaseolus vulgaris L. can significantly improve the parkinson’s relevant L-DOPA content.

AAS and spectrophotometric determination of propranolol HCl and metoprolol tartrate.

Science.gov (United States)

El-Ries, M A; Abou Attia, F M; Ibrahim, S A

2000-12-15

Two simple and accurate spectrophotometric methods are described for the determination of propranolol hydrochloride (I) and metoprolol tartrate (II). The methods are based on the reaction of each drug as a secondary amine: (a) with carbon disulphide, the formed complex extracted into iso-butyl methyl ketone (IBMK) after chelation with Cu(II) ions at pH 7.5, followed by measuring the absorbance at 435.4 nm or indirectly for the drug by flame atomic absorption spectrophotometry (AAS). The calibration graph is linear up to 40 and 60 microg ml(-1) with apparent molar absorptivities of 6.89 x 10(3) and 1.08 x 104 l mol(-1) cm(-1) and correlation coefficients of 0.9994 and 0.9995 for propranolol and metoprolol, respectively; (b) with pi-acceptors, tetracyanoethylene (TCNE), or chloranilic acid (CLA) to give highly coloured complex species. The coloured products are quantitated spectrophotometrically at 415 or 510 nm for the two drugs with TCNE and CLA, respectively, and obey Beer's Law with RSD less than 2.0. The methods were applied to the determination of these drugs in pharmaceutical preparation without interferences.

Simultaneous kinetic spectrometric determination of three flavonoid antioxidants in fruit with the aid of chemometrics

Science.gov (United States)

Sun, Ruiling; Wang, Yong; Ni, Yongnian; Kokot, Serge

2014-03-01

A simple, inexpensive and sensitive kinetic spectrophotometric method was developed for the simultaneous determination of three anti-carcinogenic flavonoids: catechin, quercetin and naringenin, in fruit samples. A yellow chelate product was produced in the presence neocuproine and Cu(I) - a reduction product of the reaction between the flavonoids with Cu(II), and this enabled the quantitative measurements with UV-vis spectrophotometry. The overlapping spectra obtained, were resolved with chemometrics calibration models, and the best performing method was the fast independent component analysis (fast-ICA/PCR (Principal component regression)); the limits of detection were 0.075, 0.057 and 0.063 mg L-1 for catechin, quercetin and naringenin, respectively. The novel method was found to outperform significantly the common HPLC procedure.

Spectrophotometric Analysis of the Kinetic of Pd(II Chloride Complex Ions Sorption Process from Diluted Aqua Solutions Using Commercially Available Activated Carbon

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Wojnicki M.

2017-12-01

Full Text Available In this paper, results of adsorption kinetic studies of Pd(II chloride complex ions on activated carbon Organosrob 10 CO are presented. Spectorphotometrical method was applied to investigate the process. Kinetic model was proposed, and fundamental thermodynamic parameters were determined. Proposed kinetic model describes well observed phenomenon in the studied range of concentration of Pd(II chloride complex ions as well, as concentration of activated carbon.

Spectrophotometric method for determination of bifunctional macrocyclic ligands in macrocyclic ligand-protein conjugates

International Nuclear Information System (INIS)

Dadachova, E.; Chappell, L.L.; Brechbiel, M.W.

1999-01-01

A simple spectrophotometric assay for determination of bifunctional polyazacarboxylate-macrocyclic ligands of different sizes that are conjugated to proteins has been developed for: 12-membered macrocycle DOTA (2-[4-nitrobenzyl]-1, 4, 7, 10-tetraazacyclododecane-N,N',N'',N'''-tetraacetic acid) and analogs, the 15-membered PEPA macrocycle (2-[4-nitrobenzyl]-1,4,7,10,13-pentaazacyclopentadecane-N,N',N'',N''',N'''' -pentaacetic acid), and the large 18-membered macrocycle HEHA (1,4,7,10,13,16-hexaazacyclooctadecane-N,N',N'',N''',N''''-hexaacetic acid). The method is based on titration of the blue-colored 1:1 Pb(II)-Arsenazo III (AAIII) complex with the polyazacarboxylate macrocyclic ligand in the concentration range of 0-2.5 μM, wherein color change occurring upon transchelation of the Pb(II) from the AAIII to the polyazamacrocyclic ligand is monitored at 656 nm. The assay is performed at ambient temperature within 20 min without any interfering interaction between the protein and Pb(II)-AA(III) complex. Thus, this method also provides a ligand-to-protein ratio (L/P ratio) that reflects the effective number of ligands per protein molecule available to radiolabeling. The method is not suitable for 14-membered TETA macrocycle (2-[4-nitrobenzyl]-1, 4, 8, 11-tetraazacyclotetradecane N,N',N'',N'''-tetraacetic acid) because of low stability constant of Pb(II)-TETA complex. The method is rapid, simple and may be customized for other polyazacarboxylate macrocyclic ligands

Development of a flow method for the determination of phosphate in estuarine and freshwaters-Comparison of flow cells in spectrophotometric sequential injection analysis

International Nuclear Information System (INIS)

Mesquita, Raquel B.R.; Ferreira, M. Teresa S.O.B.; Toth, Ildiko V.; Bordalo, Adriano A.; McKelvie, Ian D.; Rangel, Antonio O.S.S.

2011-01-01

Highlights: → Sequential injection determination of phosphate in estuarine and freshwaters. → Alternative spectrophotometric flow cells are compared. → Minimization of schlieren effect was assessed. → Proposed method can cope with wide salinity ranges. → Multi-reflective cell shows clear advantages. - Abstract: A sequential injection system with dual analytical line was developed and applied in the comparison of two different detection systems viz; a conventional spectrophotometer with a commercial flow cell, and a multi-reflective flow cell coupled with a photometric detector under the same experimental conditions. The study was based on the spectrophotometric determination of phosphate using the molybdenum-blue chemistry. The two alternative flow cells were compared in terms of their response to variation of sample salinity, susceptibility to interferences and to refractive index changes. The developed method was applied to the determination of phosphate in natural waters (estuarine, river, well and ground waters). The achieved detection limit (0.007 μM PO 4 3- ) is consistent with the requirement of the target water samples, and a wide quantification range (0.024-9.5 μM) was achieved using both detection systems.

Development of a flow method for the determination of phosphate in estuarine and freshwaters-Comparison of flow cells in spectrophotometric sequential injection analysis

Energy Technology Data Exchange (ETDEWEB)

Mesquita, Raquel B.R. [CBQF/Escola Superior de Biotecnologia, Universidade Catolica Portuguesa, R. Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Laboratory of Hydrobiology, Institute of Biomedical Sciences Abel Salazar (ICBAS) and Institute of Marine Research (CIIMAR), Universidade do Porto, Lg. Abel Salazar 2, 4099-003 Porto (Portugal); Ferreira, M. Teresa S.O.B. [CBQF/Escola Superior de Biotecnologia, Universidade Catolica Portuguesa, R. Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal); Toth, Ildiko V. [REQUIMTE, Departamento de Quimica, Faculdade de Farmacia, Universidade de Porto, Rua Anibal Cunha, 164, 4050-047 Porto (Portugal); Bordalo, Adriano A. [Laboratory of Hydrobiology, Institute of Biomedical Sciences Abel Salazar (ICBAS) and Institute of Marine Research (CIIMAR), Universidade do Porto, Lg. Abel Salazar 2, 4099-003 Porto (Portugal); McKelvie, Ian D. [School of Chemistry, University of Melbourne, Victoria 3010 (Australia); Rangel, Antonio O.S.S., E-mail: aorangel@esb.ucp.pt [CBQF/Escola Superior de Biotecnologia, Universidade Catolica Portuguesa, R. Dr. Antonio Bernardino de Almeida, 4200-072 Porto (Portugal)

2011-09-02

Highlights: {yields} Sequential injection determination of phosphate in estuarine and freshwaters. {yields} Alternative spectrophotometric flow cells are compared. {yields} Minimization of schlieren effect was assessed. {yields} Proposed method can cope with wide salinity ranges. {yields} Multi-reflective cell shows clear advantages. - Abstract: A sequential injection system with dual analytical line was developed and applied in the comparison of two different detection systems viz; a conventional spectrophotometer with a commercial flow cell, and a multi-reflective flow cell coupled with a photometric detector under the same experimental conditions. The study was based on the spectrophotometric determination of phosphate using the molybdenum-blue chemistry. The two alternative flow cells were compared in terms of their response to variation of sample salinity, susceptibility to interferences and to refractive index changes. The developed method was applied to the determination of phosphate in natural waters (estuarine, river, well and ground waters). The achieved detection limit (0.007 {mu}M PO{sub 4}{sup 3-}) is consistent with the requirement of the target water samples, and a wide quantification range (0.024-9.5 {mu}M) was achieved using both detection systems.

Optimization and Validation of Quantitative Spectrophotometric Methods for the Determination of Alfuzosin in Pharmaceutical Formulations

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M. Vamsi Krishna

2007-01-01

Full Text Available Three accurate, simple and precise spectrophotometric methods for the determination of alfuzosin hydrochloride in bulk drugs and tablets are developed. The first method is based on the reaction of alfuzosin with ninhydrin reagent in N, N'-dimethylformamide medium (DMF producing a colored product which absorbs maximally at 575 nm. Beer’s law is obeyed in the concentration range 12.5-62.5 µg/mL of alfuzosin. The second method is based on the reaction of drug with ascorbic acid in DMF medium resulting in the formation of a colored product, which absorbs maximally at 530 nm. Beer’s law is obeyed in the concentration 10-50 µg/mL of alfuzosin. The third method is based on the reaction of alfuzosin with p-benzoquinone (PBQ to form a colored product with λmax at 400 nm. The products of the reaction were stable for 2 h at room temperature. The optimum experimental parameters for the reactions have been studied. The validity of the described procedures was assessed. Statistical analysis of the results has been carried out revealing high accuracy and good precision. The proposed methods could be used for the determination of alfuzosin in pharmaceutical formulations. The procedures were rapid, simple and suitable for quality control application.

Thermodynamic and kinetic characterization of a zirconium chelate

International Nuclear Information System (INIS)

Stumpf, H.O.; Ekman, M.F.; Souza, R.F.; Costa, V.H.; Dick, Y.P.

1980-01-01

The chemical preparation, composition and characteristics of a zirconium complex with hemateine was studied. Hematein is the common name of an organic compound containing hydroxy-aromatic and hydroxyquinonic groups. The stability constant of this complex was determined spectrophotometrically. Other thermodynamic parameters for the complex formation were also determined; the effect of temperature on these parameters was examined. Reaction kinetics was investigated, as well as the charge of reacting species for the formation of the activated complex. (C.L.B.) [pt

Spectrophotometric investigation into iodine-electron donor systems at low temperature

International Nuclear Information System (INIS)

Gorodyskij, V.A.; Morachevskij, A.A.

1978-01-01

Iodine-sec. butanol (n-donor) and iodine - hexene - 1 (π-donor) have been investigated for the first time by the spectrophotometric method in the wide temeprature range (77-293 K). The existence of complexes with a charge transfer of the type, which is characterized by the long-wave absorption band in electron spectra, is determined in the systems

SPECTROPHOTOMETRIC ASSESSMENT OF FERRIC REDUCING POWER OF THE INSTANT COFFEE

OpenAIRE

Tsiupko, T. G.; Tishchenko, E. A.; Voronova, O. B.

2016-01-01

The methods of antioxidant activity determination of foodstuffs using different indicator systems were discussed. The investigation of ferric reducing power (FRP) of coffee and its individual phenolic components such as chlorogenic (CGA), caffeic (СА), ferulic (FA), gallic (GA), vanillic (VA), protocatechuic (PCA) and uric (UA) acids as well as quercetin (Qu) and catechol (C) using the spectrophotometric method with Fe(III) - o-Phen indicator system was carried out. It was shown that the sens...

Spectrophotometric determination of trace carbaryl in water and grain samples by inhibition of the rhodamine-B oxidation.

Science.gov (United States)

Gupta, Nirja; Pillai, Ajai Kumar; Parmar, Prachi

2015-03-15

A novel, sensitive, selective and simple kinetic spectrophotometric method has been developed for determination of trace levels of carbaryl based on its inhibitory effect on the oxidation of rhodamine-B by chlorine and bromine released from reaction of potassium bromate with hydrochloric acid in micellar medium. A linear relationship was observed between the inhibitory effect and the concentration of the compound. The absorbance was monitored at the maximum wavelength of 555 nm. The effect of different parameters such as pH, temperature and concentration of rhodamine-B, potassium bromate and surfactant on the reaction were investigated and optimum conditions were established. Under the selected experimental conditions, carbaryl was determined in the range of 0.04-0.4 μg mL(-1). Sandell's sensitivity and molar absorptivity were found to be 0.00055 μg cm(-2) and 3.658×10(5) L mol(-1) cm(-1) respectively. The proposed method was applied satisfactorily for the determination of carbaryl in water and different grain samples. The results were compared with those obtained by reference method and were found to be in agreement. Copyright © 2014 Elsevier B.V. All rights reserved.

Spectrophotometric determination of procainamide hydrochloride using sodium periodate

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S. Al-Tamrah

2015-09-01

Full Text Available A simple spectrophotometric method has been described for the determination of procainamide hydrochloride. The method is based on the oxidation of procainamide hydrochloride by sodium periodate in the presence of sulfuric acid and measurement of the absorbance of the violet color formed at 531 nm. Parameters affecting the reaction were studied and conditions were optimized. Linear calibration graph was obtained from 50 to 700 μg ml−1 of procainamide hydrochloride and the limit of detection was 25 μg ml−1. The method was successfully applied for the determination of procainamide hydrochloride in pharmaceutical preparation.

Spectrophotometric Quantification of Vilazodone Hydrochloride in Pharmaceutical Dosage Form Using Quality by Design Approach

International Nuclear Information System (INIS)

Panda, S.S.; Kumar, B.V.V.R.K.; Beg, S.; Behera, S.

2015-01-01

The present work deals with development and validation of a novel, robust, precise and accurate spectrophotometric method, for the estimation of vilazodone hydrochloride in tablets using the principle of Quality by Design (QbD). A fractional factorial design (FFD) was employed for initial parameter screening. Further the screened parameters were subjected to central composite design (CCD) for evaluating method robustness and method optimization. Different statistical parameters were evaluated to decide appropriateness of experimental data. Vilazodone shows absorption maximum at 285 nm using methanol. Factor screening slit width and sampling interval were identified as critical method variables, which were further evaluated by a CCD. Good linearity was obtained for vilazodone in the range of 5-60 μg/ mL with R"2 > 0.999. The method was found to be accurate with good average % recovery (more than 100 %). Developed method was validated as per ICH guidelines. Based on QbD development of spectrophotometric method ensured that quality is built into the method. The method was robust and can be applied for determination of the vilazodone in pharmaceutical dosage form. (author)

Development and validation of new spectrophotometric ratio H-point standard addition method and application to gastrointestinal acting drugs mixtures

Science.gov (United States)

Yehia, Ali M.

2013-05-01

New, simple, specific, accurate and precise spectrophotometric technique utilizing ratio spectra is developed for simultaneous determination of two different binary mixtures. The developed ratio H-point standard addition method (RHPSAM) was managed successfully to resolve the spectral overlap in itopride hydrochloride (ITO) and pantoprazole sodium (PAN) binary mixture, as well as, mosapride citrate (MOS) and PAN binary mixture. The theoretical background and advantages of the newly proposed method are presented. The calibration curves are linear over the concentration range of 5-60 μg/mL, 5-40 μg/mL and 4-24 μg/mL for ITO, MOS and PAN, respectively. Specificity of the method was investigated and relative standard deviations were less than 1.5. The accuracy, precision and repeatability were also investigated for the proposed method according to ICH guidelines.

Simultaneous spectrophotometric determination of uranium and zirconium using cloud point extraction and multivariate methods

International Nuclear Information System (INIS)

Ghasemi, Jahan B.; Hashemi, Beshare; Shamsipur, Mojtaba

2012-01-01

A cloud point extraction (CPE) process using the nonionic surfactant Triton X-114 to simultaneous extraction and spectrophotometric determination of uranium and zirconium from aqueous solution using partial least squares (PLS) regression is investigated. The method is based on the complexation reaction of these cations with Alizarin Red S (ARS) and subsequent micelle-mediated extraction of products. The chemical parameters affecting the separation phase and detection process were studied and optimized. Under the optimum experimental conditions (i.e. pH 5.2, Triton X-114 = 0.20%, equilibrium time 10 min and cloud point 45 C), calibration graphs were linear in the range of 0.01-3 mg L -1 with detection limits of 2.0 and 0.80 μg L -1 for U and Zr, respectively. The experimental calibration set was composed of 16 sample solutions using an orthogonal design for two component mixtures. The root mean square error of predictions (RMSEPs) for U and Zr were 0.0907 and 0.1117, respectively. The interference effect of some anions and cations was also tested. The method was applied to the simultaneous determination of U and Zr in water samples.

Chromium speciation in environmental samples using a solid phase spectrophotometric method

Science.gov (United States)

Amin, Alaa S.; Kassem, Mohammed A.

2012-10-01

A solid phase extraction technique is proposed for preconcentration and speciation of chromium in natural waters using spectrophotometric analysis. The procedure is based on sorption of chromium(III) as 4-(2-benzothiazolylazo)2,2'-biphenyldiol complex on dextran-type anion-exchange gel (Sephadex DEAE A-25). After reduction of Cr(VI) by 0.5 ml of 96% concentrated H2SO4 and ethanol, the system was applied to the total chromium. The concentration of Cr(VI) was calculated as the difference between the total Cr and the Cr(III) content. The influences of some analytical parameters such as: pH of the aqueous solution, amounts of 4-(2-benzothiazolylazo)2,2'-biphenyldiol (BTABD), and sample volumes were investigated. The absorbance of the gel, at 628 and 750 nm, packed in a 1.0 mm cell, is measured directly. The molar absorptivities were found to be 2.11 × 107 and 3.90 × 107 L mol-1 cm-1 for 500 and 1000 ml, respectively. Calibration is linear over the range 0.05-1.45 μg L-1 with RSD of <1.85% (n = 8.0). Using 35 mg exchanger, the detection and quantification limits were 13 and 44 ng L-1 for 500 ml sample, whereas for 1000 ml sample were 8.0 and 27 ng L-1, respectively. Increasing the sample volume can enhance the sensitivity. No considerable interferences have been observed from other investigated anions and cations on the chromium speciation. The proposed method was applied to the speciation of chromium in natural waters and total chromium preconcentration in microwave digested tobacco, coffee, tea, and soil samples. The results were simultaneously compared with those obtained using an ET AAS method, whereby the validity of the method has been tested.

A validated fast difference spectrophotometric method for 5-hydroxymethyl-2-furfural (HMF) determination in corn syrups.

Science.gov (United States)

de Andrade, Jucimara Kulek; de Andrade, Camila Kulek; Komatsu, Emy; Perreault, Hélène; Torres, Yohandra Reyes; da Rosa, Marcos Roberto; Felsner, Maria Lurdes

2017-08-01

Corn syrups, important ingredients used in food and beverage industries, often contain high levels of 5-hydroxymethyl-2-furfural (HMF), a toxic contaminant. In this work, an in house validation of a difference spectrophotometric method for HMF analysis in corn syrups was developed using sophisticated statistical tools by the first time. The methodology showed excellent analytical performance with good selectivity, linearity (R 2 =99.9%, r>0.99), accuracy and low limits (LOD=0.10mgL -1 and LOQ=0.34mgL -1 ). An excellent precision was confirmed by repeatability (RSD (%)=0.30) and intermediate precision (RSD (%)=0.36) estimates and by Horrat value (0.07). A detailed study of method precision using a nested design demonstrated that variation sources such as instruments, operators and time did not interfere in the variability of results within laboratory and consequently in its intermediate precision. The developed method is environmentally friendly, fast, cheap and easy to implement resulting in an attractive alternative for corn syrups quality control in industries and official laboratories. Copyright © 2017 Elsevier Ltd. All rights reserved.

A multisyringe flow injection method for the determination of thorium in water samples using spectrophotometric detection

International Nuclear Information System (INIS)

Guzman-Mar, J.L.; Aracely Hernandez-Ramirez; Lopez-Chuken, U.J.; Lopez-de-Alba, P.L.; Victor Cerda

2011-01-01

A fast and simple multisyringe flow injection analysis (MSFIA) method for routine determination of thorium in water samples was developed. The methodology was based on the complexation reaction of thorium with arsenazo (III) at pH 2.0. Thorium concentrations were spectrophotometrically detected at 665 nm. Under optimal conditions, Beer's law was obeyed over the range from 0.2 to 4.5 μg mL -1 thorium, a 3σ detection limit of 0.05 μg mL -1 , and a 10σ quantification limit of 0.2 μg mL -1 were obtained. The relative standard deviations (RSD, %) at 0.5, 2.5 and 4.5 μg mL -1 was 2.8, 1.5 and 0.8%, respectively (n = 10). It was found that most of the common metal ions and anions did not interfere with the thorium determination. The proposed method was successfully applied to its analysis in various water samples. (author)

Novel Spectrophotometric Methods for Determination of Salicylamide and Ascorbic acid in their binary mixture

International Nuclear Information System (INIS)

Ali, N.W.; Zaazaa, H.E.S.; Abdelrahman, M.M.

2014-01-01

Simple, selective and precise four spectrophotometric methods were developed and validated for quantitative determination of Salicylamide (SAD) and Ascorbic acid (ASC, Vitamin C) in their binary mixture. Method A is Area under curve spectrophotometry, in which the area under curve in the wavelength ranges 225-245 nm and 265-285 nm were selected for determination of SAD and ASC. Method B is based on dual wavelength spectrophotometry, where ASC can be determined by difference in absorbance at 249.8 and 285.8 nm. On the same way; SAD is measured by difference in absorbance at 240.4 and 286.4 nm. Method C utilizes isoabsorptive point spectrophotometry where total concentration of SAD and ASC was calculated at their isoabsorptive points at 246.4 and 287 nm, while SAD concentration alone can be determined by first derivative spectrophotometry (1D) at 315.4 nm, then ASC concentration can be determined by subtraction. Method D is ratio subtraction spectrophotometry, where ASC can be determined by dividing the spectrum of the mixture by the spectrum of the SAD (as a divisor) followed by subtracting the constant absorbance value of the plateau region, then finally multiplying the obtained spectrum by the spectrum of the divisor. The developed methods have been successfully applied for determination of the studied drugs in different laboratory prepared mixtures and in their pharmaceutical formulation. Statistical comparison between the results obtained by applying the proposed methods and the reported HPLC method was done, and it was found that there was no significant difference between them regarding both accuracy and precision. (author)

New Methods for Processing and Quantifying VO2 Kinetics to Steady State: VO2 Onset Kinetics

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Craig R. McNulty

2017-09-01

Full Text Available Current methods of oxygen uptake (VO2 kinetics data handling may be too simplistic for the complex physiology involved in the underlying physiological processes. Therefore, the aim of this study was to quantify the VO2 kinetics to steady state across the full range of sub-ventilatory threshold work rates, with a particular focus on the VO2 onset kinetics. Ten healthy, moderately trained males participated in five bouts of cycling. Each bout involved 10 min at a percentage of the subject's ventilation threshold (30, 45, 60, 75, 90% from unloaded cycling. The VO2 kinetics was quantified using the conventional mono-exponential time constant (tau, τ, as well as the new methods for VO2 onset kinetics. Compared to linear modeling, non-linear modeling caused a deterioration of goodness of fit (main effect, p < 0.001 across all exercise intensities. Remainder kinetics were also improved using a modified application of the mono-exponential model (main effect, p < 0.001. Interestingly, the slope from the linear regression of the onset kinetics data is similar across all subjects and absolute exercise intensities, and thereby independent of subject fitness and τ. This could indicate that there are no functional limitations between subjects during this onset phase, with limitations occurring for the latter transition to steady state. Finally, the continuing use of mono-exponential modeling could mask important underlying physiology of more instantaneous VO2 responses to steady state. Consequently, further research should be conducted on this new approach to VO2 onset kinetics.

Reactor kinetics methods development. Final report

International Nuclear Information System (INIS)

Hansen, K.F.; Henry, A.F.

1978-01-01

This report is a qualitative summary of research conducted at MIT from 1967 to 1977 in the area of reactor kinetics methods. The objectives of the research were to find methods of integration of various mathematical models of nuclear reactor transients. From the beginning the work was aimed at numerical integration methods. Specific areas of research, discussed in more detail following, included: integration of multigroup diffusion theory models by finite difference and finite element methods; response matrix and nodal methods; coarse-mesh homogenization; and special treatment of boundary conditions

Complexation equilibria and spectrophotometric determination of iron(III) with 1-amino-4-hydroxyanthraquinone.

Science.gov (United States)

Abu-Bakr, M S; Sedaira, H; Hashem, E Y

1994-10-01

The complex equilibria of iron(III) with 1-amino-4-hydroxyanthraquinone (AMHA) were studied spectrophotometrically in 40% (v/v) ethanol and an ionic strength of 0.1M (NaClO(4)). The complexation reactions were demonstrated and characterized using graphical logarithmic analysis of the absorbance-pH graphs. A simple, rapid, selective and sensitive method for the spectrophotometric determination of trace amounts of Fe(III) is developed based on the formation of Fe(AMHA) complex at pH 2.5 (lambda(max) = 640 nm, epsilon approximately = 2.1 x 10(4) L. mol(-1) . cm(-1)) in the presence of a large number of foreign ions. Interferences caused by palladium(II) was masked by the addition of cyanide ions. The method has been applied to the determination of iron in some synthetic samples and polymetallic iron ores.

Simultaneous determination of piracetam and vincamine by spectrophotometric and high-performance liquid chromatographic methods.

Science.gov (United States)

El-Saharty, Yasser Shaker Ibrahim

2008-01-01

A mixture of piracetam and vincamine was determined by 3 different methods. The first was the determination of piracetam and vincamine using the ratio-spectra first-derivative (DD1) spectrophotometric technique at 209 and 293 nm in concentration ranges of 10-45 and 2-14 microg/mL with mean recoveries of 99.22 +/- 0.72 and 99.67 +/- 0.79%, respectively. The second method was based on the resolution of the 2 components by bivariate calibration depending on a mathematic algorithm that provides simplicity and rapidity. The method depended on quantitative evaluation of the absorbencies at 210 and 225 nm in concentration ranges of 5-45 and 2-14 microg/mL, with mean recoveries of 100.33 +/- 0.54 and 100.44 +/- 0.98% for piracetam and vincamine, respectively. The third method was reversed-phase liquid chromatography using 0.05 M potassium dihydrogen phosphate-methanol (50 + 50, v/v) as the mobile phase, with the pH adjusted to 3.5 with phosphoric acid. The eluent was monitored at 215 nm in concentration ranges of 5-100 and 2-200 microg/mL, with mean recoveries of 99.62 +/- 0.67 and 99.32 +/- 0.85% for piracetam and vincamine, respectively. The suggested procedures were checked using laboratory-prepared mixtures and were successfully applied for the analysis of their pharmaceutical preparation. The methods retained their accuracy and precision when applying the standard addition technique. The results obtained by applying the proposed methods were statistically analyzed and compared with those obtained by the manufacturer's method.

Validation of high performance liquid chromatographic and spectrophotometric methods for the determination of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products

Directory of Open Access Journals (Sweden)

Serpil Sevim

2015-12-01

Full Text Available abstract The antiparkinson agent pramipexole dihydrochloride monohydrate was quantified in pharmaceutical products by high performance liquid chromatography (HPLC and derivative spectrophotometry. The first method was based on HPLC using tamsulosin HCl as an internal standard. In this method, chromatographic separation was achieved using a LiChrospher 60 RP column at 25°C, with a flow rate of 1.0 mL/min at 263 nm. The eluent comprised 0.01 mol/L ammonium acetate (pH 4.4 and acetonitrile (35:65 by volume. The linearity range was found to be 10.0-30.0 µg/mL with a mean recovery of 100.5 ± 1.10. The limit of detection (8 ng/mL and limit of quantification (50 ng/mL were calculated. In the second method, the first derivative spectrophotometric technique for the determination of pramipexole dihydrochloride monohydrate was performed by measuring the amplitude at 249 and 280 nm. In the first derivative technique, the absorbance and concentration plot was rectilinear over the 5.0-35.0 µg/mL range with a lower detection limit of 1.5 ng/mL and quantification limit of 4.5 ng/mL. The typical excipients included in the pharmaceutical product do not interfere with the selectivity of either method. The developed methods were validated for robustness, selectivity, specificity, linearity, precision, and accuracy as per the ICH and FDA guidelines (ICH Q2B, 1996; FDA,2000. In conclusion, the developed methods were successful in determining the quantity of the antiparkinson agent pramipexole dihydrochloride monohydrate in pharmaceutical products. The RSD values for the pharmaceutical product used in this study were found to be 0.97% for the HPLC method and 0.00% for the first derivative spectrophotometric method.

Flame Spectrophotometric Determination of Strontium in Water and Biological Material

Energy Technology Data Exchange (ETDEWEB)

Joensson, G

1964-10-15

A flame spectrophotometric method has been developed for the determination of strontium in biological material and water samples. Strontium is determined in the presence of calcium at a wavelength of 4607 A. The intensity of the strontium emission from the sample is increased if n-butanol is added to a solution of the sample in water. With a 6 vol% solution of n-butanol in water, an optimum intensity of 3.5 times that obtained with pure water solution is obtained. Anions and alkali metals which might interfere with the flame spectrophotometric determination are separated from the sample by a simple ion exchange operation. The method allows determination of strontium in solutions down to 0.1{mu}g/ml. In this case the standard deviation is 3.1 % and with a strontium concentration of 1 {mu}g/ml the deviation is 0.9 %. This method has been used for the determination of strontium in samples of varying composition such as bone, meat and skin from fishes, samples of human bones, shell-fish, milk, and water, in which case Sr quantities of 5{mu}g were determined with an analytical error of less than 5 % and Sr{sub q}uantities greater than 10 {mu}g with an error of less than 3 %.

Flame Spectrophotometric Determination of Strontium in Water and Biological Material

International Nuclear Information System (INIS)

Joensson, G.

1964-10-01

A flame spectrophotometric method has been developed for the determination of strontium in biological material and water samples. Strontium is determined in the presence of calcium at a wavelength of 4607 A. The intensity of the strontium emission from the sample is increased if n-butanol is added to a solution of the sample in water. With a 6 vol% solution of n-butanol in water, an optimum intensity of 3.5 times that obtained with pure water solution is obtained. Anions and alkali metals which might interfere with the flame spectrophotometric determination are separated from the sample by a simple ion exchange operation. The method allows determination of strontium in solutions down to 0.1μg/ml. In this case the standard deviation is 3.1 % and with a strontium concentration of 1 μg/ml the deviation is 0.9 %. This method has been used for the determination of strontium in samples of varying composition such as bone, meat and skin from fishes, samples of human bones, shell-fish, milk, and water, in which case Sr quantities of 5μg were determined with an analytical error of less than 5 % and Sr q uantities greater than 10 μg with an error of less than 3 %

Spectrophotometric and spectrofluorimetric determination of some drugs containing secondary amino group in bulk drug and dosage forms via derivatization with 7-Chloro-4-Nitrobenzofurazon

Directory of Open Access Journals (Sweden)

Armaan Önal

2011-01-01

Full Text Available Sensitive and selective spectrophotometric and spectrofluorimetric methods have been developed for determination of some drugs such as Pramipexole, Nebivolol, Carvedilol, and Eletriptan, which commonly contain secondary amino group. The subject methods were developed via derivatization of the secondary amino groups with 7-Chloro-4-Nitrobenzofurazon in borate buffer where a yellow colored reaction product was obtained and measured spectrophotometrically or spectrofluorimetrically. Concentration ranges were found as 2.0 to 250 μg mL-1 and 0.1 to 3.0 μg mL-1, for spectrophotometric and spectrofluorimetric study, respectively. The described methods can be easily applied by the quality control laboratories in routine analyses of these drugs in pharmaceutical preparations.

Zeolite - a possible substitute of silica gel in spectrophotometric determination of uranium?

International Nuclear Information System (INIS)

Foeldesova, M; Dillinger, P.

2006-01-01

Zeolites sorption abilities differ from the ones of the silica gel, which is normally used for uranium determination by spectrophotometric method. The difference is obvious mainly in the case of zeolites chemically modified with 1 or 2 mol/L NaOH solution. Absorbances measured using these zeolites on an radioactive water samples were 4 to 4.2 times bigger than the ones with silica gel. This avoids a use of one universal calibration curve for experimental data evaluation. Within delivered experimental data only a calibration curve for silica gel was provided. Its application to zeolites caused substantial misinterpretation of the results. Calculational construction of individual calibration curves made at this work shaw, that zeolites have a potential to replace the silica gel. This possibility is necessary to confirm by more experiments. Better sorption abilities of the modified zeolites would be utilized to reduce the lower limit for uranium determination by spectrophotometric method. (authors)

Liquid chromatographic and ultraviolet spectrophotometric determination of bevantolol and hydrochlorothiazide in feeds.

Science.gov (United States)

Spurlock, C H; Schneider, H G

1984-01-01

Separate assay methods have been developed for the 2 components of an 80 + 20 drug blend of bevantolol and hydrochlorothiazide (HCT) in admixtures with animal feed. Drug/diet admixtures are extracted with methanol for reverse phase ion-pair liquid chromatographic (LC) assay of bevantolol, and with acetonitrile for ultraviolet spectrophotometric assay of HCT. Bevantolol, a cardioselective beta blocker, is separated from soluble feed components with an RP-18 column, using methanol-water-acetic acid (60 + 40 + 1) containing 0. 005M octane-sulfonic acid, sodium salt, as ion-pairing reagent. HCT is determined spectrophotometrically in acetonitrile extracts, using a suitable blank extract as reference. Average recovery of HCT from an admixture of 0.5 mg blend/g diet is 94.5% +/- 4.3 RSD and at 2.0 mg/g, 101.5% +/- 3.5 RSD. Bevantolol recovery from the same admixtures is 101.8% +/- 2.7 RSD and 99.0% +/- 3.5 RSD, respectively, using the method as described.

Spectrophotometric determination of fluorides in water with Hach equipment

International Nuclear Information System (INIS)

Acosta L, E.

1994-11-01

The spectrophotometric method for the determination of the fluoride ion in water, demineralized water, raw waters, laundry waters and waters treated with ion exchange resins , using the technique and the SPADNS coloring indicated in the operation manual of the Hach equipment is described. This method covers the determination of the fluoride ion in the range from 0 to 2 mg/l on 25 ml. of radioactive base sample. These limits can be variable if the size of the used aliquot one is changed for the final determination of the fluoride ion. (Author)

Taylor's series method for solving the nonlinear point kinetics equations

International Nuclear Information System (INIS)

Nahla, Abdallah A.

2011-01-01

Highlights: → Taylor's series method for nonlinear point kinetics equations is applied. → The general order of derivatives are derived for this system. → Stability of Taylor's series method is studied. → Taylor's series method is A-stable for negative reactivity. → Taylor's series method is an accurate computational technique. - Abstract: Taylor's series method for solving the point reactor kinetics equations with multi-group of delayed neutrons in the presence of Newtonian temperature feedback reactivity is applied and programmed by FORTRAN. This system is the couples of the stiff nonlinear ordinary differential equations. This numerical method is based on the different order derivatives of the neutron density, the precursor concentrations of i-group of delayed neutrons and the reactivity. The r th order of derivatives are derived. The stability of Taylor's series method is discussed. Three sets of applications: step, ramp and temperature feedback reactivities are computed. Taylor's series method is an accurate computational technique and stable for negative step, negative ramp and temperature feedback reactivities. This method is useful than the traditional methods for solving the nonlinear point kinetics equations.

Spectrophotometric determination of association constant

DEFF Research Database (Denmark)

2016-01-01

Least-squares 'Systematic Trial-and-Error Procedure' (STEP) for spectrophotometric evaluation of association constant (equilibrium constant) K and molar absorption coefficient E for a 1:1 molecular complex, A + B = C, with error analysis according to Conrow et al. (1964). An analysis of the Charge...

A nondissipative simulation method for the drift kinetic equation

International Nuclear Information System (INIS)

Watanabe, Tomo-Hiko; Sugama, Hideo; Sato, Tetsuya

2001-07-01

With the aim to study the ion temperature gradient (ITG) driven turbulence, a nondissipative kinetic simulation scheme is developed and comprehensively benchmarked. The new simulation method preserving the time-reversibility of basic kinetic equations can successfully reproduce the analytical solutions of asymmetric three-mode ITG equations which are extended to provide a more general reference for benchmarking than the previous work [T.-H. Watanabe, H. Sugama, and T. Sato: Phys. Plasmas 7 (2000) 984]. It is also applied to a dissipative three-mode system, and shows a good agreement with the analytical solution. The nondissipative simulation result of the ITG turbulence accurately satisfies the entropy balance equation. Usefulness of the nondissipative method for the drift kinetic simulations is confirmed in comparisons with other dissipative schemes. (author)

Kinetics of hydroxyethylethylenediaminetriacetate exchange of neodymium (3) with ytterbium (3) and gadolinium (3) aquaions

International Nuclear Information System (INIS)

Nikitenko, S.I.; Martynenko, L.I.; Petsurova, N.I.

1985-01-01

The exchange kinetic in the NdX-Ln 3+ , where X 3- is hydroxyethylethylenediamine triacetate, Ln 3+ -Yb 3+ , Cd 3+ is studied spectrophotometrically. It has been found that the stationary exchange reate is described by the kinetic equation: W=Ksub(1)csub.(NdX)sup(0)csub(H)+Ksub(2)csub(NdX)sup(0)csub(Ln)sup(0)(1). The exchange rate constant values are calulated at t=20 deg C and μ=0.1: K 1 =(4.5+-0.2)x10 3 (Yb 3+ ), (4.8+-0.3)x10 3 .(Gd 3+ ), K 2 =1.7+-0.2(Yb 3+ ), 0.9+-0.1(Gd 3+ ) l/molxmin. It is shown that the acidic dissociation mechanism corresponds to augend (1), the exchange associative mechanism - to addend. It is shown by the method of segments that Ln 3+ in intermediate complexes (NdXLn) 3+ is coordinated by X 3- hydroxyethylglicine group

Optimization and validation of spectrophotometric methods for determination of finasteride in dosage and biological forms

Science.gov (United States)

Amin, Alaa S.; Kassem, Mohammed A.

2012-01-01

Aim and Background: Three simple, accurate and sensitive spectrophotometric methods for the determination of finasteride in pure, dosage and biological forms, and in the presence of its oxidative degradates were developed. Materials and Methods: These methods are indirect, involve the addition of excess oxidant potassium permanganate for method A; cerric sulfate [Ce(SO4)2] for methods B; and N-bromosuccinimide (NBS) for method C of known concentration in acid medium to finasteride, and the determination of the unreacted oxidant by measurement of the decrease in absorbance of methylene blue for method A, chromotrope 2R for method B, and amaranth for method C at a suitable maximum wavelength, λmax: 663, 528, and 520 nm, for the three methods, respectively. The reaction conditions for each method were optimized. Results: Regression analysis of the Beer plots showed good correlation in the concentration ranges of 0.12–3.84 μg mL–1 for method A, and 0.12–3.28 μg mL–1 for method B and 0.14 – 3.56 μg mL–1 for method C. The apparent molar absorptivity, Sandell sensitivity, detection and quantification limits were evaluated. The stoichiometric ratio between the finasteride and the oxidant was estimated. The validity of the proposed methods was tested by analyzing dosage forms and biological samples containing finasteride with relative standard deviation ≤ 0.95. Conclusion: The proposed methods could successfully determine the studied drug with varying excess of its oxidative degradation products, with recovery between 99.0 and 101.4, 99.2 and 101.6, and 99.6 and 101.0% for methods A, B, and C, respectively. PMID:23781478

Stability and kinetics of uranyl ion complexation by macrocycles in propylene carbonate

International Nuclear Information System (INIS)

Fux, P.

1984-06-01

A thermodynamic study of uranyl ion complexes formation with different macrocyclic ligands was realized in propylene carbonate as solvent using spectrophotometric and potentiometric techniques. Formation kinetics of two UO 2 complexes: a crown ether (18C6) and a coronand (22) was studied by spectrophotometry in propylene carbonate with addition of tetraethylammonium chlorate 0.1M at 25 0 C. Possible structures of complexes in solution are discussed [fr

Measurement of peroxisomal enzyme activities in the liver of brown trout (Salmo trutta, using spectrophotometric methods

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Resende Albina D

2003-03-01

Full Text Available Abstract Background This study was aimed primarily at testing in the liver of brown trout (Salmo trutta spectrophotometric methods previously used to measure the activities of catalase and hydrogen peroxide producing oxidases in mammals. To evaluate the influence of temperature on the activities of those peroxisomal enzymes was the second objective. A third goal of this work was the study of enzyme distribution in crude cell fractions of brown trout liver. Results The assays revealed a linear increase in the activity of all peroxisomal enzymes as the temperature rose from 10° to 37°C. However, while the activities of hydrogen peroxide producing oxidases were strongly influenced by temperature, catalase activity was only slightly affected. A crude fraction enriched with peroxisomes was obtained by differential centrifugation of liver homogenates, and the contamination by other organelles was evaluated by the activities of marker enzymes for mitochondria (succinate dehydrogenase, lysosomes (aryl sulphatase and microsomes (NADPH cytochrome c reductase. For peroxisomal enzymes, the activities per mg of protein (specific activity in liver homogenates were strongly correlated with the activities per g of liver and with the total activities per liver. These correlations were not obtained with crude peroxisomal fractions. Conclusions The spectrophotometric protocols originally used to quantify the activity of mammalian peroxisomal enzymes can be successfully applied to the study of those enzymes in brown trout. Because the activity of all studied peroxisomal enzymes rose in a linear mode with temperature, their activities can be correctly measured between 10° and 37°C. Probably due to contamination by other organelles and losses of soluble matrix enzymes during homogenisation, enzyme activities in crude peroxisomal fractions do not correlate with the activities in liver homogenates. Thus, total homogenates will be used in future seasonal and

Method of molybdenum kinetic determination

International Nuclear Information System (INIS)

Krejngol'd, S.U.; Dzotsenidze, N.E.; Ruseishviyai, T.G.; Nelen', I.M.

1980-01-01

The method molybdenum kinetic determination according to oxidation of pyrogallol with bromate in the medium of 0.05-0.15 M perchloric or sulphuric acids is presented. 1 mg of Ni, Co, Mn, Mg, Zn, Cr(3); 100 μg of Ca, Al, Cu, 10 μg of Cr(4), W; 10 μg of Fe in the presence of 22x10 - 4 M solution of EDTA, as well as 10 - 4 M solutions of chlorides and fluorides, 10 - 5 M solutions of bromides do not interfere with molybdenum determination using the given method. The method is rather simple, it takes 30 min to carry out the analysis. Determination limit of molybdenum constitutes 0.01 μg/ml

Stiffness Confinement Method with Pseudo Absorption for Spatial Kinetics

International Nuclear Information System (INIS)

Park, Beom Woo; Joo, Han Gyu; Chao, Yungan

2013-01-01

The primary advantage of the SCM is that it is possible to use larger time step sizes. This advantage comes from the fact because the SCM involves the solution of an eigenvalue problem instead of the ordinary form of a fixed source problem. Since using a large time step size is strongly desired in the direct whole core transport calculation for transient problems, we investigate here the SCM for spatial kinetics first with a simple one-dimensional, one-group diffusion equation and propose an improved formulation. The performance of the improved SCM for spatial kinetics is assessed by comparing the SCM solutions with the standard method solutions employing the Crank-Nicholson method with exponential transform. The stiffness confinement method for spatial kinetics was refined with the pseudo absorption term representing the dynamic frequencies. It was verified that the proposed SCM works much better than the Crank-Nicholson method with exponential transform in that time step sizes larger than 20 msec can be using in a super prompt-critical transient involving 1.5$ reactivity insertion

Stiffness Confinement Method with Pseudo Absorption for Spatial Kinetics

Energy Technology Data Exchange (ETDEWEB)

Park, Beom Woo; Joo, Han Gyu [Seoul National Univ., Seoul (Korea, Republic of); Chao, Yungan [Retired in China, Beijing (China)

2013-05-15

The primary advantage of the SCM is that it is possible to use larger time step sizes. This advantage comes from the fact because the SCM involves the solution of an eigenvalue problem instead of the ordinary form of a fixed source problem. Since using a large time step size is strongly desired in the direct whole core transport calculation for transient problems, we investigate here the SCM for spatial kinetics first with a simple one-dimensional, one-group diffusion equation and propose an improved formulation. The performance of the improved SCM for spatial kinetics is assessed by comparing the SCM solutions with the standard method solutions employing the Crank-Nicholson method with exponential transform. The stiffness confinement method for spatial kinetics was refined with the pseudo absorption term representing the dynamic frequencies. It was verified that the proposed SCM works much better than the Crank-Nicholson method with exponential transform in that time step sizes larger than 20 msec can be using in a super prompt-critical transient involving 1.5$ reactivity insertion.

Development and validation of RP-HPLC and UV-spectrophotometric methods for rapid simultaneous estimation of amlodipine and benazepril in pure and fixed dose combination

Directory of Open Access Journals (Sweden)

Abhi Kavathia

2017-05-01

Full Text Available High-performance liquid chromatographic (HPLC and UV spectrophotometric methods were developed and validated for the quantitative determination of amlodipine besylate (AM and benazepril hydrochloride (BZ. Different analytical performance parameters such as linearity, precision, accuracy, specificity, limit of detection (LOD and limit of quantification (LOQ were determined according to International Conference on Harmonization ICH Q2B guidelines. The RP-HPLC method was developed by the isocratic technique on a reversed-phase Shodex C-18 5e column. The retention time for AM and BZ was 4.43 min and 5.70 min respectively. The UV spectrophotometric determinations were performed at 237 nm and 366 nm for AM and at 237 nm for BZ. Correlation between absorbance of AM at 237 nm and 366 nm was established and based on developed correlation equation estimation of BZ at 237 nm was carried out. The linearity of the calibration curves for each analyte in the desired concentration range was good (r2 > 0.999 by both the HPLC and UV methods. The method showed good reproducibility and recovery with percent relative standard deviation less than 5%. Moreover, the accuracy and precision obtained with HPLC co-related well with the UV method which implied that UV spectroscopy can be a cheap, reliable and less time consuming alternative for chromatographic analysis. The proposed methods are highly sensitive, precise and accurate and hence successfully applied for determining the assay and in vitro dissolution of a marketed formulation.

Development of an indirect spectrophotometric method for determination of methamidophos insecticide in soil, water and vegetable samples

Directory of Open Access Journals (Sweden)

J. Shah

2015-07-01

Full Text Available A simple and rapid indirect spectrophotometric method for determination of methamidophos in water, soil and vegetable samples has been described. Methamidophos reacts with acid produced from p-dimethylaminobenzaldehyde (p-DMAB as a result of Cannizaro’s reaction. The resultant adduct undergoes condensation reaction in acidic medium forming a yellow colored product. Absorbance of the colored product was measured at 405 nm and pH 3 against a reagent blank. The Beer’s law range is obeyed in the range 1-30 µg mL-1 with molar absorptivity of 2.8 ×103 L mol-1 cm-1. The limit of detection and quantification were found to be 0.20±0.03 and 0.60±0.04 µg mL-1 respectively. The proposed method was effectively applied for determination of methamidophos in various samples with percent recoveries in the range of 96±0.08 to 102±0.06 %.

Kinetic and thermodynamic study of the reaction catalyzed by glucose-6-phosphate dehydrogenase with nicotinamide adenine dinucleotide

International Nuclear Information System (INIS)

Martin del Campo, Julia S.; Patino, Rodrigo

2011-01-01

Research highlights: → The reaction catalyzed by one enzyme of the pentose phosphate pathway was studied. → A spectrophotometric method is proposed for kinetic and thermodynamic analysis. → The pH and the temperature influences are reported on physical chemical properties. → Relative concentrations of substrates are also important in the catalytic process. - Abstract: The enzyme glucose-6-phosphate dehydrogenase (G6PD, EC 1.1.1.49) from Leuconostoc mesenteroides has a dual coenzyme specificity with oxidized nicotinamide adenine dinucleotide (NAD ox ) and oxidized nicotinamide adenine dinucleotide phosphate as electron acceptors. The G6PD coenzyme selection is determined by the metabolic cellular prevailing conditions. In this study a kinetic and thermodynamic analysis is presented for the reaction catalyzed by G6PD from L. mesenteroides with NAD ox as coenzyme in phosphate buffer. For this work, an in situ spectrophotometric technique was employed based on the detection of one product of the reaction. Substrate and coenzyme concentrations as well as temperature and pH effects were evaluated. The apparent equilibrium constant, the Michaelis constant, and the turnover number were determined as a function of each experimental condition. The standard transformed Gibbs energy of reaction was determined from equilibrium constants at different initial conditions. For the product 6-phospho-D-glucono-1,5-lactone, a value of the standard Gibbs energy of formation is proposed, Δ f G o = -1784 ± 5 kJ mol -1 .

Kinetic and thermodynamic study of the reaction catalyzed by glucose-6-phosphate dehydrogenase with nicotinamide adenine dinucleotide

Energy Technology Data Exchange (ETDEWEB)

Martin del Campo, Julia S. [Departamento de Fisica Aplicada, Centro de Investigacion y de Estudios Avanzados - Unidad Merida, Carretera antigua a Progreso Km. 6, A.P. 73 Cordemex, 97310, Merida, Yucatan (Mexico); Patino, Rodrigo, E-mail: rtarkus@mda.cinvestav.mx [Departamento de Fisica Aplicada, Centro de Investigacion y de Estudios Avanzados - Unidad Merida, Carretera antigua a Progreso Km. 6, A.P. 73 Cordemex, 97310, Merida, Yucatan (Mexico)

2011-04-20

Research highlights: {yields} The reaction catalyzed by one enzyme of the pentose phosphate pathway was studied. {yields} A spectrophotometric method is proposed for kinetic and thermodynamic analysis. {yields} The pH and the temperature influences are reported on physical chemical properties. {yields} Relative concentrations of substrates are also important in the catalytic process. - Abstract: The enzyme glucose-6-phosphate dehydrogenase (G6PD, EC 1.1.1.49) from Leuconostoc mesenteroides has a dual coenzyme specificity with oxidized nicotinamide adenine dinucleotide (NAD{sub ox}) and oxidized nicotinamide adenine dinucleotide phosphate as electron acceptors. The G6PD coenzyme selection is determined by the metabolic cellular prevailing conditions. In this study a kinetic and thermodynamic analysis is presented for the reaction catalyzed by G6PD from L. mesenteroides with NAD{sub ox} as coenzyme in phosphate buffer. For this work, an in situ spectrophotometric technique was employed based on the detection of one product of the reaction. Substrate and coenzyme concentrations as well as temperature and pH effects were evaluated. The apparent equilibrium constant, the Michaelis constant, and the turnover number were determined as a function of each experimental condition. The standard transformed Gibbs energy of reaction was determined from equilibrium constants at different initial conditions. For the product 6-phospho-D-glucono-1,5-lactone, a value of the standard Gibbs energy of formation is proposed, {Delta}{sub f}G{sup o} = -1784 {+-} 5 kJ mol{sup -1}.

Simultaneous determination of atorvastatin calcium and olmesartan medoxomil in a pharmaceutical formulation by reversed phase high-performance liquid chromatography, high-performance thin-layer chromatography, and UV spectrophotometric methods.

Science.gov (United States)

Soni, Hiral; Kothari, Charmy; Khatri, Deepak; Mehta, Priti

2014-01-01

Validated RP-HPLC, HPTLC, and UV spectrophotometric methods have been developed for the simultaneous determination of atorvastatin calcium (ATV) and olmesartan medoxomil (OLM) in a pharmaceutical formulation. The RP-HPLC separation was achieved on a Kromasil C18 column (250 x 4.6 mm, 5 microm particle size) using 0.01 M potassium dihydrogen o-phosphate (pH 4 adjusted with o-phosphoric acid)-acetonitrile (50 + 50, v/v) as the mobile phase at a flow rate of 1.5 mL/min. Quantification was achieved by UV detection at 276 nm. The HPTLC separation was achieved on precoated silica gel 60F254 plates using chloroform-methanol-acetonitrile (4 + 2+ 4, v/v/v) mobile phase. Quantification was achieved with UV detection at 276 nm. The UV-Vis spectrophotometric method was based on the simultaneous equation method that involves measurement of absorbance at two wavelengths, i.e., 255 nm (lambda max of OLM) and 246.2 nm (lambda max of ATV) in methanol. All three methods were validated as per International Conference on Harmonization guidelines. The proposed methods were simple, precise, accurate, and applicable for the simultaneous determination of ATV and OLM in a marketed formulation. The results obtained by applying the proposed methods were statistically analyzed and were found satisfactory.

Spectrophotometric determination of substrate-borne polyacrylamide.

Science.gov (United States)

Lu, Jianhang; Wu, Laosheng

2002-08-28

Polyacrylamides (PAMs) have wide application in many industries and in agriculture. Scientific research and industrial applications manifested a need for a method that can quantify substrate-borne PAM. The N-bromination method (a PAM analytical technique based on N-bromination of amide groups and spectrophotometric determination of the formed starch-triiodide complex), which was originally developed for determining PAM in aqueous solutions, was modified to quantify substrate-borne PAM. In the modified method, the quantity of substrate-borne PAM was converted to a concentration of starch-triiodide complex in aqueous solution that was then measured by spectrophotometry. The method sensitivity varied with substrates due to sorption of reagents and reaction intermediates on the substrates. Therefore, separate calibration for each substrate was required. Results from PAM samples in sand, cellulose, organic matter burnt soils, and clay minerals showed that this method had good accuracy and reproducibility. The PAM recoveries ranged from 95.8% to 103.7%, and the relative standard deviations (n = 4) were application and facilitating PAM-related research.

Spectrophotometric-isotope dilution determination of arsenic in soils and rock

Science.gov (United States)

Brown, F.W.; Simon, F.O.; Greenland, L.P.

1975-01-01

Arsenic in soil and rock samples may be determined in part-per-million concentrations using a radiochemical-isotope dilution method. Arsenic in the sample plus added As76 tracer is separated as arsine and determined spectrophotometrically as a molybdenum blue complex. The As76 activity in the absorbing solution allows corrections for chemical losses. A lower limit of 1 ppm is determinate in a 0.5-g sample.

Spectrophotometric Method for Determination of Five 1,4-Dihydropyridine Drugs Using N-Bromosuccinimide and Indigo Carmine Dye

Directory of Open Access Journals (Sweden)

Mohamed A. El Hamd

2013-01-01

Full Text Available Indirect spectrophotometric method is described for quantification of five of 1,4-dihydropyridine (1,4-DHP drugs using N-bromosuccinimide (NBS with the aid of indigo carmine (INC dye. The method is based on addition of known excess of NBS to an acidified solution of 1,4-DHP drugs and determining the residual of NBS through its ability to bleach the colour of the used dye; the amount of NBS that reacted corresponded to the amount of drugs. Beer’s law is obeyed in the concentration range 1.25–13.00 μg/mL. Good correlation coefficients (0.998-0.999 were found between the absorbance values and the corresponding concentrations. Limits of detections ranged from 0.141 to 0.500 μg/mL. The proposed method was successfully applied to the analysis of dosage forms; percent of recoveries ranged from 97.31 to 99.46% without interference from any common excipients. The statistical comparison by Student’s t-test and variance ratio F-test showed no significant difference between the proposed and official or reported methods.

Spectrophotometric determination of Sn+2 in lyophilized kit for labeling with 99mTc

International Nuclear Information System (INIS)

Araujo, Elaine Bortoleti; Sampel, Carolina Judith; Melo, Ivani Bortoleti; Okamoto, Miriam R.Y; Silva, Constancia P.G

2004-01-01

The preparation of 99 mTc labeled radiopharmaceuticals depends on the reduction of the technetium pertechnetate, commonly by stannous chloride (SnCl 2 ). The determination of the Sn +2 contents in the lyophilized preparations represents an important quality control procedure that may be applied to the process and to the final product. The objective os this work is the optimization of an spectrophotometric assay to the determination os Sn +2 contents in a citrate-stannous lyophilized kit for 99 mTc labeling. The spectrophotometric methodology employed is based in the colour development when Sn +2 reacts with sodium molybdate in the presence of potasium thiocyanate in chloridric medium. The colourfull reaction studied showed high stability after 60 minutes of the mixtures preparation. The sequence of reagents introduction in the reaction mixture was determinant to the assay. The molibdenium-stannous-tiocianate sequence produces calibration curves with good correlations (R2 ≥ 0.99). The concentrations of the molibdenium solution was also studied, in order to determine a ideal concentration for the Sn +2 range. The spectrophotometric method studied was usefull to the determination of Sn +2 content in different batches of citrate-stannous preparations. The method was fast and easy and can be applied to different stages of the production process, in order to guarantee the content of Sn +2 in the preparations (Au)

Spectrophotometric study of holmium complexation in KOH solutions at 25 Deg C

International Nuclear Information System (INIS)

Stepanchikova, S.A.; Bitejkina, R.P.

2006-01-01

Complexation of Ho 3+ in solutions of HoCl 3 and KOH at 25 Deg C is studied by indicator spectrophotometric method. Within the range of pH 9.25-10.10 and μ≤4 x 10 -4 stability constants of Ho 3+ hydroxocomplexes are measured and are extrapolated on zero ion strength [ru

Kinetics of tetravalent plutonium oxidation by cerium (4)

Energy Technology Data Exchange (ETDEWEB)

Nikitina, G P; Shumakov, V G; Egorova, V P

1975-01-01

Stoichiometry and kinetics of the Pu(4) + Ce(4) reaction is studied by spectrophotometric method at 5-30 deg C in nitric acid solutions (..mu..=(HNO/sub 3/)+(NaNO/sub 3/) = 1.0 - 5.7; (Ce(4)) = 5.10/sup -5/ - 1.2.10/sup -3/ g-ion/1, (Pu(4)) =1.10/sup -5/ - 8.5.10/sup -4/ g-ion/1. Oxidation of one Pu(4) ion to a hexavalent state requires two Ce(4) ions. The plutonium oxidation is not complicated by by-processes. Reverse Ce(3) + PuO/sub 2//sup +/ reaction does not contribute essentially to the process at (Ce(3)) 2.6.10/sup -2/ g-ion/1. The reaction rate obeys the kinetic equation - d(Pu(4))/dt = ksub(eff)(Pu(4))(Ce(4))/a sub(+-HNO/sub 3/). The thermodynamical activation parameters are found for solutions at the varied nitric acid concentrations:..delta..Gsup(not equal) = 17.0+-0.2 and ..delta..Hsup(not equal) = 21.8+-2 kcal/mole(..mu..=1.0); ..delta..Gsup(not equal) = 19.1+-0.1 and ..delta..Hsup(not equal) = 23.1+-1 kcal/mole(..mu..=4.9). The reaction mechanism is discussed in terms of the theory of absolute reaction rates and the model of long-range charge transfer.

Prediction of free turbulent mixing using a turbulent kinetic energy method

Science.gov (United States)

Harsha, P. T.

1973-01-01

Free turbulent mixing of two-dimensional and axisymmetric one- and two-stream flows is analyzed by a relatively simple turbulent kinetic energy method. This method incorporates a linear relationship between the turbulent shear and the turbulent kinetic energy and an algebraic relationship for the length scale appearing in the turbulent kinetic energy equation. Good results are obtained for a wide variety of flows. The technique is shown to be especially applicable to flows with heat and mass transfer, for which nonunity Prandtl and Schmidt numbers may be assumed.

Spectrophotometric determination of catecholamine using vanadium and eriochrome cyanine r

International Nuclear Information System (INIS)

Nagaraja, Padmarajaiah; Shrestha, Ashwinee Kumar; Shivakumar, Anantharaman; Al-Tayar, Naef Ghallab Saeed; Gowda, Avinask K.

2011-01-01

highly sensitive spectrophotometric method for the analysis of catecholamine drugs; L-dopa and methyldopa, is described. The analysis is based on the reaction of drug molecules with vanadium (V) which is reduced to vanadium (IV) and form complex with eriochrome cyanine R to give products having maximum absorbance (λ max ) at 565 nm. Beer's law is obeyed in the range 0.028-0.84 and 0.099-0.996 μg mL -1 for L-dopa and methyldopa, respectively. The statistical analysis as well as comparison with reported methods demonstrated high precision and accuracy of the proposed method. The method was successfully applied in the analysis of pharmaceutical preparations. (author)

Spectro-photometric determinations of Mn, Fe and Cu in aluminum master alloys

Science.gov (United States)

Rehan; Naveed, A.; Shan, A.; Afzal, M.; Saleem, J.; Noshad, M. A.

2016-08-01

Highly reliable, fast and cost effective Spectro-photometric methods have been developed for the determination of Mn, Fe & Cu in aluminum master alloys, based on the development of calibration curves being prepared via laboratory standards. The calibration curves are designed so as to induce maximum sensitivity and minimum instrumental error (Mn 1mg/100ml-2mg/100ml, Fe 0.01mg/100ml-0.2mg/100ml and Cu 2mg/100ml-10mg/ 100ml). The developed Spectro-photometric methods produce accurate results while analyzing Mn, Fe and Cu in certified reference materials. Particularly, these methods are suitable for all types of Al-Mn, Al-Fe and Al-Cu master alloys (5%, 10%, 50% etc. master alloys).Moreover, the sampling practices suggested herein include a reasonable amount of analytical sample, which truly represent the whole lot of a particular master alloy. Successive dilution technique was utilized to meet the calibration curve range. Furthermore, the workout methods were also found suitable for the analysis of said elements in ordinary aluminum alloys. However, it was observed that Cush owed a considerable interference with Fe, the later one may not be accurately measured in the presence of Cu greater than 0.01 %.

The kinetics of colour change in textiles and fibres treated with detergent solutions Part II - Spectrophotometric measurements.

Science.gov (United States)

Was-Gubala, Jolanta; Grzesiak, Edyta

2010-06-01

The aim of this study was to assess colour variations that occur in several types of textiles and their constituent fibres, resulting from the long-term influence of various laundry detergents. A 14-day experiment was conducted using blue, red and grey/black cotton, wool, acrylic and polyester textiles. The spectrophotometric measurement of colour changes in fabric samples and test solutions, as well as the microspectrophotometric analysis of colour changes in single fibres were described. An evaluation of the observed colour changes from a forensic fibre analysis expert's point of view, as well as that of an average user/consumer of the textiles and laundry detergents is also provided. Copyright 2009 Forensic Science Society. Published by Elsevier Ireland Ltd. All rights reserved.

Extractive spectrophotometric determination of uranium with malachite green

International Nuclear Information System (INIS)

Dubey, S.C.; Nadkarni, M.N.

1977-01-01

A sensitive spectrophotometric method based on the extraction of a uranium-benzoate-Malachite Green complex by chlorobenzene is described. The absorption maximum is at 635 nm and the molar absorptivity is 8.3 x 10 4 1. mole -1 cm -1 . A preliminary separation of uranium by extraction with methyl isobutyl ketone from acid-deficient aluminium nitrate solution is used to avoid interferences. An aliquot of the extract in then diluted with chlorobenzene and shaken with benzoate buffer containing Malachite Green (MG). The method has been applied for the determination of uranium in a synthetic leach solution. The complex extracted is probably [U0 2 (C 6 H 5 C00 3 - ][MG + ]. (author)

Extraction spectrophotometric analyzer

International Nuclear Information System (INIS)

Batik, J.; Vitha, F.

1985-01-01

Automation is discussed of extraction spectrophotometric determination of uranium in a solution. Uranium is extracted from accompanying elements in an HCl medium with a solution of tributyl phosphate in benzene. The determination is performed by measuring absorbance at 655 nm in a single-phase ethanol-water-benzene-tributyl phosphate medium. The design is described of an analyzer consisting of an analytical unit and a control unit. The analyzer performance promises increased productivity of labour, improved operating and hygiene conditions, and mainly more accurate results of analyses. (J.C.)

Microchemical analysis of materials based on Y-Ba-Cu by spectrophotometric titration

International Nuclear Information System (INIS)

Kuznetsov, V.V.; Samorukova, O.L.; Zakharov, Eh.K.

1990-01-01

A complex method for analysis of superconductor and similar materials on Y-Ba-Cu basis has been developed, which comprises yttrium and copper determination by their indicator spectrophotometric titration by EDTA and/or complexone 4 in the presence of arsenazo 3. The use of complexone 4 is more favourable. Titration is carried out at λ=650 nm. The method has a sufficient accuracy, provides for rapid determination and does not reguire preliminary separation of components

Alanine dosimetry using a spectrophotometric ferric-xylenol orange complex readout

International Nuclear Information System (INIS)

Laere, K. van; Buysse, J.; Berkvens, P.

1989-01-01

The spectrophotometric dosimetric method using the indirect oxidation of ferrous ions after dissolution of irradiated DL-and L-alanine has been thoroughly investigated with respect to its composition, read-out procedure and dose-response. Optimal concentration of 0.10 N H 2 SO 4 , 0.2 mM xylenol orange and 0.2 mM Fe 2+ were found, giving an absorption maximum at 547 nm. Standardization of chemical processing procedures allows a reproducibility better than 0.5%. The useful dose range has been extended to 0.03-12 kGy by means of slightly different read-out procedure. The quantitative concept of ''indirect yield'', G id , was introduced for this procedure as a measure of the indirect oxidation capacity of the radicals. It was found to be G id,0 (Fe 3+ ) 7.1 ions/100 eV transferred into the alanine. The spectrophotometric readout combines the highly advantageous use of alanine as a dosemeter with the straightforwardness, accuracy and low costs of the chemical procedure. (author)

Entry of Nd+3 ions into the LiYF4 matrix and determination of Nd+3 concentration by the nondestructing spectrophotometric method

International Nuclear Information System (INIS)

Tkachuk, A.M.; Poletimova, A.V.; Petrova, M.A.; Egorov, V.Yu.; Korolev, N.E.

1991-01-01

Entering of Nd 3+ ions into LiYF 4 lattice was investigation. Nondestructive spectrophotometric method for determining activator concentration in the crystal was developed. It enables to determine both the average integral concentration in the active element. Absorption cross sections were determined for a series of reference lines λ i with the lowest polarization degree. Values of β(λ i ) coefficients, enabling to determine the average neodymium concentration in the sample, are presented. Coefficient of neodymium entering into LiYF 4 lattice was determined: K nd =0.31+-0.02

OPTIMIZING CONDITIONS FOR SPECTROPHOTOMETRIC DETERMINATION OF TOTAL POLYPHENOLS IN WINES USING FOLIN-CIOCALTEU REAGENT

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Daniel Bajčan

2013-02-01

Full Text Available Wine is a complex beverage that obtains its properties mainly due to synergistic effect of alcohol, organic acids, arbohydrates, as well as the phenolic and aromatic substances. At present days, we can observe an increased interest in the study of polyphenols in wines that have antioxidant, antimicrobial, anti-inflammatory, anti-cancer and many other beneficial effects. Moderate and regular consumption of the red wine especially, with a high content of phenolic compounds, has a beneficial effect on human health. The aim of this work was to optimize conditions for spectrophotometric determination of total polyphenols in winwas to optimize conditions for spectrophotometric determination of total polyphenols in winwas to optimize conditions for spectrophotometric determination of total polyphenols in winwas to optimize conditions for pectrophotometric determination of total polyphenols in wine using Folin-Ciocaulteu reagent. Based on several studies, in order to minimize chemical use and optimize analysis time, we have proposed a method for the determination of total polyphenols using 0.25 ml Folin-Ciocaulteu reagent, 3 ml of 20% Na2CO3 solution and time of coloring complex 1.5 hour. We f

Spectrophotometric studies of transcurium element halides and oxyhalides in the solid state

International Nuclear Information System (INIS)

Young, J.P.; Haire, R.G.; Fellows, R. L.; Peterson, J.R.

1978-01-01

The present state of a microscale spectrophotometric technique is described. The application of spectrophotometry to transcurium elements (Bk, Cf, Es) requires some rather specialized microtechniques for the following reasons: only small amounts of these elements are available; their radioactivity makes the use of μg-sized samples desirable; and spectral study of solids requires thin samples. A schematic diagram of the microscope-spectrophotometer used for spectrophotometric study of the transcurium element compounds is shown. The spectrophotometer, of local design, consists of two microscopes equipped with Cassegrainian reflecting microscope objective lenses, a quartz field lens, and a Jarrell Ash 1/2 meter scanning monochromator equipped with a 1180 line/mm grating blazed at 4000 A. The photomultiplier used in this system is an S-1 type RCA 7102 operated at approximately -50 deg C. This grating-photomultiplier combination provides a continuous response free of discontinuities over the useful wavelength range of the system from 3000 to 11 000 A. The microscope-spectrophotometer is a single beam instrument. Each spectral trace is registered as photomultiplier current on a strip chart recorder. In order to obtain true absorption spectra, however, the output from the photometer is also simultaneously digitized for on-line processing. The unique advantages of applying both spectrophotometric and X-ray powder diffraction methods on the sample, in order to identify and characterize newly synthesized compounds, are also discussed. (T.G.)

A Simple Spectrophotometric Method for the Determination of Copper in Some Real, Environmental, Biological, Food and Soil Samples Using Salicylaldehyde Benzoyl Hydrazone

Directory of Open Access Journals (Sweden)

M. Jamaluddin Ahmed

2012-06-01

Full Text Available A very simple, ultra-sensitive, highly selective and non-extractive spectrophotometric method for the determination of trace amounts copper(II has been developed. Salicylaldehy debenzoyl hydrazone (SAL-BH has been proposed as a new analytical reagent for the direct non-extractive spectrophotometric determination of copper(II. SAL-BH reacts with copper in a slightly acidic (0.0001-0.005 M H2SO4 in 40% 1,4-dioxane media with copper(II to give a highly absorbent greenish yellow chelate with a molar ratio 1:1(CuII: SAL-BH The reaction is instantaneous and the maximum absorption was obtained at 404 nm and remains stable for 72 h. The average molar absorptivity and Sandell’s sensitivity were found to be 1.4×105 L mol-1 cm-1 and 5.0 ng cm-2 of copper(II, respectively. Linear calibration graphs were obtained for 0.01 – 18 mg L-1 of CuII. The detection limit and quantification limit of the reaction system were found to be 1 ng mL-1 and 10 µg L-1, respectively. A large excess of over 50 cations, anions and complexing agents (e.g., tartrate, oxalate, citrate, phosphate, thiocyanate etc. do not interfere in the determination. The method is highly selective for copper and was successfully used for the determination of copper in several standard reference materials (steels and alloys as well as in some environmental waters (portable and polluted, biological (human blood and urine, food and soil samples and solutions containing both copper(I and copper(II as well as some complex synthetic mixtures. The results of the proposed method for biological and food samples were comparable with AAS and were found to be in good agreement. The method has high precision and accuracy (s = ± 0.01 for 0.5 mg L-1.

Microwave-assisted of dispersive liquid-liquid microextraction and spectrophotometric determination of uranium after optimization based on Box-Behnken design and chemometrics methods

Science.gov (United States)

Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

2015-01-01

In this study an analytical procedure based on microwave-assisted dispersive liquid-liquid microextraction (MA-DLLME) and spectrophotometric coupled with chemometrics methods is proposed to determine uranium. In the proposed method, 4-(2-pyridylazo) resorcinol (PAR) is used as a chelating agent, and chloroform and ethanol are selected as extraction and dispersive solvent. The optimization strategy is carried out by using two level full factorial designs. Results of the two level full factorial design (24) based on an analysis of variance demonstrated that the pH, concentration of PAR, amount of dispersive and extraction solvents are statistically significant. Optimal condition for three variables: pH, concentration of PAR, amount of dispersive and extraction solvents are obtained by using Box-Behnken design. Under the optimum conditions, the calibration graphs are linear in the range of 20.0-350.0 ng mL-1 with detection limit of 6.7 ng mL-1 (3δB/slope) and the enrichment factor of this method for uranium reached at 135. The relative standard deviation (R.S.D.) is 1.64% (n = 7, c = 50 ng mL-1). The partial least squares (PLS) modeling was used for multivariate calibration of the spectrophotometric data. The orthogonal signal correction (OSC) was used for preprocessing of data matrices and the prediction results of model, with and without using OSC, were statistically compared. MA-DLLME-OSC-PLS method was presented for the first time in this study. The root mean squares error of prediction (RMSEP) for uranium determination using PLS and OSC-PLS models were 4.63 and 0.98, respectively. This procedure allows the determination of uranium synthesis and real samples such as waste water with good reliability of the determination.

Microwave-assisted of dispersive liquid-liquid microextraction and spectrophotometric determination of uranium after optimization based on Box-Behnken design and chemometrics methods.

Science.gov (United States)

Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

2015-01-25

In this study an analytical procedure based on microwave-assisted dispersive liquid-liquid microextraction (MA-DLLME) and spectrophotometric coupled with chemometrics methods is proposed to determine uranium. In the proposed method, 4-(2-pyridylazo) resorcinol (PAR) is used as a chelating agent, and chloroform and ethanol are selected as extraction and dispersive solvent. The optimization strategy is carried out by using two level full factorial designs. Results of the two level full factorial design (2(4)) based on an analysis of variance demonstrated that the pH, concentration of PAR, amount of dispersive and extraction solvents are statistically significant. Optimal condition for three variables: pH, concentration of PAR, amount of dispersive and extraction solvents are obtained by using Box-Behnken design. Under the optimum conditions, the calibration graphs are linear in the range of 20.0-350.0 ng mL(-1) with detection limit of 6.7 ng mL(-1) (3δB/slope) and the enrichment factor of this method for uranium reached at 135. The relative standard deviation (R.S.D.) is 1.64% (n=7, c=50 ng mL(-1)). The partial least squares (PLS) modeling was used for multivariate calibration of the spectrophotometric data. The orthogonal signal correction (OSC) was used for preprocessing of data matrices and the prediction results of model, with and without using OSC, were statistically compared. MA-DLLME-OSC-PLS method was presented for the first time in this study. The root mean squares error of prediction (RMSEP) for uranium determination using PLS and OSC-PLS models were 4.63 and 0.98, respectively. This procedure allows the determination of uranium synthesis and real samples such as waste water with good reliability of the determination. Copyright © 2014. Published by Elsevier B.V.

Spectrophotometric determination of boron in water with prior distillation and hydrolysis of the methyl borate

International Nuclear Information System (INIS)

Monzo, J.; Pomares, F.; Guardia, M. de la

1988-01-01

A procedure for the determination of boron in irrigation waters is proposed, involving the prior distillation and hydrolysis of methyl borate and subsequent spectrophotometric determination with azomethine-H. The selectivity is better than that of the direct analysis method. (author)

Spectrophotometric Determination of Phenolic Antioxidants in the Presence of Thiols and Proteins

Directory of Open Access Journals (Sweden)

Aslı Neslihan Avan

2016-08-01

Full Text Available Development of easy, practical, and low-cost spectrophotometric methods is required for the selective determination of phenolic antioxidants in the presence of other similar substances. As electron transfer (ET-based total antioxidant capacity (TAC assays generally measure the reducing ability of antioxidant compounds, thiols and phenols cannot be differentiated since they are both responsive to the probe reagent. In this study, three of the most common TAC determination methods, namely cupric ion reducing antioxidant capacity (CUPRAC, 2,2′-azinobis(3-ethylbenzothiazoline-6-sulfonic acid diammonium salt/trolox equivalent antioxidant capacity (ABTS/TEAC, and ferric reducing antioxidant power (FRAP, were tested for the assay of phenolics in the presence of selected thiol and protein compounds. Although the FRAP method is almost non-responsive to thiol compounds individually, surprising overoxidations with large positive deviations from additivity were observed when using this method for (phenols + thiols mixtures. Among the tested TAC methods, CUPRAC gave the most additive results for all studied (phenol + thiol and (phenol + protein mixtures with minimal relative error. As ABTS/TEAC and FRAP methods gave small and large deviations, respectively, from additivity of absorbances arising from these components in mixtures, mercury(II compounds were added to stabilize the thiol components in the form of Hg(II-thiol complexes so as to enable selective spectrophotometric determination of phenolic components. This error compensation was most efficient for the FRAP method in testing (thiols + phenols mixtures.

Study of imidaclopride removal from aqueous solution by adsorption onto granular activated carbon using an on-line spectrophotometric analysis system

International Nuclear Information System (INIS)

Daneshvar, N.; Aber, S.; Khani, A.; Khataee, A.R.

2007-01-01

The removal of imidaclopride as a pesticide by granular activated carbon (GAC) and its adsorption kinetics were studied at different pH values and temperatures. In all experiments, the amount of GAC and initial concentration of imidaclopride were 2 g and 25 ppm, respectively. The adsorption process was followed by an on-line spectrophotometric analysis system, which consisted of UV-spectrophotometer, a designed absorption cell, peristaltic pump and special glassy reactor. The effect of pH and temperature on adsorption was studied over 90 min adsorption periods. The obtained data were treated according to various kinetic models. The results showed that second order model was the most suitable one on the overall. The our results also showed that the adsorption rate constants for first order, second order and intraparticle diffusion models followed decreasing order: pH = 7 > 4 > 10 > 1, T = 25 > 35 > 45 > 55 deg. C

Study of imidaclopride removal from aqueous solution by adsorption onto granular activated carbon using an on-line spectrophotometric analysis system

Energy Technology Data Exchange (ETDEWEB)

Daneshvar, N. [Water and Wastewater Treatment Research Laboratory, Department of Applied Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: nezam_daneshvar@yahoo.com; Aber, S. [Water and Wastewater Treatment Research Laboratory, Department of Applied Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: soheil_aber@yahoo.com; Khani, A. [Water and Wastewater Treatment Research Laboratory, Department of Applied Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: alikhani_chemwt@yahoo.com; Khataee, A.R. [Water and Wastewater Treatment Research Laboratory, Department of Applied Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz (Iran, Islamic Republic of)]. E-mail: ar_khataee@yahoo.com

2007-06-01

The removal of imidaclopride as a pesticide by granular activated carbon (GAC) and its adsorption kinetics were studied at different pH values and temperatures. In all experiments, the amount of GAC and initial concentration of imidaclopride were 2 g and 25 ppm, respectively. The adsorption process was followed by an on-line spectrophotometric analysis system, which consisted of UV-spectrophotometer, a designed absorption cell, peristaltic pump and special glassy reactor. The effect of pH and temperature on adsorption was studied over 90 min adsorption periods. The obtained data were treated according to various kinetic models. The results showed that second order model was the most suitable one on the overall. The our results also showed that the adsorption rate constants for first order, second order and intraparticle diffusion models followed decreasing order: pH = 7 > 4 > 10 > 1, T = 25 > 35 > 45 > 55 deg. C.

Spectrophotometric Determination Of Heavy Metals In Cosmetics

African Journals Online (AJOL)

ISSN 1597-6343. Spectrophotometric Determination Of Heavy Metals In Cosmetics ... analysed using atomic absorption spectrophotometer – coupled with a hydride ... presence of arsenic (As), mercury (Hg), cadmium (Cd) and lead. (Pb) in ...

Receptor binding kinetics equations: Derivation using the Laplace transform method.

Science.gov (United States)

Hoare, Sam R J

Measuring unlabeled ligand receptor binding kinetics is valuable in optimizing and understanding drug action. Unfortunately, deriving equations for estimating kinetic parameters is challenging because it involves calculus; integration can be a frustrating barrier to the pharmacologist seeking to measure simple rate parameters. Here, a well-known tool for simplifying the derivation, the Laplace transform, is applied to models of receptor-ligand interaction. The method transforms differential equations to a form in which simple algebra can be applied to solve for the variable of interest, for example the concentration of ligand-bound receptor. The goal is to provide instruction using familiar examples, to enable investigators familiar with handling equilibrium binding equations to derive kinetic equations for receptor-ligand interaction. First, the Laplace transform is used to derive the equations for association and dissociation of labeled ligand binding. Next, its use for unlabeled ligand kinetic equations is exemplified by a full derivation of the kinetics of competitive binding equation. Finally, new unlabeled ligand equations are derived using the Laplace transform. These equations incorporate a pre-incubation step with unlabeled or labeled ligand. Four equations for measuring unlabeled ligand kinetics were compared and the two new equations verified by comparison with numerical solution. Importantly, the equations have not been verified with experimental data because no such experiments are evident in the literature. Equations were formatted for use in the curve-fitting program GraphPad Prism 6.0 and fitted to simulated data. This description of the Laplace transform method will enable pharmacologists to derive kinetic equations for their model or experimental paradigm under study. Application of the transform will expand the set of equations available for the pharmacologist to measure unlabeled ligand binding kinetics, and for other time

Discussion of the Investigation Method on the Reaction Kinetics of Metallurgical Reaction Engineering

Science.gov (United States)

Du, Ruiling; Wu, Keng; Zhang, Jiazhi; Zhao, Yong

Reaction kinetics of metallurgical physical chemistry which was successfully applied in metallurgy (as ferrous metallurgy, non-ferrous metallurgy) became an important theoretical foundation for subject system of traditional metallurgy. Not only the research methods were very perfect, but also the independent structures and systems of it had been formed. One of the important tasks of metallurgical reaction engineering was the simulation of metallurgical process. And then, the mechanism of reaction process and the conversion time points of different control links should be obtained accurately. Therefore, the research methods and results of reaction kinetics in metallurgical physical chemistry were not very suitable for metallurgical reaction engineering. In order to provide the definite conditions of transmission, reaction kinetics parameters and the conversion time points of different control links for solving the transmission and reaction equations in metallurgical reaction engineering, a new method for researching kinetics mechanisms in metallurgical reaction engineering was proposed, which was named stepwise attempt method. Then the comparison of results between the two methods and the further development of stepwise attempt method were discussed in this paper. As a new research method for reaction kinetics in metallurgical reaction engineering, stepwise attempt method could not only satisfy the development of metallurgical reaction engineering, but also provide necessary guarantees for establishing its independent subject system.

Development of a derivative spectrophotometric method for the determination of fungicide zinc ethylenebisdithiocarbamate using sodium molybdate

International Nuclear Information System (INIS)

Kaur, Manpreet; Kaur, Varinder; Malik, Ashok K.; Singh, Baldev; Rao, A.L.J.; Verma, Neelam

2009-01-01

A derivative spectrophotometric procedure was developed for the determination of zinc(II) ethylenebisdithiocarbamate, Zineb, after formation of its blue colored complex with sodium molybdate in acidic medium. The Beer's law is obeyed up to 40 μg mL -1 of Zineb at 956 nm. The detection limit was 0.006 μg mL -1 for Zineb when S/N ratio is 3 taking into account various parameters, such as the effect of acid concentration. The interference of a large number of ions on the determination of Zineb was evaluated. Most of the alkaline metals and metal salts did not interfere. The procedure presented proper sensitivity and it was applied for determining Zineb in food stuffs and commercial samples of Dithane Z 78 and Hexathane 75% W.P.. Results were compared with earlier reported methods. Zineb was successfully determined without any interferences in the presence of other dithiocarbamates like Ziram, Thiram, Ferbam etc. (author)

A novel visible spectrophotometric method for the determination of ethamsylate in pharmaceutical preparations and biological samples

Science.gov (United States)

Zhang, Meiyun; Zhang, Yan; Li, Quanmin

2010-03-01

A highly sensitive visible spectrophotometric method has been developed to determine ethamsylate in this paper, which is based on using Cu(II) as spectroscopic probe reagent. The study indicates that in the presence of SCN - and KNO 3, Cu(II) is reduced to Cu(I) by ethamsylate at pH 5.0, and the in situ formed Cu(I) reacts with SCN - to form into the white emulsion CuSCN that could be stayed upon the surface of water. According to the amount of residual Cu(II), the amount of ethamsylate can be indirectly determined. Under the optimal conditions, Beer's law is applicable in the range of 0.2-9.0 μg/mL (7.60 × 10 -7-3.42 × 10 -5 mol/L) for aqueous standard solution of ethamsylate with linear correlation coefficient of 0.9998. The detection limit and relative standard deviation are 0.12 μg/mL and 1.5%, respectively. And the molar absorption coefficient of the indirect determination of ethamsylate is 1.0 × 10 5 L/mol cm. The method is successfully applied to determine ethamsylate in pharmaceutical preparations and biological samples.

Development of indirect spectrophotometric method for quantification of cephalexin in pure form and commercial formulation using complexation reaction

International Nuclear Information System (INIS)

Khan, M.N.; Hussain, R.; Kalsoom, S.; Saadiq, M.

2016-01-01

A simple, accurate and indirect spectrophotometric method was developed for the quantification of cephalexin in pure form and pharmaceutical products using complexation reaction. The developed method is based on the oxidation of the cephalexin with Fe/sup 3+/ in acidic medium. Then 1, 10- phenanthroline reacts with Fe/sup 2+/ and a red colored complex was formed. The absorbance of the complex was measured at 510 nm by spectrophotometer. Different experimental parameters affecting the complexation reactions were studied and optimized. Beer law was obeyed in the concentration range 0.4 -10 micro gmL/sup -1/ with a good correlation of 0.992. The limit of detection and limit of quantification were found to be 0.065 micro gmL/sup -1/ and 0.218 micro gmL/sup -1/ , respectively. The method have good reproducibility with a relative standard deviation of 6.26 percent (n = 6). The method was successfully applied for the determination of cephalexin in bulk powder and commercial formulation. Percent recoveries were found to range from 95.47 to 103.87 percent for the pure form and 98.62 to 103.35 percent for commercial formulations. (author)

Shedding light on food fraud: spectrophotometric and spectroscopic methods as a tool against economically motivated adulteration of food

Science.gov (United States)

Petronijević, R. B.; Velebit, B.; Baltić, T.

2017-09-01

Intentional modification of food or substitution of food ingredients with the aim of gaining profit is food fraud or economically motivated adulteration (EMA). EMA appeared in the food supply chain, and following the global expansion of the food market, has become a world-scale problem for the global economy. Food frauds have involved oils, milk and meat products, infant formula, honey, juices, spices, etc. New legislation was enacted in the last decade in order to fight EMA. Effective analytical methods for food fraud detection are few and still in development. The majority of the methods in common use today for EMA detection are time consuming and inappropriate for use on the production line or out of the laboratory. The next step in the evolution of analytical techniques to combat food fraud is development of fast, accurate methods applicable using portable or handheld devices. Spectrophotometric and spectroscopic methods combined with chemometric analysis, and perhaps in combination with other rapid physico-chemical techniques, could be the answer. This review discusses some analytical techniques based on spectrophotometry and spectroscopy, which are used to reveal food fraud and EMA.

Spectrophotometric characterization of hemozoin as a malaria biomarker

Science.gov (United States)

Silva, Ivo; Lima, Rui; Minas, Graça.; Catarino, Susana O.

2017-08-01

Malaria is a parasitic disease with more than a billion people worldwide at risk of contraction. The disease is predominantly widespread in regions with precarious healthcare conditions and resources. Despite the several available malaria diagnostic methods, only two are predominantly used in the field in malaria-endemic countries: microscopy and rapid diagnostic tests. In this work, an alternative diagnostic system is proposed, based on optical absorption spectrophotometry. The main objective of this paper is the spectrophotometric study of hemozoin as a malaria biomarker, since it is a sub-product of the malaria infection. The optical absorbance of hemoglobin and hemozoin solutions in purified water was measured in the visible spectrum range using a spectrophotometric setup. The results showed main absorbance peaks at 540 nm and 574 nm for hemoglobin, and at 672 nm for hemozoin. The tests performed in aqueous solutions have shown that both hemoglobin and synthetic hemozoin, when alone in solution, were detected by absorbance, with sensitivity of 0.05 g/L, and with a high linearity (R2> 0.92 for all wavelength peaks). Furthermore, it was found that the whole blood and the hemoglobin spectra have similar absorption peaks. By combining whole blood and synthetic hemozoin solutions, it was proved that both the hemozoin and the hemoglobin absorbance peaks could still be detected by spectrophotometry. For instance, in polydimethylsiloxane wells, the proposed method was able to detect hemozoin in whole blood samples for optical paths as low as 3 mm in cylindrical wells, thus proving the capability for this method's miniaturization. With this work, it is possible to conclude that hemozoin is a viable candidate as a biomarker for malaria detection by optical absorption spectrophotometry and also, that an autonomous, fully integrated and low cost miniaturized system, based on such a principle, could provide an efficient diagnosis of malaria.

Spectrophotometric determination of trace and ultratrace levels of boron in silicon and chlorosilane samples

International Nuclear Information System (INIS)

Chen, J.S.; Lin, H.M.; Yang, M.H.

1991-01-01

Spectrophotometric methods for the determination of boron in the low μg/g and ng/g range in high-purity silicon and dichloro- and trichlorosilanes were investigated in detail. The procedures established involve dissolution of silicon samples and the hydrolyzed products of chlorosilane samples in hydrofluoric acid-containing reagents followed by evaporation of the silicon matrix as H 2 SiF 6 . The boron retained in the treated sample solution was then determined by a spectrophotometric method using carminic acid as a chromatic reagent. Special effort has been paid to the control of the analytical blank and reproducible determination of boron. The results indicate that addition of mannitol and proper control of the evaporation process are effective in preventing volatilization of boron during the evaporation of silicon matrix and can thus attain high recovery of boron and reproducible analysis. Through meticulous control of the analytical blank and experimental conditions, the limit of detection for boron determination with the established method can be as low as ng/g levels. Application of the methods to the determination of boron in various stages of purification of silicon and trichlorosilane as well as in borophosphosilicate film was conducted. (orig.)

Spectrophotometric studies on complex formation of 5-nitro-3-sulpho-salicylic acid with niobium(V)

International Nuclear Information System (INIS)

Parmar, D.S.; Shivahare, G.C.

1975-01-01

5-nitro-3-sulpho-salicylic acid forms a yellow complex witn niobium(V) at pH 9.9 and the reaction has been successfully studied spectrophotometrically. The results of the Job's continuous variation method and the mole ratio method indicate a composition of 1:2 for the complex. Stability constant of the complex has also been determined. (author)

Spectrophotometric studies on complex formation of 5-nitro-3-sulpho-salicylic acid with niobium(V)

Energy Technology Data Exchange (ETDEWEB)

Parmar, D S; Shivahare, G C [Rajasthan Univ., Jaipur (India). Dept. of Chemistry

1975-11-01

5-nitro-3-sulpho-salicylic acid forms a yellow complex witn niobium(V) at pH 9.9 and the reaction has been successfully studied spectrophotometrically. The results of the Job's continuous variation method and the mole ratio method indicate a composition of 1:2 for the complex. Stability constant of the complex has also been determined.

Development and Validation of Spectrophotometric Methods for Simultaneous Estimation of Valsartan and Hydrochlorothiazide in Tablet Dosage Form

Directory of Open Access Journals (Sweden)

Monika L. Jadhav

2014-01-01

Full Text Available Two UV-spectrophotometric methods have been developed and validated for simultaneous estimation of valsartan and hydrochlorothiazide in a tablet dosage form. The first method employed solving of simultaneous equations based on the measurement of absorbance at two wavelengths, 249.4 nm and 272.6 nm, λmax for valsartan and hydrochlorothiazide, respectively. The second method was absorbance ratio method, which involves formation of Q-absorbance equation at 258.4 nm (isoabsorptive point and also at 272.6 nm (λmax of hydrochlorothiazide. The methods were found to be linear between the range of 5–30 µg/mL for valsartan and 4–24 μg/mL for hydrochlorothiazide using 0.1 N NaOH as solvent. The mean percentage recovery was found to be 100.20% and 100.19% for the simultaneous equation method and 98.56% and 97.96% for the absorbance ratio method, for valsartan and hydrochlorothiazide, respectively, at three different levels of standard additions. The precision (intraday, interday of methods was found within limits (RSD<2%. It could be concluded from the results obtained in the present investigation that the two methods for simultaneous estimation of valsartan and hydrochlorothiazide in tablet dosage form are simple, rapid, accurate, precise and economical and can be used, successfully, in the quality control of pharmaceutical formulations and other routine laboratory analysis.

Extractive spectrophotometric determination of uranium with malachite green

Energy Technology Data Exchange (ETDEWEB)

Dubey, S C; Nadkarni, M N [Bhabha Atomic Research Centre, Bombay (India). Fuel Reprocessing Div.

1977-04-01

A sensitive spectrophotometric method based on the extraction of a uranium-benzoate-Malachite Green complex by chlorobenzene is described. The absorption maximum is at 635 nm and the molar absorptivity is 8.3 x 10/sup 4/1. mole /sup -1/ cm/sup -1/. A preliminary separation of uranium by extraction with methyl isobutyl ketone from acid-deficient aluminium nitrate solution is used to avoid interferences. An aliquot of the extract in then diluted with chlorobenzene and shaken with benzoate buffer containing Malachite Green (MG). The method has been applied for the determination of uranium in a synthetic leach solution. The complex extracted is probably (U0/sub 2/(C/sub 6/H/sub 5/C00/sub 3//sup -/)(MG/sup +/).

Effect of the substitutional groups on the electrochemistry, kinetic of thermal decomposition and kinetic of substitution of some uranyl Schiff base complexes

Energy Technology Data Exchange (ETDEWEB)

Asadi, Zahra; Nasrollahi, Rahele; Ranjkeshshorkaei, Mohammad; Firuzabadi, Fahimeh Dehghani [Shiraz Univ. (Iran, Islamic Republic of). Chemistry Dept.; Dusek, Michal; Fejfarova, Karla [ASCR, Prague (Czech Republic). Inst. of Physics

2016-05-15

Uranyl(VI) complexes, [UO{sub 2}(X-saloph)(solvent)], where saloph denotes N,N{sup '}-bis(salicylidene)-1,2-phenylenediamine and X = NO{sub 2}, Cl, Me, H; were synthesized and characterized by 61H NMR, IR, UV-Vis spectroscopy, thermal gravimetry (TG), cyclic voltammetry, elemental analysis (C.H.N) and X-ray crystallography. X-ray crystallography of [UO{sub 2}(4-nitro-saloph)(DMF)] revealed coordination of the uranyl by the tetradentate Schiff base ligand and one solvent molecule, resulting in seven-coordinated uranium. The complex of [UO{sub 2}(4-nitro-saloph)(DMF)] was also synthesized in nano form. Transmission electron microscopy image showed nano-particles with sizes between 30 and 35 nm. The TG method and analysis of Coats-Redfern plots revealed that the kinetics of thermal decomposition of the complexes is of the first-order in all stages. The kinetics and mechanism of the exchange reaction of the coordinated solvent with tributylphosphine was investigated by spectrophotometric method. The second-order rate constants at four temperatures and the activation parameters showed an associative mechanism for all corresponding complexes with the following trend: 4-Nitro > 4-Cl > H > 4-Me. It was concluded that the steric and electronic properties of the complexes were important for the reaction rate. For analysis of anticancer properties of uranyl Schiff base complexes, cell culture and MTT assay was carried out. These results showed a reduction of jurkat cell line concentration across the complexes.

Determination of rhenium (7) trace amounts by spectrophotometric titration in medium of mixed solvents

International Nuclear Information System (INIS)

Kuznetsov, V.V.; Samorukova, O.L.

1978-01-01

The method has been proposed of determining rhenium (7) microamounts by spectrophotometric titration in the medium water-dimethyl-sulphoxide with the reagent nitrochromazo. The method is based on the formation of ionic pairs K + ReO 4 - in water-organic solvents. The results of rhenium determination are satisfactory in a wide concentration range up to 0.3 mkg in 15 ml which makes the method proposed close in sensitivity to photometric methods and much better in reproducibility

Uranium fluorides analysis. Titanium spectrophotometric determination

International Nuclear Information System (INIS)

Anon.

Titanium determination in uranium hexafluoride in the range 0.7 to 100 microgrammes after transformation of uranium fluoride in sulfate. Titanium is separated by extraction with N-benzoylphenylhydroxylamine, reextracted by hydrochloric-hydrofluoric acid. The complex titanium-N-benzoylphenylhydroxylamine is extracted by chloroform. Spectrophotometric determination at 400 nm [fr

HF effect on dissociation kinetics of plutonium and neptunium complexes with 1,2-diaminocyclohexanetetraacetic acid in nitric acid solutions

International Nuclear Information System (INIS)

Nikitina, S.A.; Stepanov, A.V.

1982-01-01

Dissociation kinetics of Pusup((4)) and Np sup((4)) complexes with DCTA were investigated in HNO 3 solutions in the presence of HF and arsenazo 3. It was found that HF or NaF produced a differentiating effect on the reactivity of the complexes at [HNO 3 ]=1-6 mol/l as well as inhibiting effect at [HNO 3 ]=0.01 mol/l. Conditions of the differential kinetic analysis of plutonium and neptunium in the mixture and differential spectrophotometric analysis of uranium (6) during the camouflage of neptunium (4) and plutonium (4) were determined

Anion-exchange enrichment and spectrophotometric determination of uranium in sea-water

International Nuclear Information System (INIS)

Kuroda, Rokuro; Oguma, Koichi; Mukai, Noriko; Iwamoto, Masatoshi

1987-01-01

A method is proposed for the determination of uranium in sea-water. The uranium is strongly sorbed on a strongly basic anion-exchange resin (Cl - form) from acidified sea-water containing sodium azide (0.3M) and is easily eluted with 1M hydrochloric acid. Uranium in the effluent can be determined spectrophotometrically with Arsenazo III. The combined method allows easy and selective determination of uranium in sea-water without using a sophisticated adsorbent. The overall recovery and precision are satisfactory at the 3 μg/1. level. (author)

Spectrophotometric retinal oximetry in pigs

DEFF Research Database (Denmark)

Traustason, Sindri; Kiilgaard, Jens Folke; Karlsson, Robert

2013-01-01

PURPOSE: To assess the validity of spectrophotometric retinal oximetry, by comparison to blood gas analysis and intra-vitreal measurements of partial pressure of oxygen (pO2). METHODS: Female domestic pigs were used for all experiments (n=8). Oxygen fraction in inspired air was changed using...... a mixture of room air, pure oxygen and pure nitrogen, ranging from 5% to 100% oxygen. Femoral arterial blood gas analysis and retinal oximetry was performed at each level of inspiratory oxygen fraction. Retinal oximetry was performed using a commercial instrument, the Oxymap Retinal Oximeter T1 (Oxymap ehf...... arterial oxygen saturation and the optical density ratio over retinal arteries revealed an approximately linear relationship (R(2) = 0.74, p = 3.4 x 10(-9)). In order to test the validity of applying the arterial calibration to veins, we compared non-invasive oximetry measurements to invasive pO2...

Selective determination of cyanide complexes of copper, zinc and cadmium in electrolytes by spectrophotometric titration

International Nuclear Information System (INIS)

Kuznetsov, V.V.; Korchagina, O.A.; Samorukova, O.L.

1986-01-01

Selective, sensitive and rapid method for determining Cd, Zn, Cu and their mixtures in cyanide electrolytes of galvanic bathes has been developed. Analysis is performed by means of indicator spectrophotometric titration with barium and strontium salts of cadmium cyanide complexes in organic-aqueous solvents

Spectrophotometric method for quantitative measuring essential oil in aromatic water and distillate with rose smell

International Nuclear Information System (INIS)

Semenova, E; Moiseeva, I; Presnyakova, V; Goncharov, D; Goncharov, M; Presnyakova, E; Presnyakov, S; Kolesnikova, S

2017-01-01

In this connection, we improved the express methods of determining the mixture of volatile aromatic substances by the spectrophotometry of aromatic water and steam distillate of essential oil raw materials (traditional or biotechnological with rose smell). Direct spectrophotometry of distillation water is impossible because it is a colloid of liquid oil and law is not observed. Therefore, it is necessary to dissolve 1 ml of distillate in ethanol in the ratio 1:4, in this case we take real solution with no lipophilic fall-out on the walls of cuvette, also the light absorption law is observed. There are stable maximums in spectrums of studied oils. Optical density of these maximums is a result of summary absorption of terpenoid components (aromatic and monoterpene alcohols, its ethers). Optical density of tested and standard solutions is measured in appropriate wavelengths. Spectrophotometric method of determination of essential oil quantity in aromatic water with rose smell differs with high sensitivity (10 -5 -10 -6 gmol/l) and allows to determine oil concentration from 0,900 to 0,008 mg with an error less than 1%. At that, 1 ml is enough for analysis. It’s expedient to apply this method while operating with small quantity of water distillate in biochemical and biotechnological researches and also as express control for extraction and hydrodistillation of essential oil raw material (rose petals and flowers from different origin, eremothecium cultural liquid etc.). (paper)

ATPase Activity Measurements by an Enzyme-Coupled Spectrophotometric Assay.

Science.gov (United States)

Sehgal, Pankaj; Olesen, Claus; Møller, Jesper V

2016-01-01

Enzymatic coupled assays are usually based on the spectrophotometric registration of changes in NADH/NAD(+) or NADPH/NADP(+) absorption at 340 nm accompanying the oxidation/reduction of reactants that by dehydrogenases and other helper enzymes are linked to the activity of the enzymatic reaction under study. The present NADH-ATP-coupled assay for ATPase activity is a seemingly somewhat complicated procedure, but in practice adaptation to performance is easily acquired. It is a more safe and elegant method than colorimetric methods, but not suitable for handling large number of samples, and also presupposes that the activity of the helper enzymes is not severely affected by the chemical environment of the sample in which it is tested.

Novel atomic absorption spectrometric and rapid spectrophotometric methods for the quantitation of paracetamol in saliva: application to pharmacokinetic studies.

Science.gov (United States)

Issa, M M; Nejem, R M; El-Abadla, N S; Al-Kholy, M; Saleh, Akila A

2008-01-01

A novel atomic absorption spectrometric method and two highly sensitive spectrophotometric methods were developed for the determination of paracetamol. These techniques based on the oxidation of paracetamol by iron (III) (method I); oxidation of p-aminophenol after the hydrolysis of paracetamol (method II). Iron (II) then reacts with potassium ferricyanide to form Prussian blue color with a maximum absorbance at 700 nm. The atomic absorption method was accomplished by extracting the excess iron (III) in method II and aspirates the aqueous layer into air-acetylene flame to measure the absorbance of iron (II) at 302.1 nm. The reactions have been spectrometrically evaluated to attain optimum experimental conditions. Linear responses were exhibited over the ranges 1.0-10, 0.2-2.0 and 0.1-1.0 mug/ml for method I, method II and atomic absorption spectrometric method, respectively. A high sensitivity is recorded for the proposed methods I and II and atomic absorption spectrometric method value indicate: 0.05, 0.022 and 0.012 mug/ml, respectively. The limit of quantitation of paracetamol by method II and atomic absorption spectrometric method were 0.20 and 0.10 mug/ml. Method II and the atomic absorption spectrometric method were applied to demonstrate a pharmacokinetic study by means of salivary samples in normal volunteers who received 1.0 g paracetamol. Intra and inter-day precision did not exceed 6.9%.

Kinetic investigation of heterogeneous catalytic reactions by means of the kinetic isotope method

Energy Technology Data Exchange (ETDEWEB)

Bauer, F; Dermietzel, J [Akademie der Wissenschaften der DDR, Leipzig. Zentralinstitut fuer Isotopen- und Strahlenforschung

1978-09-01

The application of the kinetic isotope method to heterogeneous catalytic processes is possible for surface compounds by using the steady-state relation. However, the characterization of intermediate products becomes ambiguous if sorption rates are of the same order of magnitude as surface reactions rates. The isotopic exchange reaction renders possible the estimation of sorption rates.

An experimental design approach for optimization of spectrophotometric method for estimation of cefixime trihydrate using ninhydrin as derivatizing reagent in bulk and pharmaceutical formulation

Directory of Open Access Journals (Sweden)

Yogita B. Wani

2017-01-01

Full Text Available The aim of the present work is to use experimental design to screen and optimize experimental variables for developing a spectrophotometric method for determining cefixime trihydrate content using ninhydrin as a derivatizing reagent. The method is based on the reaction of the amino group of cefixime with ninhydrin in an alkaline medium to form a yellow-colored derivative (λmax 436 nm. A two-level full factorial design was utilized to screen the effect of ninhydrin reagent concentration (X1, volume of ninhydrin reagent (X2, heating temperature (X3 and heating time (X4 on the formation of the cefixime–ninhydrin complex Y (absorbance. One way ANOVA and Pareto ranking analyses have shown that the ninhydrin reagent concentration (X1, volume of ninhydrin reagent (X2 and heating temperature (X3 were statistically significant factors (P < 0.05 affecting the formation of the cefixime–ninhydrin complex Y (absorbance. A Box-Behnken experimental design with response surface methodology was then utilized to evaluate the main, interaction and quadratic effects of these three factors on the selected response. With the help of a response surface plot and contour plot the optimum values of the selected factors were determined and used for further experiments. These values were a ninhydrin reagent concentration (X1 of 0.2% w/v, volume of ninhydrin reagent (X2 of 1 mL and heating temperature (X3 of 80 °C. The proposed method was validated according to the ICH Q2 (R1 method validation guidelines. The results of the present study have clearly shown that an experimental design concept may be effectively applied to the optimization of a spectrophotometric method for estimating the cefixime trihydrate content in bulk and pharmaceutical formulation with the least number of experimental runs possible.

Spectrophotometric determination of Fe(II) in Geological Materials by Using Ferrozine as Cromogenic Reagent

International Nuclear Information System (INIS)

Sanchez, D. M.; Martin, R.; Marin, J.; Morante, R.; Gutierrez, L.; Bayon, A.

1999-12-01

A rapid and sensitive spectrophotometric method for the determination of labile ferrous iron in geological materials is described. Samples are treated by boiling with hydrochloric acid for 60 min. in an atmosphere of carbon dioxide. Systematic erroneous results due to high concentrations of ferric iron are resolved. The limit of detection for the method was 0.02% of FeO. International standard granites analysed by the proposed method showed recoveries ranged from 81-102%. (Author) 9 refs

Spectrophotometric reading of EUCAST antifungal susceptibility testing of Aspergillus fumigatus

DEFF Research Database (Denmark)

Meletiadis, J.; Leth Mortensen, K.; Verweij, P. E.

2017-01-01

with spectrophotometrically determined MICs and essential (±1 twofold dilution) and categorical (susceptible/intermediate/resistant or wild-type/non-wild-type) agreement was calculated. Spectrophotometric data were analysed with regression analysis using the Emax model, and the effective concentration corresponding to 5% (EC......5) was estimated. Results Using the 5% cut-off, high essential (92%–97%) and categorical (93%–99%) agreement (

Decoloration Kinetics of Waste Cooking Oil by 60Co γ-ray/H2O2

Science.gov (United States)

Xiang, Yulin; Xiang, Yuxiu; Wang, Lipeng

2016-03-01

In order to decolorize, waste cooking oil, a dark red close to black solution from homes and restaurants, was subjected to 60Co γ-ray/H2O2 treatment. By virtue of UV/Vis spectrophotometric method, the influence of Gamma irradiation to decoloration kinetics and rate constants of the waste cooking oil in the presence of H2O2 was researched. In addition, the influence of different factors such as H2O2 concentration and irradiation dose on the decoloration rate of waste cooking oil was investigated. Results indicated that the decoloration kinetics of waste cooking oil conformed to the first-order reaction. The decoloration rate increased with the increase of irradiation dose and H2O2 concentration. Saponification analysis and sensory evaluation showed that the sample by 60Co γ-ray/H2O2 treatment presented better saponification performance and sensory score. Furthermore, according to cost estimate, the cost of the 60Co γ-ray/H2O2 was lower and more feasible than the H2O2 alone for decoloration of waste cooking oil.

Novel spectrophotometric method for the determination of aluminum in soda drinks packed in cans and plastic bottles

Energy Technology Data Exchange (ETDEWEB)

Francisco, Barbara Bruna A.; Caldas, Luiz Fernando S.; Brum, Daniel M. [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de Sao Joao Batista s/n, Centro, Niteroi/RJ 24020-141 (Brazil); Cassella, Ricardo J., E-mail: cassella@vm.uff.br [Departamento de Quimica Analitica, Universidade Federal Fluminense, Outeiro de Sao Joao Batista s/n, Centro, Niteroi/RJ 24020-141 (Brazil)

2010-09-15

In the present work, a new spectrophotometric method was developed for the determination of aluminum in soda drinks packed in different materials. Reaction among Al(III), phenylfluorone (PF) and cetylpyridinium chloride (CPC) in slightly alkaline medium was explored for this purpose. The method was optimized regarding to its chemical parameters in order to establish better conditions in terms of sensitivity and selectivity. The results obtained showed that the concentration of CPC presented remarkable influence on the sensitivity and acted as a sensitizer for the studied system. The possible interferences of some metallic cations were evaluated and the cations Cu(II), Mn(II), and Zn(II) presented noticed interference on the Al(III) signal. So, their interference was eliminated by using EDTA with minimum loss of sensitivity. The results obtained in the determination of total aluminum in soda drinks by the developed methodology were not statistically different from those obtained by electrothermal atomic absorption spectrometry. In the optimized conditions the method presented a linear range of 5-100 {mu}g L{sup -1}. The limits of detection and quantification were 0.81 and 2.7 {mu}g L{sup -1}, respectively. The methodology was successfully applied in the determination of aluminum in 10 samples of soda drinks packed in cans and plastic bottles.

Study on the Solid Phase Extraction and Spectrophotometric ...

African Journals Online (AJOL)

NJD

Spectrophotometric Determination of Mercury in Water and. Biological ... 1Department of Chemistry, Yunnan University, Kunming, 650091, P.R. China. 2Department of ... (such as higher enrichment factor, reduced contamination of the.

Investigation of synthesis, thermal properties and curing kinetics of fluorene diamine-based benzoxazine by using two curing kinetic methods

International Nuclear Information System (INIS)

He, Xuan-yu; Wang, Jun; Ramdani, Noureddine; Liu, Wen-bin; Liu, Li-jia; Yang, Lei

2013-01-01

Graphical abstract: - Highlights: • A novel diamine-based benzoxazine monomer containing aryl ether and bulky fluorene groups (BEF-p) is synthesized. • Kinetic parameters can be calculated by Starink-LSR method and direct LSR method. • Cure reaction could be successfully described with the autocatalytic model. • The poly(BEF-p) exhibits high T g and superior thermal stability. • Aryl ether linkages had little influence on the thermal stability. - Abstract: A novel diamine-based benzoxazine monomer containing aryl ether and bulky fluorene groups (BEF-p) was prepared from the reaction of 9,9-bis-[4-(p-aminophenoxy)-phenyl]fluorene with paraformaldehyde and phenol. The chemical structure of monomer was confirmed by Fourier-transform infrared (FTIR) and 1 H and 13 C nuclear magnetic resonance spectroscopy ( 1 H and 13 C NMR). The polymerization behavior of monomer was analyzed by differential scanning calorimetry (DSC) and FTIR. The curing kinetics was studied by non-isothermal DSC, and the kinetic parameters were determined. The autocatalytic model based on two kinetic methods (Starink-LSR method and direct LSR method) showed good agreement with experimental results. The thermal and mechanical properties of poly(BEF-p) were evaluated with DSC, dynamic mechanical thermal analysis (DMTA), and thermogravimetric analysis (TGA). The results showed that the cured polymer exhibited higher glass transition temperature (T g ) and better thermal stability compared with diaminodiphenylmethane-based benzoxazine(P-ddm), and was slightly lower than those of fluorene diamine-phenol-based polybenzoxazine (poly(BF-p))

Determination of Nitrite and Nitrate in Natural Waters Using Flow Injection with Spectrophotometric Detection

International Nuclear Information System (INIS)

Yaqoob, M.; Nabi, A.

2013-01-01

A simple and sensitive flow injection spectrophotometric method is reported for the room temperature determination of nitrite and nitrate based on the Griess reaction and a copperised cadmium column for reduction of nitrate. Calibration graphs were linear over the range 2 - 1000 micro g N L /sup -1/ (R2 = 0.9997 and 0.9999, n = 9) with a limit of detection (3 s.d.) of 1.0 micro g N L and relative standard deviations (n = 10) of 0.9 and 1.2% for 50 micro g N L nitrite and nitrate respectively. The sample throughput was 50 h. The effect of reagent concentrations, physical parameters (flow rate, sample volume, reaction coil and copperised cadmium column length) and the potential interferences are reported. The effect of salinity on the blank and on the determination of nitrite and nitrate are also presented. The method was applied to natural waters (rainwater, freshwater and estuarine water) and the results for nitrite + nitrate (140 - 7310 micro g N L/sup -1/) were not significantly different (95% confidence interval) from results obtained using a segmented flow analyser reference method with spectrophotometric detection. (author)

Spectrophotometric study of the complexation reaction between niobium(V) and 5-sulpho-3-nitro-salicylic acid

Energy Technology Data Exchange (ETDEWEB)

Parmar, D S; Shivahare, G C [Rajasthan Univ., Jaipur (India). Dept. of Chemistry

1975-04-01

5-sulpho-3 nitro-salicylic acid forms a yellow complex with niobium(V) at pH 8.5 and the reaction has been successfully studied spectrophotometrically. The results of the Job's continuous variation method and the molar ratio method indicate a composition of 1:2 for the complex. Stability constant of the complex has also been determined. (auth)

Determination of equilibration kinetics of oxide electrode materials using a manometric method

International Nuclear Information System (INIS)

Badwal, S.P.S.; Jiang, S.P.; Love, J.; Nowotny, J.; Rekas, M.

1998-01-01

The gas/solid equilibration kinetics for electrode oxide materials, such as (La 0.8 Sr 0.2 )MnO 3 , using a manometric method, was determined. The reaction kinetics between oxygen and the oxide material was monitored using the measurements of the P(O 2 ) changes during isothermic experiments of oxidation and reduction. The procedure of the determination will be described and relevant kinetic equations was derived. The equilibration kinetic data obtained can be used to determine the chemical diffusion coefficient. Copyright (1998) Australasian Ceramic Society

Development and validation of a simple spectrophotometric method for the determination of methyldopa in both bulk and marketed dosage formulations

Directory of Open Access Journals (Sweden)

Paulo Roberto da Silva Ribeiro

2014-09-01

Full Text Available A simple, precise, sensitive, rapid, specific and economical spectrophotometric method was developed to determine methyldopa (MTD content in bulk and pharmaceutical dosage formulations. The proposed method was based on the formation of a colored product from the nitrosation reaction of MTD with sodium nitrite in an acid medium. The resultant nitroso derivative species reacts further with sodium hydroxide and is converted it into a more stable compound. This yellow nitrosation product exhibited an absorption maximum at 430 nm. Beer's Law was obeyed in a concentration range of 6.37 to 82.81 μg mL-1 MTD with an excellent coefficient of determination (R2 = 0.9998. No interference was observed from common excipients in formulations. The results showed the method to be simple, accurate and readily applied for the determination of MTD in pure form and in pharmaceutical preparations. The analytical results obtained for these products using the proposed method are in agreement with those of the Brazilian Pharmacopoeia procedure at a 95% confidence level.

PCA-based algorithm for calibration of spectrophotometric analysers of food

International Nuclear Information System (INIS)

Morawski, Roman Z; Miekina, Andrzej

2013-01-01

Spectrophotometric analysers of food, being instruments for determination of the composition of food products and ingredients, are today of growing importance for food industry, as well as for food distributors and consumers. Their metrological performance significantly depends of the numerical performance of available means for spectrophotometric data processing; in particular – the means for calibration of analysers. In this paper, a new algorithm for this purpose is proposed, viz. the algorithm using principal components analysis (PCA). It is almost as efficient as PLS-based algorithms of calibration, but much simpler

Spectrophotometric determination of the first hydrolysis constant of praseodymium (III)

International Nuclear Information System (INIS)

Gonzalez M, R.; Lopez G, H.; Rojas H, A.

2010-01-01

The behavior of the trivalent ion praseodymium in 2 M of NaCl at 303 K and in CO 2 free conditions, was studied. Spectrophotometric titrations of the soluble species were used, in order to obtain the value of the first hydrolysis constant of Pr(III). The data obtained were treated with both the program Squad and by a graphic method, respectively. The result obtained using Squad was log*β 1 = -8.94 ± 0.03, while it was log*β 1 = -8.77 ± 0.03, when calculated graphically. These results are similar to the value obtained previously with the potentiometric method. (Author)

Spectrophotometric determination of the first hydrolysis constant of praseodymium (III)

Energy Technology Data Exchange (ETDEWEB)

Gonzalez M, R.; Lopez G, H. [ININ, Carretera Mexico-Toluca s/n, 52750 Ocoyoacac, Estado de Mexico (Mexico); Rojas H, A., E-mail: hilario.lopez@inin.gob.m [Universidad Autonoma Metropolitana, Unidad Iztapalapa, Departamento de Quimica, Av. San Rafael Atlixco No. 186, Col. Vicentina, 09340 Mexico D. F. (Mexico)

2010-07-01

The behavior of the trivalent ion praseodymium in 2 M of NaCl at 303 K and in CO{sub 2} free conditions, was studied. Spectrophotometric titrations of the soluble species were used, in order to obtain the value of the first hydrolysis constant of Pr(III). The data obtained were treated with both the program Squad and by a graphic method, respectively. The result obtained using Squad was log*{beta}{sub 1}= -8.94 {+-} 0.03, while it was log*{beta}{sub 1}= -8.77 {+-} 0.03, when calculated graphically. These results are similar to the value obtained previously with the potentiometric method. (Author)

A simple method for determination of carmine in food samples based on cloud point extraction and spectrophotometric detection.

Science.gov (United States)

Heydari, Rouhollah; Hosseini, Mohammad; Zarabi, Sanaz

2015-01-01

In this paper, a simple and cost effective method was developed for extraction and pre-concentration of carmine in food samples by using cloud point extraction (CPE) prior to its spectrophotometric determination. Carmine was extracted from aqueous solution using Triton X-100 as extracting solvent. The effects of main parameters such as solution pH, surfactant and salt concentrations, incubation time and temperature were investigated and optimized. Calibration graph was linear in the range of 0.04-5.0 μg mL(-1) of carmine in the initial solution with regression coefficient of 0.9995. The limit of detection (LOD) and limit of quantification were 0.012 and 0.04 μg mL(-1), respectively. Relative standard deviation (RSD) at low concentration level (0.05 μg mL(-1)) of carmine was 4.8% (n=7). Recovery values in different concentration levels were in the range of 93.7-105.8%. The obtained results demonstrate the proposed method can be applied satisfactory to determine the carmine in food samples. Copyright © 2015 Elsevier B.V. All rights reserved.

Experimental methods of investigation of kinetics and dynamics of nuclear reactors

International Nuclear Information System (INIS)

Costa Oliveira, Jaime M.

1969-03-01

The author presents experimental methods used to study kinetic and dynamic properties of nuclear reactors. Kinetic methods aim at determining characteristic parameters of the behaviour in time of neutrons. Dynamic methods aim at establishing the relationships between the reactor behaviour and its internal and external causes (notably the measurement of transfer functions). The author proposes a classification with respect to the excitation type: periodic excitation (reactivity sinusoidal modulation, source sinusoidal modulation, periodic pulse excitation), non periodic excitation (reactivity monitoring, reactivity linear variation, reactivity variation according to any given law, removal of starting source), random excitation (random reactivity or source excitation), natural fluctuations (alpha-Rossi method, methods of reduced variance, probabilistic methods, correlation methods, spectral analysis method). He also addresses space and energy effects. Applications are reported for low power and power reactors

Titrimetric and Spectrophotometric Determination of Metaprolol tartrate in Pharmaceuticals Using N-Bromosuccinimide

Directory of Open Access Journals (Sweden)

K. Basavaiah

2007-01-01

Full Text Available One titrimetric and two spectrophotometric methods are presented for the assay of metaprolol tartrate (MPT in bulk drug and in tablets. The methods employ N-bromosuccinimide (NBS as the oxidimetric reagent and two dyes, methyl orange and indigo carmine as spectrophotometric reagents. In titrimetry, an acidified solution of MPT is treated with a known excess amount of NBS and after a definite time, the unreacted oxidant is determined by iodometric back titration. Spectrophotometry involves adding a measured excess of NBS to MPT in acid medium followed by determination of residual NBS by reacting with a fixed amount of either methyl orange and measuring the absorbance at 520 nm (Method A or indigo carmine and measuring the absorbance at 610 nm (Method B. In all the methods, the amount of NBS reacted corresponds to the amount of MPT. Reaction conditions have been optimized. Titrimetry allows the determination of 1 - 12 mg of MPT and the calculations are based on a 1: 4 (MPT: NBS reaction stoichiometry. In spectrophotometry, the measured absorbance is found to increase linearly with the concentration of MPT serving as basis for quantitation. The systems obey Beer’s law for 0.5 - 4.0 μg mL-1 and 1.25 - 10.0 μg mL-1 for method A and method B, respectively. The apparent absorptivities are calculated to 1.07 × 105 be and 4.22 × 104 L mol cm-1 for method A and method B, respectively. The methods developed were applied to the assay of MPT in commercial tablet formulations, and the results were compared statistically with those of a reference method. The accuracy and reliability of the methods were further ascertained by performing recovery tests via standard-addition method.

Implementing atomic force microscopy (AFM) for studying kinetics of gold nanoparticle's growth

DEFF Research Database (Denmark)

Georgiev, P.; Bojinova, A.; Kostova, B.

2013-01-01

In a novel experimental approach Atomic Force Microscopy (AFM) was applied as a tool for studying the kinetics of gold nanoparticle growth. The gold nanoparticles were obtained by classical Turkevich citrate synthesis at two different temperatures. From the analysis of AFM images during...... the synthesis process the nanoparticle s' sizes were obtained. To demonstrate the applicability and the reliability of the proposed experimental approach we studied the nanoparticles growth at two different temperatures by spectrophotometric measurements and compared them with the results from AFM experimental...

Comparative study of three modified numerical spectrophotometric methods: An application on pharmaceutical ternary mixture of aspirin, atorvastatin and clopedogrel

Science.gov (United States)

Issa, Mahmoud Mohamed; Nejem, R.'afat Mahmoud; Shanab, Alaa Abu; Hegazy, Nahed Diab; Stefan-van Staden, Raluca-Ioana

2014-07-01

Three novel numerical methods were developed for the spectrophotometric multi-component analysis of capsules and synthetic mixtures of aspirin, atorvastatin and clopedogrel without any chemical separation. The subtraction method is based on the relationship between the difference in absorbance at four wavelengths and corresponding concentration of analyte. In this method, the linear determination ranges were 0.8-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 0.5-30 μg mL-1 clopedogrel. In the quotient method, 0.8-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 1.0-30 μg mL-1 clopedogrel were determine from spectral data at the wavelength pairs that show the same ratio of absorbance for other two species. Standard addition method was used for resolving ternary mixture of 1.0-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 2.0-30 μg mL-1 clopedogrel. The proposed methods were validated. The reproducibility and repeatability were found satisfactory which evidence was by low values of relative standard deviation (atorvastatin and clopedogrel in capsule dosage forms and results were in good concordance with alternative liquid chromatography.

Chlorine Dioxide-Iodide-Methyl Acetoacetate Oscillation Reaction Investigated by UV-Vis and Online FTIR Spectrophotometric Method

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Laishun Shi

2012-01-01

Full Text Available In order to study the chemical oscillatory behavior and mechanism of a new chlorine dioxide-iodide ion-methyl acetoacetate reaction system, a series of experiments were done by using UV-Vis and online FTIR spectrophotometric method. The initial concentrations of methyl acetoacetate, chlorine dioxide, potassium iodide, and sulfuric acid and the pH value have great influence on the oscillation observed at wavelength of 289 nm. There is a preoscillatory or induction period, and the amplitude and the number of oscillations are associated with the initial concentration of reactants. The equations for the triiodide ion reaction rate changing with reaction time and the initial concentrations in the oscillation stage were obtained. Oscillation reaction can be accelerated by increasing temperature. The apparent activation energies in terms of the induction period and the oscillation period were 26.02 KJ/mol and 17.65 KJ/mol, respectively. The intermediates were detected by the online FTIR analysis. Based upon the experimental data in this work and in the literature, a plausible reaction mechanism was proposed for the oscillation reaction.

Comparative analysis among several methods used to solve the point kinetic equations

International Nuclear Information System (INIS)

Nunes, Anderson L.; Goncalves, Alessandro da C.; Martinez, Aquilino S.; Silva, Fernando Carvalho da

2007-01-01

The main objective of this work consists on the methodology development for comparison of several methods for the kinetics equations points solution. The evaluated methods are: the finite differences method, the stiffness confinement method, improved stiffness confinement method and the piecewise constant approximations method. These methods were implemented and compared through a systematic analysis that consists basically of confronting which one of the methods consume smaller computational time with higher precision. It was calculated the relative which function is to combine both criteria in order to reach the goal. Through the analyses of the performance factor it is possible to choose the best method for the solution of point kinetics equations. (author)

Comparative analysis among several methods used to solve the point kinetic equations

Energy Technology Data Exchange (ETDEWEB)

Nunes, Anderson L.; Goncalves, Alessandro da C.; Martinez, Aquilino S.; Silva, Fernando Carvalho da [Universidade Federal, Rio de Janeiro, RJ (Brazil). Coordenacao dos Programas de Pos-graduacao de Engenharia. Programa de Engenharia Nuclear; E-mails: alupo@if.ufrj.br; agoncalves@con.ufrj.br; aquilino@lmp.ufrj.br; fernando@con.ufrj.br

2007-07-01

The main objective of this work consists on the methodology development for comparison of several methods for the kinetics equations points solution. The evaluated methods are: the finite differences method, the stiffness confinement method, improved stiffness confinement method and the piecewise constant approximations method. These methods were implemented and compared through a systematic analysis that consists basically of confronting which one of the methods consume smaller computational time with higher precision. It was calculated the relative which function is to combine both criteria in order to reach the goal. Through the analyses of the performance factor it is possible to choose the best method for the solution of point kinetics equations. (author)

A spectrophotometric method of determining nobium, ranging from 0,01 to 0,10% Nb, in steel with xylene orange after precipitation by tannin

International Nuclear Information System (INIS)

Jurczyk, J.; Capalla, K.; Szeja, K.

1980-01-01

A spectrophotometric method is presented of determining 0,1 to 0,10% niobium content in steel. The dissolution of steel was made by means of a mixture of hydrochloric and nitric acids. Niobium was precipitated by hydrolysis in the presence of tannin, gelatine and ascorbic acid and then was determined in the form of a coloured complex compound at pH 3. The concentration of niobium in the examined solution cannot exceed 1,6 μg/cm 3 . Standard deviation for niobium content 0,017% Nb is 0,0007% and for 0,100% Nb - 0,0025%. (author)

Treating experimental data of inverse kinetic method by unitary linear regression analysis

International Nuclear Information System (INIS)

Zhao Yusen; Chen Xiaoliang

2009-01-01

The theory of treating experimental data of inverse kinetic method by unitary linear regression analysis was described. Not only the reactivity, but also the effective neutron source intensity could be calculated by this method. Computer code was compiled base on the inverse kinetic method and unitary linear regression analysis. The data of zero power facility BFS-1 in Russia were processed and the results were compared. The results show that the reactivity and the effective neutron source intensity can be obtained correctly by treating experimental data of inverse kinetic method using unitary linear regression analysis and the precision of reactivity measurement is improved. The central element efficiency can be calculated by using the reactivity. The result also shows that the effect to reactivity measurement caused by external neutron source should be considered when the reactor power is low and the intensity of external neutron source is strong. (authors)

HF effect on dissociation kinetics of plutonium and neptunium complexes with 1,2-diaminocyclohexanetetraacetic acid in nitric acid solutions

Energy Technology Data Exchange (ETDEWEB)

Nikitina, S.A.; Stepanov, A.V.

1982-01-01

Dissociation kinetics of Pusup((4)) and Np sup((4)) complexes with DCTA were investigated in HNO/sub 3/ solutions in the presence of HF and arsenazo 3. It was found that HF or NaF produced a differentiating effect on the reactivity of the complexes at (HNO/sub 3/)=1-6 mol/l as well as inhibiting effect at (HNO/sub 3/)=0.01 mol/l. Conditions of the differential kinetic analysis of plutonium and neptunium in the mixture and differential spectrophotometric analysis of uranium (6) during the camouflage of neptunium (4) and plutonium (4) were determined.

SPECTROPHOTOMETRIC DETERMINATION OF ACETYLCYSTEINE IN PHARMACEUTICAL FORMULATIONS USING 2,3-DICHLORO-1,4-NAPTHOQUINONE

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A. O. Donchenko

2015-04-01

Full Text Available The aim of research was the development and validation ofspectrophotometric method foracetylcysteine assay in pharmaceutical formulations.Тhe proposed method is based on the reaction with 2,3-dichloro-1,4-naphthoquinone and the formation of colored products that exhibit absorption maxima at 425 nm. Introduction Many analytical methods have been published for acetylcysteine assay in pharmaceutical formulations as high-performance liquid chromatography (HPLC, fluorimetry and chemiluminescence. Some of these methods are time consuming or require expensive equipment. Other published methods suffer from lack of selectivity and sensitivity. Spectrophotometry is the most widely used technique in pharmaceutical analysis because it is simple, economic, and easily available to most quality control laboratories. In the present work, we propose a simple and accurate spectrophotometric method for acetylcysteine assay in pharmaceutical formulations. Materials and Methods Reagents: Reference standard acetylcysteinesubstance; 2,3-dichloro-1,4-naphthoquinone. All chemicals and solvents were of analytical grade. DMFA was used as a solvent. Pharmaceutical preparations:powder for oral solution «ACC 200» 200 mgseries number50026151 (Salutas Pharma CmbH, Germany; effervescent tablets «Fluimucil» 600 mg (Zambon S.P.A., Italy and «ACC LONG» 600 mg (Salutas Pharma CmbH, Germany series numbers 321284 and DH2740; solution for injections «Fluimucil» 100 mg/ml (Zambon S.P.A., Italyseries number28002492. Solutions: Acetylcysteine stock solution (0,16%; DMFAsolution of 2,3-dichloro-1,4-naphthoquinone (4%. Equipment Analytical balance (ABT-120-5DM; UV-VIS spectrophotometer (Specord 200; water bath (MemmertWNB 7-45;quartz cells. Results Acetylcysteine was determined using a spectrophotometric method based on the reaction with 2,3-dichloro-1,4-naphthoquinone to form yellow colored reaction products with absorption maxima at 425 nm. The effect of reaction time and

A PLS-based extractive spectrophotometric method for simultaneous determination of carbamazepine and carbamazepine-10,11-epoxide in plasma and comparison with HPLC

Science.gov (United States)

Hemmateenejad, Bahram; Rezaei, Zahra; Khabnadideh, Soghra; Saffari, Maryam

2007-11-01

Carbamazepine (CBZ) undergoes enzyme biotransformation through epoxidation with the formation of its metabolite, carbamazepine-10,11-epoxide (CBZE). A simple chemometrics-assisted spectrophotometric method has been proposed for simultaneous determination of CBZ and CBZE in plasma. A liquid extraction procedure was operated to separate the analytes from plasma, and the UV absorbance spectra of the resultant solutions were subjected to partial least squares (PLS) regression. The optimum number of PLS latent variables was selected according to the PRESS values of leave-one-out cross-validation. A HPLC method was also employed for comparison. The respective mean recoveries for analysis of CBZ and CBZE in synthetic mixtures were 102.57 (±0.25)% and 103.00 (±0.09)% for PLS and 99.40 (±0.15)% and 102.20 (±0.02)%. The concentrations of CBZ and CBZE were also determined in five patients using the PLS and HPLC methods. The results showed that the data obtained by PLS were comparable with those obtained by HPLC method.

Contributions te the study of methods and factors affecting the spectrophotometric determination of boron traces with carmin uranium compounds

International Nuclear Information System (INIS)

Fernandez Cellini, R.; Gasco Sanchez, L.

1956-01-01

The study of some factors affecting the spectrophotometric determination of boron traces with carmin is made; the influence of carmin from different origin, the stability of complex carmin-boric acid in relation with the sulphuric acid concentration, the interference produced by ion nitrate, and the ion uraline and light influence are discussed. (Author) 36 refs

Spectrophotometric determination of uranium by previous extraction chromatography separation in polimetalic mineral, phosphorites and technological licours

International Nuclear Information System (INIS)

Moreno Bermudez, J.; Cabrera Quevedo, C.; Alfonso Mendez, L.; Rodriguez Aguilera, M.

1994-01-01

The development of an analytical procedure for spectrophotometric determination of uranium in polimetalic mineral, phosphorites and technological licours is described. The method is based on the previous separation of interfering elements by extraction chromatography and on spectrophotometric determination of uranium (IV) with arsenazo III in concentrated hydrochloric acid. Tributyl phosphate impregnate on politetrafluoroethylene is used as stationary phase and 5.5 M nitric acid is used as movie phase. The influence of matrix-component elements was studies. The development procedure was applied to real samples, being the results compared with those obtained by other well established analytical methods like gamma-spectrometry, laser fluorimetric, spectrophotometry previous uranium separation by liquid liquid extraction and anion exchange. The reproducibility is evaluated and the detection limited has been established for each studied matrix. A procedure for correcting the thorium interference has been developed for samples with a Th/ 3U8O higher than 0.2

Spectrophotometric determination of triclosan in personal care products

Science.gov (United States)

Lu, Huihui; Ma, Hongbing; Tao, Guanhong

2009-09-01

A spectrophotometric method for the determination of triclosan in personal care products was proposed. It was based on the reaction of sodium nitrite with p-sulfanilic acid in an acidic medium to form diazonium ion, with which triclosan further formed an azo compound in an alkaline medium. The resulting yellow colored product has a maximum absorption at 452 nm. A good linear relationship ( r = 0.9999) was obtained in the range of 0-30 mg L -1 triclosan. A detection limit of 0.079 g L -1 was achieved and the relative standard deviation was 0.24% ( n = 11) at 14 mg L -1 triclosan. The proposed method has been applied to the analyses of triclosan in several personal care products and the results were in good agreement with those obtained by high-performance liquid chromatography.

Highly Selective and Sensitized Spectrophotometric Determination of Iron (3) Following Potentiometric Study

International Nuclear Information System (INIS)

Shokrollahi, A.; Ghaedi, M.; Rajabi, H.R.

2007-01-01

A simple, selective and sensitized spectrophotometric method for determination of trace amounts of Fe 3+ ion in tap and waste water solutions has been described. The spectrophotometric determination of Fe 3+ ion using Ferron in the presence of N,N-Dodecy trimethylammonium bromide (DTAB) has been carried out. The Beer's law is obeyed over the concentration range of 0.05-2.6 μg mL -1 of Fe 3+ ion with the relative standard deviation (RSD %) 3 L mol -1 cm -1 . Potentiometric pH titration has been used for prediction of protonation constants of ferron, and evaluating its stoichiometry and respective stability constant with Fe 3+ ion. As it is obvious the most likely species of ferron alone and its complexes are LH (log=7.64), LH 2 (logK=10.52), LH 3 (logK=11.74) and ML 2 (logβ= 23.68), ML 3 (logβ23.68), ML 3 H (logβ= 23.68), ML 3 H 2 (logβ= 23.68) and ML(OH) 2 (logβ=23.68) respectively

The rapid spectrophotometric determination of vanadium in tool steel with 9(6-methyl-2-pyridyl)azo5

International Nuclear Information System (INIS)

Beaupre, P.W.; Holland, W.J.

1980-01-01

An extractive-spectrophotometric method for the determination of vanadium in tool steel is described. The only sample pretreatment required is dissolution. An average vanadium of 2.06% was obtained on a standard sample compared to the recommended value of 2.06%. (author)

Differential equation methods for simulation of GFP kinetics in non-steady state experiments.

Science.gov (United States)

Phair, Robert D

2018-03-15

Genetically encoded fluorescent proteins, combined with fluorescence microscopy, are widely used in cell biology to collect kinetic data on intracellular trafficking. Methods for extraction of quantitative information from these data are based on the mathematics of diffusion and tracer kinetics. Current methods, although useful and powerful, depend on the assumption that the cellular system being studied is in a steady state, that is, the assumption that all the molecular concentrations and fluxes are constant for the duration of the experiment. Here, we derive new tracer kinetic analytical methods for non-steady state biological systems by constructing mechanistic nonlinear differential equation models of the underlying cell biological processes and linking them to a separate set of differential equations governing the kinetics of the fluorescent tracer. Linking the two sets of equations is based on a new application of the fundamental tracer principle of indistinguishability and, unlike current methods, supports correct dependence of tracer kinetics on cellular dynamics. This approach thus provides a general mathematical framework for applications of GFP fluorescence microscopy (including photobleaching [FRAP, FLIP] and photoactivation to frequently encountered experimental protocols involving physiological or pharmacological perturbations (e.g., growth factors, neurotransmitters, acute knockouts, inhibitors, hormones, cytokines, and metabolites) that initiate mechanistically informative intracellular transients. When a new steady state is achieved, these methods automatically reduce to classical steady state tracer kinetic analysis. © 2018 Phair. This article is distributed by The American Society for Cell Biology under license from the author(s). Two months after publication it is available to the public under an Attribution–Noncommercial–Share Alike 3.0 Unported Creative Commons License (http://creativecommons.org/licenses/by-nc-sa/3.0).

Sensitive inexpensive spectrophotometric and spectrofluorimetric analysis of ezogabine, levetiracetam and topiramate in tablet formulations using Hantzsch condensation reaction

Science.gov (United States)

Ibrahim, F. A.; El-Yazbi, A. F.; Wagih, M. M.; Barary, M. A.

2017-09-01

Two highly sensitive, simple and selective spectrophotometric and spectrofluorimetric assays have been investigated for the analysis of ezogabine, levetiracetam and topiramate in their pure and in pharmaceutical dosage forms. The suggested methods depend on the condensation of the primary amino-groups in the three drugs with acetylacetone and formaldehyde according to Hantzsch reaction yielding highly fluorescent yellow colored dihydropyridine derivatives. The reaction products of ezogabine, levetiracetam and topiramate were measured spectrophotometrically at 418, 390 and 380 nm or spectrofluorimetrically at λem/ex of 495/425 nm, 490/415 nm and 488/410 nm, respectively. Various experimental conditions have been carefully studied to maximize the reaction yield. At the optimum reaction conditions, the calibration curves were rectilinear over the concentration ranges of 8-25, 60-180 and 80-200 μg/mL spectrophotometrically and 0.02-0.2, 0.2-1.2 and 0.2-1.5 μg/mL spectrofluorimetrically for ezogabine, levetiracetam and topiramate, respectively with good correlation coefficients. The suggested methods were applied successfully for the analysis of ezogabine, levetiracetam and topiramate in their commercial tablets with high percentage recoveries and negligible interference from various excipients in pharmaceutical dosage forms. The results were statistically analyzed and showed the absence of any significant difference between both developed and published methods. The procedures were validated and evaluated by the ICH guidelines revealing good reproducibility and accuracy. Therefore, the two proposed methods may be considered of high interest for practical and reliable analysis of ezogabine, levetiracetam and topiramate in pharmaceutical dosage forms.

Evaluation of the Esthetic Properties of Developmental Defects of Enamel: A Spectrophotometric Clinical Study

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Fabrizio Guerra

2015-01-01

Full Text Available Objectives. Detailed clinical quantification of optical properties of developmental defect of enamel is possible with spectrophotometric evaluation. Developmental defects of enamel (DDE are daily encountered in clinical practice. DDE are an alteration in quality and quantity of the enamel, caused by disruption and/or damage to the enamel organ during amelogenesis. Methods. Several clinical indices have been developed to categorize enamel defects based on their nature, appearance, microscopic features, or cause. A sample of 39 permanent teeth presenting DDE on labial surface was examined using the DDE Modified Index and SpectroShade evaluation. The spectrophotometric approach quantifies L* (luminosity, a* (quantity of green-red, and b* (quantity of blue-yellow of different DDE. Conclusions. SpectroShade evaluation of the optical properties of the enamel defect enhances clinical understanding of severity and extent of the defect and characterizes the enamel alteration in terms of color discrepancy and surface characterization.

Indirect spectrophotometric determination of arbutin, whitening agent through oxidation by periodate and complexation with ferric chloride

Science.gov (United States)

Barsoom, B. N.; Abdelsamad, A. M. E.; Adib, N. M.

2006-07-01

A simple and accurate spectrophotometric method for the determination of arbutin (glycosylated hydroquinone) is described. It is based on the oxidation of arbutin by periodate in presence of iodate. Excess periodate causes liberation of iodine at pH 8.0. The unreacted periodate is determined by measurement of the liberated iodine spectrophotometrically in the wavelength range (300-500 nm). A calibration curve was constructed for more accurate results and the correlation coefficient of linear regression analysis was -0.9778. The precision of this method was better than 6.17% R.S.D. ( n = 3). Regression analysis of Bear-Lambert plot shows good correlation in the concentration range 25-125 ug/ml. The identification limit was determined to be 25 ug/ml a detailed study of the reaction conditions was carried out, including effect of changing pH, time, temperature and volume of periodate. Analyzing pure and authentic samples containing arbutin tested the validity of the proposed method which has an average percent recovery of 100.86%. An alternative method is also proposed which involves a complexation reaction between arbutin and ferric chloride solution. The produced complex which is yellowish-green in color was determined spectophotometrically.

A study of pH-dependent photodegradation of amiloride by a multivariate curve resolution approach to combined kinetic and acid-base titration UV data.

Science.gov (United States)

De Luca, Michele; Ioele, Giuseppina; Mas, Sílvia; Tauler, Romà; Ragno, Gaetano

2012-11-21

Amiloride photostability at different pH values was studied in depth by applying Multivariate Curve Resolution Alternating Least Squares (MCR-ALS) to the UV spectrophotometric data from drug solutions exposed to stressing irradiation. Resolution of all degradation photoproducts was possible by simultaneous spectrophotometric analysis of kinetic photodegradation and acid-base titration experiments. Amiloride photodegradation showed to be strongly dependent on pH. Two hard modelling constraints were sequentially used in MCR-ALS for the unambiguous resolution of all the species involved in the photodegradation process. An amiloride acid-base system was defined by using the equilibrium constraint, and the photodegradation pathway was modelled taking into account the kinetic constraint. The simultaneous analysis of photodegradation and titration experiments revealed the presence of eight different species, which were differently distributed according to pH and time. Concentration profiles of all the species as well as their pure spectra were resolved and kinetic rate constants were estimated. The values of rate constants changed with pH and under alkaline conditions the degradation pathway and photoproducts also changed. These results were compared to those obtained by LC-MS analysis from drug photodegradation experiments. MS analysis allowed the identification of up to five species and showed the simultaneous presence of more than one acid-base equilibrium.

Variational methods in the kinetic modeling of nuclear reactors: Recent advances

International Nuclear Information System (INIS)

Dulla, S.; Picca, P.; Ravetto, P.

2009-01-01

The variational approach can be very useful in the study of approximate methods, giving a sound mathematical background to numerical algorithms and computational techniques. The variational approach has been applied to nuclear reactor kinetic equations, to obtain a formulation of standard methods such as point kinetics and quasi-statics. more recently, the multipoint method has also been proposed for the efficient simulation of space-energy transients in nuclear reactors and in source-driven subcritical systems. The method is now founded on a variational basis that allows a consistent definition of integral parameters. The mathematical structure of multipoint and modal methods is also investigated, evidencing merits and shortcomings of both techniques. Some numerical results for simple systems are presented and the errors with respect to reference calculations are reported and discussed. (authors)

Quantitative HPLC Analysis of Rosmarinic Acid in Extracts of "Melissa officinalis" and Spectrophotometric Measurement of Their Antioxidant Activities

Science.gov (United States)

Canelas, Vera; da Costa, Cristina Teixeira

2007-01-01

The students prepare tea samples using different quantities of lemon balm leaves ("Melissa officinalis") and measure the rosmarinic acid contents by an HPLC-DAD method. The antioxidant properties of the tea samples are evaluated by a spectrophotometric method using a radical-scavenging assay with DPPH. (2,2-diphenyl-1-picrylhydrazyl). Finally the…

Spectrophotometric determination of silicon in silumin matrix

International Nuclear Information System (INIS)

Samanta, Papu; Pandey, K.L.; Kumar, Pradeep; Bagchi, A.C.; Abdulla, K.K.

2015-01-01

In dispersion fuel, fissile material is dispersed in inert matrix. Aluminum-silicon-nickel (silumin) alloy is employed as inert matrix owing to its high thermal conductivity, high castability, high corrosion resistance. All these properties depend on the chemical composition and the structure of silumin. Silicon is stringent specification in silumin. A spectrophotometric method has been developed for the determination of silicon content in silumin matrix. Silumin matrix was fused with LiOH and subsequent dissolution in water along with few drops of conc. sulphuric acid. The molybodo-silicic formed by the addition of ammonium molybdate is reduced to molybdenum blue by ascorbic acid in the presence of antimony. The absorbance was measured at 810 nm. Aluminum and nickel were found to be non-interfering with the silicon determination. (author)

Kinetics of isotopic exchanges by using radioactive indicators

International Nuclear Information System (INIS)

May, S.

1958-12-01

After having noticed that iodine 131 under the form of sodium iodide has always been used as radioactive indicator in the CEA atomic pile located in Chatillon, this research report recalls the counting technique and some historical aspects of the notion of isotopic exchange and qualitative works, and presents some generalities on isotopic exchanges (reactions and calculation of rate constants of order 1 and 2, calculation of activation energy, spectro-photometric studies, Walden inversion, alkaline hydrolysis, influence of solvent on exchange kinetics, influence of the nature of the mineral halide). The author then addresses exchanges in aliphatic series (exchange with sodium iodide and with molecular iodine), exchanges in olefin series, exchanges in alicyclic series, and exchanges in aromatic series

Multi-wavelength spectrophotometric analysis for detection of xanthochromia in cerebrospinal fluid and accuracy for the diagnosis of subarachnoid hemorrhage.

Science.gov (United States)

Smith, Andrew; Wu, Alan H B; Lynch, Kara L; Ko, Nerissa; Grenache, David G

2013-09-23

Cerebrospinal fluid (CSF) was examined for bilirubin, an important indicator for diagnosis of subarachnoid hemorrhage (SAH). A multi-wavelength (340, 415, and 460 nm) spectrophotometric assay was developed for the quantitative measurement of bilirubin in CSF, enabling the mathematical correction for absorbance of hemoglobin and proteins. Bilirubin and hemoglobin results were correlated to HPLC and a standard colorimetric assay, respectively. A subset of samples was sent for an absorbance reading at 450 nm following baseline correction. The multi-wavelength bilirubin assay was validated on 70 patients with confirmed SAH and 70 patients with neurologic symptoms who ruled out for SAH. The multi-wavelength spectrophometric assay demonstrated no interferences due to proteins (albumin) up to 30 g/l or oxyhemoglobin up to 260 mg/l. The assay limit of detection was 0.2 mg/l, linear to 20 mg/l, and CVs ranged from 1 to 6% at bilirubin concentrations of 0.84 and 2.1mg/l. The spectrophotometric assay correlated to HPLC and the colorimetric assay for bilirubin and hemoglobin, respectively. Results also correlated to the absorbance method (with removal of samples with high hemoglobin and proteins). The area under the ROC curve for diagnosis of SAH was 0.971 and 0.954 for the HPLC and spectrophotometric assay, respectively. At a cutoff of 0.2mg/l, the clinical specificity was 100% for both assays, and the clinical sensitivity was 94.3% and 88.6% for SAH for the HPLC and spectrophotometric asays, respectively. The multi-wavelength spectrophotometric assay is an objective alternative to visual inspection, HPLC, and absorbance for CSF bilirubin. Copyright © 2013 Elsevier B.V. All rights reserved.

Development and validation of indirect visible spectrophotometric methods for oxcarbazepine in pure and the tablet dosage form

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Hemavathi N. Deepakumari

2016-09-01

Full Text Available Three simple, accurate and highly sensitive indirect spectrophotometric methods have been developed for the determination of oxcarbazepine (OXC in both pure and in pharmaceutical preparations. The methods are based on the oxidation of oxcarbazepine by a known excess of cerium(IV in acid medium. This was followed by the determination of unreacted cerium(IV, which oxidizes leuco dyes to colored dyes in the same acid medium. In method A, an unreacted cerium(IV oxidizes leuco crystal violet to crystal violet dye which is measured at 580 nm. A bluish-colored malachite green with a maximum absorption at 610 nm is developed in method B. In method C, cerium(IV oxidizes leuco xylene cyanol FF to blue colored xylene cyanol FF having absorption maximum at 610 nm. In all these methods, the amount of cerium(IV reacted corresponds to the amount of OXC and the absorbance is found to decrease linearly with OXC concentration. Beer’s law was obeyed in the concentration range of 0–2.5, 0–2.0 and 0–2.5 μg ml−1 for methods A, B and C, respectively, and the corresponding molar absorptivity values are 3.86 × 104, 4.41 × 104 and 2.16 × 104 l mol−1cm−1. All variables have been optimized and the results were statistically compared with those of a literature method by employing the student’s t-test and F-test. No interference was observed from excipients normally added to the tablets.

Study the oxidation kinetics of uranium using XRD and Rietveld method

Science.gov (United States)

Zhang, Yanzhi; Guan, Weijun; Wang, Qinguo; Wang, Xiaolin; Lai, Xinchun; Shuai, Maobing

2010-03-01

The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50~300°C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO2 was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO2 can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

Spectrophotometric Determination of Lamivudine in Pure and Tablet Forms

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A. Biksham Babu

2012-01-01

Full Text Available Two visible spectrophotometric methods have been developed for the determination of Lamivudine(LMV in pure and tablet forms. Method-A is based on oxidation of 3-methyl-2-benzathiazolinone hydrazone (MBTH in the presence of iodoso benzene diacetate (IBDA to form electrophilic intermediate which is an active coupling species that reacts with the coupler (LMV by electrophillic attack on the most nucleophilic site on cyclic ring of the coupler. Method-B depends on diazonium salt formation and consequent reaction with resorcinol producing colored product. The absorbances are measured at 590 nm and 540 nm for Method-A and Method-B respectively. Beer's law is obeyed in the concentration range of 10.0-60.0 μg/mL for both the methods. The correlation coefficient which is very close to unity indicates that there is good correlation between concentration and absorbance. LOD, LOQ, confidence levels and relative standard deviation are calculated for the developed methods. The developed methods were successfully applied to tablet forms.

Modeling systematic errors: polychromatic sources of Beer-Lambert deviations in HPLC/UV and nonchromatographic spectrophotometric assays.

Science.gov (United States)

Galli, C

2001-07-01

It is well established that the use of polychromatic radiation in spectrophotometric assays leads to excursions from the Beer-Lambert limit. This Note models the resulting systematic error as a function of assay spectral width, slope of molecular extinction coefficient, and analyte concentration. The theoretical calculations are compared with recent experimental results; a parameter is introduced which can be used to estimate the magnitude of the systematic error in both chromatographic and nonchromatographic spectrophotometric assays. It is important to realize that the polychromatic radiation employed in common laboratory equipment can yield assay errors up to approximately 4%, even at absorption levels generally considered 'safe' (i.e. absorption <1). Thus careful consideration of instrumental spectral width, analyte concentration, and slope of molecular extinction coefficient is required to ensure robust analytical methods.

Spectrophotometric method for the analysis of rare earths by first and second order derivatives

International Nuclear Information System (INIS)

Deshpande, S.M.; Singh, H.

1997-01-01

Spectrophotometric methods are widely used for the analysis of rare earth elements as they are simple, fast, precise and accurate. Many of the rare earth ions in acidic solutions absorb in ultraviolet and visible region of the electromagnetic spectrum. Because of the restricted transition of the 4f electrons the absorption peaks are very sharp and these peaks are used for the qualitative and quantitative analysis of rare elements. When analysis of one or two minor constituents in the mixture of rare earths is involved, it is a straightforward and simple matter, but the analysis of multiple elements from a complex mixture is very difficult because of the mutual interference of the absorption bands. Simultaneous equations of the type: (OD) 1 = C A X Φ A1 + C B X Φ B1 and (OD) 2 = C A X Φ A2 + C B X Φ B2 are also employed to overcome the mutual interference. In this paper first order and second order derivative spectra are used for the analysis of rare earths. It is a simple and effective technique for accurate analysis of rare earths from a complex mixture. Absorption data in the first derivative mode is also presented. Analysis of Nd-Pr-Sm from their synthetic mixtures is reported. (author). 4 refs., 1 tab., 1 ill

DLLME-spectrophotometric determination of glyphosate residue in legumes.

Science.gov (United States)

Çetin, Emine; Şahan, Serkan; Ülgen, Ahmet; Şahin, Uğur

2017-09-01

A new separation and pre-concentration method for spectrophotometric determination of glyphosate herbicide was developed. Glyphosate was converted into dithiocarbamic acid with CS 2 , followed by copper in the presence of ammonia to promote complex formation. This complex was collected in a CH 2 Cl 2 organic drop and absorbance measured at 435nm. The analytical parameters, such as the amount of NH 3 , Cu(II) and CS 2 , type of extraction solutions, and the ratio of dispersive and organic liquids were optimized. The calibration curve was linear in the range 0.5-10mgl -1 . The limits of detection and quantification were calculated from 3s to 10s criterions as 0.21mgl -1 and 0.70mgl -1 , respectively. The developed method was applied to legume samples with the satisfactory recovery values of 98±4-102±3%. Copyright © 2017 Elsevier Ltd. All rights reserved.

Spectrophotometric Determination of Thorium in Low Grade Minerals and Ores

Energy Technology Data Exchange (ETDEWEB)

Arnfelt, A L; Edmundsson, I

1960-08-15

The following method is intended for the determination of microgram quantities of thorium in samples of minerals and ores. The mineral sample is decomposed by repeated sintering with sodium peroxide. After digestion with water thorium peroxide hydrate is recovered by centrifugation and dissolved in hydrochloric acid. Thorium is determined spectrophotometrically with naphtarson after its separation from metals forming chloro complexes which are adsorbed on a strongly basic anion exchange resin. Interferences from a few different ions have been studied. The time required for the analysis of one sample is about 4 hours, when analysing 12 samples simultaneously

Spectrophotometric Determination of Thorium in Low Grade Minerals and Ores

International Nuclear Information System (INIS)

Arnfelt, A.L.; Edmundsson, I.

1960-08-01

The following method is intended for the determination of microgram quantities of thorium in samples of minerals and ores. The mineral sample is decomposed by repeated sintering with sodium peroxide. After digestion with water thorium peroxide hydrate is recovered by centrifugation and dissolved in hydrochloric acid. Thorium is determined spectrophotometrically with naphtarson after its separation from metals forming chloro complexes which are adsorbed on a strongly basic anion exchange resin. Interferences from a few different ions have been studied. The time required for the analysis of one sample is about 4 hours, when analysing 12 samples simultaneously

Split kinetic energy method for quantum systems with competing potentials

International Nuclear Information System (INIS)

Mineo, H.; Chao, Sheng D.

2012-01-01

For quantum systems with competing potentials, the conventional perturbation theory often yields an asymptotic series and the subsequent numerical outcome becomes uncertain. To tackle such a kind of problems, we develop a general solution scheme based on a new energy dissection idea. Instead of dividing the potential energy into “unperturbed” and “perturbed” terms, a partition of the kinetic energy is performed. By distributing the kinetic energy term in part into each individual potential, the Hamiltonian can be expressed as the sum of the subsystem Hamiltonians with respective competing potentials. The total wavefunction is expanded by using a linear combination of the basis sets of respective subsystem Hamiltonians. We first illustrate the solution procedure using a simple system consisting of a particle under the action of double δ-function potentials. Next, this method is applied to the prototype systems of a charged harmonic oscillator in strong magnetic field and the hydrogen molecule ion. Compared with the usual perturbation approach, this new scheme converges much faster to the exact solutions for both eigenvalues and eigenfunctions. When properly extended, this new solution scheme can be very useful for dealing with strongly coupling quantum systems. - Highlights: ► A new basis set expansion method is proposed. ► Split kinetic energy method is proposed to solve quantum eigenvalue problems. ► Significant improvement has been obtained in converging to exact results. ► Extension of such methods is promising and discussed.

Spectrophotometric determination of copper with ascorbic acid

International Nuclear Information System (INIS)

Majeed, A.; Mustafa, M.M.; Asma, R.N.; Sareecha, N.

1996-01-01

Copper has been determined spectrophotometrically by using ascorbic acid as a chromagenic reagent. The complex formed in basic medium is measured for its absorbance at 340 n.m. Interference for 23 cations and 9 anions has also been checked. Effect of pH, time, temperature, ammonia, reagent concentration and interferents has been report. (author)

Spectrophotometric determination of copper with ascorbic acid

Energy Technology Data Exchange (ETDEWEB)

Majeed, A; Mustafa, M M; Asma, R N; Sareecha, N [Islamia Univ., Bahawalpur (Pakistan). Chemistry Dept.

1996-06-01

Copper has been determined spectrophotometrically by using ascorbic acid as a chromagenic reagent. The complex formed in basic medium is measured for its absorbance at 340 n.m. Interference for 23 cations and 9 anions has also been checked. Effect of pH, time, temperature, ammonia, reagent concentration and interferents has been report. (author).

Kinetics of cancer: a method to test hypotheses of genetic causation

Directory of Open Access Journals (Sweden)

Lipkin Steven M

2005-12-01

Full Text Available Abstract Background Mouse studies have recently compared the age-onset patterns of cancer between different genotypes. Genes associated with earlier onset are tentatively assigned a causal role in carcinogenesis. These standard analyses ignore the great amount of information about kinetics contained in age-onset curves. We present a method for analyzing kinetics that measures quantitatively the causal role of candidate genes in cancer progression. We use our method to demonstrate a clear association between somatic mutation rates of different DNA mismatch repair (MMR genotypes and the kinetics of cancer progression. Methods Most experimental studies report age-onset curves as the fraction diagnosed with tumors at each age for each group. We use such data to estimate smoothed survival curves, then measure incidence rates at each age by the slope of the fitted curve divided by the fraction of mice that remain undiagnosed for tumors at that age. With the estimated incidence curves, we compare between different genotypes the median age of cancer onset and the acceleration of cancer, which is the rate of increase in incidence with age. Results The direction of change in somatic mutation rate between MMR genotypes predicts the direction of change in the acceleration of cancer onset in all 7 cases (p ˜ 0.008, with the same result for the association between mutation rate and the median age of onset. Conclusion Many animal experiments compare qualitatively the onset curves for different genotypes. If such experiments were designed to analyze kinetics, the research could move to the next stage in which the mechanistic consequences of particular genetic pathways are related to the dynamics of carcinogenesis. The data we analyzed here were not collected to test mechanistic and quantitative hypotheses about kinetics. Even so, a simple reanalysis revealed significant insights about how DNA repair genotypes affect separately the age of onset and the

Development and validation of a UV-spectrophotometric method for the determination of pheniramine maleate and its stability studies

Science.gov (United States)

Raghu, M. S.; Basavaiah, K.; Ramesh, P. J.; Abdulrahman, Sameer A. M.; Vinay, K. B.

2012-03-01

A sensitive, precise, and cost-effective UV-spectrophotometric method is described for the determination of pheniramine maleate (PAM) in bulk drug and tablets. The method is based on the measurement of absorbance of a PAM solution in 0.1 N HCl at 264 nm. As per the International Conference on Harmonization (ICH) guidelines, the method was validated for linearity, accuracy, precision, limits of detection (LOD) and quantification (LOQ), and robustness and ruggedness. A linear relationship between absorbance and concentration of PAM in the range of 2-40 μg/ml with a correlation coefficient (r) of 0.9998 was obtained. The LOD and LOQ values were found to be 0.18 and 0.39 μg/ml PAM, respectively. The precision of the method was satisfactory: the value of relative standard deviation (RSD) did not exceed 3.47%. The proposed method was applied successfully to the determination of PAM in tablets with good accuracy and precision. Percentages of the label claims ranged from 101.8 to 102.01% with the standard deviation (SD) from 0.64 to 0.72%. The accuracy of the method was further ascertained by recovery studies via a standard addition procedure. In addition, the forced degradation of PAM was conducted in accordance with the ICH guidelines. Acidic and basic hydrolysis, thermal stress, peroxide, and photolytic degradation were used to assess the stability-indicating power of the method. A substantial degradation was observed during oxidative and alkaline degradations. No degradation was observed under other stress conditions.

Spectrophotometric determination of phosphorus in iron alloys employing a flow injection system

OpenAIRE

Gervasio,Ana P. G.; Miranda,Carlos E. S.; Luca,Gilmara C.; Tumang,Cristiane A.; Campos,Luis F. P.; Reis,Boaventura F.

2001-01-01

A flow-injection procedure for spectrophotometric determination of phosphorus in electrolytic iron and iron alloys is proposed. The method is based on the ammonium molybdate reaction followed by stannous chloride reduction in acidic medium. In order to circumvent the severe interference caused by the major constituents such as Fe(III) and Cr(III), a mini-column packed with AG50W-X8 resin was coupled to the manifold. A sample throughput of 40 determinations per hour, a dynamical range from P 0...

Study the oxidation kinetics of uranium using XRD and Rietveld method

Energy Technology Data Exchange (ETDEWEB)

Zhang Yanzhi; Guan Weijun; Wang Qinguo; Wang Xiaolin; Lai Xinchun; Shuai Maobing, E-mail: yanzhizh@163.com [China Academy of Engineering Physics, PO Box 919-71, Mianyang, Sichuan, 621900 (China)

2010-03-15

The surface oxidation of uranium metal has been studied by X-ray diffraction (XRD) and Rietveld method in the range of 50{approx}300deg. C in air. The oxidation processes are analyzed by XRD to determine the extent of surface oxidation and the oxide structure. The dynamics expression for the formation of UO{sub 2} was derived. At the beginning, the dynamic expression was nonlinear, but switched to linear subsequently for uranium in air and humid oxygen. That is, the growth kinetics of UO{sub 2} can be divided into two stages: nonlinear portion and linear portion. Using the kinetic data of linear portion, the activation energy of reaction between uranium and air was calculated about 46.0 kJ/mol. However the content of oxide as a function of time was linear in humid helium ambience. Contrast the dynamics results, it prove that the absence of oxygen would accelerate the corrosion rate of uranium in the humid gas. We can find that the XRD and Rietveld method are a useful convenient method to estimate the kinetics and thermodynamics of solid-gas reaction.

DETERMINATION OF KINETICS OF DEGRADATION AND MOBILITY OF DITHIOCARBAMATES FUNGICIDES IN AQUEOUS MEDIA AND IN MOROCCAN SOIL

Directory of Open Access Journals (Sweden)

Said El Antri

2010-07-01

Full Text Available Contribution analysis of dithiocarbamates pesticides used on tomatoes treatment has been reported. The study is focused on analysis and determination of some dithiocarbamates like, Maneb, Mancozeb, Zineb and Propineb, in order to achieve accurate impact of theses pesticides on water and soil. Analysis method is based on decomposition of dithiocarbamate by heating under acidic attack to give carbon disulfide complexed with copper acetate solution in presence of diethanolamine. Complex formed is dosed spectrophotometrically at 435 nm. Degradation kinetic of dithiocarbamate in aqueous media have been realized and proved that dithiocarbamate are degraded by simple air exposition. In the other hand, pH affects also dithiocarbamate degradation by increasing hydroxyl ions to participate for dithiocarbamate instability. Dithiocarbamate mobility on Moroccan soils samples have been realised and don’t have the same degradation mode.

A comparative study between three stability indicating spectrophotometric methods for the determination of diatrizoate sodium in presence of its cytotoxic degradation product based on two-wavelength selection

Science.gov (United States)

Riad, Safaa M.; El-Rahman, Mohamed K. Abd; Fawaz, Esraa M.; Shehata, Mostafa A.

2015-06-01

Three sensitive, selective, and precise stability indicating spectrophotometric methods for the determination of the X-ray contrast agent, diatrizoate sodium (DTA) in the presence of its acidic degradation product (highly cytotoxic 3,5-diamino metabolite) and in pharmaceutical formulation, were developed and validated. The first method is ratio difference, the second one is the bivariate method, and the third one is the dual wavelength method. The calibration curves for the three proposed methods are linear over a concentration range of 2-24 μg/mL. The selectivity of the proposed methods was tested using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of DTA in pharmaceutical dosage forms without interference from other dosage form additives. The results were statistically compared with the official US pharmacopeial method. No significant difference for either accuracy or precision was observed.

Possibilities and limitations of the kinetic plot method in supercritical fluid chromatography.

Science.gov (United States)

De Pauw, Ruben; Desmet, Gert; Broeckhoven, Ken

2013-08-30

Although supercritical fluid chromatography (SFC) is becoming a technique of increasing importance in the field of analytical chromatography, methods to compare the performance of SFC-columns and separations in an unbiased way are not fully developed. The present study uses mathematical models to investigate the possibilities and limitations of the kinetic plot method in SFC as this easily allows to investigate a wide range of operating pressures, retention and mobile phase conditions. The variable column length (L) kinetic plot method was further investigated in this work. Since the pressure history is identical for each measurement, this method gives the true kinetic performance limit in SFC. The deviations of the traditional way of measuring the performance as a function of flow rate (fixed back pressure and column length) and the isopycnic method with respect to this variable column length method were investigated under a wide range of operational conditions. It is found that using the variable L method, extrapolations towards other pressure drops are not valid in SFC (deviation of ∼15% for extrapolation from 50 to 200bar pressure drop). The isopycnic method provides the best prediction but its use is limited when operating closer towards critical point conditions. When an organic modifier is used, the predictions are improved for both methods with respect to the variable L method (e.g. deviations decreases from 20% to 2% when 20mol% of methanol is added). Copyright © 2013 Elsevier B.V. All rights reserved.

Sensitive flow-injection spectrophotometric analysis of bromopride

Science.gov (United States)

Lima, Liliane Spazzapam; Weinert, Patrícia Los; Pezza, Leonardo; Pezza, Helena Redigolo

2014-12-01

A flow injection spectrophotometric procedure employing merging zones is proposed for direct bromopride determination in pharmaceutical formulations and biological fluids. The proposed method is based on the reaction between bromopride and p-dimethylaminocinnamaldehyde (p-DAC) in acid medium, in the presence of sodium dodecyl sulfate (SDS), resulting in formation of a violet product (λmax = 565 nm). Experimental design methodologies were used to optimize the experimental conditions. The Beer-Lambert law was obeyed in a bromopride concentration range of 3.63 × 10-7 to 2.90 × 10-5 mol L-1, with a correlation coefficient (r) of 0.9999. The limits of detection and quantification were 1.07 × 10-7 and 3.57 × 10-7 mol L-1, respectively. The proposed method was successfully applied to the determination of bromopride in pharmaceuticals and human urine, and recoveries of the drug from these media were in the ranges 99.6-101.2% and 98.6-102.1%, respectively. This new flow injection procedure does not require any sample pretreatment steps.

Mean centering of ratio spectra and successive derivative ratio spectrophotometric methods for determination of isopropamide iodide, trifluoperazine hydrochloride and trifluoperazine oxidative degradate

Directory of Open Access Journals (Sweden)

Maha M. Abdelrahman

2016-09-01

Full Text Available Two sensitive, selective and precise stability indicating methods for the determination of isopropamide iodide (ISO, trifluoperazine hydrochloride (TPZ and trifluoperazine oxidative degradate (DEG were developed and validated. Method A is a successive derivative ratio spectrophotometric one, which depends on the successive derivative of ratio spectra in two steps using 0.1 N HCl as a solvent and measuring TPZ at 250.4 and 257.2 nm, ISO at 223 and 228 nm and DEG at 210.6, 213 and 270.2 nm. Method B is mean centering of ratio spectra which depends on using the mean centered ratio spectra in two successive steps and measuring the mean centered values of the second ratio spectra at 322, 355 and 339 nm for TPZ, ISO and DEG, respectively. Factors affecting the developed methods were studied and optimized, moreover, they have been validated as per ICH guidelines and the results demonstrated that the suggested methods are reliable, reproducible and suitable for routine use with short analysis time. Statistical analysis of the two developed methods with the reported one using F- and Student’s t-test showed no significant difference regarding accuracy and precision.

Spectrophotometric determination of nitrite in simulated Purex Process solutions

Energy Technology Data Exchange (ETDEWEB)

Araujo, I.daC. de; Matsuda, H T; Araujo, B.F. de; Araujo, J.A. de

1984-01-01

A spectrophotometric method for nitrite determination in simulated Purex Process solutions is presented, utilizing the Griess reagent for the formation of the coloured azocompound with an absorption maximum at 525 nm. Molar absortivity was 36,262 and the sensitivity of the method 10/sup -6/M for nitrite. The calibration curve is linear in the range of 2 to 30..mu..g NO/sup -//sub 2//25 ml in cells of 1 cm optical path. The method can be used in the presence of uranium up to limits of an U/NO/sup -//sub 2/ ratio of 150. Test solutions were prepared to simulate composition and concentrations as obtained by irradiating standard fuel with a neutro flux of 3.2 x 10/sup 13/ n.s/sup -1/.cm/sup -2/, with a burn-up value of 33,000 Mwd/T and cooling time of two years. Nitrite determinations in these solutions were accurate within limits of 5%.

The kinetics of the reduction reaction of plutonium(IV) with N,N-dimethylhydroxylamine

International Nuclear Information System (INIS)

Yanxin Chen; Honbing Tang; Jinping Liu; Hui He

2011-01-01

The kinetics of reduction reactions between N,N-dimethylhydroxylamine (DMHAN) and plutonium(IV) in nitric acid solution have been studied spectrophotometrically. The kinetic equation of the reaction is determined to be -d[Pu(IV)]/dt = k 0 [Pu(IV)][DMHAN] 1.18 /[H + ] 2.22 at the beginning, where, the rate constant of the reaction (k 0 ) is 10.5 ± 1.8(mol/L) 1.04 s -1 at 14.5 deg C. By regressing of the time-concentration curve of the reaction, The complete rate equation is calculated as -d[Pu(IV)] / dt = k[Pu(IV)] 2 [DMHAN] 1.18 /[H + ] 2.22 / 8.12[Pu(III)]+95.9[Pu(IV)] with the reaction constant k about 1,000(mol/L) 1.04 s -1 at 14.5 deg C and an ionic strength (μ) of 4.0 mol/L. (author)

New method for the determination of precipitation kinetics using a laminar jet reactor

NARCIS (Netherlands)

Al Tarazi, M.Y.M.; Heesink, Albertus B.M.; Versteeg, Geert

2005-01-01

In this paper a new experimental method for determining the kinetics of fast precipitation reactions is introduced. Use is made of a laminar jet reactor, which is also frequently applied to determine the kinetics of homogeneous gas–liquid reactions. The liquid containing one or more of the

New method for the determination of precipitation kinetics using a laminar jet reactor

NARCIS (Netherlands)

Al-Tarazi, Mousa; Heesink, A. Bert M.; Versteeg, Geert F.

2005-01-01

In this paper a new experimental method for determining the kinetics of fast precipitation reactions is introduced. Use is made of a laminar jet reactor, which is also frequently applied to determine the kinetics of homogeneous gas-liquid reactions. The liquid containing one or more of the

Determination of the kinetic parameters of BeO thermoluminescent samples using different methods

Energy Technology Data Exchange (ETDEWEB)

Algarve, Fábio J.; Caldas, Linda V.E., E-mail: fjalgarve@ipen.br, E-mail: lcaldas@ipen.br [Instituto de Pesquisas Energéticas e Nucleares (IPEN/CNEN-SP), São Paulo, SP (Brazil)

2017-07-01

The objective of this work was to determine the kinetic parameters of BeO thermoluminescent (TL) samples. The knowledge of the kinetic parameters is important for the general description of the physical characteristics of a thermoluminescent material. Using a linear heating rate of 5K/s{sup -1}, the BeO peak temperatures obtained were (474.7 ± 1.2) K and (620.5 ± 1.2) K, respectively, for the first and second TL peaks. The peak shape and the glow curve area measurement methods and the Urbach formula have been used for the trap parameter determination. A kinetic order of about two was determined for the first peak, whereas the second peak followed the first-order kinetics according to the geometrical factor. The energy activation values obtained using different kinds of measurements are in good agreement, including the Kitis method for deconvolution of the glow curve. Furthermore the results agree with those presented by other authors. (author)

Spectrophotometric Determination of Doxycycline Hyclate in Pure and Capsule using Diazotization Reaction

Directory of Open Access Journals (Sweden)

Ruba Fahmi Abbas

2017-07-01

Full Text Available A sensitive spectrophotometric method has been developed for the determination of Doxycycline hyclate (DCH as pure and  capsule forms. This method is based on diazotization of primary amine group of benzocaine with sodium nitrite in hydrochloric acid medium; the formed diazonium salt is then reacted with DCH in sodium hydroxide medium, to form yellow – orange Azo dye. Beer's law is obeyed in the concentration rang 16-34mg. ml-1 at 480 nm with detection limit LOD and molar absorptivity Є were found to be 0.418 mg.ml-1 and 2.214× 10+4 L.mol-1.cm-1, respectively.

Yonsei Evolutionary Population Synthesis (YEPS). II. Spectro-photometric Evolution of Helium-enhanced Stellar Populations

Energy Technology Data Exchange (ETDEWEB)

Chung, Chul; Yoon, Suk-Jin; Lee, Young-Wook, E-mail: chulchung@yonsei.ac.kr, E-mail: sjyoon0691@yonsei.ac.kr [Center for Galaxy Evolution Research, Yonsei University, Seoul 03722 (Korea, Republic of)

2017-06-20

The discovery of multiple stellar populations in Milky Way globular clusters (GCs) has stimulated various follow-up studies on helium-enhanced stellar populations. Here we present the evolutionary population synthesis models for the spectro-photometric evolution of simple stellar populations (SSPs) with varying initial helium abundance ( Y {sub ini}). We show that Y {sub ini} brings about dramatic changes in spectro-photometric properties of SSPs. Like the normal-helium SSPs, the integrated spectro-photometric evolution of helium-enhanced SSPs is also dependent on metallicity and age for a given Y {sub ini}. We discuss the implications and prospects for the helium-enhanced populations in relation to the second-generation populations found in the Milky Way GCs. All of the models are available at http://web.yonsei.ac.kr/cosmic/data/YEPS.htm.

Yonsei Evolutionary Population Synthesis (YEPS). II. Spectro-photometric Evolution of Helium-enhanced Stellar Populations

International Nuclear Information System (INIS)

Chung, Chul; Yoon, Suk-Jin; Lee, Young-Wook

2017-01-01

The discovery of multiple stellar populations in Milky Way globular clusters (GCs) has stimulated various follow-up studies on helium-enhanced stellar populations. Here we present the evolutionary population synthesis models for the spectro-photometric evolution of simple stellar populations (SSPs) with varying initial helium abundance ( Y ini ). We show that Y ini brings about dramatic changes in spectro-photometric properties of SSPs. Like the normal-helium SSPs, the integrated spectro-photometric evolution of helium-enhanced SSPs is also dependent on metallicity and age for a given Y ini . We discuss the implications and prospects for the helium-enhanced populations in relation to the second-generation populations found in the Milky Way GCs. All of the models are available at http://web.yonsei.ac.kr/cosmic/data/YEPS.htm.

SPECTROPHOTOMETRIC STUDIES OF SANGUINARINE-Β-CYCLODEXTRIN COMPLEX FORMATION

Directory of Open Access Journals (Sweden)

Veaceslav Boldescu

2008-06-01

Full Text Available The main aim of this study was to investigate the influence of pH and the presence of hydrophilic polymer polyvinylpyrrolidone on the formation of sanguinarine-β-cyclodextrin (SANG-β-CD inclusion complex. Spectrophotometric studies of the SANG-β-CD systems in the presence and without 0.1 % PVP at the pH 5.0 did not show any evidence of the complex formation. However, the same systems showed several obvious evidences at the pH 8.0: the hyperchromic and the hypochromic effects and the presence of the isosbestic point in the region of 200 – 210 nm. The association constants calculated by three linear methods: Benesi-Hildebrand, Scott and Scatchard, were two times higher for the systems with addition of 0.1% PVP than for the systems without it.

A novel flow-based strategy for implementing differential kinetic analysis

International Nuclear Information System (INIS)

Fortes, Paula R.; Meneses, Silvia R.P.; Zagatto, Elias A.G.

2006-01-01

Differential kinetic analysis can be implemented in a multi-pumping flow system, and this was demonstrated in relation to an improved spectrophotometric catalytic determination of iron and vanadium in Fe-V alloys. The method exploited the influence of Fe(II) and V(IV) on the rate of iodide oxidation by Cr(VI) under acidic conditions; therefore the Jones reductor was needed. The sample was inserted into an acidic KI stream that acted also as carrier stream, and a Cr(VI) solution was added by confluence. Successive measurements were performed during sample passage through the detector, each one related to a different yet reproducible condition for reaction development. Data treatment involved multivariate calibration by the PLS algorithm. The proposed system is very simple and rugged, allowing about 50 samples to be run per hour, meaning 48 mg KI per determination. The first two latent variables carry ca. 94% of the analytical information, pointing out that the intrinsic dimensionality of the data set is two. Results are in agreement with inductively coupled argon plasma-optical emission spectrometry

Spectrophotometric assay of creatinine in human serum sample

Directory of Open Access Journals (Sweden)

Avinash Krishnegowda

2017-05-01

Full Text Available A new spectrophotometric method for the analysis of creatinine concentration in human serum samples is developed. The method explores the oxidation of p-methylamino phenol sulfate (Metol in the presence of copper sulfate and creatinine which yields an intense violet colored species with maximum absorbance at 530 nm. The calibration graph of creatinine by fixed time assay ranged from 4.4 to 620 μM. Recovery of creatinine in human serum samples varied from 101% to 106%. Limit of detection and limit of quantification were 0.145 μM and 0.487 μM respectively. Sandell’s sensitivity was 0.112 μg cm−2 and molar absorptivity was 0.101 × 104 L mol−1 cm−1. Within day precision was 2.5–4.8% and day-to-day precision range was 3.2–7.8%. The robustness and ruggedness of the method expressed in RSD values ranged from 0.78% to 2.12% and 1.32% to 3.46% respectively, suggesting that the developed method was rugged. This method provides good sensitivity and is comparable to standard Jaffe’s method with comparatively less interference from foreign substances.

Simultaneous spectrophotometric determination of tungsten and molybdenum with dithiol

International Nuclear Information System (INIS)

Navale, A.S.

1987-01-01

Toluene-3,4-dithiol is a very sensitive reagent for the spectrophotometric determination of tungsten and molybdenum. Since the absorption spectra of the dithiol complexes of these two elements overlap, a separation of the two elements is carried out. This leads to time consuming extraction procedures. Measuring the absorption of the mixed complexes at two wavelengths and solving a set of simultaneous equations is also not favorable because a lot of time and effort is required for solving the simultaneous equations for each sample. A faster and simpler method is described here for the simultaneous determination of the two elements. The method is based on measurement of absorbance of the mixed complexes at three pre-selected wavelengths and simple calculations involving the absorbance differences. The criteria for selecting the three wavelengths and the theory are described. Application of the method for the determination of tungsten and molybdenum in ore samples is presented. The method is applicable to any similar system consisting of two interfering components. 4 figures, 2 tables, 6 refs. (author)

Spectrophotometric Analysis of Phosphoric Acid Leakage in High-Temperature Phosphoric Acid-Doped Polybenzimidazole Membrane Fuel Cell Application

Directory of Open Access Journals (Sweden)

Seungyoon Han

2016-01-01

Full Text Available High-temperature proton exchange membrane fuel cells (HT-PEMFCs utilize a phosphoric acid- (PA- doped polybenzimidazole (PBI membrane as a polymer electrolyte. The PA concentration in the membrane can affect fuel cell performance, as a significant amount of PA can leak from the membrane electrode assembly (MEA by dissolution in discharged water, which is a byproduct of cell operation. Spectrophotometric analysis of PA leakage in PA-doped polybenzimidazole membrane fuel cells is described here. This spectrophotometric analysis is based on measurement of absorption of an ion pair formed by phosphomolybdic anions and the cationoid color reagent. Different color reagents were tested based on PA detection sensitivity, stability of the formed color, and accuracy with respect to the amount of PA measured. This method allows for nondestructive analysis and monitoring of PA leakage during HT-PEMFCs operation.

Spectrophotometric and spectrofluorometric determination of uranium using a flotation process with benzoate and rivanol

Energy Technology Data Exchange (ETDEWEB)

Lopez Herroz, C.; Hernandez, M.; Sanchez-Pedreno, C.

1988-01-01

Tribenzouranyl anion forms with rivnol an ion-association compound which is floated with isopropyl ether and dissolved in ethanol. As a consequence, new spectrophotometric and spectrofluorimetric methods for the determination of trace amounts of uranium are developed. At 373 nm Beer's law is obeyed over the range 10-150 /mu/g of uranium. When the spectrofluorimetric technique is used, calibration graph is linear in the 2-25 /mu/g range.

Spectrophotometric determination of silica in water. Low range; Determinacion espectrofotometrica de silicio en aguas. Rango bajo

Energy Technology Data Exchange (ETDEWEB)

Acosta L, E. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)]. e-mail: eal@nuclear.inin.mx

1992-07-15

The spectrophotometric method for the determination of the silica element in water, demineralized water, raw waters, laundry waters, waters treated with ion exchange resins and sea waters is described. This method covers the determination of the silica element in the interval from 20 to 1000 {mu}g/l on 50 ml. of base sample. These limits its can be variable if the size of the used aliquot one is changed for the final determination of the silica element. (Author)

Determination of dissolved inorganic species of iodine by spectrophotometric titration

Energy Technology Data Exchange (ETDEWEB)

Pesavento, Maria; Profumo, Antonella; Biesuz, Raffaela

1987-09-01

A method for determining iodate and iodine (+1) in aqueous solutions is proposed. The assay is similar to a previously described method for the determination of iodide and iodine (O), which were titrated with standard iodate in hydrochloric acid solution. A sample solution made 0.5-1.5 M in hydrochloric acid is titrated with a standard iodide solution and monitored spectrophotometrically at 230 nm. The species involved have strong absorbances that are well differentiated at this wavelength. By combining the two titrations it is possible to resolve any mixture of species of iodine in different oxidation states. The precision of the method (standard deviation) is the same both when determining a single species (IO/sub 3/-,I+,1/sub 2/ or I-) and a mixture, and is equal to 2 x 10/sup -7/ M. Chloride and bromide, even at very high concentrations, do not interfere.

Determination of dissolved inorganic species of iodine by spectrophotometric titration

International Nuclear Information System (INIS)

Pesavento, Maria; Profumo, Antonella

1987-01-01

A method for determining iodate and iodine (+1) in aqueous solutions is proposed. The assay is similar to a previously described method for the determination of iodide and iodine (O), which were titrated with standard iodate in hydrochloric acid solution. A sample solution made 0.5-1.5 M in hydrochloric acid is titrated with a standard iodide solution and monitored spectrophotometrically at 230 nm. The species involved have strong absorbances that are well differentiated at this wavelength. By combining the two titrations it is possible to resolve any mixture of species of iodine in different oxidation states. The precision of the method (standard deviation) is the same both when determining a single species (IO 3 -,I+,1 2 or I-) and a mixture, and is equal to 2 x 10 -7 M. Chloride and bromide, even at very high concentrations, do not interfere. (author)

A simple method for simultaneous spectrophotometric determination of brilliant blue fcf and sunset yellow fcf in food samples after cloud point extraction

International Nuclear Information System (INIS)

Heydari, R.

2016-01-01

In this study, a simple and low-cost method for extraction and pre-concentration of brilliant blue FCF and sunset yellow FCF in food samples using cloud point extraction (CPE) and spectrophotometric detection was developed. The effects of main factors such as solution pH, surfactant concentration, salt and its concentration, incubation time and temperature on the CPE of both dyes were investigated and optimized. Linear range of calibration graphs were obtained in the range of 16.0-1300 ng mL-1 for brilliant blue FCF and 25.0-1300 ng mL/sup -1/ for sunset yellow FCF under the optimum conditions. Limit of detection values for brilliant blue FCF and sunset yellow FCF were 3 and 6 ng mL-1, respectively. The relative standard deviation (RSD) values of both dyes for repeated measurements (n=6) were less than 4.57 %. The obtained results were demonstrated the proposed method can be applied satisfactory to determine these dyes in different food samples. (author)

On-line Speciation of Cr(III) and Cr(VI) by Flow Injection Analysis With Spectrophotometric Detection and Chemometrics

DEFF Research Database (Denmark)

Diacu, Elena; Andersen, Jens Enevold Thaulov

2003-01-01

A flow injection system has been developed, for on-line speciation. of Cr(III) and Cr(VI) by the Diphenylcarbazide (DPC) method with H2O2 oxidation followed by spectrophotometric detection at the 550 nm wavelength. The data thus obtained were subjected to a chemometric analysis (PLS), which showe...

Effect of bilirubin on the spectrophotometric and radionuclide assay for serum angiotensin-converting enzyme

International Nuclear Information System (INIS)

Saxe, A.W.; Hollinger, M.A.; Essam, T.

1986-01-01

The effect of bilirubin on serum angiotensin-converting enzyme (ACE) activity was studied with spectrophotometric and radionuclide assays. In the spectrophotometric assay addition of bilirubin to normal serum from dog, mouse, and human produced a dose-related inhibition of ACE activity. A 50% decrease in human ACE activity was produced by the addition of approximately 250 mg/L in vitro. Serum from icteric patients with elevated bilirubin was also associated with a reduction in ACE activity in the spectrophotometric assay. A 50% decrease in ACE activity in these samples was associated with a serum bilirubin of approximately 220 mg/L. In the radionuclide assay, however, addition of bilirubin to normal human serum failed to reduce measured ACE activity. The use of a radionuclide assay for serum ACE in clinical samples offers the advantage of less interference from serum bilirubin

Rapid and specific spectrophotometric and RP-HPLC methods for the determination of ascorbic acid in fruits juices and in human plasma

International Nuclear Information System (INIS)

Arayne, M.S.; Bibi, Z.; Sultana, N.

2009-01-01

Ascorbic acid (AA) is one of the most important water soluble vitamin in the human diet, present naturally in a wide range of foods, especially fruits and vegetables. The objective of this study was to develop a rapid, sensitive and specific method for the determination of ascorbic acid (vitamin C) from a variety of sources like fresh fruits or from human plasma using spectrophotometric technique or by RP-HPLC. Initially, estimation of vitamin C was carried out spectrophotometrically as UV spectroscopy is a trusted technique to monitor small quantities of drugs and vitamins. The assay was linear over the concentration range of 0.05-100 mi cro g/mL/sup -I/. In the second procedure, we attempted to separate and quantitate ascorbic acid from fruit juices as well as from human plasma by RP-HPLC with UV detection. This has been possible because of the diversity of columns and conditions of analysis available. Chromatographic separation was successfully achieved on a pre-packed Kromasil 100, C/sub 18/ (5 macro m 25 x 0.46) column using acetonitrile water (60:40; v/v) as mobile phase at a flow rate of 0.75 mL/sup -min/ and effluent monitored at 265 nm. The assay was also linear over the concentration range of 0.05-100 micro g/mL/sub -1/, with recovery ranging from 99.0-100.0 % and intra and inter day CV <3 % when applied to the analysis of ascorbic acid from fruit juice available in Pakistan at the time of study Grape fruit, malta, mosami, sweetlemon, fruiter, lemon, lime, custard apple, orange, lemon, guava and papaya juice were found to be very rich in as ascorbic acid, while chikoo, pear, apricot, peach, carrot and some other fruits were found to be poor sources of ascorbic acid. (author)

Spectrophotometric determination of Tl carrier in 201Tl-TlCl injection

International Nuclear Information System (INIS)

Gong Quansheng; Jing Lie

1997-01-01

A simple and sensitive method for the spectrophotometric determination of carrier content (Thallium) in 201 Tl-TlCl injection is described. Thallium (I) is oxidised to Thallium (III) by aqueous bromine, then excess bromine is removed by adding sulfosalicylic acid. In buffer solution (NH 4 Cl-NH 4 OH) at pH 11.7 with the presence of emulsifier OP, thallium (III) and cadion form a complex having an absorption maximum at 469 nm with a molar absorptivity of 1.37 x 10 4 m 2 /mol. Beer's law is obeyed in the concentration range of 0-7 μg/5 mL. The effect of impurity elements in 201 Tl-TlCl injection is examined. It is an ideal method for the analysis of radioactive solution

Gas-Kinetic Theory Based Flux Splitting Method for Ideal Magnetohydrodynamics

Science.gov (United States)

Xu, Kun

1998-01-01

A gas-kinetic solver is developed for the ideal magnetohydrodynamics (MHD) equations. The new scheme is based on the direct splitting of the flux function of the MHD equations with the inclusion of "particle" collisions in the transport process. Consequently, the artificial dissipation in the new scheme is much reduced in comparison with the MHD Flux Vector Splitting Scheme. At the same time, the new scheme is compared with the well-developed Roe-type MHD solver. It is concluded that the kinetic MHD scheme is more robust and efficient than the Roe- type method, and the accuracy is competitive. In this paper the general principle of splitting the macroscopic flux function based on the gas-kinetic theory is presented. The flux construction strategy may shed some light on the possible modification of AUSM- and CUSP-type schemes for the compressible Euler equations, as well as to the development of new schemes for a non-strictly hyperbolic system.

Perturbative method for the derivation of quantum kinetic theory based on closed-time-path formalism

International Nuclear Information System (INIS)

Koide, Jun

2002-01-01

Within the closed-time-path formalism, a perturbative method is presented, which reduces the microscopic field theory to the quantum kinetic theory. In order to make this reduction, the expectation value of a physical quantity must be calculated under the condition that the Wigner distribution function is fixed, because it is the independent dynamical variable in the quantum kinetic theory. It is shown that when a nonequilibrium Green function in the form of the generalized Kadanoff-Baym ansatz is utilized, this condition appears as a cancellation of a certain part of contributions in the diagrammatic expression of the expectation value. Together with the quantum kinetic equation, which can be derived in the closed-time-path formalism, this method provides a basis for the kinetic-theoretical description

Spectrophotometric determination of nitrite based on its catalytic effect on the reaction of nuclear fast red and potassium bromate

Directory of Open Access Journals (Sweden)

HASSAN ZAVVAR MOUSAVI

2009-08-01

Full Text Available A highly selective and sensitive catalytic spectrophotometric method was developed for the determination of nitrite in water samples. The method is based on its catalytic effect on the nuclear fast red–potassium bromate redox reaction in acidic medium. The reaction was followed spectrophotometrically by measuring the change in the absorbance at 518 nm of nuclear fast red 5 min after initiation of the reaction. In this study, the experimental parameters were optimized and the effects of other cations and anions on the determination of nitrite were examined. The calibration graph was linear in the range 2.0–45 µg mL-1 of nitrite. The relative standard deviations for the determination of 15 and 30 µg mL-1 of nitrite were 3.1 and 1.75 %, respectively (n = 8. The detection limit calculated from three times the standard deviation of the blank 3Sb was 0.7 µg mL-1. The method was successfully applied to the determination of nitrite in spiked tap, natural and wastewater samples.

Second-order kinetic model for the sorption of cadmium onto tree fern: a comparison of linear and non-linear methods.

Science.gov (United States)

Ho, Yuh-Shan

2006-01-01

A comparison was made of the linear least-squares method and a trial-and-error non-linear method of the widely used pseudo-second-order kinetic model for the sorption of cadmium onto ground-up tree fern. Four pseudo-second-order kinetic linear equations are discussed. Kinetic parameters obtained from the four kinetic linear equations using the linear method differed but they were the same when using the non-linear method. A type 1 pseudo-second-order linear kinetic model has the highest coefficient of determination. Results show that the non-linear method may be a better way to obtain the desired parameters.

The relationship between the Wigner-Weyl kinetic formalism and the complex geometrical optics method

OpenAIRE

Maj, Omar

2004-01-01

The relationship between two different asymptotic techniques developed in order to describe the propagation of waves beyond the standard geometrical optics approximation, namely, the Wigner-Weyl kinetic formalism and the complex geometrical optics method, is addressed. More specifically, a solution of the wave kinetic equation, relevant to the Wigner-Weyl formalism, is obtained which yields the same wavefield intensity as the complex geometrical optics method. Such a relationship is also disc...

Spectrophotometric titration of sulfates in the presence of zirconium

International Nuclear Information System (INIS)

Kuznetsov, V.V.; Kotova, S.S.; Molokanova, L.G.; Chekmarev, A.M.; Yagodin, G.A.

1978-01-01

The procedure has been proposed for express determination of sulphate ions in the presence of zirconium by spectrophotometric titration with the use of barium chloride and nitrochromazo as an indicator. The procedure is based on bonding zirconium into a more stable complex with EDTA (ethylenediaminotetraacetic acid). The presence of excess of EDTA and zirconium (4) complexonate in the solution being titrated does not affect the titration curve shape and the character of break on the curve in the equivalence point. A complete demasking of SO 4 2- is observed in the case of 1O-fold excess of EDTA with respect to zirconium (4). Statistic evaluation of the method has shown that the results of titration can be distorted by chance errors only

SPECTROPHOTOMETRIC DETERMINATION OF CHLOROPHYLLS AND CAROTENOIDS. AN EFFECT OF SONICATION AND SAMPLE PROCESSING

Directory of Open Access Journals (Sweden)

Jana Braniša

2014-02-01

Full Text Available Chlorophylls and carotenoids are abundant pigments in plants, algae and cyanobacteria. In this study we verified the applicability of two previously developed UV-vis spectrophotometric methods for simultaneous quantitative determination of chlorophylls (a, b and carotenoids (lycopene, β-carotene or total carotenoids. The pigments were extracted from the strawberries, apricots and raspberries in both the acetone-water and acetone-hexane mixtures. Based on the statistical evaluation of the results the combination of mechanical disruption and sonication of fruit samples seems to be a suitable way to improve the pigment extraction efficiency from fruits in both types of solvents. In the case of apricot and raspberry fruit extracts the amount of chlorophylls and carotenoids calculated from the proposed equations was comparable to those published by other authors. However, the spectrophotometric determination of β-carotene content in strawberry acetone-hexane extract appeared to be problematic mainly due to the fact that carotenoids exhibited overlapping chlorophyll absorption bands. Overlap of bands leads to the negative values calculated from the proposed equation for the β-carotene content. The results indicate the limitations in use of the proposed set of equations for plant samples with comparable amounts of studied pigments.

Improvement of neutron kinetics module in TRAC-BF1code: one-dimensional nodal collocation method

Energy Technology Data Exchange (ETDEWEB)

Jambrina, Ana; Barrachina, Teresa; Miro, Rafael; Verdu, Gumersindo, E-mail: ajambrina@iqn.upv.es, E-mail: tbarrachina@iqn.upv.es, E-mail: rmiro@iqn.upv.es, E-mail: gverdu@iqn.upv.es [Universidade Politecnica de Valencia (UPV), Valencia (Spain); Soler, Amparo, E-mail: asoler@iberdrola.es [SEA Propulsion S.L., Madrid (Spain); Concejal, Alberto, E-mail: acbe@iberdrola.es [Iberdrola Ingenieria y Construcion S.A.U., Madrid (Spain)

2013-07-01

The TRAC-BF1 one-dimensional kinetic model is a formulation of the neutron diffusion equation in the two energy groups' approximation, based on the analytical nodal method (ANM). The advantage compared with a zero-dimensional kinetic model is that the axial power profile may vary with time due to thermal-hydraulic parameter changes and/or actions of the control systems but at has the disadvantages that in unusual situations it fails to converge. The nodal collocation method developed for the neutron diffusion equation and applied to the kinetics resolution of TRAC-BF1 thermal-hydraulics, is an adaptation of the traditional collocation methods for the discretization of partial differential equations, based on the development of the solution as a linear combination of analytical functions. It has chosen to use a nodal collocation method based on a development of Legendre polynomials of neutron fluxes in each cell. The qualification is carried out by the analysis of the turbine trip transient from the NEA benchmark in Peach Bottom NPP using both the original 1D kinetics implemented in TRAC-BF1 and the 1D nodal collocation method. (author)

Micellar modified spectrophotometric determination of nitrobenzenes based upon reduction with tin(II), diazotisation and coupling with the Bratton-Marshall reagent.

Science.gov (United States)

Escrig-Tena, I; Alvarez Rodríguez, L; Esteve-Romero, J; García-Alvarez-Coque, M C

1998-09-01

Nitrobenzenes, such as the antibiotic chloramphenicol, the vasodilator nicardipine, and the herbicides dinitramin, dinobuton, fenitrothion, methylparathion, oxyfluorfen, parathion, pendimethalin, quintozene, and trifluralin, were determined by using a spectrophotometric method in the visible region (540 nm). The method was based on the reduction of the nitrobenzenes to arylamines with tin(II) chloride, diazotisation of the arylamines and coupling of the diazonium ions with the Bratton-Marshall reagent. The two latter reactions were performed in a micellar medium of sodium dodecyl sulphate. The linear calibration range was 2x10(-6) to 7x10(-5) M (r>0.999), with limits of detection in the 10(-7) M level, which is 2-6 fold lower with respect to the corresponding spectrophotometric procedure in non-micellar medium. The procedure was applied to the analysis of the compounds in commercial preparations (pharmaceuticals and herbicide formulations) and in water samples, with good recoveries.

The mass angular scattering power method for determining the kinetic energies of clinical electron beams

International Nuclear Information System (INIS)

Blais, N.; Podgorsak, E.B.

1992-01-01

A method for determining the kinetic energy of clinical electron beams is described, based on the measurement in air of the spatial spread of a pencil electron beam which is produced from the broad clinical electron beam. As predicted by the Fermi-Eyges theory, the dose distribution measured in air on a plane, perpendicular to the incident direction of the initial pencil electron beam, is Gaussian. The square of its spatial spread is related to the mass angular scattering power which in turn is related to the kinetic energy of the electron beam. The measured spatial spread may thus be used to determine the mass angular scattering power, which is then used to determine the kinetic energy of the electron beam from the known relationship between mass angular scattering power and kinetic energy. Energies obtained with the mass angular scattering power method agree with those obtained with the electron range method. (author)

New method for evaluating the kinetic constant of thermal protection materials

International Nuclear Information System (INIS)

Bae, Ji Yeul; Yi, Jong Ju; Park, Sul Ki; Cho, Hyung Hee; Bae, Ju Chan; Ham, Hee Cheol

2013-01-01

Thermal protection material (TPM) is used to protect rocket structures from extreme conditions created by the hot exhaust of the rocket. Designing TPM is an important step in the rocket design process. Considering that an increase in the system weight decreases the overall performance of a rocket, the amount of TPM is carefully determined during the design process. Therefore, the precise properties of TPM guarantee an accurate thermal analysis and the successful design of the rocket. Among the many properties of TPM, the kinetic constant and activation energy, which govern the thermochemical reaction of the TPM, are the most important. Thus, an experiment to measure the kinetic constant and activation energy is conducted as part of this research. A theoretical approach to deduce the properties from measured data is discussed, and a method to apply the theory to experimental data, termed the R 2 method, is developed. Compared to a previous method which was difficult to apply, the R 2 method reduces unclear selections of the reaction time and does not require intervention by an interpreter. The properties deduced by the R 2 method show good agreement with the other method despite the limited number of experimental results.

A new optical sensor for spectrophotometric determination of uranium (VI) and thorium (IV) in acidic medium

Energy Technology Data Exchange (ETDEWEB)

Elhefnawy, O.A. [Nuclear and Radiological Regulatory Authority (NRRA), Cairo (Egypt). Nuclear Safeguards and Physical Protection Dept.

2017-07-01

A spectrophotometric method was developed for U(VI) and Th(IV) determination in acidic medium by using proposed optical sensor. This sensor is base on the complexation reaction of the ionophore midodrine hydrochloride (L) with U(VI)/Th(IV) in plasticized (o-NPOE) high molecular weight (PVC). Several parameters such as effect of acidic medium, response time and sensor compositions were studied. The determination of the complexes stoichiometry was also studied using Job's method. The complexes stoichiometry were measured at the absorbance spectra 302 nm and the results were found to be 1:1 for both complexes U(VI)-L and Th(IV)-L. The complexation reaction was extremely rapid at room temperature; it takes 5, 10 min to complete the complexation reaction in U(VI) and Th(IV), respectively. Under the optimum conditions the calibration curves of U(VI)/Th(IV) determination, have good linearity at different acidic medium nitric, sulfuric, and phosphoric acids with low detection and quantification limits. The accuracy and precision studies proved that the proposed optical sensor is valid and qualified for U(VI)/Th(IV) spectrophotometric determination in different acidic medium. The selectivity of the proposed optical sensor was studied. The proposed optical sensor was applied successfully for U(VI)/Th(IV) determination in research and development (R and D) nuclear waste samples with satisfactory results. A comparative study of the proposed optical sensor with other previous spectrophotometric sensors for U(VI)/Th(IV) determination, proved the high efficiency of the proposed optical sensor, that it presents wide linear range and low detection limit. The proposed optical sensor could be applied for a quantitative determination of U(VI)/Th(IV) in acidic waste samples.

A new optical sensor for spectrophotometric determination of uranium (VI) and thorium (IV) in acidic medium

International Nuclear Information System (INIS)

Elhefnawy, O.A.

2017-01-01

A spectrophotometric method was developed for U(VI) and Th(IV) determination in acidic medium by using proposed optical sensor. This sensor is base on the complexation reaction of the ionophore midodrine hydrochloride (L) with U(VI)/Th(IV) in plasticized (o-NPOE) high molecular weight (PVC). Several parameters such as effect of acidic medium, response time and sensor compositions were studied. The determination of the complexes stoichiometry was also studied using Job's method. The complexes stoichiometry were measured at the absorbance spectra 302 nm and the results were found to be 1:1 for both complexes U(VI)-L and Th(IV)-L. The complexation reaction was extremely rapid at room temperature; it takes 5, 10 min to complete the complexation reaction in U(VI) and Th(IV), respectively. Under the optimum conditions the calibration curves of U(VI)/Th(IV) determination, have good linearity at different acidic medium nitric, sulfuric, and phosphoric acids with low detection and quantification limits. The accuracy and precision studies proved that the proposed optical sensor is valid and qualified for U(VI)/Th(IV) spectrophotometric determination in different acidic medium. The selectivity of the proposed optical sensor was studied. The proposed optical sensor was applied successfully for U(VI)/Th(IV) determination in research and development (R and D) nuclear waste samples with satisfactory results. A comparative study of the proposed optical sensor with other previous spectrophotometric sensors for U(VI)/Th(IV) determination, proved the high efficiency of the proposed optical sensor, that it presents wide linear range and low detection limit. The proposed optical sensor could be applied for a quantitative determination of U(VI)/Th(IV) in acidic waste samples.

Determination of the kinetic parameters of BeO using isothermal decay method

International Nuclear Information System (INIS)

Nieto, Juan Azorin; Vega, Claudia Azorin; Montalvo, Teodoro Rivera; Cabrera, Eugenio Torijano

2016-01-01

Most of the existing methods for obtaining the frequency factors make use of the trap depth (activation energy) making some assumptions about the order of the kinetics. This causes inconsistencies in the reported values of trapping parameters due that the values of the activation energy obtained by different methods differ appreciably among them. Then, it is necessary to use a method independent of the trap depth making use of the isothermal luminescence decay (ILD) method. The trapping parameters associated with the prominent glow peak of BeO (280 °C) are reported using ILD method. As a check, the trap parameters are also calculated by glow curve shape (Chen's) method after isolating the prominent glow peak by thermal cleaning technique. Our results show a very good agreement between the trapping parameters calculated by the two methods. ILD method was used for determining the trapping parameters of BeO. Results obtained applying this method are in good agreement with those obtained using other methods, except in the value of the frequency factor. - Highlights: • Kinetic parameters of BeO were determined. • Isothermal decay method was used. • Frecuency factor not agree with those obtained by other methods.

Stability of generalized Runge-Kutta methods for stiff kinetics coupled differential equations

International Nuclear Information System (INIS)

Aboanber, A E

2006-01-01

A stability and efficiency improved class of generalized Runge-Kutta methods of order 4 are developed for the numerical solution of stiff system kinetics equations for linear and/or nonlinear coupled differential equations. The determination of the coefficients required by the method is precisely obtained from the so-called equations of condition which in turn are derived by an approach based on Butcher series. Since the equations of condition are fewer in number, free parameters can be chosen for optimizing any desired feature of the process. A further related coefficient set with different values of these parameters and the region of absolute stability of the method have been introduced. In addition, the A(α) stability properties of the method are investigated. Implementing the method in a personal computer estimated the accuracy and speed of calculations and verified the good performances of the proposed new schemes for several sample problems of the stiff system point kinetics equations with reactivity feedback

THE SPECTROPHOTOMETRIC DETERMINATION OF NITRITES WITH N,N-DIETHYLANILINE

Directory of Open Access Journals (Sweden)

O. S. Pogrebnyak

2015-11-01

Full Text Available A new spectrophotometric method for nitrite determination was proposed. The method is based on the measurement of absorbance of the N,N-diethylaniline nitrosation product at 475 nm in the hydrochloric acid medium. The optimum concentrations and the influence of various conditions on the determination sensitivity have been determined. The detection limit (blank + 3s for nitrite is 0.98 mg∙L–1 where sis the standard deviation of blank estimation. The linearity range of the calibration graph was over 1.0–100 mg∙L–1 of  nitrite (sr≤ 0.029, n = 8. The metrological characteristics of the procedure were checked by means of method of additives on the control samples and natural waters. The relative error did not exceed 0.06 for nitrite determination on the control samples. The effect of foreign ions in nitrite determination of 1,0∙10−3 mol∙L–1 has been studied. The proposed procedure is simple  and suitable for nitrite determination in various objects.

Investigation of Chemical Equilibrium Kinetics by the Electromigration Method

CERN Document Server

Bozhikov, G A; Bontchev, G D; Maslov, O D; Milanov, M V; Dmitriev, S N

2002-01-01

Measurement of the chemical reaction rates for complex formation as well as hydrolysis type reactions by the method of horizontal zone electrophoresis is outlined. The correlation between chemical equilibrium kinetics and electrodiffusion processes in a constant d.c. electric field is described. In model electromigration experiments the reaction rate constant of the complex formation of Hf(IV) and DTPA is determined.

Standard test methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions

CERN Document Server

American Society for Testing and Materials. Philadelphia

2010-01-01

1.1 These test methods cover procedures for the chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade plutonium nitrate solutions to determine compliance with specifications. 1.2 The analytical procedures appear in the following order: Sections Plutonium by Controlled-Potential Coulometry Plutonium by Amperometric Titration with Iron(II) Plutonium by Diode Array Spectrophotometry Free Acid by Titration in an Oxalate Solution 8 to 15 Free Acid by Iodate Precipitation-Potentiometric Titration Test Method 16 to 22 Uranium by Arsenazo I Spectrophotometric Test Method 23 to 33 Thorium by Thorin Spectrophotometric Test Method 34 to 42 Iron by 1,10-Phenanthroline Spectrophotometric Test Method 43 to 50 Impurities by ICP-AES Chloride by Thiocyanate Spectrophotometric Test Method 51 to 58 Fluoride by Distillation-Spectrophotometric Test Method 59 to 66 Sulfate by Barium Sulfate Turbidimetric Test Method 67 to 74 Isotopic Composition by Mass Spectrom...

A new integral method for solving the point reactor neutron kinetics equations

International Nuclear Information System (INIS)

Li Haofeng; Chen Wenzhen; Luo Lei; Zhu Qian

2009-01-01

A numerical integral method that efficiently provides the solution of the point kinetics equations by using the better basis function (BBF) for the approximation of the neutron density in one time step integrations is described and investigated. The approach is based on an exact analytic integration of the neutron density equation, where the stiffness of the equations is overcome by the fully implicit formulation. The procedure is tested by using a variety of reactivity functions, including step reactivity insertion, ramp input and oscillatory reactivity changes. The solution of the better basis function method is compared to other analytical and numerical solutions of the point reactor kinetics equations. The results show that selecting a better basis function can improve the efficiency and accuracy of this integral method. The better basis function method can be used in real time forecasting for power reactors in order to prevent reactivity accidents.

Eliminating amino acid interference during spectrophotometric NH4+ analysis

NARCIS (Netherlands)

Ros, G.H.; Leeuwen, van A.G.; Temminghoff, E.J.M.

2011-01-01

Amino acids can interfere with NH4+ in spectrophotometric NH4+ determination hampering accurate quantification of the fate of NH4+ and dissolved organic N in soils. Serious interference has been reported for soils rich in organic matter, and for soils that have been fumigated, oven-dried or

Simple spectrophotometric methods for determination of fluoxetine and clomipramine hydrochlorides in dosage forms and in some post-mortem biological fluids samples

Directory of Open Access Journals (Sweden)

Emam A. Ali

2016-12-01

Full Text Available Sensitive, simple and rapid spectrophotometric methods for micro determination of fluoxetine hydrochloride (FLU and clomipramine hydrochloride (CLO. The methods are based on the reaction between the examined drugs and acid dyes, namely; bromocresol green (BCG, phenol red (PhR and metanil yellow (MY producing yellow ion-pair complexes followed by their extraction with methylene chloride and measured at 412, 407 and 409 nm for FLU with BCG, PhR and MY, respectively; whereas for CLO at 409, 406 and 407 nm, respectively. All variables that affect the performance of the proposed methods were carefully studied and optimized. Beer’s law was obeyed in the concentration ranges 0.86–24.32 μg/mL, 8.64–41.30 μg/mL, 0.86–34.76 μg/mL for FLU and 1.75–24.55 μg/mL, 7.0–50 μg/mL, 1.65–34.78 μg/mL for CLO using BCG, PhR and MY respectively. The methods were validated in terms of accuracy and precision. The proposed methods were successfully applied to the determination of fluoxetine hydrochloride and clomipramine hydrochloride in pure samples, pharmaceutical formulations, spiked post-mortem urine and blood samples.

Sensitive spectrophotometric determination of aceclofenac following azo dye formation with 4-carboxyl-2,6-dinitrobenzene diazonium ion.

Science.gov (United States)

Aderibigbe, Segun A; Adegoke, Olajire A; Idowu, Olakunle S; Olaleye, Sefiu O

2012-01-01

The study is a description of a sensitive spectrophotometric determination of aceclofenac following azo dye formation with 4-carboxyl-2,6-dinitrobenzenediazonium ion (CDNBD). Spot test and thin layer chromatography revealed the formation of a new compound distinct from CDNBD and aceclofenac. Optimization studies established a reaction time of 5 min at 30 degrees C after vortex mixing the drug/CDNBD for 10 s. An absorption maximum of 430 nm was selected as analytical wavelength. A linear response was observed over 1.2-4.8 μg/mL of aceclofenac with a correlation coefficient of 0.9983 and the drug combined with CDNBD at stoichiometric ratio of 2 : 1. The method has a limit of detection of 0.403 μg/mL, limit of quantitation of 1.22 μg/mL and is reproducible over a three day assessment. The method gave Sandell's sensitivity of 3.279 ng/cm2. Intra- and inter-day accuracies (in terms of errors) were less than 6% while precisions were of the order of 0.03-1.89% (RSD). The developed spectrophotometric method is of equivalent accuracy (p > 0.05) with British Pharmacopoeia, 2010 potentiometric method. It has the advantages of speed, simplicity, sensitivity and more affordable instrumentation and could found application as a rapid and sensitive analytical method of aceclofenac. It is the first described method by azo dye derivatization for the analysis of aceclofenac in bulk samples and dosage forms.

Calculation of statistic estimates of kinetic parameters from substrate uncompetitive inhibition equation using the median method

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Pedro L. Valencia

2017-04-01

Full Text Available We provide initial rate data from enzymatic reaction experiments and tis processing to estimate the kinetic parameters from the substrate uncompetitive inhibition equation using the median method published by Eisenthal and Cornish-Bowden (Cornish-Bowden and Eisenthal, 1974; Eisenthal and Cornish-Bowden, 1974. The method was denominated the direct linear plot and consists in the calculation of the median from a dataset of kinetic parameters Vmax and Km from the Michaelis–Menten equation. In this opportunity we present the procedure to applicate the direct linear plot to the substrate uncompetitive inhibition equation; a three-parameter equation. The median method is characterized for its robustness and its insensibility to outlier. The calculations are presented in an Excel datasheet and a computational algorithm was developed in the free software Python. The kinetic parameters of the substrate uncompetitive inhibition equation Vmax, Km and Ks were calculated using three experimental points from the dataset formed by 13 experimental points. All the 286 combinations were calculated. The dataset of kinetic parameters resulting from this combinatorial was used to calculate the median which corresponds to the statistic estimator of the real kinetic parameters. A comparative statistical analyses between the median method and the least squares was published in Valencia et al. [3].

Variation of iron redox kinetics and its relation with molecular composition of standard humic substances at circumneutral pH

OpenAIRE

Lee, Ying Ping; Fujii, Manabu; Kikuchi, Tetsuro; Terao, Koumei; Yoshimura, Chihiro

2017-01-01

Oxidation and reduction kinetics of iron (Fe) and proportion of steady-state Fe(II) concentration relative to total dissolved Fe (steady-state Fe(II) fraction) were investigated in the presence of various types of standard humic substances (HS) with particular emphasis on the photochemical and thermal reduction of Fe(III) and oxidation of Fe(II) by dissolved oxygen (O2) and hydrogen peroxide (H2O2) at circumneutral pH (pH 7-8). Rates of Fe(III) reduction were spectrophotometrically determined...

Effect of medium acidity on the thermodynamics and kinetics of the reaction of pyridoxal 5'-phosphate with isoniazid in an aqueous solution

Science.gov (United States)

Gamov, G. A.; Zavalishin, M. N.; Usacheva, T. R.; Sharnin, V. A.

2017-05-01

Thermodynamic characteristics of the formation of the Schiff base between isoniazid and pyridoxal 5'-phosphate in an aqueous solution at different pH values of a medium are determined by means of spectrophotometry and calorimetric titration. The process kinetics is studied spectrophotometrically, and the reaction rate constants for the formation of the imine at different acidities of a medium are determined. Biochemical aspects of the binding of pyridoxal 5'-phosphate into stable compounds are discussed.

Iron oxide nanoparticle-based magnetic resonance method to monitor release kinetics from polymeric particles with high resolution.

Science.gov (United States)

Chan, Minnie; Schopf, Eric; Sankaranarayanan, Jagadis; Almutairi, Adah

2012-09-18

A new method to precisely monitor rapid release kinetics from polymeric particles using super paramagnetic iron oxide nanoparticles, specifically by measuring spin-spin relaxation time (T(2)), is reported. Previously, we have published the formulation of logic gate particles from an acid-sensitive poly-β-aminoester ketal-2 polymer. Here, a series of poly-β-aminoester ketal-2 polymers with varying hydrophobicities were synthesized and used to formulate particles. We attempted to measure fluorescence of released Nile red to determine whether the structural adjustments could finely tune the release kinetics in the range of minutes to hours; however, this standard technique did not differentiate each release rate of our series. Thus, a new method based on encapsulation of iron oxide nanoparticles was developed, which enabled us to resolve the release kinetics of our particles. Moreover, the kinetics matched the relative hydrophobicity order determined by octanol-water partition coefficients. To the best of our knowledge, this method provides the highest resolution of release kinetics to date.

Spectrophotometric and chemometric methods for determination of imipenem, ciprofloxacin hydrochloride, dexamethasone sodium phosphate, paracetamol and cilastatin sodium in human urine

Science.gov (United States)

El-Kosasy, A. M.; Abdel-Aziz, Omar; Magdy, N.; El Zahar, N. M.

2016-03-01

New accurate, sensitive and selective spectrophotometric and chemometric methods were developed and subsequently validated for determination of Imipenem (IMP), ciprofloxacin hydrochloride (CIPRO), dexamethasone sodium phosphate (DEX), paracetamol (PAR) and cilastatin sodium (CIL) in human urine. These methods include a new derivative ratio method, namely extended derivative ratio (EDR), principal component regression (PCR) and partial least-squares (PLS) methods. A novel EDR method was developed for the determination of these drugs, where each component in the mixture was determined by using a mixture of the other four components as divisor. Peak amplitudes were recorded at 293.0 nm, 284.0 nm, 276.0 nm, 257.0 nm and 221.0 nm within linear concentration ranges 3.00-45.00, 1.00-15.00, 4.00-40.00, 1.50-25.00 and 4.00-50.00 μg mL- 1 for IMP, CIPRO, DEX, PAR and CIL, respectively. PCR and PLS-2 models were established for simultaneous determination of the studied drugs in the range of 3.00-15.00, 1.00-13.00, 4.00-12.00, 1.50-9.50, and 4.00-12.00 μg mL- 1 for IMP, CIPRO, DEX, PAR and CIL, respectively, by using eighteen mixtures as calibration set and seven mixtures as validation set. The suggested methods were validated according to the International Conference of Harmonization (ICH) guidelines and the results revealed that they were accurate, precise and reproducible. The obtained results were statistically compared with those of the published methods and there was no significant difference.

Oxytetracycline as a new analytical reagent for the spectrophotometric determination of boron

Energy Technology Data Exchange (ETDEWEB)

Narayana, G L

1984-05-01

Oxytetracycline hydrochloride, Terramycin, is introduced as a new reagent for the spectrophotometric determination of trace quantities of boron in concentrated sulphuric acid medium. The reagent has an absorption maximum at 430 nm, and that of the boron complex at 520 nm. The colored system conformed to Beer's law between 2 and 10 ..mu..g of boron at 520 nm. The molar absorptivity calculated on the basis of boron is 10,800 1 mol/sup -1/ cm/sup -1/. The composition of the complex has been shown to be 1:1 both by the slope ratio and molar ratio methods. 16 references.

Oxytetracycline as a new analytical reagent for the spectrophotometric determination of boron

International Nuclear Information System (INIS)

Narayana, G.L.

1984-01-01

Oxytetracycline hydrochloride, Terramycin, is introduced as a new reagent for the spectrophotometric determination of trace quantities of boron in concentrated sulphuric acid medium. The reagent has an absorption maximum at 430 nm, and that of the boron complex at 520 nm. The coloured system conformed to Beer's law between 2 and 10 μg of boron at 520 nm. The molar absorptivity calculated on the basis of boron is 10,800 1 mol -1 cm -1 . The composition of the complex has been shown to be 1:1 both by the slope ratio and molar ratio methods. (author)

Spectrophotometric assay of phenylephrine hydrochloride using 4-aminoantipyrine and copper (II)