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.

Spectrophotometric determination of aluminium in steel with xylenol orange

International Nuclear Information System (INIS)

Majeed, A.; Javed, N.; Khan, M.S.

1996-01-01

Spectrophotometric determination of Aluminium in steel based on colour reaction between Aluminium and xylenol orange has been carried out. Red coloured complex formed in weak acidic solution is measured for its absorbance at 550 nm. The various optimum experimental conditions for Aluminium xylenol orange (Al-Xo) complex have been studied. (author)

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

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.

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.

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

Spectrophotometric calibration system for DECam

Science.gov (United States)

Rheault, J.-P.; DePoy, D. L.; Marshall, J. L.; Prochaska, T.; Allen, R.; Wise, J.; Martin, E.; Williams, P.

2012-09-01

We describe a spectrophotometric calibration system that is being implemented as part of the DES DECam project at the Blanco 4 meter at CTIO. Our calibration system uses a 1nm wide tunable source to measure the instrumental response function of the telescope optics and detector from 300nm up to 1100nm. This calibration will be performed regularly to monitor any change in the transmission function of the telescope during the 5 year survey. The system consists of a monochromator based tunable light source that provides illumination on a dome flat that is monitored by calibrated photodiodes that allow us to measure the telescope throughput as a function of wavelength. Our system has a peak output power of 2 mW, equivalent to a flux of approximately 800 photons/s/pixel on DECam.

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.)

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.

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.

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.

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.

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

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

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...

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.

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, 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.

Indications of Segmental Flow in Straight Pipes by Flow Injection with Spectrophotometric Detection

DEFF Research Database (Denmark)

Andersen, Jens Enevold Thaulov

2000-01-01

A procedure of spectrophotometric analysis of fluid flow in pipes is described and its performance is tested on three different dye compounds. The procedure follows measurement and mathematical de-convolution of the signal with an exponential function that is associated with molecular diffusion. ...

Kinetic Spectrophotometric Determination of Certain Cephalosporins in Pharmaceutical Formulations

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Mahmoud A. Omar

2009-01-01

Full Text Available A simple, reliable, and sensitive kinetic spectrophotometric method was developed for determination of eight cephalosporin antibiotics, namely, Cefotaxime sodium, Cephapirin sodium, Cephradine dihydrate, Cephalexin monohydrate, Ceftazidime pentahydrate, Cefazoline sodium, Ceftriaxone sodium, and Cefuroxime sodium. The method depends on oxidation of each of studied drugs with alkaline potassium permanganate. The reaction is followed spectrophotometrically by measuring the rate of change of absorbance at 610 nm. The initial rate and fixed time (at 3 minutes methods are utilized for construction of calibration graphs to determine the concentration of the studied drugs. The calibration graphs are linear in the concentration ranges 5–15 g mL−1 and 5–25 g mL−1 using the initial rate and fixed time methods, respectively. The results are validated statistically and checked through recovery studies. The method has been successfully applied for the determination of the studied cephalosporins in commercial dosage forms. Statistical comparisons of the results with the reference methods show the excellent agreement and indicate no significant difference in accuracy and precision.

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 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...

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)

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.

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.

Thorium spectrophotometric analysis with high precision

International Nuclear Information System (INIS)

Palmieri, H.E.L.

1983-06-01

An accurate and precise determination of thorium is proposed. Precision of about 0,1% is required for the determination of macroquantities of thorium processed. After an extensive literature search concerning this subject, spectrophotometric titration has been chosen, using disodium ethylenediaminetetraacetate (EDTA) solution and alizarin S as indicator. In order to obtain such a precision, an amount of 0,025 M EDTA solution precisely measured has been added and the titration was completed with less than 5 ml of 0,0025 M EDTA solution. It is usual to locate the end-point graphically, by plotting added titrant versus absorbance. The non-linear minimum square fit, using the Fletcher e Powell's minimization process and a computer program. (author)

DECal: A Spectrophotometric Calibration System For DECam.

Science.gov (United States)

Rheault, Jean-Philippe; DePoy, D. L.; Marshall, J. L.; Prochaska, T.; Allen, R.; Wise, J.; Martin, E.

2012-01-01

We present preliminary results for a spectrophotometric calibration system that is being implemented as part of the DES DECam project at the Blanco 4 meter at CTIO. Our calibration system uses a 2nm wide tunable source to measure the instrumental response function of the telescope from 300nm up to 1100nm. This calibration will be performed regularly to monitor any change in the transmission function. The system consists of a monochromator based tunable light source that provides illumination on a dome flat that is monitored by calibrated photodiodes and allow us to measure the throughput as a function of wavelength. Our system has an output power of 2 mW, equivalent to a flux of approximately 800 photons/s/pixel on DECam. Preliminary results of the measure of the throughput of the telescope will be presented.

Spectrophotometric determination of plutonium with chlorophosphonazo III in n-pentanol

International Nuclear Information System (INIS)

Saponara, N.M.; Marsh, S.F.

1982-03-01

Microgram amounts of plutonium are measured spectrophotometrically as the plutonium-chlorophosphonazo III complex after extraction into n-pentanol from 1.5 M HCl. The relative standard deviation is 1.5% for the range of 2.5 to 17.5 μg. The tolerance is excellent for many metals and nonmetals present in nuclear fuel-cycle materials. A preceding anion-exchange-column separation increases tolerance for certain metals and nonmetals

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

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

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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.

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)

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 ...

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

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

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 ...

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)

Spectrophotometric determination of the ASTM color of diesel oil

Energy Technology Data Exchange (ETDEWEB)

Douglas Willian Emanuel Alves Santana; Marcelle Prates Sepulveda; Paulo Jorge Sanches Barbeira

2007-03-15

One of the parameters analyzed to determine the quality of diesel oil is its ASTM color. Changes in color may be indicative of problems in the production process, contamination, degradation or the oxidation of diesel. The methodology recommended for determining the color of automotive diesel oil samples is the colorimetry according to standard ASTM D1500, in which a sample is introduced into a glass cell and the color of the sample is compared with an optical filter color scale. Although it is very simple, the manual method requires good visual acuity from the operator. This procedure becomes somewhat subjective in some cases since different operators can make distinct evaluations of the same sample. In this way, this work proposes the development of a spectrophotometric analysis methodology to eliminate the subjectiveness in the determination of ASTM color of diesel oil samples by using operator-independent parameters and making quality assay more accurate and precise. Short communication. 7 refs., 2 figs., 2 tabs.

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.

Spectrophotometric Rapid-Response Classification of Near-Earth Objects

Science.gov (United States)

Mommert, Michael; Trilling, David; Butler, Nat; Axelrod, Tim; Moskovitz, Nick; Jedicke, Robert; Pichardo, Barbara; Reyes-Ruiz, Mauricio

2015-08-01

Small NEOs are, as a whole, poorly characterized, and we know nothing about the physical properties of the majority of all NEOs. The rate of NEO discoveries is increasing each year, and projects to determine the physical properties of NEOs are lagging behind. NEOs are faint, and generally even fainter by the time that follow-up characterizations can be made days or weeks after their discovery. There is a need for a high-throughput, high-efficiency physical characterization strategy in which hundreds of faint NEOs can be characterized each year. Broadband photometry in the near-infrared is sufficiently diagnostic to assign taxonomic types, and hence constrain both the individual and ensemble properties of NEOs.We present results from our rapid response near-infrared spectrophotometric characterization program of NEOs. We are using UKIRT (on Mauna Kea) and the RATIR instrument on the 1.5m telescope at the San Pedro Martir Observatory (Mexico) to allow us to make observations most nights of the year in robotic/queue mode. We derive taxonomic classifications for our targets using machine-learning techniques that are trained on a large sample of measured asteroid spectra. For each target we assign a probability for it to belong to a number of different taxa. Target selection, observation, data reduction, and analysis are highly automated, requiring only a minimum of user interaction, making this technique powerful and fast. Our targets are NEOs that are generally too faint for other characterization techniques, or would require many hours of large telescope time.

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 ...

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

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)

How Much Cranberry Juice Is in Cranberry-Apple Juice? A General Chemistry Spectrophotometric Experiment

Science.gov (United States)

Edionwe, Etinosa; Villarreal, John R.; Smith, K. Christopher

2011-01-01

A laboratory experiment that spectrophotometrically determines the percent of cranberry juice in cranberry-apple juice is described. The experiment involves recording an absorption spectrum of cranberry juice to determine the wavelength of maximum absorption, generating a calibration curve, and measuring the absorbance of cranberry-apple juice.…

Determination of loratadine in pharmaceuticals by a spectrophotometric method

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Pavalache Georgeta

2015-06-01

Full Text Available The spectrophotometric method for determination of loratadine using tetraiodomercurate has been applied in various pharmaceutical formulations. The results confirmed that recovery value is optimum and the method is valid, thus it can be used in quality control and evaluation of loratadine tablets, oral formulations of mixed composition, oral solutions, etc. The method is easy and simple to apply, does not require complicated equipment and spectrophotometric reading time is reduced, which allows a large number of analyzes in a relatively short time.

Kinetic spectrophotometric determination of some fluoroquinolone ...

African Journals Online (AJOL)

A simple and sensitive kinetic spectrophotometric method was developed for the determination of some fluoroquinolonea antibiotics; gemifloxacin mesylate, moxifloxacin hydrochloride and gatifloxacin in bulk and in pharmaceutical preparations. The method is based upon a kinetic investigation of the oxidation reaction of ...

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)

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 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

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 ...

Development of Ultraviolet Spectrophotometric Method for Analysis ...

African Journals Online (AJOL)

HP

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.

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.

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)

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.

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

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

Directory of Open Access Journals (Sweden)

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

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.

Spectrophotometric determination of procainamide hydrochloride using sodium periodate

Directory of Open Access Journals (Sweden)

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.

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...

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 ...

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

Directory of Open Access Journals (Sweden)

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 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 DETERMINATION OF NITRITE BY ITS ...

African Journals Online (AJOL)

Preferred Customer

sources of nitrite include intensive use of chemical nitrogenous fertilizers, ... The current paper describes another kinetic spectrophotometric method for determination of ... s at λmax = 570 nm (allowing a lag time of 5 s) against water as reference. ... samples and the total amount of the analyte was estimated by applying the ...

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 ...

The spectrophotometric determination of boron in tourmalines

Directory of Open Access Journals (Sweden)

LJILJANA JAKSIC

2005-02-01

Full Text Available A procedure for the spectrophotometric determination of macro amounts of boron in tourmaline with azomethine H is described. The used tourmaline concentrate was obtained by magnetic separation and heavy-liquids purification of the schorl zone of pegmatite or granite aplite. The samples of tourmaline were decomposed by fusion with anhydrous sodium carbonate and taken up in dilute hydrochloric acid. The interfering effects of iron and aluminium were eliminated by masking with an EDTA – NTA solution. After pH adjustment, the boron was reacted with azomethine H and the absorbance of the obtained coloured complex was measured at 415 nm. The results are compared with those obtained by other procedures. The relative error of the determination was less than 3 %.

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 (

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

Science.gov (United States)

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.

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.

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 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.

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.

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 ...

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), ...

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)

High precision spectrophotometric analysis of thorium

International Nuclear Information System (INIS)

Palmieri, H.E.L.

1984-01-01

An accurate and precise determination of thorium is proposed. Precision of about 0,1% is required for the determination of macroquantities of thorium when processed. After an extensive literature search concerning this subject, spectrophotometric titration has been chosen, using dissodium ethylenediaminetetraacetate (EDTA) solution and alizarin-S as indicator. In order to obtain such a precision, an amount of 0,025 M EDTA solution precisely measured has been added and the titration was completed with less than 5 ml of 0,0025 M EDTA solution. It is usual to locate the end-point graphically, by plotting added titrant versus absorbance. The non-linear minimum square fit, using the Fletcher e Powell's minimization process and a computer programme. Besides the equivalence point, other parameters of titration were determined: the indicator concentration, the absorbance of the metal-indicator complex, and the stability constants of the metal-indicator and the metal-EDTA complexes. (Author) [pt

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.

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 ...

Development and Application of Kinetic Spectrophotometric Method ...

African Journals Online (AJOL)

Purpose: To develop an improved kinetic-spectrophotometric procedure for the determination of metronidazole (MNZ) in pharmaceutical formulations. Methods: The method is based on oxidation reaction of MNZ by hydrogen peroxide in the presence of Fe(II) ions at pH 4.5 (acetate buffer). The reaction was monitored ...

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...

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 ...

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

Spectrophotometric Analysis of Phenolic Compounds in Grapes and Wines.

Science.gov (United States)

Aleixandre-Tudo, Jose Luis; Buica, Astrid; Nieuwoudt, Helene; Aleixandre, Jose Luis; du Toit, Wessel

2017-05-24

Phenolic compounds are of crucial importance for red wine color and mouthfeel attributes. A large number of enzymatic and chemical reactions involving phenolic compounds take place during winemaking and aging. Despite the large number of published analytical methods for phenolic analyses, the values obtained may vary considerably. In addition, the existing scientific knowledge needs to be updated, but also critically evaluated and simplified for newcomers and wine industry partners. The most used and widely cited spectrophotometric methods for grape and wine phenolic analysis were identified through a bibliometric search using the Science Citation Index-Expanded (SCIE) database accessed through the Web of Science (WOS) platform from Thompson Reuters. The selection of spectrophotometry was based on its ease of use as a routine analytical technique. On the basis of the number of citations, as well as the advantages and disadvantages reported, the modified Somers assay appears as a multistep, simple, and robust procedure that provides a good estimation of the state of the anthocyanins equilibria. Precipitation methods for total tannin levels have also been identified as preferred protocols for these types of compounds. Good reported correlations between methods (methylcellulose precipitable vs bovine serum albumin) and between these and perceived red wine astringency, in combination with the adaptation to high-throughput format, make them suitable for routine analysis. The bovine serum albumin tannin assay also allows for the estimation of the anthocyanins content with the measurement of small and large polymeric pigments. Finally, the measurement of wine color using the CIELab space approach is also suggested as the protocol of choice as it provides good insight into the wine's color properties.

Reliability and accuracy of Crystaleye spectrophotometric system.

Science.gov (United States)

Chen, Li; Tan, Jian Guo; Zhou, Jian Feng; Yang, Xu; Du, Yang; Wang, Fang Ping

2010-01-01

to develop an in vitro shade-measuring model to evaluate the reliability and accuracy of the Crystaleye spectrophotometric system, a newly developed spectrophotometer. four shade guides, VITA Classical, VITA 3D-Master, Chromascop and Vintage Halo NCC, were measured with the Crystaleye spectrophotometer in a standardised model, ten times for 107 shade tabs. The shade-matching results and the CIE L*a*b* values of the cervical, body and incisal regions for each measurement were automatically analysed using the supporting software. Reliability and accuracy were calculated for each shade tab both in percentage and in colour difference (ΔE). Difference was analysed by one-way ANOVA in the cervical, body and incisal regions. range of reliability was 88.81% to 98.97% and 0.13 to 0.24 ΔE units, and that of accuracy was 44.05% to 91.25% and 1.03 to 1.89 ΔE units. Significant differences in reliability and accuracy were found between the body region and the cervical and incisal regions. Comparisons made among regions and shade guides revealed that evaluation in ΔE was prone to disclose the differences. measurements with the Crystaleye spectrophotometer had similar, high reliability in different shade guides and regions, indicating predictable repeated measurements. Accuracy in the body region was high and less variable compared with the cervical and incisal regions.

Single peak parameters technique for simultaneous measurements: Spectrophotometric sequential injection determination of Fe(II) and Fe(III).

Science.gov (United States)

Kozak, J; Paluch, J; Węgrzecka, A; Kozak, M; Wieczorek, M; Kochana, J; Kościelniak, P

2016-02-01

Spectrophotometric sequential injection system (SI) is proposed to automate the method of simultaneous determination of Fe(II) and Fe(III) on the basis of parameters of a single peak. In the developed SI system, sample and mixture of reagents (1,10-phenanthroline and sulfosalicylic acid) are introduced into a vessel, where in an acid environment (pH≅3) appropriate compounds of Fe(II) and Fe(III) with 1,10-phenanthroline and sulfosalicylic acid are formed, respectively. Then, in turn, air, sample, EDTA and sample again, are introduced into a holding coil. After the flow reversal, a segment of air is removed from the system by an additional valve and as EDTA replaces sulfosalicylic acid forming a more stable colorless compound with Fe(III), a complex signal is registered. Measurements are performed at wavelength 530 nm. The absorbance measured at minimum of the negative peak and the area or the absorbance measured at maximum of the signal can be used as measures corresponding to Fe(II) and Fe(III) concentrations, respectively. The time of the peak registration is about 2 min. Two-component calibration has been applied to analysis. Fe(II) and Fe(III) can be determined within the concentration ranges of 0.04-4.00 and 0.1-5.00 mg L(-1), with precision less than 2.8% and 1.7% (RSD), respectively and accuracy better than 7% (RE). The detection limit is 0.04 and 0.09 mg L(-1) for Fe(II) and Fe(III), respectively. The method was applied to analysis of artesian water samples. Copyright © 2015 Elsevier B.V. All rights reserved.

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

Speciation and spectrophotometric determination of uranium in seawater

Directory of Open Access Journals (Sweden)

M. KONSTANTINOU

2004-06-01

Full Text Available A series of ion-exchange and extraction procedures for the separation of uranium from seawater samples and subsequent spectrophotometric determination of uranium in seawater by means of arsenazo(III is described. According to the measurements performed by means of traced samples at every stage of separation, the yield of the pre-analytical procedures is generally over 90% and the separation of uranium very selective. The mean uranium concentration in seawater samples collected from five different coastal areas in Cyprus was found to be 3.2 ± 0.2 & micro; g L-1. Uranium in seawater is stable in its hexavalent oxidation state and UO2 (CO334- is the predominant species under normal coastal conditions (pH ≥ 8, EH ≥ 0.35 mV, 1 atm and 0.03% CO2.

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

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 ...

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.

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.

Dose intercomparison for 400–500 keV electrons using FWT-60 film and glutamine (spectrophotometric readout) dosimeters

DEFF Research Database (Denmark)

Gupta, B. L.; Nilekani, S. R.; Gehringer, P.

1986-01-01

This paper describes the dose and the depth dose measurements with FWT-60 film and glutamine (Spectrophotometric readout) dosimeters for 400–500 keV electrons. The glutamine powder was spread uniformly in polyethylene bags and the powder thickness in each bag was 5 mg cm−2. Both techniques show...

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)

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.

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.

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.

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.

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.

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.

Spectrophotometric Examination of Rough Print Surfaces

Directory of Open Access Journals (Sweden)

Erzsébet Novotny

2011-05-01

Full Text Available The objective was to assess the impact of the surface texture of individual creative paper types (coated or patternedon the quality of printing and to identify to what extent the various creative paper types require specific types ofspectrophotometers. We used stereomicroscopic images to illustrate unprinted and printed surfaces of creative papertypes. Surface roughness was measured to obtain data on the unevenness of surfaces. Spectrophotometric tests wereused to select the most suitable spectrophotometer from meters with different illumination setup for testing anygiven print. For the purpose of testing, we used spectrophotometers which are commonly available generally used totest print products for colour accuracy. With the improvement of measuring geometries, illumination setup, colourmeasurement becomes more and more capable of producing reliable results unaffected by surface textures. Our testshave proved this fact by showing that the GretagMacbeth Spectrolino with annular illumination is less sensitive tosurface texture than the X-Rite Spetrodensitometer and the Techkon SpetroDens with directional illumination. Furthertests have brought us to the conclusion that there is a difference even between the two devices with directionalillumination. While the X-Rite 530 Spectrodensitometer is more suitable for testing coated surfaces, the TechkonSpectroDens can come close to ΔE*ab values produced by the annular illuminated device for textured surfaces.

[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.

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.

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 %.

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 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.

The Spectrophotometric Analysis and Modeling of Sunscreens

Science.gov (United States)

Walters, Christina; Keeney, Allen; Wigal, Carl T.; Johnston, Cynthia R.; Cornelius, Richard D.

1997-01-01

Sunscreens and their SPF (Sun Protection Factor) values are the focus of this experiment that includes spectrophotometric measurements and molecular modeling. Students suspend weighed amounts of sunscreen lotions graded SPF 4, 6, 8, 15, 30, and 45 in water and dissolve aliquots of the aqueous suspensions in propanol. The expected relationship of absorbance proportional to log10(SPF) applies at 312 nm where a maximum in absorbance occurs for the sunscreen solutions. Results at 330 nm give similar results and are more accessible using spectrometers routinely available in the introductory laboratory. Sunscreens constitute a suitable class of compounds to use for modeling electronic spectra, and using the computer for the active ingredients ethylhexyl para-methoxycinnamate, oxybenzone, 2-ethylhexyl salicylate, and octocrylene found in commercially available formulations typically predicts the absorption maxima within 10 nm. This experiment lets students explore which compounds have the potential to function as sunscreen agents and thereby see the importance of a knowledge of chemistry to the formulation of household items.

IMPROVED SPECTROPHOTOMETRIC CALIBRATION OF THE SDSS-III BOSS QUASAR SAMPLE

Energy Technology Data Exchange (ETDEWEB)

Margala, Daniel; Kirkby, David [Frederick Reines Hall, Department of Physics and Astronomy, University of California, Irvine, CA (United States); Dawson, Kyle [Department of Physics and Astronomy, University of Utah, Salt Lake City, UT 84112 (United States); Bailey, Stephen [Lawrence Berkeley National Laboratory, One Cyclotron Road, Berkeley, CA 94720 (United States); Blanton, Michael [Center for Cosmology and Particle Physics, Department of Physics, New York University, 4 Washington Place, New York, NY 10003 (United States); Schneider, Donald P., E-mail: dmargala@uci.edu [Department of Astronomy and Astrophysics, The Pennsylvania State University, University Park, PA 16802 (United States)

2016-11-10

We present a model for spectrophotometric calibration errors in observations of quasars from the third generation of the Sloan Digital Sky Survey Baryon Oscillation Spectroscopic Survey (BOSS) and describe the correction procedure we have developed and applied to this sample. Calibration errors are primarily due to atmospheric differential refraction and guiding offsets during each exposure. The corrections potentially reduce the systematics for any studies of BOSS quasars, including the measurement of baryon acoustic oscillations using the Ly α forest. Our model suggests that, on average, the observed quasar flux in BOSS is overestimated by ∼19% at 3600 Å and underestimated by ∼24% at 10,000 Å. Our corrections for the entire BOSS quasar sample are publicly available.

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)

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

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)

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 ...

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

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 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

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 ...

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

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)

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 and computerized evaluation of tooth bleaching employing 10 different home-bleaching procedures: In-vitro study

Science.gov (United States)

Peskersoy, Cem; Tetik, Ayhan; Ozturk, Veli Ozgen; Gokay, Necmi

2014-01-01

Objective: The aim of this in-vitro study was to evaluate the efficacy of bleaching products, determine the applicability and validation of the measurement methods. Materials and Methods: Freshly extracted 110 human incisor teeth were stained with whole blood and hemolysate solution prior to the application of 10 different home-bleaching products. Spectrophotometric measurements of the tooth shades were performed for each specimen before and after bleaching at the 1st, 3rd, 7th, and 14 days. Differences in lightness (Δl), chroma (Δc), hue (Δh) values and shade changes were measured to evaluate process. Computerized digital imaging analyses to determine the color changes were performed with Photoshop CS4 software (Adobe, San Jose, CA, USA). Statistical analyses were performed with analysis of variance, Scheffe and Tukey tests. Results: In all of the test groups regardless of the material used, a significant increase in lightness and hue, and decrease of chroma were observed, as compared to the control group. After recommended bleaching applications, Δl and Δh values respectively increased in group Zaris White and Brite (ZWB) and group Pola Night and Δc values showed significant decrease in groups ZWB and Rembrandt REM3 (P bleaching systems showed slower but almost permanent bleaching effect likewise office-based methods. Both software and spectrophotometric analyses have advantages such as evaluating the results objectively and numerically, also treatment outcomes could be preserved. PMID:25512738

Rapid and direct spectrophotometric method for kinetics studies and routine assay of peroxidase based on aniline diazo substrates.

Science.gov (United States)

Mirazizi, Fatemeh; Bahrami, Azita; Haghbeen, Kamahldin; Shahbani Zahiri, Hossein; Bakavoli, Mehdi; Legge, Raymond L

2016-12-01

Peroxidases are ubiquitous enzymes that play an important role in living organisms. Current spectrophotometrically based peroxidase assay methods are based on the production of chromophoric substances at the end of the enzymatic reaction. The ambiguity regarding the formation and identity of the final chromophoric product and its possible reactions with other molecules have raised concerns about the accuracy of these methods. This can be of serious concern in inhibition studies. A novel spectrophotometric assay for peroxidase, based on direct measurement of a soluble aniline diazo substrate, is introduced. In addition to the routine assays, this method can be used in comprehensive kinetics studies. 4-[(4-Sulfophenyl)azo]aniline (λmax = 390 nm, ɛ = 32 880 M(-1) cm(-1) at pH 4.5 to 9) was introduced for routine assay of peroxidase. This compound is commercially available and is indexed as a food dye. Using this method, a detection limit of 0.05 nmol mL(-1) was achieved for peroxidase.

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 determination of metals in Pakistani and foreign brand cigarette tobacco

International Nuclear Information System (INIS)

Ikram, M.; Rauf, M.A.; Ali, S.; Iqbal, M.

2001-01-01

Tobacco smoking and related uses are major cause of various diseases in human beings. In the present study forty one various brands of cigarettes from Pakistan, United States, United Kingdom and Japan have been selected for determination of iron, nickel and copper spectrophotometrically. The concentration of Fe, Ni and Cu in tobacco of each forty-one brands of national and foreign brands cigarette is given in this article. The spectrophotometric determination of Fe, Ni and Cu in forty one brands of national and foreign cigarettes reveals that the concentrations of these metals depends on different conditions, such as soil condition, fertilizer and sprays during the tobacco growth. However, Cigarette manufacturing companies could have a significant role in their concentration levels. The results obtained by this technique are in good agreement with the reported literature values. (A.B.)

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

Spectrophotometric determination of some metal ions using hydrazones

International Nuclear Information System (INIS)

Mohammed, M. S.

2000-05-01

In this research many starting materials were prepared, like methyl salicylate and salicylic acid hydrazide from which different derivatives of hydrazones were synthesized by coupling with carbonyl compounds like benzil monoxime and benzil mono hydrazone which are prepared and others like salicylaldehyde and benzoin. The hydrazones that were synthesized are salicylaldehyde salicylic acid hydrazone, benzoin salicylic acid hydrazone, benzil mono hydrazone salicylic acid hydrazone and benzil monoxime salicylic acid hydrazone. These reagents were determined by different methods, IR spectrophotometric determination, the nitrogen content method and melting point determination. These hydrazones act as ligands for determination of some metal ions by making different coloured complexes that were prepared for eight hydrazones with eight metal ions U (VI), Fe (II), Fe (III), Co (II), V (II), Mo (VI), Ni (II) and Cu (II). These complexes were determined by ultraviolet and visible spectrophotometer (UV/VIS) to detect their absorbance and wavelengths (λ max). The two hydrazones salicylaldehyde salicylic acid-hydrazone and benzoin salicylic acid hydrazone, were selected for determination of five metal ions (Fe (II), Fe (III), U (VI), Ni (II) and Cu (II)), using two micelles sodium n-dodecyl sulphate and pyridinium hexa decyl bromide mono hydrate. Their absorbance and wavelengths were detected using UV/VIS spectrophotometer. (Author)

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 Determination of Phenolic Antioxidants in the Presence of Thiols and Proteins

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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.

Convergent validity of two decision making style measures

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Berisha, Gentrit

2018-04-01

Full Text Available Decision making research has witnessed a growing number of studies on individual differences and decision making styles, yet the lack of comprehensive frameworks and widely accepted measures has hindered research for a long time. There is an ongoing debate on whether individuals’ styles dynamically change across time and situations according to circumstances. Furthermore, it is an open question whether these styles are mutually exclusive. Decision style measures seek to determine one’s dominant style as well as less used styles. To our knowledge this is the first study of the convergent validity of two widely used decision making style measures: The Decision Style Inventory (DSI and the General Decision Making Style (GDMS. The direction and strength of correlation between directive, analytical, conceptual and behavioral styles as measured by DSI and rational, intuitive, dependent, avoidant and spontaneous styles as measured by GDMS have been tested. Results of the current study are compared with previous studies that have used one or both of the instruments. Correlations between styles are consistent with findings from other studies using one of the decision style measures, but the strength of correlations indicates that there is no convergent validity between DSI and GDMS.

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.

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)

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.)

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.

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 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)

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.

Spectrophotometric readout for an alanine dosimeter for food irradiation applications

International Nuclear Information System (INIS)

Ebraheem, S.; Beshir, W.B.; Eid, S.; Sobhy, R.; Kovacs, A.

2003-01-01

The alanine-electron spin resonance (EPR) readout system is well known as a reference and transfer dosimetry system for the evaluation of high doses in radiation processing. The high cost of an EPR/alanine dosimetry system is a serious handicap for large-scale routine application in irradiation facilities. In this study, the use of a complex produced by dissolving irradiated L-alanine in 1,4-phenyl diammonium dichloride solution was investigated for dosimetry purposes. This complex--having a purple colour--has an increasing absorbance with increasing dose in the range of 1-20 kGy. The applicability of spectrophotometric evaluation was studied by measuring the absorbance intensity of this complex at 360 and 505 nm, respectively. Fluorimetric evaluation was also investigated by measuring the emission of the complex at 435 nm as a function of dose. The present method is easy for routine application. The effect of the dye concentration as well as the suitable amount of irradiated alanine has been studied. With respect to routine application, the stability of the product complex after its formation was also investigated

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.

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)

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.

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

Flow analysis methods for the direct ultra-violet spectrophotometric measurement of nitrate and total nitrogen in freshwaters

Energy Technology Data Exchange (ETDEWEB)

Gentle, Brady S.; Ellis, Peter S.; Grace, Michael R. [Water Studies Centre, School of Chemistry, Monash University, Victoria 3800 (Australia); McKelvie, Ian D., E-mail: iandm@unimelb.edu.au [School of Chemistry, University of Melbourne, Victoria 3010 (Australia); School of Geography, Earth and Environmental Sciences, University of Plymouth, Drake Circus, Plymouth PL4 8AA (United Kingdom)

2011-10-17

Highlights: {yields} Second derivative UV spectrophotometry has been used to determine nitrate and total N using flow analysis techniques. {yields} A simple flow system with a single-reflection flow-through cell was used for the UV measurement of nitrate. {yields} Total N was determined after on-line UV photooxidation with alkaline peroxodisulfate. {yields} Analyses carried out using the developed flow systems show a high degree of agreement with comparative analyses. {yields} This method requires no colorimetric reagents and eliminates the requirement for a toxic cadmium reduction column. - Abstract: Second derivative ultra-violet spectrophotometric methods are described for the measurement of nitrate and total nitrogen in freshwaters using flow analysis techniques. A simple flow system consisting of a peristaltic pump and a single-reflection flow-through cell was used for the measurement of nitrate. Quantification of total nitrogen using alkaline peroxodisulfate photo-digestion was achieved by incorporating an ultra-violet photo-reactor, a hollow-fibre filter and a debubbler into the flow system. The nitrate system featured a limit of detection of 0.04 mg N L{sup -1}, 0.4%RSD (1 mg N L{sup -1} as nitrate, n = 10), a coefficient of determination (R{sup 2}) of 0.9995 over the calibration range 0.0-2.0 mg N L{sup -1}, and a data acquisition time of 1.5 s per spectrum. The total nitrogen system featured a limit of detection of 0.05 mg N L{sup -1}, 1%RSD (1 mg N L{sup -1} as ammonium chloride, n = 10), a coefficient of determination of 0.9989 over the calibration range 0.0-2.0 mg N L{sup -1}, and a throughput of 5 sample h{sup -1} measured in triplicate. Digestions of five model nitrogen compounds returned recoveries of >88%. Determinations carried out using the developed systems show a high degree of agreement with data obtained using reference methods. These methods require no colorimetric reagents and eliminate the requirement for a toxic cadmium reduction column

Flow analysis methods for the direct ultra-violet spectrophotometric measurement of nitrate and total nitrogen in freshwaters

International Nuclear Information System (INIS)

Gentle, Brady S.; Ellis, Peter S.; Grace, Michael R.; McKelvie, Ian D.

2011-01-01

Highlights: → Second derivative UV spectrophotometry has been used to determine nitrate and total N using flow analysis techniques. → A simple flow system with a single-reflection flow-through cell was used for the UV measurement of nitrate. → Total N was determined after on-line UV photooxidation with alkaline peroxodisulfate. → Analyses carried out using the developed flow systems show a high degree of agreement with comparative analyses. → This method requires no colorimetric reagents and eliminates the requirement for a toxic cadmium reduction column. - Abstract: Second derivative ultra-violet spectrophotometric methods are described for the measurement of nitrate and total nitrogen in freshwaters using flow analysis techniques. A simple flow system consisting of a peristaltic pump and a single-reflection flow-through cell was used for the measurement of nitrate. Quantification of total nitrogen using alkaline peroxodisulfate photo-digestion was achieved by incorporating an ultra-violet photo-reactor, a hollow-fibre filter and a debubbler into the flow system. The nitrate system featured a limit of detection of 0.04 mg N L -1 , 0.4%RSD (1 mg N L -1 as nitrate, n = 10), a coefficient of determination (R 2 ) of 0.9995 over the calibration range 0.0-2.0 mg N L -1 , and a data acquisition time of 1.5 s per spectrum. The total nitrogen system featured a limit of detection of 0.05 mg N L -1 , 1%RSD (1 mg N L -1 as ammonium chloride, n = 10), a coefficient of determination of 0.9989 over the calibration range 0.0-2.0 mg N L -1 , and a throughput of 5 sample h -1 measured in triplicate. Digestions of five model nitrogen compounds returned recoveries of >88%. Determinations carried out using the developed systems show a high degree of agreement with data obtained using reference methods. These methods require no colorimetric reagents and eliminate the requirement for a toxic cadmium reduction column. The overlap of chloride and nitrate spectra in seawater is

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.

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.

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 thorium using arsenazo III in water

International Nuclear Information System (INIS)

Rio, M.A.P. do; Godoy, J.M. de.

1985-01-01

A spectrophotometric determination of thorium with arsenazo III (1,8 dihidroxynaphtaline - 3,6 sulfanic acid - 2,7 bis (azo-2) - phenil argonic acid) was carried out aiming to analyse this element in water. In order to eliminate possible interferences, a coprecipitation with lantanium fluoride was used followed by an extration with 0,2 M TTA (tenoil-trifluor - aceton) / Benzen. The results showed a good agreement with the ones obtained by alfa-spectrometry. (Author) [pt

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.

Spectrophotometric determination of nitrite based on its catalytic effect on the reaction of nuclear fast red and potassium bromate

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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.

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.

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.

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.

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.

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 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 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.

THE SPECTROPHOTOMETRIC DETERMINATION OF NITRITES WITH N,N-DIETHYLANILINE

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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.

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 Determination of Labetalol and Lercanidipine in Pure Form and in Pharmaceutical Preparations Using Ferric-1,10-Phenanthroline

OpenAIRE

Abu El-Enin, M. A.; El-Wasseef, D. R.; El-Sherbiny, D. T.; El-Ashry, S. M.

2009-01-01

A simple and sensitive spectrophotometric method was developed for the determination of labetalol HCl (LBT) and lercanidipine HCl (LER) in pure form and in dosage forms. The method was based upon oxidation of the LBT and LER with Fe+3 and the estimation of the produced Fe+2 with 1,10-phenanthroline. The absorbance of the tris(1,10-phenanthroline) Fe+2 complex was measured at 510 nm. Reaction conditions were optimized to obtain colored complex of higher sensitivity and longer stability. The ab...

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

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.

Using measurement uncertainty in decision-making and conformity assessment

Science.gov (United States)

Pendrill, L. R.

2014-08-01

Measurements often provide an objective basis for making decisions, perhaps when assessing whether a product conforms to requirements or whether one set of measurements differs significantly from another. There is increasing appreciation of the need to account for the role of measurement uncertainty when making decisions, so that a ‘fit-for-purpose’ level of measurement effort can be set prior to performing a given task. Better mutual understanding between the metrologist and those ordering such tasks about the significance and limitations of the measurements when making decisions of conformance will be especially useful. Decisions of conformity are, however, currently made in many important application areas, such as when addressing the grand challenges (energy, health, etc), without a clear and harmonized basis for sharing the risks that arise from measurement uncertainty between the consumer, supplier and third parties. In reviewing, in this paper, the state of the art of the use of uncertainty evaluation in conformity assessment and decision-making, two aspects in particular—the handling of qualitative observations and of impact—are considered key to bringing more order to the present diverse rules of thumb of more or less arbitrary limits on measurement uncertainty and percentage risk in the field. (i) Decisions of conformity can be made on a more or less quantitative basis—referred in statistical acceptance sampling as by ‘variable’ or by ‘attribute’ (i.e. go/no-go decisions)—depending on the resources available or indeed whether a full quantitative judgment is needed or not. There is, therefore, an intimate relation between decision-making, relating objects to each other in terms of comparative or merely qualitative concepts, and nominal and ordinal properties. (ii) Adding measures of impact, such as the costs of incorrect decisions, can give more objective and more readily appreciated bases for decisions for all parties concerned. Such

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

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L. Yu. Klimenko

2014-08-01

dictated by the primary orientation of all studied international guidances on the work exactly by this method. The next criteria and the order of acceptability estimation of linearity for UV-spectrophotometric methods of quantitative determination analyses in biological fluids used in forensic and toxicological analysis have been offered: acceptability estimation of linear dependence parameters is carried out in two stages – for the lines obtained using model solutions (without matrix and calibration samples respectively; two approaches has been suggested for parameters estimation of linear dependence obtained using model solutions; they are based on: 1 assumption of equality of the uncertainty related to the procedure of sample preparation of calibration standards, and the uncertainty of the calibration curve plotted by model solutions; 2 assumption of insignificance of the uncertainty of the calibration curve plotted by model solutions; for both approaches the acceptability criteria have been offered for residual standard deviation and correlation coefficient ; for estimation of parameters of linear dependence obtained using calibration samples it has been suggested to proceed from assumption of equality of the calibration uncertainty and the uncertainty of measuring the absorbance and sample preparation of the sample to be analysed; within this approach the acceptability criteria have been offered for residual standard deviation RSD0 and correlation coefficient Rс; the parameters of within-run (within-day and between-run (between-day linearity should satisfy these criteria. Conclusion. The criteria and order of acceptability estimation of linearity for UV-spectrophotometric methods of quantitative determination analyses in biological fluids used in forensic and toxicological analysis have been formed. Offered approaches have been tested by example of UV-spectrophotometric method of doxylamine quantitative determination in blood.

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 %.

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.

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 %

Polarographic, spectrophotometric and coulometric studies of MoO=4 in H2SO4

International Nuclear Information System (INIS)

Tokoro, R.; Bertotti, M.

1990-01-01

This study characterizes the polarographic process of Mo O sup(=) sub(4) in H sub(2)SO sub(4) medium, determining which species is responsible by catalytic cycle. Spectrophotometric and coulometric studies are also described. (author)

Spectrophotometric observations of symbiotic stars

International Nuclear Information System (INIS)

Ipatov, A.P.; Yudin, B.F.

1985-01-01

The data of spectrophotometric observations of symbiotic stars Z And, AX Per, CI Cyg, BF Cyg, YY Her, V 443 Her, AG Dra, AG Peg, AS 296, EG And, V 1016 Cyg, and HM Sge are presented. The spectral range of observations is 3300-7500 A, resolution is 50 A. The data obtained allowed to reveal specific characteristics inherent to the radiation of symbiotic stars and to estimate the parameters of their individual components. Analysis of the spectra of symbiotic stars in the range of 1300-7500 A wavelengths suggests a hypothesis, according to which a hot source in the Rayleigh - Jeans spectral range has a less steep inclination in the energy distribution, than a black-body one. A disk, formed during cold star substance accretion through an internal Lagrangian point onto a denser component of the system, can play the role of the source. In this case one manages to obtain the energy distribution in the symbiotic star spectrum consistent with the observed distribution

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...

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...

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.

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.

Kinetic spectrophotometric method for the determination of perindopril erbumine in pure and commercial dosage forms

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Nafisur Rahman

2017-02-01

Full Text Available A kinetic spectrophotometric method has been developed for the determination of perindopril erbumine in pure and commercial dosage forms. The method is based on the reaction of drug with potassium permanganate in alkaline medium at room temperature (30 ± 1 °C. The reaction was followed spectrophotometrically by measuring the increase in absorbance with time at 603 nm and the initial rate, fixed time (at 8.0 min and equilibrium time (at 90.0 min methods were adopted for constructing the calibration graphs. All the calibration graphs are linear in the concentration range of 5.0–50.0 μg/ml. The limits of detection for initial rate, fixed time and equilibrium time methods were 0.752, 0.882 and 1.091 μg/ml, respectively. The activation parameters such as Ea, ΔH‡, ΔS‡ and ΔG‡ were also determined for the reaction and found to be 60.93 kJ/mol, 56.45 kJ/mol, 74.16 J/K mol and −6.53 kJ/mol, respectively. The variables were optimized and the proposed methods are validated as per ICH guidelines. The method has been further applied to the determination of perindopril erbumine in commercial dosage forms. The analytical results of the proposed methods when compared with those of the reference method show no significant difference in accuracy and precision and have acceptable bias.

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

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.

Construção de uma cela de fluxo de longo caminho óptico para medidas espectrofotométricas Construction of a long-pathlength flow cell for spectrophotometric measurements

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Wanessa Roberto Melchert

2008-01-01

Full Text Available A simple and low-cost flow cell with 30 cm optical path for spectrophotometric measurements is described. It presents desirable characteristics such as low attenuation of the radiation beam and internal volume (75 µL comparable to that of a 1-cm conventional cell (80 µL. Despite the increase in optical path, the effect on sample dispersion was also similar to that attained in the commercial cell. The performance of the cell was assessed by the determination of phosphate based on the molybdenum blue method, yielding a linear response range between 0.05 and 0.8 mg L-1 phosphorus (r=0.999. The increase in sensitivity (30.4-fold in comparison with that obtained with a conventional 1-cm flow cell agreed with that estimated by the Lambert-Beer law.

A modified spectrophotometric assay to estimate deglycosylation of steroidal saponin to sapogenin by mixed ruminal microbes.

Science.gov (United States)

Wang, Yuxi; McAllister, Tim A

2010-08-30

The lack of a method for measuring deglycosylation of saponins in ruminal fluid has limited the ability to investigate the impact of these compounds on rumen microorganisms. A simple spectrophotometric assay was adapted and a protocol developed to enable measurement of steroidal saponin and sapogenin in ruminal fluid. The procedure was used for in vitro determination of deglycosylation activity of rumen bacteria obtained from cattle fed or not fed Yucca schidigera saponin, and to determine the relative deglycosylase activities of extracellular and cell-associated enzymes from ruminal content. Modifications to the spectrophotometric assay (i.e. heating time shortened to 10 min and 0.5 mL dH(2)O added to the reaction mixture) improved the stability of the optical density (425 nm) of the chromophore for up to 24 h post-reaction. Centrifugation (12 000 x g, 20 min) enabled differential estimations of steroidal saponin and sapogenin in ruminal fluid. Steroidal saponin added to defaunated ruminal fluid (dRF) or clarified ruminal fluid (cRF) was recovered completely from the mixture as saponin + sapogenin (99.1% and 100.6%, respectively), whereas saponin recovery from the supernatant of dRF was greatly reduced (P ruminal extracellular enzyme preparation was recoverable in supernatant after 24 h, compared with only 26-32% remaining in supernatant from incubation with a cell-associated enzymes fraction. Mixed rumen bacteria deglycosylate steroidal saponin to sapogenin, at activity levels unaffected by prior exposure to saponin, but they were unable to degrade the sapogenin core structure. Deglycosylation activity occurred primarily in the cell-associated enzyme fraction of ruminal content. Copyright (c) 2008 Crown in the right of Canada. Published by John Wiley & Sons, Ltd.

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.

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)

The Development of a New Inhibition Kinetic Spectrophotometric Method for the Determination of Phenylhydrazine Based on its Inhibitory Effect on Oxidation of Methyl Red by Bromate in Micellar Medium

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Mohsen Keyvanfard

2010-01-01

Full Text Available A new, simple, sensitive and selective kinetic spectrophotometric method was developed for the determination of trace amounts of phenylhydrazine over the range of 0.02-0.30 μg/mL. The method is based on the inhibitory effect of phenylhydrazine on the oxidation of methyl red by bromate in acidic and micellar medium. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of methyl red at 518 nm with a fixed-time 0.5–2.0 min from initiation of the reaction..The relative standard deviation of 0.08 and 0.2 μg/mL phenylhydrazine was 1.7 and 2.4%, respectively. The method was applied to the determination of phenylhydrazine in water samples.

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

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.

Measurement of shared decision making - a review of instruments

NARCIS (Netherlands)

Scholl, I.; Koelewijn-van Loon, M.; Sepucha, K.; Elwyn, G.; Legare, F.; Harter, M.; Dirmaier, J.

2011-01-01

The last years have seen a clear move towards shared decision making (SDM) and increased patient involvement in many countries. However, as the field of SDM research is still relatively young, new instruments for the measurement of (shared) decision making (process, outcome and surrounding elements)

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.

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)

Spectro-photometric calibration of the SuperNova Integral Field Spectrograph in the Nearby Supernova Factory collaboration framework

International Nuclear Information System (INIS)

Buton, Clement

2009-01-01

Ten years ago, type Ia supernovae used as distances indicators led to the discovery of the accelerating expansion of the universe. Today, a second generation of surveys has significantly increased the high-redshift type Ia supernovae sample. The low-redshift sample was however still limiting the cosmological analysis using SNe. In this framework, the Nearby Supernova Factory has followed 200 nearby type Ia supernovae using the dedicated Supernovae Integral Field Spectrograph with spectro-photometric capacities. My PhD thesis has been carried out at the Institut de Physique Nucleaire de Lyon and at the Lawrence Berkeley National Laboratory in the framework of the international cosmological project SNfactory. In order to reach the design spectrophotometric accuracy, attention has been focused on several key aspects of the calibration procedure, including: determination of a dedicated point spread function for 3D point source extraction, estimating the nightly photometric quality, derivation of the nightly sky extinction over the extended optical domain, its modeling in terms of physical components and its variability within a given night. A full multi-standards calibration pipeline has been implemented using approximately 4000 observations of spectrophotometric standard stars taken throughout the night over nearly 500 individual nights. Preliminary scientific results of the whole SNfactory collaboration will be presented at the end of this thesis. (author)

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

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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.

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

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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 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)

Sensitive flotation-spectrophotometric determination of gold, based on the gold(I)-iodide-methylene blue system.

Science.gov (United States)

Marczenko, Z; Jankowski, K

1985-04-01

The gold(I)-iodide-Methylene Blue (MB) system is suitable for flotation separation and spectrophotometric determination of gold. Under the optimum conditions [(MB(+))(AuI(2)(-))].3[(MB(+))(I(3)(-))] is formed, and floated with cyclohexane. The product is dissolved in methanol and its absorbance measured. The molar absorptivity is 3.4 x 10(5)1.mole(-1).cm(-1) at 655 nm. The proposed method is more than three times as sensitive as the Rhodamine B method. Pt, Pd, Ag and Hg interfere seriously, and Ir, Rh, Bi and Cd to a smaller extent. Preliminary separation of gold by precipitation with tellurium as a collector is recommended. The method has been applied to determination of gold traces (about 1 x 10(-4)%) in a copper sample.

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)

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

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.

Measuring local autonomy: A decision-making approach

NARCIS (Netherlands)

Fleurke, F.; Willemse, R.

2006-01-01

In studies on central-local relations it is common to assess local autonomy in a deductive way. The extent of local autonomy is determined by measuring the central legal and financial competence, after which the remaining room for local decision-making is determined. The outcome of this indirect

Spectrophotometric determination of boric acid in boron powder with curcumin

International Nuclear Information System (INIS)

Grotheer, E.W.

1979-01-01

A rapid and accurate method was needed to determine trace amounts of boric acid for quality control and specification testing of elemental boron. The reaction between boric acid and curcumin occurs at a measurable rate only when the curcumin molecule is protonated. Protonation takes place at the carbonyl groups in the presence of a strong acid and occurs completely and rapidly when sulfuric acid is added to a solution of curcumin in acetic acid. Spectrophotometric measurements were made. The extraction of boric acid from boron powder was found to be complete within 2h when either water or the diol solution was used. Whatman No. 40 cr 42 filter paper was used to obtain diol samples free of boron particles. The extraction efficiency of 2-ethyl-1,3-hexanediol was evaluated by adding 1 ml of 500 ppM aqueous boric acid and 1 drop of 10% NaOH to accurately weighed samples of boron powder. The water then was evaporated at room temperature and the samples were extracted with diol solution. The data obtained are included. The extraction efficiency also was evaluated by determining the boric acid content of boron which had been recovered from a previous extraction and boric acid determination. The determination of boric acid using curcumin is unaffected by the presence of other compounds, except for fluoride and nitrate ions. 2 tables

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 study of the complexation equilibria of lanthanum(III) with 1,4-bis(4'-methylanilino)anthraquinone and the determination of lanthanum(III)

International Nuclear Information System (INIS)

Idriss, K.A.-R; El-Shahawy, A.S.; Sedaira, H.; Harfoush, A.A.

1985-01-01

The complexation equilibria of lanthanum(III) with 1,4-bis(4'-methylanilino)anthraquinone (Quinizarin Green) were studied spectrophotometrically in 40% V/V dimethylformamide using graphical analysis of the absorbance curves. The reaction mechanism of lanthanum with the bisarylaminoanthraquinone dye within the pH range 6 to 9.25 was demonstrated. The thermodynamic stabilities and the molar absorptivities of the complexes formed were determined. The optimum conditions for the spectrophotometric determination of La(III) with this reagent were found. (author)

Make-or-buy decisions and the manipulability of performance measures

OpenAIRE

Andersson, Fredrik

2009-01-01

Abstract in Undetermined The make-or-buy decision is analyzed in a simple framework combining contractual incompleteness with the existence of an imperfect but contractible performance measure. Contractual incompleteness gives rise to two regimes, identified with make and buy. The performance measure on which comprehensive contracts can be written is imperfect in the sense of being subject to manipulation. The performance incentives faced by the agent are stronger in the “buy” regime. A posit...

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

A simple spectrophotometric determination of trace amounts of vanadium using thionin

Directory of Open Access Journals (Sweden)

Tom Cherian

2005-12-01

Full Text Available A simple and sensitive spectrophotometric method has been developed for the determination of trace amounts of vanadium using thionin as a chromogenic reagent. The proposed method is based on the reaction of vanadium(V with potassium iodide in acid medium to liberate iodine, which bleaches the violet colour of thionin and is measured at 600 nm. This decrease in absorbance is directly proportional to the vanadium(V concentration and obeys Beer's law in the range of 0.2-10 μgmL-1 of V(V. The molar absorptivity, Sandell's sensitivity, detection limit and quantitation limit of the method were found to be 2.298 x 104 Lmol-1cm-1, 0.52 x 10-2 μgcm-2, 0.035 μgmL-1 and 0.11 μgmL-1, respectively. The optimum reaction conditions and other analytical conditions were evaluated. The effect of interfering ions on the determination is described. The developed method has been successfully applied to the analysis of the vanadium in synthetic and alloy samples.

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.

Kinetic spectrophotometric determination of trace amounts of selenium and vanadium

Energy Technology Data Exchange (ETDEWEB)

Safavi, A.; Sedghy, H.R.; Shams, E. [Dept. of Chemistry, Shiraz Univ. (Iran)

1999-11-01

A sensitive kinetic spectrophotometric method has been developed for the determination of Se(IV) over the range of 45 to 4000 ng in 10 mL of solution. The method is based on the catalytic effect of Se(IV) on the reduction reaction of bromate by hydrazinium dichloride, with subsequent reaction of Ponceau S with products of the above reaction (chlorine and bromine), causing color changing of Ponceau S. Method development includes optimization of time interval for measurement of slope, pH, reagents concentration, and temperature. The optimized conditions yielded a theoretical detection limit of 33 ng/10 mL of solution of Se(IV). The interfering effects were studied and removed. The method was applied to the determination of selenium in spiked water, Kjeldahl tablet, selenium tablet, and shampoo. Vanadium(V) has an inhibition effect on the catalyzed reaction of bromate and hydrazine by selenium. Using this effect, V(V) can be determined in the range of 70 to 2500 ng in 10 mL of solution. The optimization procedure includes pH and selenium concentration. An extraction method was used for interference removal. The method was applied to the determination of vanadium in petroleum. (orig.)

Sensitization of glycine (spectrophotometric read-out) dosimetric system using sorbitol

International Nuclear Information System (INIS)

Shinde, S.H.; Mukherjee, T.

2009-01-01

Glycine spectrophotometric read-out systems have a useful dose range of 15-4000 Gy. An attempt was made to sensitize it using sorbitol as a sensitizer. Optimum compositions of aqueous acidic solutions of ferrous ammonium sulphate-xylenol orange (XO), i.e. FX and sorbitol-ferrous ammonium sulphate-xylenol orange, i.e. SFX, for 400 mg of glycine, which gives maximum dosimetric response for any given dose, were established. Molar absorption coefficient values of ferric-XO-glycine complex, i.e. ε-values, were determined for glycine system in FX and SFX. These values were found to be 8410 and 15,000 m 2 mol -1 respectively, indicating that an enhancement or sensitivity factor of about 1.78 can be achieved by sorbitol for glycine in SFX. This factor was further confirmed by measuring the gamma dose response of glycine in FX and in SFX for four different doses, viz. 37.8, 75.5, 151 and 302 Gy. It was observed that dose response of glycine in SFX is about 77% more than that of glycine in FX. The maximum variation observed in response of glycine in FX or SFX was found to be within ±1.5%.

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 +/).

Simultaneous determination of rifampicin, isoniazid and pyrazinamide in tablet preparations by multivariate spectrophotometric calibration.

Science.gov (United States)

Goicoechea, H C; Olivieri, A C

1999-08-01

The use of multivariate spectrophotometric calibration is presented for the simultaneous determination of the active components of tablets used in the treatment of pulmonary tuberculosis. The resolution of ternary mixtures of rifampicin, isoniazid and pyrazinamide has been accomplished by using partial least squares (PLS-1) regression analysis. Although the components show an important degree of spectral overlap, they have been simultaneously determined with high accuracy and precision, rapidly and with no need of nonaqueous solvents for dissolving the samples. No interference has been observed from the tablet excipients. A comparison is presented with the related multivariate method of classical least squares (CLS) analysis, which is shown to yield less reliable results due to the severe spectral overlap among the studied compounds. This is highlighted in the case of isoniazid, due to the small absorbances measured for this component.

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)

Optical spectrophotometric atlas of Supernova 1987A in the LMC. I. The first 130 days

International Nuclear Information System (INIS)

Phillips, M.M.; Heathcote, S.R.; Hamuy, M.; Navarrete, M.

1988-01-01

Optical spectrophotometry of SN 1987A in the Large Magellanic Cloud (LMC) covering the first 5 months since outburst is presented. More than 80 spectra were obtained at Cerro Tololo over this period, mostly with the 2D-Frutti two-dimensional photon-counting detector on the 1-m telescope. The spectrophotometric calibration of the 2D-Frutti data is considered in detail. Through a comparison with broadband photometry, it is shown that the accuracy of the 2D-Frutti spectrophotometry is + or - 5 percent in absolute terms, and that the relative calibration for any single spectrum is accurate to + or - 3 percent. CCD spectrophotometry obtained on the first night of observation (Feb. 25, 1987) is also briefly discussed. Radial velocities for several prominent absorption and emission features are measured from these combined data. 13 references

Spectrophotometric determination of boron by solvent extraction with 2-hydroxy-2-methylbutyric acid and malachite green

International Nuclear Information System (INIS)

Sato, Shigeya; Uchikawa, Sumio

1984-01-01

A very simple and sensitive method for the spectrophotometric determination of boron was developed. Boron was found to react with 2-hydroxy-2-methylbutyric acid in weak acidic aqueous solution at room temperature to form a complex anion which can be extracted into chlorobenzene with malachite green in a single extraction; boron is determined indirectly by measuring the absorbance of malachite green in the extract at 629 nm. The calibration graph is linear over the range (7.50 x 10 -7 - 2.00 x 10 -5 ) mol dm -3 boron; the apparent molar absorptivity is 6.50 x 10 4 dm 3 mol -1 cm -1 . The method is applied to the determination of micro amounts of boron in natural waters with satisfactory results. (author)

SPECTROPHOTOMETRIC DETERMINATION OF CHLOROPHYLLS AND CAROTENOIDS. AN EFFECT OF SONICATION AND SAMPLE PROCESSING

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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.

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)

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

Spectrophotometric observations of very low ionization HII regions in the LMC

International Nuclear Information System (INIS)

Pena, M.; Ruiz, M.T.; Rubio, M.

1987-01-01

Optical spectrophotometric observations of 17 very low ionization HII regions of the LMC are reported. Physical conditions and chemical composition of these objects are derived from the emission line intensities. The average chemical abundances obtained are: log O/H=8.49+-0.08, log N/H=6.91+-0.07 and log S/H=6.89+-0.10. We do not find evidence of any composition gradient in the LMC. The HII regions in the vicinity of the detected molecular cloud complexes show higher nebular reddening. (Author)

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

Derivative spectrophotometric determination of trace amounts of Tungsten(VI) in real water samples

International Nuclear Information System (INIS)

Viswanatha, C.; Ramakrishna Reddy, K.; Devanna, N.; Praveen Kumar, M.D.

2012-01-01

2,4-Dimethoxybenzaldehydeisonicotinoylhydrazone (DMBHIH) has been synthesized and characterized with IR, NMR and Mass Spectroscopic methods. A simple and derivative spectrophotometric method has been developed for the determination of trace amounts of W(VI). The reagent forms a yellow coloured water soluble complex with W(VI) in basic medium (pH 8.0). The molar absorptivity and Sandell's sensitivity of coloured species are 3.43 x 10 4 L.mol -1 cm -1 and 0.0049 μg/cm 2 respectively. Beer's law is obeyed in the range 0.4113-6.2138 μg/ml of W(VI) at λ max 394 nm. W(VI) forms 1:1 complex with DMBHIH and stability constant of the complex was 5.22x10 6 . The first and second derivative amplitude was measured at 453 nm and 468 nm. The developed method applied for the determination of W(VI) in alloys and biological samples. (author)

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.

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 study of the complexation equilibria of uranium(VI) with 1,4-bis(4'-methylanilino)anthraquinone and determination of uranium(VI)

International Nuclear Information System (INIS)

Idriss, K.A.; Seleim, M.M.; Abu-Bakr, M.S.; Sedaira, H.

1985-01-01

The reaction of U(VI) with 1,4-bis(4'-methylanilino)anthraquinone (quinizarin green) in water-dimethylformamide medium was investigated spectrophotometrically. The complexation equilibria in solution were demonstrated. The study of the reaction in presence of equimolar concentrations or in solutions containing metal or ligand excess gave evidence for the formation of complexes with stoichiometric ratios of UO 2 :L = 1:1 and 1:2 in dependence on the pH of the medium. Their thermodynamic stabilities and the values of their molar absorption coefficients were determined. The optimum conditions for spectrophotometric determination of U(VI) with this reagent were found. (author)

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%.

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)

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...

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)

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

Validation of a spectrophotometric methodology for the quantification of polysaccharides from roots of Operculina macrocarpa (jalapa

Directory of Open Access Journals (Sweden)

Marcos A.M. Galvão

Full Text Available The roots from Operculina macrocarpa (L. Urb., Convolvulaceae, are widely used in Brazilian traditional medicine as a laxative and purgative. The biological properties of this drug material have been attributed to its polysaccharides content. Thus, the aim of this study was to evaluate the polysaccharide content in drug material from O. macrocarpa by spectrophotometric quantitative analysis. The root was used as plant material and the botanical identification was performed by macro and microscopic analysis. The plant material was used to validate the spectrophotometric procedures at 490 nm for the quantification of the reaction product from drug polysaccharides and phenol-sulfuric acid solution. The analytical procedure was evaluated in order to comply with the necessary legal requirements by the determination of the following parameters: specificity, linearity, selectivity, precision, accuracy and robustness. This study provides with a simple and valid analytical procedure (linear, precise, accurate and reproducible, which can be satisfactorily used for quality control and standardization of herbal drug from O. macrocarpa.

Spectrophotometric determination of boron by solvent extraction with 2-hydroxy-2-methylbutyric acid and malachite green

Energy Technology Data Exchange (ETDEWEB)

Sato, Shigeya; Uchikawa, Sumio [Kumamoto Univ. (Japan). Faculty of Education

1984-03-01

A very simple and sensitive method for the spectrophotometric determination of boron was developed. Boron was found to react with 2-hydroxy-2-methylbutyric acid in weak acidic aqueous solution at room temperature to form a complex anion which can be extracted into chlorobenzene with malachite green in a single extraction; boron is determined indirectly by measuring the absorbance of malachite green in the extract at 629 nm. The calibration graph is linear over the range (7.50 x 10/sup -7/ - 2.00 x 10/sup -5/) mol dm/sup -3/ boron; the apparent molar absorptivity is 6.50 x 10/sup 4/ dm/sup 3/ mol/sup -1/ cm/sup -1/. The method is applied to the determination of micro amounts of boron in natural waters with satisfactory results.

Spectrophotometric determination of low levels arsenic species in beverages after ion-pairing vortex-assisted cloud-point extraction with acridine red.

Science.gov (United States)

Altunay, Nail; Gürkan, Ramazan; Kır, Ufuk

2016-01-01

A new, low-cost, micellar-sensitive and selective spectrophotometric method was developed for the determination of inorganic arsenic (As) species in beverage samples. Vortex-assisted cloud-point extraction (VA-CPE) was used for the efficient pre-concentration of As(V) in the selected samples. The method is based on selective and sensitive ion-pairing of As(V) with acridine red (ARH(+)) in the presence of pyrogallol and sequential extraction into the micellar phase of Triton X-45 at pH 6.0. Under the optimised conditions, the calibration curve was highly linear in the range of 0.8-280 µg l(-1) for As(V). The limits of detection and quantification of the method were 0.25 and 0.83 µg l(-1), respectively. The method was successfully applied to the determination of trace As in the pre-treated and digested samples under microwave and ultrasonic power. As(V) and total As levels in the samples were spectrophotometrically determined after pre-concentration with VA-CPE at 494 nm before and after oxidation with acidic KMnO4. The As(III) levels were calculated from the difference between As(V) and total As levels. The accuracy of the method was demonstrated by analysis of two certified reference materials (CRMs) where the measured values for As were statistically within the 95% confidence limit for the certified values.

Spectrophotometric study on beryllium complex with Chromazurol S in the presence of zephiramine

International Nuclear Information System (INIS)

Nishida, Hiroshi

1982-01-01

Beryllium(II) reacted with Chromazurol S (CAS, H 4 L) to produce two types of 1:2 complexes in the presence of zephiramine, one of which was in a form of mononuclear Be(HL) 2 4 - showing an absorption maximum at 612 nm and other was in binuclear Be 2 (OH)(HL) 4 9 - showing an absorption maximum at 525 nm. The formation equilibrium of these complexes in the range of pH 5 to 10 was examined by the spectrophotometric method. The binuclear complex was found to be produced from the hydrolysis of the mononuclear complex through the following equation; Be(HL) 2 4 - + 1/2H 2 O reversible 1/2Be 2 (OH)(HL) 4 9 - + 1/2H + where zephiramine ion was not shown. The effect of anions such as chloride and sulfate ions on this equilibrium was observed. The apparent equilibrium constant decreased with the increase of the anion concentrations. The equilibrium constant was larger in the presence of sulfate ion than in chloride ion at the same concentration. In the practical spectrophotometric determination, however, these effects by such diverse ions could be successfully elimination by raising the pH to 10 so high as the above equilibrium was shifted rightward thoroughly. (author)

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...

AN APPLICATION OF FLOW INJECTION ANALYSIS WITH GAS DIFFUSION AND SPECTROPHOTOMETRIC DETECTION FOR THE MONITORING OF DISSOLVED SULPHIDE CONCENTRATION IN ENVIRONMENTAL SAMPLES

Directory of Open Access Journals (Sweden)

Malwina Cykowska

2014-10-01

Full Text Available The monitoring of the concentration of sulphide is very important from the environment point of view because of high toxicity of hydrogen sulphide. What is more hydrogen sulphide is an important pollution indicator. In many cases the determination of sulphide is very difficult due to complicated matrix of some environmental samples, which causes that most analytical methods cannot be used. Flow injection analysis allows to avoid matrix problem what makes it suitable for a wide range of applications in analytical laboratories. In this paper determination of dissolved sulphide in environmental samples by gas-diffusion flow injection analysis with spectrophotometric detection was presented. Used gas-diffusion separation ensures the elimination of interferences caused by sample matrix and gives the ability of determination of sulphides in coloured and turbid samples. Studies to optimize the measurement conditions and to determine the value of the validation parameters (e.g. limit of detection, limit of quantification, precision, accuracy were carried out. Obtained results confirm the usefulness of the method for monitoring the concentration of dissolved sulphides in water and waste water. Full automation and work in a closed system greatly reduces time of analysis, minimizes consumption of sample and reagents and increases safety of analyst’s work.

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.)

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 determination of volautile inorganic hydrides in binary gaseous mixtures

International Nuclear Information System (INIS)

Rezchikov, V.G.; Skachkova, I.N.; Kuznetsova, T.S.; Khrushcheva, V.V.

1985-01-01

A study was made on possibility of single and continuons analysis of binary mixtures (hydride-gas) for the content of volatile inorganic hydrides (VIH) from absorption spectra in the 185-280 nm band. Dependences of the percentage of VIH transmission on the wavelength are presented. It is shown that the maximum of their absorption depends on the element-hydrogen the bond length and binding energy. Detection limit for boron hydride was established to be n x 10 -3 % vol at 185-190 nm wavelength. Technique for spectrophotometric hydride determination in binary mixtures with hydrogen, argon, helium was developed. The technique provides the continuous control of gaseous mixture composition

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)

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)

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)

Residual gravimetric method to measure nebulizer output.

Science.gov (United States)

Vecellio None, Laurent; Grimbert, Daniel; Bordenave, Joelle; Benoit, Guy; Furet, Yves; Fauroux, Brigitte; Boissinot, Eric; De Monte, Michele; Lemarié, Etienne; Diot, Patrice

2004-01-01

The aim of this study was to assess a residual gravimetric method based on weighing dry filters to measure the aerosol output of nebulizers. This residual gravimetric method was compared to assay methods based on spectrophotometric measurement of terbutaline (Bricanyl, Astra Zeneca, France), high-performance liquid chromatography (HPLC) measurement of tobramycin (Tobi, Chiron, U.S.A.), and electrochemical measurements of NaF (as defined by the European standard). Two breath-enhanced jet nebulizers, one standard jet nebulizer, and one ultrasonic nebulizer were tested. Output produced by the residual gravimetric method was calculated by weighing the filters both before and after aerosol collection and by filter drying corrected by the proportion of drug contained in total solute mass. Output produced by the electrochemical, spectrophotometric, and HPLC methods was determined after assaying the drug extraction filter. The results demonstrated a strong correlation between the residual gravimetric method (x axis) and assay methods (y axis) in terms of drug mass output (y = 1.00 x -0.02, r(2) = 0.99, n = 27). We conclude that a residual gravimetric method based on dry filters, when validated for a particular agent, is an accurate way of measuring aerosol output.

A New Technique for Quantitative Determination of Dexamethasone in Pharmaceutical and Biological Samples Using Kinetic Spectrophotometric Method

Directory of Open Access Journals (Sweden)

Ali Mohammad Akhoundi-Khalafi

2015-01-01

Full Text Available Dexamethasone is a type of steroidal medications that is prescribed in many cases. In this study, a new reaction system using kinetic spectrophotometric method for quantitative determination of dexamethasone is proposed. The method is based on the catalytic effect of dexamethasone on the oxidation of Orange G by bromate in acidic media. The change in absorbance as a criterion of the oxidation reaction progress was followed spectrophotometrically. To obtain the maximum sensitivity, the effective reaction variables were optimized. Under optimized experimental conditions, calibration graph was linear over the range 0.2–54.0 mg L−1. The calculated detection limit (3sb/m was 0.14 mg L−1 for six replicate determinations of blank signal. The interfering effect of various species was also investigated. The present method was successfully applied for the determination of dexamethasone in pharmaceutical and biological samples satisfactorily.

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.

Extraction-spectrophotometric study of ruthenium (4) and osmium (4,8) reaction with 2-mercaptobenzimidazole, 2-mercaptobenzoxazole and 2-mercaptobenzothiazole in acetate buffer solutions

Energy Technology Data Exchange (ETDEWEB)

Lomakina, L N; Ignat' eva, T I; Busev, A I [Moskovskij Gosudarstvennyj Univ. (USSR)

1978-03-01

The complex formation of Ru(4) and Os(4, 8) with 2-mercaptobenzimidazole (MBI), 2-mercaptobenzoxazole (MBO) and 2-mercaptobenzothiazole (MBT) has been studied spectrophotometrically in acetate buffer solutions. As it has been shown earlier, Os and Ru react with the reagents in the oxidation state of three . Compound polinuclear structures of Ru and Os with MBI and MBO are suggested. A spectrophotometric procedure has been developed of determining Ru and Os (>=10/sup -4/%) with MBO in natural and industrial materials after selective absorption of the tetraoxides during distillation.

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.

Individual v. community-level measures of women's decision-making ...

African Journals Online (AJOL)

Individual v. community-level measures of women's decision-making involvement and ... participation for child survival in sub-Saharan Africa is limited. ... Multilevel discrete-time hazard models were employed to investigate the net effect of ...

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

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.

Challenges and solutions for the analysis of in situ, in crystallo micro-spectrophotometric data

International Nuclear Information System (INIS)

Dworkowski, Florian S. N.; Hough, Michael A.; Pompidor, Guillaume; Fuchs, Martin R.

2015-01-01

The particular challenge of the analysis of optical absorption and Raman spectroscopic data measured from protein crystals and how the SLS-APE software toolbox supports scientists in dealing with such data is described. Combining macromolecular crystallography with in crystallo micro-spectrophotometry yields valuable complementary information on the sample, including the redox states of metal cofactors, the identification of bound ligands and the onset and strength of undesired photochemistry, also known as radiation damage. However, the analysis and processing of the resulting data differs significantly from the approaches used for solution spectrophotometric data. The varying size and shape of the sample, together with the suboptimal sample environment, the lack of proper reference signals and the general influence of the X-ray beam on the sample have to be considered and carefully corrected for. In the present article, how to characterize and treat these sample-dependent artefacts in a reproducible manner is discussed and the SLS-APEin situ, in crystallo optical spectroscopy data-analysis toolbox is demonstrated

Spectrophotometric determination of hydrogen peroxide with osmium(VIII) and m-carboxyphenylfluorone.

Science.gov (United States)

Hoshino, Mitsuru; Kamino, Shinichiro; Doi, Mitsunobu; Takada, Shingo; Mitani, Shota; Yanagihara, Rika; Asano, Mamiko; Yamaguchi, Takako; Fujita, Yoshikazu

2014-01-03

Spectrophotometric determination of hydrogen peroxide was accomplished with osmium(VIII) and m-carboxyphenylfluorone (MCPF) in the presence of cetyltrimethylammonium chloride (CTAC). In the determination of hydrogen peroxide based on the fading of the color of osmium(VIII)-MCPF complex, Beer's law was obeyed in the range 20-406 ng mL(-1), with an effective molar absorption coefficient (at 580 nm) of 5.21×10(4) L mol(-1) cm(-1) and a relative standard deviation of 0.33% (n=6). Further, we performed the characterization of MCPF and obtained the crystal structure. Copyright © 2013 Elsevier B.V. All rights reserved.

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.

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.

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.

SHARDS: a spectro-photometric analysis of distant red and dead massive galaxies

Science.gov (United States)

Pérez-González, P. G.; Cava, A.; The Shards Team

2013-05-01

SHARDS, an ESO/GTC Large Program, is an ultra-deep (26.5 mag) spectro-photometric survey carried out with GTC/OSIRIS and designed to select and study massive passively evolving galaxies at z= 1.0--2.5 in the GOODS-N field. The survey uses a set of 24 medium band filters (FWHM ˜15 nm) covering the 500--950 nm spectral range. Our observing strategy has been planned to detect, for z>1 sources, the prominent Mg absorption feature (at rest-frame ˜280 nm), a distinctive, necessary, and sufficient feature of evolved stellar populations (older than 0.5 Gyr). These observations are being used to: (1) construct for the first time an unbiased sample of high-z quiescent galaxies, which extends to fainter magnitudes the samples selected with color techniques and spectroscopic surveys; (2) derive accurate ages and stellar masses based on robust measurements of spectral features such as the Mg(UV) or D(4000) indices; (3) measure their redshift with an accuracy Δ z/(1+z)<0.02; and (4) study emission-line galaxies (starbursts and AGN) up to very high redshifts. The well-sampled optical SEDs provided by SHARDS for all sources in the GOODS-N field are a valuable complement for current and future surveys carried out with other telescopes (e.g., Spitzer, HST, and Herschel).

Study of extraction-spectrophotometric micro-determination of boron with methylene blue and its application

International Nuclear Information System (INIS)

Zhu Daohong

1990-08-01

A sensitive extraction-spectrophotometric method for microdetermination of boron with methylene blue was investigated. The method was based on the extraction of a BF 4 - -methylene blue complex into dichloroethane. Boron was determined directly by measuring the absorbance at 658 nm. The calibration graph was linear over the range of 2.5 x 10 -9 to 8 x 10 -8 g/mL. The blank, mechanism of the reactions, interference of other ions and some optimum conditions of the method were studied in detail. The main source of the blank resulted from methylene blue and the complex of F - -methylene blue. In order to reduce the blank, the amounts of methylene blue, H 2 SO 4 and HF were used as less as possible. Only one to one complex BF 4 - -methylene blue was formed in the medium of H 2 SO 4 . About 90% of methylene blue and F - -methylene blue complex was removre with 5 ml of water and only a little amount of BF 4 -methylene blue complex was decomposed. The extraction-spectrophotometric method with methylene blue was first applied to the microdetermination of boron in sodium metal and UF 6 . The sample of sodium metal was taken and weighed in the glovebox filled with argon. Then sodium metal was oxidized, hydrolyzed, netralized and fluorizated with H 2 O, H 2 SO 4 and HF, respectively. The 0.5 ppm of boron in sodium metal was determined with a relative error about ±4%. This method can be applied to the determination of boron in sodium metal, sodium sulfate and sodium hydroxide at diffeent grades. The species of boron in the hydrolysate of UF 6 is BF 4 - anion, so the sample can be directly analyzed. Boron contents in the range of 0.1 to 0.5 ppm was determined with a relative error about ±3%. Six samples could be analysed in 2h

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...

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

Directory of Open Access Journals (Sweden)

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.

Oxygen consumption in Plasmodium berghei-infected murine red cells: a direct spectrophotometric assay in intact erythrocytes.

Science.gov (United States)

Deslauriers, R; Moffatt, D J; Smith, I C

1986-05-29

A spectrophotometric assay has been devised to measure oxygen consumption non-invasively in intact murine red cells parasitized by Plasmodium berghei. The method uses oxyhemoglobin in the erythrocytes both as a source of oxygen and as an indicator of oxygen consumption. Spectra of intact cells show broad peaks and sloping baselines due to light-scattering. In order to ascertain the number of varying components in the 370-450 nm range, the resolution of the spectra was enhanced using Fourier transforms of the frequency domain spectra. Calculation of oxygen consumption was carried out for two-component systems (oxyhemoglobin, deoxyhemoglobin) using absorbances at 415 and 431 nm. Samples prepared from highly parasitized mice (greater than 80% parasitemia, 5% hematocrit) showed oxygen consumption rates of (4-8) X 10(-8) microliter/cell per h. This rate was not attributable to the presence of white cells or reticulocytes. The rate of oxygen consumption in the erythrocytes is shown to be modulated by various agents: the respiratory inhibitors NaN3 and KCN (1 mM) reduced oxygen consumption 2-3-fold; salicylhydroxamic acid (2.5 mM) caused a 20% reduction in rate and 10 mM NaN3, completely blocked deoxygenation. Antimalarial drugs and metal-chelating agents were also tested. Chloroquine, EDTA and desferal (desferoxamine mesylate) did not decrease the deoxygenation rate of hemoglobin in parasitized cells. Quinacrine, quinine and primaquine reduced the rate of formation of deoxyhemoglobin but also produced substantial quantities of methemoglobin. The lipophilic chelator, 5-hydroxyquinoline, decreased the rate of deoxygenation one-third. The spectrophotometric assay provides a convenient means to monitor oxygen consumption in parasitized red cells, to test the effects of various agents thereon, and potentially to explore possible mechanisms for oxygen utilization.

K4 Fe(CN)6 as a spectrophotometric agent for uranium analysis

International Nuclear Information System (INIS)

Soedyartomo; Tarwita.

1976-01-01

The properties of K 4 Fe(CN) 6 as a spectrophotometric agent for Uranium analysis was observed by putting some experiment into practice. The experiment covers the observation of expanding colour stability, the optimization of operating condition (p,H. and wavelength), the effect of K 4 Fe(CN) 6 concentration and the preparation of its standard curves (transmitansion vs uranium concentration) and the observation of the interfering metal spectra s (Cu ++ , Fe ++ ) either of its mixtures or themselves alone, has been carried out. The result and discussion on it are given. (author)

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.

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 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...

Acidity Constants Determination of Triazine Dye Derivative in the presence of some Surfactants by Multiwavelength Spectrophotometric and Spectrofluorimetric

Directory of Open Access Journals (Sweden)

Ali Yeganeh Faal

2014-03-01

Full Text Available In this work, acidity constants protonated form of 4.4'-bis astilbene-2,2'-disulfonic-disodium salts (TRIAZ have been determined spectrophotometrically and spectrofluorimetrically at 25◦C and ionic strength of 0.1M KNO3. A program based on MCR-ALS applied for determination of acidity constants. The results show that the peak values of dye are influenced by the presence of anionic, cationic, and nonionic surfactants. The effects of sodium dodecyl sulfate (SDS, Triton X-100 (TX-100 and cetyl trimethyl ammonium bromide (CTAB as a surface-active agent on the acidic and basic forms, and the spectral properties of dye were studied. Also, we determined the critical micelle concentration (CMC for these surfactants by spectrophotometric and spectrofluorimetric triazine dye probes. In addition, by using of evolving factor analysis (EFA and multivariate curve resolution alternative least squares (MCR-ALS methods, acidity constants were acquired.

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

Directory of Open Access Journals (Sweden)

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.

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.

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.

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)

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.

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

Directory of Open Access Journals (Sweden)

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.

Spectrophotometric studies of marine surfactants in the southern Baltic Sea

Directory of Open Access Journals (Sweden)

Violetta Drozdowska

2015-04-01

Full Text Available It is well known that surfactants in the southern Baltic Sea constitute the organic matter from riverine waters discharges as well as the secondary degradation products of marine phytoplankton excretion. They reach the surface microlayer by the upwellings and turbulent motions of water and in the membranes of the vesicles as well as from the atmosphere. To assess concentration and spatial distribution of marine surfactants in the southern Baltic Sea, the steady-state spectrophotometric and spectrofluorometric measurements of water samples taken from a surface film and a depth of 0.5 m were carried out. Water samples were collected during windless days of the cruise of r/v ‘Oceania’ in November 2012, from the open and the coastal waters having regard to the vicinity of the Vistula and Łeba mouths. In the present paper, fractions of dissolved organic matter having chromophores (CDOM or fluorophores (FDOM are recognized through their specific spectroscopic behavior, i.e., steady-state absorption, fluorescence excitation and fluorescence spectra. The steady-state spectroscopic measurements revealed the CDOM and FDOM molecules characteristic to both the land and marine origin. Moreover, the concentration and spatial distribution of marine surfactants significantly depend on the distance from the river mouth. Finally, higher values of absorbance and fluorescence intensity observed in a surface film in comparison to these values in a depth of 0.5 m clearly suggest the higher concentration of organic matter in a marine film. On the other hand, our results revealed that a surface microlayer is composed of the same CDOM and FDOM as bulk water.

Sensitive spectrophotometric determination of ascorbic acid in drugs and foods using surface plasmon resonance band of silver nanoparticles

Directory of Open Access Journals (Sweden)

Kobra Zarei

2015-12-01

Full Text Available A simple and sensitive procedure was proposed for spectrophotometric determination of ascorbic acid. It was found that the reduction of Ag+ to silver nanoparticles (Ag-NPs by ascorbic acid in the presence of polyvinylpyrrolidone (PVP as a stabilizing agent produce very intense surface plasmon resonance peak of Ag-NPs. The plasmon absorbance of the Ag-NPs at λ = 440 nm allows the quantitative spectrophotometric detection of the ascorbic acid. The calibration curve was linear with concentration of ascorbic acid in the range of 0.5–60 μM. The detection limit was obtained as 0.08 μM. The influence of potential interfering substances on the determination of ascorbic acid was studied. The proposed method was successfully applied for the determination of ascorbic acid in some powdered drink mixtures, commercial orange juice, natural orange juice, vitamin C injection, effervescent tablet, and multivitamin tablet.

Spectrophotometric analysis of flavonoid-DNA binding interactions at physiological conditions

Science.gov (United States)

Janjua, Naveed Kausar; Siddiqa, Asima; Yaqub, Azra; Sabahat, Sana; Qureshi, Rumana; Haque, Sayed ul

2009-12-01

Mode of interactions of three flavonoids [morin (M), quercetin (Q), and rutin (R)] with chicken blood ds.DNA (ck.DNA) has been investigated spectrophotometrically at different temperatures including body temperature (310 K) and at two physiological pH values, i.e. 7.4 (human blood pH) and 4.7 (stomach pH). The binding constants, Kf, evaluated using Benesi-Hildebrand equation showed that the flavonoids bind effectively through intercalation at both pH values and body temperature. Quercetin, somehow, showed greater binding capabilities with DNA. The free energies of flavonoid-DNA complexes indicated the spontaneity of their binding. The order of binding constants of three flavonoids at both pH values were found to be Kf(Q) > Kf(R) > Kf(M) and at 310 K.

Spectrophotometric determination of La (III) with sulphamethoxazole based hydroxy triazene

International Nuclear Information System (INIS)

Manwani, Sapana; Chauhan, R.S.; Goswami, A.K.

2015-01-01

In the present study, 3-hydroxy-3-p-chlorophenyll-1-(4-amino-N-(5-methyl-1,2-oxazole-3- yl) benzenesulphonamide-methane) triazene has been synthesized by coupling of hydroxylamine obtained by reduction of nitro compound with diazonium salt obtained from sulphamethoxazole taking hydroxylamine in excess at temperature between 0-5°C. Chemical structure of the synthesized compound was confirmed by IR, 1 H NMR, MASS and by elemental analysis. The complex of the reagent with La (III) has been studied. 3-hydroxy-3-p-chlorophenyll-1-(4-amino-N-(5-methyl-1,2-oxazole-3-yl) benzenesulphonamide-methane) triazene has been used for spectrophotometric determination of lanthanum (III) at 392 nm, keeping the pH between 8.5 to 8.9

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

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 study of the complexation equilibria of zirconium(IV) with 1-amino-4-hydroxyanthraquinone and the determination of zirconium

Energy Technology Data Exchange (ETDEWEB)

Idriss, K A; Seleim, M M; Saleh, M S; Abu-Bakr, M S; Sedaira, Hassan

1988-11-01

The spectral absorption and acid-base characteristics of 1-amino-4-hydroxyanthraquinone (AMHA) were studied in water -ethanol media. The composition, molar absorptivities, equilibrium constants and stability constants of the chelates of this reagent with zirconium(IV) have been determined spectrophotometrically in 40% V/V ethanol at 20/sup 0/C and an ionic strength of 0.1 M (NaClO/sub 4/). Graphical logarithmic analysis of the absorbance graphs was used to demonstrate and characterise the complexation equilibria in solution. A simple, rapid, selective and sensitive method for the spectrophotometric determination of trace amounts of zirconium is proposed based on the formation of the Zr(AMHA)/sub 2/ complex at pH 3.5 (lambda/sub max/ = 600 nm, epsilon 1.621 x 10/sup 4/ l mol/sup -1/ cm/sup -1/). Interference caused by a number of ions was masked by the addition of cyanide ions.

Integrating fMRI with psychophysiological measurements in the study of decision-making

OpenAIRE

Wong, Savio W.H.; Xue, Gui; Bechara, Antoine

2011-01-01

Neuroimaging techniques have recently been used to examine the neural mechanism of decision-making. Nevertheless, most of the neuroimaging studies overlook the importance of emotion and autonomic response in modulating the process of decision-making. In this paper, we discussed how to integrating fMRI with psychophysiological measurements in studying decision-making. We suggested that psychophysiological data would complement with fMRI findings in providing a more comprehensive understanding ...

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.

A simple and selective spectrophotometric flow injection determination of trace amounts of ruthenium by catalytic oxidation of safranin-O

Energy Technology Data Exchange (ETDEWEB)

Rezaei, Behzad [Department of Chemistry, Isfahan University of Technology, Isfahan 84156-84111 (Iran, Islamic Republic of)], E-mail: rezaei@cc.iut.ac.ir; Keyvanfard, Mohsen [Faculty of Science, Majlesi Campus, Islamic Azad University, Isfahan (Iran, Islamic Republic of)

2008-03-01

In this work, a simple, selective and rapid flow injection method has been developed for determination of ruthenium. The method is based on its catalytic effect on the oxidation of safranin-O by metaperiodate. The reaction was monitored spectrophotometrically by measuring safranin-O absorbance at {lambda}{sub max} = 521. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine ruthenium in the ranges of 0.4-20.0 ng/mL ({delta}A = 0.2819C{sub Ru} + 1.1840) and 20.0-100.0 ng/mL ({delta}A = 0.0984C{sub Ru} + 7.9391) with a detection limit of 0.095 ng/mL and a sample rate of 30 {+-} 5 samples/h. Relative standard deviation for the five replicate measurements was less than 1.84%. The proposed method has been successfully applied for analysis of ultra trace amounts of ruthenium in real samples.

A simple and selective spectrophotometric flow injection determination of trace amounts of ruthenium by catalytic oxidation of safranin-O

International Nuclear Information System (INIS)

Rezaei, Behzad; Keyvanfard, Mohsen

2008-01-01

In this work, a simple, selective and rapid flow injection method has been developed for determination of ruthenium. The method is based on its catalytic effect on the oxidation of safranin-O by metaperiodate. The reaction was monitored spectrophotometrically by measuring safranin-O absorbance at λ max = 521. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine ruthenium in the ranges of 0.4-20.0 ng/mL (ΔA = 0.2819C Ru + 1.1840) and 20.0-100.0 ng/mL (ΔA = 0.0984C Ru + 7.9391) with a detection limit of 0.095 ng/mL and a sample rate of 30 ± 5 samples/h. Relative standard deviation for the five replicate measurements was less than 1.84%. The proposed method has been successfully applied for analysis of ultra trace amounts of ruthenium in real samples

Spectrophotometric study of bio-sorption of uranium on glass grade spodumene shell powder

International Nuclear Information System (INIS)

Parakudyil, A.S.; Pillai, A.K.; Reddy, A.V.R.; Singal, R.K.; Sharma, P.K.; Michael, K.M.

2012-01-01

Separation of uranium found in iron ore leachates was done by extraction chromatography using glass grade spodumene shellpowder (GSS) in nitric acid medium and analyzed spectrophotometrically. The influences of metal ion concentration, pH and adsorption capacity of biomass were investigated. Biosorption is a potential method of separation of heavy and trace metals from waste water and effluents from various sources. The adsorption capacities of biomass were investigated by batch experiments and column experiments. In the present study, glass grade spodumene shell powder (GSS) in acidic medium is being used as a biosorbent

Potentiometric and spectrophotometric titration study of interaction of tungstovanadophosphoric heteropolyacids with sodium hydroxide

International Nuclear Information System (INIS)

Borkoyakov, S.A.; Fisun, L.A.

1988-01-01

The methods of potentiometric and spectrophotometric titration are used to study H s+n PW 12-n V n O 40 (n=1,2) (P-W-V HPA) decomposition by sodium hydroxide. It is shown that at the first stage of heteropolyanion interaction with alkali (pH) > 4 P-W-V HPA structural reconstruction takes place. It is accompanied by the formation of complexes with a higher content of vanadium atoms stable at pH 4-7/ P-W-V HPA decomposition to initial salts occurs at pH > 8

Influence of all-ceramic and porcelain-fused-to-metal restorations on peri-implant gingival discoloration:a spectrophotometric comparison

DEFF Research Database (Denmark)

Peng, Min; Fei, Wei; Hosseini, Mandana

2013-01-01

discoloration scores were evaluated by clinician. SPSS17.0 was used to analyze the data. RESULTS: There was no significant difference between the all-ceramic group (3.4+1.8) and PFM group (4.9+3.4) spectrophotometrically. No significant difference was found between the all-ceramic restorations and PFM...

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...

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

Science.gov (United States)

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.

From thermometric to spectrophotometric kinetic-catalytic methods of analysis. A review.

Science.gov (United States)

Cerdà, Víctor; González, Alba; Danchana, Kaewta

2017-05-15

Kinetic-catalytic analytical methods have proved to be very easy and highly sensitive strategies for chemical analysis, that rely on simple instrumentation [1,2]. Molecular absorption spectrophotometry is commonly used as the detection technique. However, other detection systems, like electrochemical or thermometric ones, offer some interesting possibilities since they are not affected by the color or turbidity of the samples. In this review some initial experience with thermometric kinetic-catalytic methods is described, up to our current experience exploiting spectrophotometric flow techniques to automate this kind of reactions, including the use of integrated chips. Procedures for determination of inorganic and organic species in organic and inorganic matrices are presented. Copyright © 2017 Elsevier B.V. All rights reserved.

Development of a Draft Core Set of Domains for Measuring Shared Decision Making in Osteoarthritis: An OMERACT Working Group on Shared Decision Making.

Science.gov (United States)

Toupin-April, Karine; Barton, Jennifer; Fraenkel, Liana; Li, Linda; Grandpierre, Viviane; Guillemin, Francis; Rader, Tamara; Stacey, Dawn; Légaré, France; Jull, Janet; Petkovic, Jennifer; Scholte-Voshaar, Marieke; Welch, Vivian; Lyddiatt, Anne; Hofstetter, Cathie; De Wit, Maarten; March, Lyn; Meade, Tanya; Christensen, Robin; Gaujoux-Viala, Cécile; Suarez-Almazor, Maria E; Boonen, Annelies; Pohl, Christoph; Martin, Richard; Tugwell, Peter S

2015-12-01

Despite the importance of shared decision making for delivering patient-centered care in rheumatology, there is no consensus on how to measure its process and outcomes. The aim of this Outcome Measures in Rheumatology (OMERACT) working group is to determine the core set of domains for measuring shared decision making in intervention studies in adults with osteoarthritis (OA), from the perspectives of patients, health professionals, and researchers. We followed the OMERACT Filter 2.0 method to develop a draft core domain set by (1) forming an OMERACT working group; (2) conducting a review of domains of shared decision making; and (3) obtaining opinions of all those involved using a modified nominal group process held at a session activity at the OMERACT 12 meeting. In all, 26 people from Europe, North America, and Australia, including 5 patient research partners, participated in the session activity. Participants identified the following domains for measuring shared decision making to be included as part of the draft core set: (1) identifying the decision, (2) exchanging information, (3) clarifying views, (4) deliberating, (5) making the decision, (6) putting the decision into practice, and (7) assessing the effect of the decision. Contextual factors were also suggested. We proposed a draft core set of shared decision-making domains for OA intervention research studies. Next steps include a workshop at OMERACT 13 to reach consensus on these proposed domains in the wider OMERACT group, as well as to detail subdomains and assess instruments to develop a core outcome measurement set.

Spectrophotometric investigation of vanadium(4) complexing with monoamine complexones

International Nuclear Information System (INIS)

Merkulov, D.A.; Kornev, V.I.

1998-01-01

Interaction of vanadium(4) with iminodiacetic (H 2 Ida) and methyliminodiacetic (H 2 Mida) acids by μ = 0.1 (NaClO 4 ) and t = 20±2 deg C is studied through the spectrophotometric method. It is established that the process of complex formation in quasi-binary systems due to competitive effect of hydroxide ions depends to a large degree on the ligands concentration and properties. The VOIda, VO(OH)Ida - , VOMida, VO(OH)Mida - complexes are identified. The stability constants logarithms of these complexes are equal correspondingly to 9.81±0.02, 18.19±0.03, 10.15±0.03, 18.34±0.02. The results of the study on the VO 2+ -HIda and VO 2+ -H 2 Mida systems agree well with the regularities, identified by the study on the vanadium(4) complex formation with other complexones of the iminodiacetate series

Development of spectrophotometric determination of beryllium in beryl minerals using chrome Azurol S

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Hisham K. Fouad

2016-09-01

Full Text Available A developed, direct, rapid, and sensitive spectrophotometric determination of beryllium in beryl minerals with Chrome Azurol S (CAS as a chromogenic reagent was developed in the present article. The determination was performed without either solvent extraction or ion exchange separation of beryllium from its matrix. The stable 1:1 Be-CAS complex was formed instantly with duration time of at least 24 h with constant absorbance. Different parameters such as wavelengths, pH, EDTA concentration and dye concentration were studied for the optimum determination of beryllium. Interference due to presence of high aluminum concentrations was overcome by adding 5% EDTA disodium salt solution. Maximum absorbance for Be-CAS complex was performed at λmax 568 NM using acetate buffer at pH 4.6. Beer’s law was obeyed in the range from 0.02 to 9 ppm with molar absorptivity ε = 0.22 × 104 mol−1 cm−1 and an average standard deviation of 0.7. The R.S.D for 10 replicate measurements of 1 ppm Be was 1.2%.

An efficient absorbing system for spectrophotometric determination of nitrogen dioxide

Science.gov (United States)

Kaveeshwar, Rachana; Amlathe, Sulbha; Gupta, V. K.

A simple and sensitive spectrophotometric method for determination of atmospheric nitrogen dioxide using o-nitroaniline as an efficient absorbing, as well as diazotizing, reagent is described. o-Nitroaniline present in the absorbing medium is diazotized by the absorbed nitrite ion to form diazonium compound. This is later coupled with 1-amino-2-naphthalene sulphonic acid (ANSA) in acidic medium to give red-violet-coloured dye,having λmax = 545 nm. The isoamyl extract of the red azo dye has λmax = 530 nm. The proposed reagents has ≈ 100% collection efficiency and the stoichiometric ratio of NO 2:NO 2- is 0.74. The other important analytical parameters have been investigated. By employing solvent extraction the sensitivity of the reaction was increased and up to 0.03 mg m -3 nitrogen dioxide could be estimated.

Determination of lisinopril in pharmaceuticals by a kinetic spectrophotometric method

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Čakar Mira

2012-01-01

Full Text Available A kinetic spectrophotometric method for determination of lisinopril in pharmaceuticals has been developed. The method is based on activator action of lisinopril on Cu(II ions catalysing the oxidation of nile blue A with hydrogen peroxide in borate buffer (pH 9.3. A decrease of the absorbance was recorded at 635 nm for 5 min at 25°C. The linearity was established applying the tangent method within the concentration range of lisinopril from 0.8-6.4 μg mL-1, the detection and quantification limits being 0.158 μg mL-1 and 0.480 μg mL-1, respectively. The method has been successfully applied in three brands of tablets containing lisinopril alone or in combination with hydrochlorothiazide.

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.

Spectrophotometric study of lanthanoid complexes with antipyrine and salicylic acid

Energy Technology Data Exchange (ETDEWEB)

Tishchenko, M A; Gerasimenko, G I; Poluehktov, N S [AN Ukrainskoj SSR, Odessa. Fiziko-Khimicheskij Inst.

1981-01-01

The extraction-spectrophotometric method has been used to study lanthanoid ion complexing (Pr, Nd, Ho and Er) with antipyrine (Ant) and salicylic acid (Sal). The component relationship in different-ligand compounds Ln:Ant:Sal=2:3:6 and solvate number equal to 5 are determined; molar extinction coefficients of binary and different-ligand compounds are calculated. Oscillator strengths of absorption bands corresponding to supersensitive transitions of neodymium, holmium, erbium and some most intensive praseodymium bands are calculated. The study of IR spectra of investigated compounds allows to conclude on formation of coordination bonds of the central atom with the antipyrine molecule through the oxygen of the carbonyl group as well as on carboxyl group hydrogen substitution for metal and formation of coordination bond with OH group in salicylic acid molecules.

Spectrophotometric study of lanthanoid complexes with antipyrine and salicylic acid

International Nuclear Information System (INIS)

Tishchenko, M.A.; Gerasimenko, G.I.; Poluehktov, N.S.

1981-01-01

The extraction-spectrophotometric method has been used to study lanthanoid ion complexing (Pr, Nd, Ho and Er) with antipyrine (Ant) and salicylic acid (Sal). The component relationship in different-ligand compounds Ln:Aut:Sal=2:3:6 and solvate number equal to 5 are determined; molar extinction coefficients of binary and different-ligand compounds are calculated. Oscillator strengths of absorption bands corresponding to supersensitive transitions of neodymium, holmium, erbium and some most intensive praseodymium bands are calculated. The study of IR spectra of investigated compounds allows to conclude on formation of coordination bonds of the central atom with the antipyrine molecule through the oxygen of the carbonyl group as well as on carboxyl group hydrogen substitution for metal and formation of coordination bond with OH group in salicylic acid molecules [ru

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.

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

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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 cerium with methylthymol blue in the presence of oxalate and cyanide as masking agents

Energy Technology Data Exchange (ETDEWEB)

Cabrera-Martin, A; Izquierdo-Hornillos, R; Quejido-Cabezas, A J; Peral-Fernandez, J L [Universidad Complutense de Madrid (Spain). Facultad de Ciencias Quimicas

1983-04-01

The spectrophotometric determination of cerium can be carried out by several methods, which involve either the formation of complexes of cerium(III) and cerium(IV) or the oxidation of suitable reagents by cerium(IV) and further measuring the intensity of the colour of the oxidised matter. The latter methods show a lack of selectivity and low sensitivity owing to the nature of the redox reaction. The methods that involve the formation of complexes have also been shown to have low selectivity and sensitivity. However, the most useful methods are those based on the complexes of cerium(III) with Xylenol Orange and Methylthymol Blue (MTB), but they are affected by many interferences. In this work the reaction of cerium(III) with MTB in the presence of oxalate and cyanide ions was studied at pH 10.2, which improves the sensitivity and the selectivity of the determination of cerium.

Sensitive and selective spectrophotometric determination of pantoprazole sodium in pharmaceuticals using permanganate

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K. B. VINAY

2010-03-01

Full Text Available A simple visible spectrophotometric method is described for the determination of pantoprazole sodium sesquihydrate (PSS. The method is based on the formation of a brown colored product on treating PSS with permanganate in neutral medium, the absorbance being measured at 350 nm. The experimental conditions for the assay were optimized. The absorbance is found to increase linearly with the concentration of PSS and the calibration graph is linear in the range of 2.5-40.0 μg ml-1 with a linear regression coefficient of 0.998. The calculated molar absorptivity value is 1.27x104 l mol-1 cm-1 and the corresponding Sandel sensitivity is 0.0341 µg cm-2. The limits of detection (LOD and quantification (LOQ are calculated to be 0.49 and 1.47 µg ml-1, respectively. Intra-day and inter-day accuracy expressed as relative error were better than 2.0% and the corresponding precision (RSD was less than 2.5 %. The developed and validated method was applied to the determination of the active ingredient in a tablet dosage form and the results obtained agreed well with those of the reference method. The accuracy and reliability of the method were ascertained by performing recovery experiments via standard-addition procedure.

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.

Simultaneous in-line concentration for spectrophotometric determination of cations and anions

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Rocha Fábio R. P

2004-01-01

Full Text Available A flow system is proposed for simultaneous in-line concentration of cations and anions. A sliding-bar commutator was employed to insert an anion and a cation exchange column into a flowing sample stream for serial retention of the analytes. In the injector alternative position, different solutions flowed through the columns for parallel elution of the species in different analytical paths. Three-way solenoid valves allowed the intermittent reagent introduction in the sample zones. Signals were measured by employing two flow-through LED-based detectors. The simultaneous retention of the sample zones in coiled reactors can be also performed to increase the residence time and the analyte conversion rate. The analytical potentiality was demonstrated by the in-line concentration of ammonium and phosphate followed by spectrophotometric detection. For a 90 s loading time, the sampling rate was estimated as 40 determinations per hour, which is three-fold higher than the obtained without performing the tasks simultaneously. Enrichment factors of 8.0 and 18 were estimated for phosphate and ammonium, respectively, yielding detection limits of 1 mg L-1 PO4(3- and 1 mg L-1 NH4+ (99.7% confidence level. The reagent consumption was lower than 2 mg per determination. Results for freshwater samples agreed with the obtained by reference APHA procedures at the 95% confidence level.

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.

Spectrophotometric Determination of Doxycycline Hyclate in Pure and Capsule using Diazotization Reaction

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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.

Indirect spectrophotometric determination of BIDA, DISIDA, DTPA and MDP in labelled compounds

International Nuclear Information System (INIS)

Van der Walt, T.N.; Coetzee, P.P.

1989-01-01

N-(4-(n-butyl)acetanilide)iminodiacetic acid (BIDA), N-(2,6-diisopropylacetanilide)iminodiacetic acid (DISDA), diethylenetriaminepentaacetic acid (DTPA) and methylene diphosphonic acid (MDP) are used in labelling kits. The contents of BIDA, DISIDA or MDP of the 99m Tc-labelled compounds can be determined (indirectly) spectrophotometrically with copper, eriochrome cyanine R (ECC) and dodecyl-ethyldimethylammonium bromide (DEDA) in a sodium barbital buffered system at pH 8.5. The calibration curves obey Beer's Law from 0 to 40 μg/25 mL for BIDA and DISIDA, 0 to 60 μg/25 mL for DTPA and 0 to 100 μg/10 mL for MDP. (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.

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

Ion exchange separation of lead from strontium in certified reference samples and spectrophotometric determination of lead as extractable ion-pair of eosin2- and the lead-cryptand (2.2.2)2+ complex

International Nuclear Information System (INIS)

Al-Merey, R.; Al-Shayah, O.

2004-01-01

A two-step procedure including anion exchange separation of lead from strontium in geological reference samples and a spectrophotometric determination of the separated lead as lead-cryptate (2.2.2) complex is presented. The exchangeable anion Cl - of the ion exchange resin (Dowex 1x4) is changed to Br - in 6M HBr solution. Lead is quantitatively retained in the column from 0.5M HBr medium, while Sr 2+ , Ba 2+ , Ca 2+ , Mg 2+ , Na + , K + , Fe 3+ , Cr 3+ , and Al 3+ are passed through. Subsequently the retained Ph is eluted from the column with 6M HBr. The separation efficiency of the resin is controlled using mixed standard solution of (Pb, Sr, Ca, Mg, Ba, Na, K, Fe, Cr and Al), and radioactive tracer of 85 Sr and 131 Ba. The resin selectivity coefficient (K) of separating Pb from Sr is found to be K S r P b∼10 9 . The Spectrophotometric method of lead determination is based on the formation of lead-crytate (2.2.2) complex at pH 8.3 using borate/HCl as a buffer solution. Then the ion-pair of eosin 2+ and lead-cryptand (2.2.2) complex is extracted with chloroform, finally the absorbance of the extractable legend is measured at 550 nm. The extraction recovery, accuracy, precision, linearity and detection limit of the spectrophotometric method are 99.58%, 1.7%, 0.080μg mL -1 , o-9μg mL -1 , and 0.060μg mL -1 , respectively. (author)

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

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

Building up a database of spectro-photometric standard stars from the UV to the near-IR: A status report

NARCIS (Netherlands)

Vernet, J.; Kerber, F.; Saitta, F.; Mainieri, V.; D'Odorico, S.; Lidman, C.; Mason, E.; Bohlin, R.C.; Rauch, T.; Ivanov, V.D.; Smette, A.; Walsh, J.R.; Fosbury, R.A.E.; Goldoni, P.; Groot, P.; Hammer, F.; Horrobin, M.; Kaper, L.; Kjaergaard-Rasmussen, P.; Pallavicini, R.; Royer, F.

2008-01-01

We present a project aimed at establishing a set of 12 spectro-photometric standards over a wide wavelength range from 320 to 2500 nm. Currently no such set of standard stars covering the near-IR is available. Our strategy is to extend the useful range of existing well-established optical flux

Development of a Draft Core Set of Domains for Measuring Shared Decision Making in Osteoarthritis: An OMERACT Working Group on Shared Decision Making

Science.gov (United States)

Toupin April, Karine; Barton, Jennifer; Fraenkel, Liana; Li, Linda; Grandpierre, Viviane; Guillemin, Francis; Rader, Tamara; Stacey, Dawn; Légaré, France; Jull, Janet; Petkovic, Jennifer; Scholte Voshaar, Marieke; Welch, Vivian; Lyddiatt, Anne; Hofstetter, Cathie; De Wit, Maarten; March, Lyn; Meade, Tanya; Christensen, Robin; Gaujoux-Viala, Cécile; Suarez-Almazor, Maria E.; Boonen, Annelies; Pohl, Christoph; Martin, Richard; Tugwell, Peter

2015-01-01

Objective Despite the importance of shared decision making for delivering patient-centred care in rheumatology, there is no consensus on how to measure its process and outcomes. The aim of this OMERACT working group is to determine the core set of domains for measuring shared decision making in intervention studies in adults with osteoarthritis (OA), from the perspective of patients, health professionals and researchers. Methods We followed the OMERACT Filter 2.0 to develop a draft core domain set, which consisted of: (i) forming an OMERACT working group; (ii) conducting a review of domains of shared decision making; and (iii) obtaining the opinions of stakeholders using a modified nominal group process held at a session activity at the OMERACT 2014 meeting. Results 26 stakeholders from Europe, North America and Australia, including 5 patient research partners, participated in the session activity. Participants identified the following domains for measuring shared decision making to be included as part of the Draft Core Set: 1) Identifying the decision; 2) Exchanging Information; 3) Clarifying views; 4) Deliberating; 5) Making the decision; 6) Putting the decision into practice; and 7) Assessing the impact of the decision. Contextual factors were also suggested. Conclusion We propose a Draft Core Set of shared decision making domains for OA intervention research studies. Next steps include a workshop at OMERACT 2016 to reach consensus on these proposed domains in the wider OMERACT group, as well as detail sub-domains and assess instruments to develop a Core Outcome Measurement Set. PMID:25877502

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%.

Attempts to develop a new nuclear measurement technique of β-glucuronidase levels in biological samples

International Nuclear Information System (INIS)

Unak, T.; Avcibasi, U.; Yildirim, Y.; Cetinkaya, B.

2003-01-01

β-Glucuronidase is one of the most important hydrolytic enzymes in living systems and plays an essential role in the detoxification pathway of toxic materials incorporated into the metabolism. Some organs, especially liver and some tumour tissues, have high level of β-glucuronidase activity. As a result the enzymatic activity of some kind of tumour cells, the radiolabelled glucuronide conjugates of cytotoxic, as well as radiotoxic compounds have potentially very valuable diagnostic and therapeutic applications in cancer research. For this reason, a sensitive measurement of β-glucuronidase levels in normal and tumour tissues is a very important step for these kinds of applications. According to the classical measurement method of β-glucuronidase activity, in general, the quantity of phenolphthalein liberated from its glucuronide conjugate, i.e. phenolphthalein-glucuronide, by β-glucuronidase has been measured by use of the spectrophotometric technique. The lower detection limit of phenolphthalein by the spectrophotometric technique is about 1-3 mg. This means that the β-glucuronidase levels could not be detected in biological samples having lower levels of β-glucuronidase activity and therefore the applications of the spectrophotometric technique in cancer research are very seriously limited. Starting from this consideration, we recently attempted to develop a new nuclear technique to measure much lower concentrations of β-glucuronidase in biological samples. To improve the detection limit, phenolphthalein-glucuronide and also phenyl-N-glucuronide were radioiodinated with 131 I and their radioactivity was measured by use of the counting technique. Therefore, the quantity of phenolphthalein or aniline radioiodinated with 131 I and liberated by the deglucuronidation reactivity of β-glucuronidase was used in an attempt to measure levels lower than the spectrophotometric measurement technique. The results obtained clearly verified that 0.01 pg level of

Process monitored spectrophotometric titration coupled with chemometrics for simultaneous determination of mixtures of weak acids.

Science.gov (United States)

Liao, Lifu; Yang, Jing; Yuan, Jintao

2007-05-15

A new spectrophotometric titration method coupled with chemometrics for the simultaneous determination of mixtures of weak acids has been developed. In this method, the titrant is a mixture of sodium hydroxide and an acid-base indicator, and the indicator is used to monitor the titration process. In a process of titration, both the added volume of titrant and the solution acidity at each titration point can be obtained simultaneously from an absorption spectrum by least square algorithm, and then the concentration of each component in the mixture can be obtained from the titration curves by principal component regression. The method only needs the information of absorbance spectra to obtain the analytical results, and is free of volumetric measurements. The analyses are independent of titration end point and do not need the accurate values of dissociation constants of the indicator and the acids. The method has been applied to the simultaneous determination of the mixtures of benzoic acid and salicylic acid, and the mixtures of phenol, o-chlorophenol and p-chlorophenol with satisfactory results.

Spectrophotometric intracutaneous analysis for differential diagnosis of pigmented skin lesions

Directory of Open Access Journals (Sweden)

Е. V. Filonenko

2013-01-01

Full Text Available The non-invasive diagnosis of pigmented skin lesions by spectrophotometric intracutaneous analysis (SIA-scopy using device for dermatoscopy (SIAscope V by Astron Clinica, Ltd was approved in P.A.Herzen Moscow Cancer Research Institute. The method is based on analysis of light interaction with wavelength of 440–960 nm anf human skin, which is recorded by change of image on scan. The comparative analysis of SIA-scopy and histological data in 327 pigmented skin lesions in 147 patients showed, that SIA had high diagnostic efficiency for cutaneous melanoma: the sensitivity was 96%, specifity – 94%, diagnostic accuracy – 94%. For study of malignant potential of pigmented lesions by SIA-scopy the most informative capacity was obtained for assessment of melanin in papillary dermis, status of blood vessels and collagen fibres (SIA-scans 3, 4, 5.

Spectrophotometric, potentiometric, and gravimetric determination of lanthanides with peri-dihydroxynaphthindenone

International Nuclear Information System (INIS)

Hassan, S.S.M.; Mahmoud, W.H.

1982-01-01

Sensitive and reasonably selective methods are described for the spectrophotometric, potentiometric, and gravimetric determination of lanthanides using peri-dihydroxynaphthindenone as a novel chromogenic and precipitating reagent. The reagent forms a stable 1:2 (metal:reagent) type of complex with light lanthanides at pH 2-7 in 1:1 ethanol-water mixture. Low metal concentrations ( 4 L mol -1 cm -1 ) which obey Beer's law. Quantitative precipitation of the complexes from metal solutions of concentrations > 100 μg/mL permits both gravimetric quantitation by igniting the precipitates to the metal oxides and potentiometric titration of the excess reagent. Results with an average recovery of 98% (standard deviation 0.7%) are obtainable for 0.1 μg to 200 mg of all light lanthanides. Many foreign ions naturally occurring or frequently associated with lanthanides do not interfere or can be tolerated

Ultra-violet Spectrophotometric Determination of Caffeine in Soft and Energy Drinks Available in Yenagoa, Nigeria

OpenAIRE

Amos-Tautua; W. Bamidele Martin; E.R.E. Diepreye

2014-01-01

This study was carried out to determine the pH and levels of caffeine in eight brands of carbonated and energy drinks available in local market in Yenagoa, Nigeria. Quantitative analysis of caffeine was performed by a simple and fast standard UV spectrophotometric method, using carbon tetrachloride as the extracting solvent. Results showed that the pH of the beverages were slightly acidic ranging from 5.92-6.44. The minimum caffeine level was observed in the carbonated soft drink Coca Cola (4...

Spectrophotometrical investigation of the NGC 3359 galaxy

International Nuclear Information System (INIS)

Burenkov, A.N.; Khchikyan, Eh.E.; AN Armyanskoj SSR, Byurakan. Astrofizicheskaya Observatoriya)

1986-01-01

Results of detailed spectrophotometrical investigations of NGC 3353, carried out with 6 m telescope of SAO Academy of Sciences of the USSR are presented (dispersion approximately 65 A/mm). Four separate condensations, the brightest of which is Mark 35, are studied. In the spectrum of Mark 35 the emission lines for Hsub(α) to H 12 , HeI lambda lambda 7065, 6678, 5876, 4922, 4472, 3820 and forbidden lines [01]lambda lambdas 6300/64, [02] lambda 3727, [03] lambda lambda 5007, 4959, 4363, [Ne3] lambda 3869, [N2] lambda lambda 6584/48, [S2] lambda lambda 6717/31, [S3] lambda 6310, [Ar3] lambda 7136 are detected. In the second central condensation, called ''nucleus'', emission lines are weaker and beginning with Hsub(β) the absorption components appear which become stronger in the late members of Balmer lines. The forbidden lines in the nucleus are strong: [Ne3], [O3], [O2], [S2][N2]. The relative intensities and equivalent widths of emission lines as well as the chemical composition of Mark 35 and ''nucleus'' are estimated. Both condensations according to their physical properties look like superassociations. It has been concluded that the source of excitation are young stars. NGC 3353 is probably the net of superassociations

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 %.

Indirect spectrophotometric determination of BIDA, DISIDA, DTPA and MDP in labelled compounds

Energy Technology Data Exchange (ETDEWEB)

Van der Walt, T.N.; Coetzee, P.P. (Rand Afrikaans Univ., Johannesburg (South Africa). Dept. of Chemistry); Fourie, P.J. (Atomic Energy Corp. of South Africa (Pty) Ltd., Pretoria (South Africa))

1989-01-01

N-(4-(n-butyl)acetanilide)iminodiacetic acid (BIDA), N-(2,6-diisopropylacetanilide)iminodiacetic acid (DISDA), diethylenetriaminepentaacetic acid (DTPA) and methylene diphosphonic acid (MDP) are used in labelling kits. The contents of BIDA, DISIDA or MDP of the {sup 99m}Tc-labelled compounds can be determined (indirectly) spectrophotometrically with copper, eriochrome cyanine R (ECC) and dodecyl-ethyldimethylammonium bromide (DEDA) in a sodium barbital buffered system at pH 8.5. The calibration curves obey Beer's Law from 0 to 40 {mu}g/25 mL for BIDA and DISIDA, 0 to 60 {mu}g/25 mL for DTPA and 0 to 100 {mu}g/10 mL for MDP. (author).

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)

Reverse flow injection spectrophotometric determination of thiram and nabam fungicides in natural water samples

International Nuclear Information System (INIS)

Asghar, M.; Yaqoob, M.; Nabi, A.

2014-01-01

A reverse flow injection (rFI) spectrophotometric method is reported for determination of thiram and nabam fungicides in natural water samples. The method is based on the reduction of iron(III) in the presence of thiram/nabam in acidic medium at 60 degree C and formation of iron(II)-ferricyanide complex was measured at 790 nm. The limits of detection (3s blank) were 0.01 and 0.05 micro g mL1 for thiram and nabam respectively with a sample throughput of 60 h1. Calibration graphs were linear over the range of 0.02 - 8.0 micro g mL1 (R2 = 0.9999, n = 8) and 0.1 - 30 micro g mL1 (R2 = 0.9982, n = 10) for thiram and nabam with relative standard deviations (RSDs; n = 3) in the range of 0.8 - 1.6% respectively. Experimental parameters and potential interferences were examined. Thiram and nabam were determined in natural water samples using solid-phase extraction (SPE) procedure and recoveries were in the range of 93+-3 - 105+-2% and 87+-4 - 102+-3% respectively. The results obtained were not significantly different compared with a HPLC method. (author)

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

Directory of Open Access Journals (Sweden)

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.

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

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

Measuring patient participation in surgical treatment decision-making from healthcare professionals' perspective.

Science.gov (United States)

Heggland, Liv-Helen; Mikkelsen, Aslaug; Øgaard, Torvald; Hausken, Kjell

2014-02-01

To develop, empirical test, and validate an instrument measuring patient participation in surgical treatment decision-making from healthcare professionals' perspective. Since the advent of New Public Management in many Western countries, patient participation in healthcare decision-making has been considered to be a best practice. A common notion is that well-educated and well-informed public want to choose their own treatments and providers and want to ask questions about the quality of their health services. Survey. A self-report-measuring instrument was designed and administered to 620 healthcare professionals. Items were developed, validated and tested by 451 nurses and physicians working in six surgical wards in a University Hospital in Norway. A 16-item scale with the following four dimensions was developed: information dissemination, formulation of options, integration of information and control. Factor analysis procedures and reliability testing were performed. A one-way, between-groups analysis of variance was conducted to compare doctors' and nurses' opinions on four dimensions of patient participation in surgical treatment decision-making. This article shows that patient participation in surgical treatment decision-making can be measured by a 16-item scale and four distinct dimensions. The analysis demonstrated a reasonable level of construct validity and reliability. Nurses and physicians have a positive attitude towards patient participation overall, but the two groups differ in the extent to which they accept the idea of patient participation in treatment decision-making. The instrument can be a tool for managers and healthcare professionals in the implementation of patient participation in clinical practice. Data from the instrument can be useful to identify health services being provided and what areas that could strengthen patient participation. © 2013 Blackwell Publishing Ltd.

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.

Distributed Fast Self-Organized Maps for Massive Spectrophotometric Data Analysis †.

Science.gov (United States)

Dafonte, Carlos; Garabato, Daniel; Álvarez, Marco A; Manteiga, Minia

2018-05-03

Analyzing huge amounts of data becomes essential in the era of Big Data, where databases are populated with hundreds of Gigabytes that must be processed to extract knowledge. Hence, classical algorithms must be adapted towards distributed computing methodologies that leverage the underlying computational power of these platforms. Here, a parallel, scalable, and optimized design for self-organized maps (SOM) is proposed in order to analyze massive data gathered by the spectrophotometric sensor of the European Space Agency (ESA) Gaia spacecraft, although it could be extrapolated to other domains. The performance comparison between the sequential implementation and the distributed ones based on Apache Hadoop and Apache Spark is an important part of the work, as well as the detailed analysis of the proposed optimizations. Finally, a domain-specific visualization tool to explore astronomical SOMs is presented.

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

Extractive Spectrophotometric Determination of Nortriptyline Hydrochloride Using Sudan II, IV and Black B.

Science.gov (United States)

Amin, A S; Saleh, H M

2017-08-17

A simple spectrophotometric methods has been developed for the determination of nortriptyline hydrochloride in pure and in pharmaceuticalformulations based on the formation of ion-pair complexes with sudun II (S II ), sudan (IV) (S IV ) and sudan black B (S BB ). The selectivity of the method was improved through extraction with chloroform. The optimum conditions for complete extracted colour development were assessed. The absorbance measurements were made at 534, 596 and 649 nm for S II , S IV and S BB complexes, respectively. The calibration graph was linear in the ranges 0.5- 280. 0.5- 37.5 and 0.5 - 31.0 μg ml -1 of the drug usiny the same reagents, respectively. The precision of the procedure was checked by calculating the relative standard deviation of ten replicate determinations on 15 μg ml -1 of nortriptyline HCI and was found to be 1.7, 1.3 and 1.55% using S II , S IV , and S BB complexes, respectively. The molar absorptivity and Sandell sensitivity for each ion-pair were calculated. The proposed methods were successfully applied to the deterniination of pure nortriptyline HCI and in pharmaceutical formulations, and the results demonstrated that the method is equally accurate, precise and reproducible as the official method.

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...

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)

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.

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)

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)).

Science.gov (United States)

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.

Micellar effect on the sensitivity of spectrophotometric Mo(VI) determination based on the formation of gallic acid complex providing evidence for the polyoxoanion structure of molybdate ions

International Nuclear Information System (INIS)

Tascioglu, Senay; Sendil, Olcay; Beyreli, Sivekar

2007-01-01

In this study effects of anionic (sodium dodecyl sulfate, SDS), cationic (cetyltrimethylammonium bromide, CTAB) and nonionic (Triton X-100, TX100) micelles on the sensitivity of spectrophotometric molybdenum(VI) (Mo) determination based on the formation of a binary complex with gallic acid (GA) were investigated. Micellar CTAB was found to enhance the formation of Mo-GA complex. SDS micelles exerted an inhibitory effect while TX100 micelles had no effect on the complex formation. By the optimization of experimental conditions, the determination limit of the method suggested in the literature was lowered from 5.2 x 10 -5 to 4.6 x 10 -6 and to 5.7 x 10 -7 M, in the absence and presence of CTAB, respectively. The mechanism of the effect of CTAB was investigated by spectrophotometric titrations and it was concluded that CTAB did not form a ternary complex with Mo and GA. The stoichiometry of the complex, deduced from the results of spectrophotometric titrations, provided evidence for the formation of para-Mo 7 O 4 6- polyanions at pH 4.5, indicating to the formation of a charge transfer complex between these ions and GA in micellar medium

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.

Derivatization of labetalol hydrochloride for its spectrofluorimetric and spectrophotometric determination inhuman plasma: Application to stability study

Science.gov (United States)

Omar, Mahmoud A.; Derayea, Sayed M.; Abdel-Lateef, Mohamed A.; El Hamd, Mohamed A.

2018-02-01

Two simple, selective and accurate methods were developed for the determination of Labetalol hydrochloride in pure form and pharmaceutical tablets. Both methods are based on derivatization of the studied drug with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazole (NBDsbnd Cl) in alkaline medium (pH 7.5).The reaction product was measured spectrofluorimetrically at 540 nm after excitation at 476 nm (method I) or spectrophotometrically at 480 nm (method II). The calibration graphs were rectilinear over the concentration ranges of 0.10-2.0 and 1.0-11.0 μg mL- 1 for methods I and II, respectively. The proposed methods were successfully applied to the analysis of commercial tablets without interference from common excipients. Furthermore, the spectrofluorimetric method was utilized for the in vitro determination of labetalol in spiked human plasma, with a percent mean recovery (n = 3) of 97.80 ± 1.29%. Moreover, the spectrofluorimetric method was extended to examine the stability study of LBT under different stress conditions such as alkaline, acidic, oxidative, photolytic and a thermal degradation.

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...

Monitoring ambient ozone with a passive measurement technique method, field results and strategy

NARCIS (Netherlands)

Scheeren, BA; Adema, EH

1996-01-01

A low-cost, accurate and sensitive passive measurement method for ozone has been developed and tested. The method is based on the reaction of ozone with indigo carmine which results in colourless reaction products which are detected spectrophotometrically after exposure. Coated glass filters are

Neuroeconomic Measures of Social Decision-Making Across the Lifespan

Directory of Open Access Journals (Sweden)

Lusha eZhu

2012-09-01

Full Text Available Social and decision-making deficits are often the first symptoms of a striking number of neurodegenerative disorders associated with aging. These includes not only disorders that directly impact dopamine and basal ganglia, such as Parkinson’s disorder, but also degeneration in which multiple neural pathways are affected over the course of normal aging. The impact of such deficits can be dramatic, as in cases of financial fraud, which disproportionately affect the elderly. Unlike memory and motor impairments, however, which are readily recognized as symptoms of more serious underlying neurological conditions, social and decision-making deficits often do not elicit comparable concern in the elderly. Furthermore, few behavioral measures exist to quantify these deficits, due in part to our limited knowledge of the core cognitive components or their neurobiological substrates. Here we probe age-related differences in decision-making using a game theory paradigm previously shown to dissociate contributions of basal ganglia and prefrontal regions to behavior. Combined with computational modeling, we provide evidence that behavioral deficits in elderly participants is driven primarily by an over-reliance in trial-and-error reinforcement learning that does not take into account the strategic context, which may underlie elderly’s susceptibility to fraud.

Neuroeconomic measures of social decision-making across the lifespan.

Science.gov (United States)

Zhu, Lusha; Walsh, Daniel; Hsu, Ming

2012-01-01

Social and decision-making deficits are often the first symptoms of a striking number of neurodegenerative disorders associated with aging. These includes not only disorders that directly impact dopamine and basal ganglia, such as Parkinson's disorder, but also degeneration in which multiple neural pathways are affected over the course of normal aging. The impact of such deficits can be dramatic, as in cases of financial fraud, which disproportionately affect the elderly. Unlike memory and motor impairments, however, which are readily recognized as symptoms of more serious underlying neurological conditions, social and decision-making deficits often do not elicit comparable concern in the elderly. Furthermore, few behavioral measures exist to quantify these deficits, due in part to our limited knowledge of the core cognitive components or their neurobiological substrates. Here we probe age-related differences in decision-making using a game theory paradigm previously shown to dissociate contributions of basal ganglia and prefrontal regions to behavior. Combined with computational modeling, we provide evidence that age-related changes in elderly participants are driven primarily by an over-reliance in trial-and-error reinforcement learning that does not take into account the strategic context, which may underlie cognitive deficits that contribute to social vulnerability in elderly individuals.

Development of a safety decision-making scenario to measure worker safety in agriculture.

Science.gov (United States)

Mosher, G A; Keren, N; Freeman, S A; Hurburgh, C R

2014-04-01

Human factors play an important role in the management of occupational safety, especially in high-hazard workplaces such as commercial grain-handling facilities. Employee decision-making patterns represent an essential component of the safety system within a work environment. This research describes the process used to create a safety decision-making scenario to measure the process that grain-handling employees used to make choices in a safety-related work task. A sample of 160 employees completed safety decision-making simulations based on a hypothetical but realistic scenario in a grain-handling environment. Their choices and the information they used to make their choices were recorded. Although the employees emphasized safety information in their decision-making process, not all of their choices were safe choices. Factors influencing their choices are discussed, and implications for industry, management, and workers are shared.

Spectrophotometric determination of cyclamate in soft drinks and desserts: complementary collaborative study.

Science.gov (United States)

Sjöberg, A M

1988-01-01

Fifteen official food control laboratories participated in a collaborative study of a spectrophotometric method to determine cyclamate in a soft drink and a dessert at concentrations of 90-311 mg/L and 202-526 mg/kg, respectively, with blind duplicates and a blank. Average recovery from the soft drink was 97.5%, and from the dessert, 98.6%. Reproducibility relative standard deviations were 4.7-6.5% and 6.9-8.5%, respectively. The outlier percentage was 5.5%. This study complements an earlier work by leading Nordic food laboratories and was designed according to the latest recommendations. The results of this study were compared with those of the earlier collaborative study and with general collaborative results obtained by AOAC.

The effect of non-aqueous solvents on spectrophotometric analysis of lead (II)

International Nuclear Information System (INIS)

Ramadan, A.A.; Bahbouh, M.; Kamuah, M.

1992-01-01

The effect of the following non-aqueous solvents: Methanol, Ethanol, Propanol, iso-propanol, dimethylsulfoxide, dimethylformamide and acetonitrile on spectrophotometric analysis of lead (II) was studied. One absorption peak at range 220-340 nm was observed. The values of maximum wave length (λ max ) and maximum molar absorptivity coefficient (ε max ) vary in accordance with the above solvents and the concentration of HC1. the analytical curves, A=f(C Pb 2+ ), for the determination of lead (II) in presence 5 M HC1 (in methanol) and 7 M HC1 (in other solvents) showed linear proportionality over the concentration range 2.5x10 -5 - 2.0x10 -4 M Pb 2+ . (author). 16 Refs., 4 figs., 2 Tabs

A new importance measure for risk-informed decision making

International Nuclear Information System (INIS)

Borgonovo, E.; Apostolakis, G.E.

2000-01-01

Recently, several authors pointed out that the traditional importance measures had limitations. In this study, the problem through an analysis at the parameter level was investigated and a new measure was introduced. The measure was based on small parameter variations and is capable of accounting for the importance of a group of components/parameters. The definition, computational steps, and an application of a new importance measure for risk-informed decision making were presented here. Unlike traditional importance measures, differential importance measure (DIM) deals with changes in the various parameters that determine the unavailability/unreliability of a component, e.g., failure rates, common-cause failure rates, individual human errors. The importance of the component unavailability/unreliability can be calculated from the importance of the parameters. DIM can be calculated for the frequency of initiating events, while risk achievement worth (RAW) is limited to binary events, e.g., component unavailability. The changes in parameters are 'small'. This is more realistic than the drastic assumption in RAW that the component is always down. DIM is additive. This allows the evaluation of the impact of changes, such as the relaxation of quality assurance requirements, which affect groups of parameters, e.g., the failure rates of a group of pumps. (M.N.)

Variation of ratio kinetic profiles as a simple and novel spectrophotometric method for the simultaneous kinetic analysis of binary mixtures

Directory of Open Access Journals (Sweden)

Naseri Abdolhossein

2012-01-01

Full Text Available In this paper, a new and very simple kinetic - spectrophotometric method is developed for the simultaneous determination of binary mixtures without prior separational steps. The method is based on the calculation of the variation of ratio kinetic profiles. The mathematical explanation of the procedure is also illustrated. The proposed method can be used for simultaneous determination of two analytes A and B that react with the same reagent to give the same absorbing species. In order to evaluate the applicability of the method, a model data as well as an experimental data were tested. The results from experimental data relating to the simultaneous spectrophotometric determination of Co (II and V (IV based on their oxidation reactions with Fe (III in the presence 1, 10- Phenanthroline (Phen in micellar media were presented as a real model for resolution of the binary systems. The applicability of the method in tap water and synthesized alloy samples was also assessed by spiking experiments with different amount of Co (II and V (IV.

Distributed Fast Self-Organized Maps for Massive Spectrophotometric Data Analysis †

Directory of Open Access Journals (Sweden)

Carlos Dafonte

2018-05-01

Full Text Available Analyzing huge amounts of data becomes essential in the era of Big Data, where databases are populated with hundreds of Gigabytes that must be processed to extract knowledge. Hence, classical algorithms must be adapted towards distributed computing methodologies that leverage the underlying computational power of these platforms. Here, a parallel, scalable, and optimized design for self-organized maps (SOM is proposed in order to analyze massive data gathered by the spectrophotometric sensor of the European Space Agency (ESA Gaia spacecraft, although it could be extrapolated to other domains. The performance comparison between the sequential implementation and the distributed ones based on Apache Hadoop and Apache Spark is an important part of the work, as well as the detailed analysis of the proposed optimizations. Finally, a domain-specific visualization tool to explore astronomical SOMs is presented.

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.

Development of a microtitre-based spectrophotometric method to monitor Babesia divergens growth in vitro.

Science.gov (United States)

Malandrin, Laurence; Marchand, Anne-Marie; Chauvin, Alain

2004-09-01

Babesia divergens multiplication cycle involves erythrocyte invasion, intracellular division, and erythrocyte lysis with the simultaneous liberation of hemoglobin. We have decided to set up a spectrophotometric protocol based on hemoglobin concentration in the culture supernatants to monitor B. divergens in vitro growth. After the selection of 405 nm as the most appropriate endpoint hemoglobin wavelength in our conditions (hemoglobin concentration in the supernatant), cultures were standardized [1 x 10(9) red blood cell (RBC)/ml, 1-2.5 x 10(5) infected red blood cell (iRBC)/ml] to allow their monitoring over 3 days. The protocol was then compared to the most commonly used growth measurement methods: parasitemia counting and [(3)H]hypoxanthine incorporation. An excellent correlation was demonstrated between A(405) of the culture supernatant and parasitemia of the iRBC, whatever the RBC concentration used in the medium. This correlation was also evidenced between A(405) and [(3)H]hypoxanthine incorporation for [(3)H]hypoxanthine concentrations lower than 4 microCi/ml. Our assays also highlighted the inhibitory effect of [(3)H]hypoxanthine on B. divergens growth even when used at low concentrations (0.8 microCi/ml) and for a short incorporation duration (24 h). This effect was confirmed by both A(405) and parasitemia counting. In conclusion, A(405) measurement of B. divergens culture supernatant represents a simple, rapid, safe, and reliable way to measure the in vitro growth of this parasite. Generation times of three different B. divergens strains were then determined by the protocol described here and varied between 8 h 36 min and 13 h 8 min.

Spectrophotometric determination of yttrium with 2-(2-thiazolylazo)-5-dimethylaminophenol

International Nuclear Information System (INIS)

Tsurumi, Chikao; Furuya, Keiichi.

1975-01-01

Spectrophotometric determination of small amounts of yttrium with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM) in the presence of zephiramine was investigated. The recommended procedures were as follows; 2.0 ml of water, 7.0 ml of TAM-methanolic solution (2x10 -4 mol/l) and 2.0 ml of zephiramine-aqueous solution (1x10 -2 mol/l) were added to a solution containing less than 35 μg of yttrium and its pH was adjusted to 8.0 with 0.1 mol/l ammonium chloride-0.1 mol/l ammonium hydroxide solution. The solution was transferred to a 25 ml volumetric flask and diluted to the mark with water. After 20 minutes, the absorbance at 575 nm against a reagent blank was measured. The color of yttrium-TAM complex is reddish-violet in the presence of zephiramine and is stable for 90 minutes after color development. The yttrium-TAM complex shows an absorption maximum at 575 nm. The absorbance at 575 nm is constant in a pH range from 7.5 to 8.3. The molar extinction coefficient at this wavelength is 7.2x10 4 l.mol -1 .cm -1 . The band obeys Beer's law up to the concentration of 1.4 μg/ml of yttrium. The molar ratio of yttrium to TAM in the complex is 1 : 2. A number of ions interfere with the determination can be masked by the addition of various masking agents and removed in terms of trioctylamine-xylene extraction. Manganese, tantalum, tin(II), citrate and tartrate ions interfere with the determination. (auth.)

Eye tracking measures of uncertainty during perceptual decision making.

Science.gov (United States)

Brunyé, Tad T; Gardony, Aaron L

2017-10-01

Perceptual decision making involves gathering and interpreting sensory information to effectively categorize the world and inform behavior. For instance, a radiologist distinguishing the presence versus absence of a tumor, or a luggage screener categorizing objects as threatening or non-threatening. In many cases, sensory information is not sufficient to reliably disambiguate the nature of a stimulus, and resulting decisions are done under conditions of uncertainty. The present study asked whether several oculomotor metrics might prove sensitive to transient states of uncertainty during perceptual decision making. Participants viewed images with varying visual clarity and were asked to categorize them as faces or houses, and rate the certainty of their decisions, while we used eye tracking to monitor fixations, saccades, blinks, and pupil diameter. Results demonstrated that decision certainty influenced several oculomotor variables, including fixation frequency and duration, the frequency, peak velocity, and amplitude of saccades, and phasic pupil diameter. Whereas most measures tended to change linearly along with decision certainty, pupil diameter revealed more nuanced and dynamic information about the time course of perceptual decision making. Together, results demonstrate robust alterations in eye movement behavior as a function of decision certainty and attention demands, and suggest that monitoring oculomotor variables during applied task performance may prove valuable for identifying and remediating transient states of uncertainty. Published by Elsevier B.V.

Spectrophotometric method for quantitative determination of triclabendazole in bulk and pharmaceutical

Directory of Open Access Journals (Sweden)

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.

Spectrophotometric determination of ruthenium (III) and rhodium (III) with 9,10-phenanthrenequinone monoxime after extraction into molten naphthalene

International Nuclear Information System (INIS)

Wasey, A.; Bansal, R.K.; Puri, B.K.; Satake, Masatada.

1983-01-01

9,10-Phenanthrenequinone monoxime has been used as a reagent for the spectrophotometric determination of ruthenium(III) and rhodium(III) after extraction into molten naphthalene. The extracted mixture of the metal complex and naphthalene was dissolved in chloroform and ruthenium and rhodium were determined spectrophotometrically. Beer's law holds in the concentration range of 0.2-4.1 μg/cm 3 for ruthenium and 0.3-5.3 μg/cm 3 for rhodium in 10 cm 3 of the final solution. The molar absorptivities and Sandell sensitivities are calculated to be 9.70 x 10 3 l mol -1 cm -1 and 0.01 μg/cmsup(2 ) (660 nm) for ruthenium and 1.13 x 10 4 l mol -1 cm -1 and 0.009 μg/cm 2 (410 nm) for rhodium respectively. Aliquots containing 2.0 μg of ruthenium and 4.1 μg of rhodium give mean absorbances of 0.192 and 0.451 with standard deviations of 0.0017 and 0.0039, respectively. Interference of various ions has been studied and the method has been applied to the determination of ruthenium and rhodium in various synthetic mixtures. This procedure is also applied to the simultaneous determination of ruthenium and rhodium present together in a solution. (author)

Comparison of numerical and physico-chemical models for on-line spectrophotometric control of uranium

International Nuclear Information System (INIS)

Corriou, J.P.; Boisde, G.

1986-04-01

In view of on-line spectrophotometric control of fuel reprocessing streams, a physico-chemical model able to predict uranium and nitric acid concentrations in an uranyl nitrate-nitric acid system has been searched. Thus the influences of the following parameters: uranium, nitrate, hydrogen ion concentrations, ionic strength, on the equilibria of complexation of uranium (VI) nitrate have been evaluated. Extinction coefficients for the uranium mononitrate and uranium dinitrate complexes are given between 410 and 440 nm. The apparent equilibrium constants are determined as a function of the ionic strength. The limitations of this predictive model are emphasized and comparisons with numerical models are discussed. (16 refs)

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

Spectrophotometric determination of uranium and plutonium in nitric acid solutions at their co-presence

International Nuclear Information System (INIS)

Levakov, B.I.; Mishenev, V.B.; Nezgovorov, N.Yu.; Ryazanova, G.K.; Timofeev, G.A.

1986-01-01

The method of spectrophotometric determination of uranium (6) and plutonium (4) in nitric acid solutions is described. Uranium is determined by light absorption of the complex with arsenazo 3 in 0.05 mol/l nitric acid at λ=654 nm, plutonium - by light absorption of the complex with xylenol orange in 0.1 mol/l nitric acid at λ=540 nm. To disguise plutonium, tetravalent and certain trivalent elements DTPA is introduced into photometered solution for uranium determination. The relative root-mean square deviation of determination results does not exceed 0.03 in uranium concenration ranges 0.5-5 μg/ml, of plutonium -1-3 μg/ml

Development of a Draft Core Set of Domains for Measuring Shared Decision Making in Osteoarthritis

DEFF Research Database (Denmark)

Toupin-April, Karine; Barton, Jennifer; Fraenkel, Liana

2015-01-01

OBJECTIVE: Despite the importance of shared decision making for delivering patient-centered care in rheumatology, there is no consensus on how to measure its process and outcomes. The aim of this Outcome Measures in Rheumatology (OMERACT) working group is to determine the core set of domains...... for measuring shared decision making in intervention studies in adults with osteoarthritis (OA), from the perspectives of patients, health professionals, and researchers. METHODS: We followed the OMERACT Filter 2.0 method to develop a draft core domain set by (1) forming an OMERACT working group; (2) conducting...... a review of domains of shared decision making; and (3) obtaining opinions of all those involved using a modified nominal group process held at a session activity at the OMERACT 12 meeting. RESULTS: In all, 26 people from Europe, North America, and Australia, including 5 patient research partners...

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

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.

Developing a Tool for Measuring the Decision-Making Competence of Older Adults

Science.gov (United States)

Finucane, Melissa L.; Gullion, Christina M.

2010-01-01

The authors evaluated the reliability and validity of a tool for measuring older adults’ decision-making competence (DMC). Two-hundred-five younger adults (25-45 years), 208 young-older adults (65-74 years), and 198 old-older adults (75-97 years) made judgments and decisions related to health, finance, and nutrition. Reliable indices of comprehension, dimension weighting, and cognitive reflection were developed. Unlike previous research, the authors were able to compare old-older with young-older adults’ performance. As hypothesized, old-older adults performed more poorly than young-older adults; both groups of older adults performed more poorly than younger adults. Hierarchical regression analyses showed that a large amount of variance in decision performance across age groups (including mean trends) could be accounted for by social variables, health measures, basic cognitive skills, attitudinal measures, and numeracy. Structural equation modeling revealed significant pathways from three exogenous latent factors (crystallized intelligence, other cognitive abilities, and age) to the endogenous DMC latent factor. Further research is needed to validate the meaning of performance on these tasks for real-life decision making. PMID:20545413

Harnessing monitoring measurements in urban environments for decision making after nuclear accidents

International Nuclear Information System (INIS)

Kaiser, J.C.; Proehl, G.

2007-01-01

This article gives an overview on the conceptual design of the Inhabited Areas Monitoring Module IA MM which will be introduced into European decision support systems for nuclear emergencies. It will improve the use of monitoring data of radioactive contamination in urban environments for decision making. IAMM converts the dated gamma dose rate (GDR) measurements from geo-referenced locations into maps of surface contamination with an enhanced spatial resolution. Depending on the availability of the monitoring data, IAMM relies on two modes of operation. If there are only a few measurements, these are taken to improve the maps from a deposition model using data assimilation. If the number of measurements is sufficient to apply spatial interpolation IAMM will rely entirely on monitoring data. Suitable geo-referenced data points will be interpreted by IAMM with respect to their detector environment using the concept of location factors. The endpoints of IAMM can be used directly for decision making or dose calculations with either simple dose models or the more refined EuRopean Model for INhabited areas (ERMIN). (orig.)

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.

Utilization of oxidation reactions for the spectrophotometric determination of captopril using brominating agents

Science.gov (United States)

El-Didamony, Akram M.; Erfan, Eman A. H.

2010-03-01

Three simple, accurate and sensitive methods (A-C) for the spectrophotometric assay of captopril (CPL) in bulk drug, in dosage forms and in the presence of its oxidative degradates have been described. The methods are based on the bromination of captopril with a solution of excess brominating mixture in hydrochloric acid medium. After bromination, the excess brominating mixture is followed by the estimation of surplus bromine by three different reaction schemes. In the first method (A), the determination of the residual bromine is based on its ability to bleach the indigo carmine dye and measuring the absorbance at 610 nm. Method B, involves treating the unreacted bromine with a measured excess of iron(II) and the remaining iron(II) is complexed with 1,10-phenanthroline and the increase in absorbance is measured at 510 nm. In method (C), the surplus bromine is treated with excess of iron(II) and the resulting iron(III) is complexed with thiocyanate and the absorbance is measured at 478 nm. In all the methods, the amount of bromine reacted corresponds to the drug content. The different experimental parameters affecting the development and stability of the color are carefully studied and optimized. Beer's law is valid within a concentration range of 0.4-6.0, 0.4-2.8 and 1.2-4.8 μg mL -1 for methods A, B and C, respectively. The calculated apparent molar absorptivity was found to be 5.16 × 10 4, 9.95 × 10 4 and 1.74 × 10 5 L mol -1 cm -1, for methods A, B and C, respectively. Sandell's sensitivity, correlation coefficients, detection and quantification limits are also reported. No interference was observed from common additives found in pharmaceutical preparations. The proposed methods are successfully applied to the determination of CPL in the tablet formulations with mean recoveries of 99.94-100.11% and the results were statistically compared with those of a reference method by applying Student's t- and F-test.

Spectrophotometric determination of boron by solvent extraction with hydrobenzoin and crystal violet

International Nuclear Information System (INIS)

Sato, Shigeya; Uchikawa, Sumio

1982-01-01

A highly sensitive and simple method for the spectrophotometric determination of boron was developed. Boron was found to react with hydrobenzoin in weak alkaline medium to form a complex anion extractable into benzene with crystal violet, and the measurement of the absorbance of crystal violet in the extract at 600 nm enabled the determination of boron indirectly. The recommended procedure is as follows: Take an aliquot of the boron solution (2.0 x 10 - 4 mol l - 1 ) into a 10-ml test tube. Add 1 ml of carbonate buffer solution (pH 9.4) and 0.25 ml of crystal violet solution (1.0 x 10 - 2 mol l - 1 ), and dilute the mixed solution to 4 ml with deionized water. Shake the solution with 4 ml of benzene solution containing hydrobenzoin (2.0 x 10 - 2 mol l - 1 ) for 2 min. Measure the absorbance of the organic phase at 600 nm using a 10-mm glass cell against benzene. The calibration curve obeyed Beer's law on the concentration range from 2.5 x 10 - 6 mol l - 1 to 2.5 x 10 - 5 mol l - 1 of boron, and the apparent molar absorptivity was 3.0 x 10 4 l mol - 1 cm - 1 at 20 0 C. It was found that many kinds of co-existing ions interfered with the determination. However, this method was applicable to the determination of boron in sea water when chloride ion and cations such as Ca(II) and Mg(II) were previously eliminated by treating the sample solution with Ag 2 O and cation exchanger resin. The proposed method is a very simple and rapid one, because this method does not require apparatus other than common laboratories and the evaporation to dryness of sample or removal of the excess of reagent. (author)

A method for the separation of sodium and iron from plutonium and other impurities in concentrated plutonium solution and their subsequent measurement

International Nuclear Information System (INIS)

Mair, M.A.; Brown, M.L.

1988-06-01

Sodium and iron are separated from plutonium and other impurities by solvent extraction. Sodium is determined by flame photometry and iron by spectrophotometric measurement of the orthophenanthroline complex. (author)

Novel kinetic spectrophotometric method for estimation of certain biologically active phenolic sympathomimetic drugs in their bulk powders and different pharmaceutical formulations

Science.gov (United States)

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

2018-03-01

A simple, selective and sensitive kinetic spectrophotometric method was described for estimation of four phenolic sympathomimetic drugs namely; terbutaline sulfate, fenoterol hydrobromide, isoxsuprine hydrochloride and etilefrine hydrochloride. This method is depended on the oxidation of the phenolic drugs with Folin-Ciocalteu reagent in presence of sodium carbonate. The rate of color development at 747-760 nm was measured spectrophotometrically. The experimental parameters controlling the color development were fully studied and optimized. The reaction mechanism for color development was proposed. The calibration graphs for both the initial rate and fixed time methods were constructed, where linear correlations were found in the general concentration ranges of 3.65 × 10- 6-2.19 × 10- 5 mol L- 1 and 2-24.0 μg mL- 1 with correlation coefficients in the following range 0.9992-0.9999, 0.9991-0.9998 respectively. The limits of detection and quantitation for the initial rate and fixed time methods were found to be in general concentration range 0.109-0.273, 0.363-0.910 and 0.210-0.483, 0.700-1.611 μg mL- 1 respectively. The developed method was validated according to ICH and USP 30 -NF 25 guidelines. The suggested method was successfully implemented to the estimation of these drugs in their commercial pharmaceutical formulations and the recovery percentages obtained were ranged from 97.63% ± 1.37 to 100.17% ± 0.95 and 97.29% ± 0.74 to 100.14 ± 0.81 for initial rate and fixed time methods respectively. The data obtained from the analysis of dosage forms were compared with those obtained by reported methods. Statistical analysis of these results indicated no significant variation in the accuracy and precision of both the proposed and reported methods.

The vexing problem of defining the meaning, role and measurement of values in treatment decision-making.

Science.gov (United States)

Charles, Cathy; Gafni, Amiram

2014-03-01

Two international movements, evidence-based medicine (EBM) and shared decision-making (SDM) have grappled for some time with issues related to defining the meaning, role and measurement of values/preferences in their respective models of treatment decision-making. In this article, we identify and describe unresolved problems in the way that each movement addresses these issues. The starting point for this discussion is that at least two essential ingredients are needed for treatment decision-making: research information about treatment options and their potential benefits and risks; and the values/preferences of participants in the decision-making process. Both the EBM and SDM movements have encountered difficulties in defining the meaning, role and measurement of values/preferences in treatment decision-making. In the EBM model of practice, there is no clear and consistent definition of patient values/preferences and no guidance is provided on how to integrate these into an EBM model of practice. Methods advocated to measure patient values are also problematic. Within the SDM movement, patient values/preferences tend to be defined and measured in a restrictive and reductionist way as patient preferences for treatment options or attributes of options, while broader underlying value structures are ignored. In both models of practice, the meaning and expected role of physician values in decision-making are unclear. Values clarification exercises embedded in patient decision aids are suggested by SDM advocates to identify and communicate patient values/preferences for different treatment outcomes. Such exercises have the potential to impose a particular decision-making theory and/or process onto patients, which can change the way they think about and process information, potentially impeding them from making decisions that are consistent with their true values. The tasks of clarifying the meaning, role and measurement of values/preferences in treatment decision-making

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...

Spectrophotometric Determination of Iron(II after Solid Phase Extraction of Its 2,2′ Bipyridine Complex on Silica Gel-Polyethylene Glycol

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Nahid Pourreza

2013-01-01

Full Text Available A new solid phase extraction procedure was developed for preconcentration of iron(II using silica gel-polyethylene glycol (silica-PEG as an adsorbent. The method is based on retention of iron(II as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1 of sulfuric acid-acetone mixture (1:2 and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1 of iron(II. The limit of detection based on 3Sb was 0.57 ng mL−1 and relative standard deviations (R.S.D for ten replicate measurements of 12 and 42 ng mL−1 of iron(II were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II in water, multivitamin tablet, and spinach samples.

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.

Spectrophotometric determination of total lactones in Andrographis paniculata Nees

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Napaporn Jantakun

2005-11-01

Full Text Available A spectrophotometric method for determination of total lactones in Andrographis paniculata was established by using dinitrobenzoic acid and potassium hydroxide solutions as colour forming agents. The absorbance of the solution was determined at 536 nm. The linearity range was 12-72 × 10-6 g.ml-1. The detection limit was 1.2 μg, the quantitation limit was 4.23 μg. The intraday variation had an average of slope 6082.97 g.ml-1, % RSD 0.10; an average intercept 0.2786, %RSD 3.66 (n=3. The interday variation had an average of 6146 g.ml-1 with the %RSD of 6.30 and an average intercept 0.2628, %RSD 4.95 (n=4. The coefficients of determination were 0.998-0.999. The total lactones content, calculated as andrographolide, determined by this method was 8.61±0.52% (n=4 and by the official method, Thai Herbal Pharmacopoeia, was 8.12±0.34% (n=2. The results of the two methods do not differ significantly at P=0.05 (P(|t|>0.903 = 0.53

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)

Rapid visual and spectrophotometric nitrite detection by cyclometalated ruthenium complex.

Science.gov (United States)

Lo, Hoi-Shing; Lo, Ka-Wai; Yeung, Chi-Fung; Wong, Chun-Yuen

2017-10-16

Quantitative determination of nitrite ion (NO 2 - ) is of great importance in environmental and clinical investigations. A rapid visual and spectrophotometric assay for NO 2 - detection was developed based on a newly designed ruthenium complex, [Ru(npy)([9]aneS3)(CO)](ClO 4 ) (denoted as RuNPY; npy = 2-(1-naphthyl)pyridine, [9]aneS3 = 1,4,7-trithiacyclononane). This complex traps NO + produced in acidified NO 2 - solution, and yields observable color change within 1 min at room temperature. The assay features excellent dynamic range (1-840 μmol L -1 ) and high selectivity, and its limit of detection (0.39 μmol L -1 ) is also well below the guideline values for drinking water recommended by WHO and U.S. EPA. Practical use of this assay in tap water and human urine was successfully demonstrated. Overall, the rapidity and selectivity of this assay overcome the problems suffered by the commonly used modified Griess assays for nitrite determination. Copyright © 2017 Elsevier B.V. All rights reserved.

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

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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.

Incipient fault diagnosis of power transformers using optical spectro-photometric technique

Science.gov (United States)

Hussain, K.; Karmakar, Subrata

2015-06-01

Power transformers are the vital equipment in the network of power generation, transmission and distribution. Mineral oil in oil-filled transformers plays very important role as far as electrical insulation for the winding and cooling of the transformer is concerned. As transformers are always under the influence of electrical and thermal stresses, incipient faults like partial discharge, sparking and arcing take place. As a result, mineral oil deteriorates there by premature failure of the transformer occurs causing huge losses in terms of revenue and assets. Therefore, the transformer health condition has to be monitored continuously. The Dissolved Gas Analysis (DGA) is being extensively used for this purpose, but it has some drawbacks like it needs carrier gas, regular instrument calibration, etc. To overcome these drawbacks, Ultraviolet (UV) -Visible and Fourier Transform Infrared (FTIR) Spectro-photometric techniques are used as diagnostic tools for investigating the degraded transformer oil affected by electrical, mechanical and thermal stresses. The technique has several advantages over the conventional DGA technique.

Extractive-spectrophotometric determination of disopyramide and irbesartan in their pharmaceutical formulation

Science.gov (United States)

Abdellatef, Hisham E.

2007-04-01

Picric acid, bromocresol green, bromothymol blue, cobalt thiocyanate and molybdenum(V) thiocyanate have been tested as spectrophotometric reagents for the determination of disopyramide and irbesartan. Reaction conditions have been optimized to obtain coloured comoplexes of higher sensitivity and longer stability. The absorbance of ion-pair complexes formed were found to increases linearity with increases in concentrations of disopyramide and irbesartan which were corroborated by correction coefficient values. The developed methods have been successfully applied for the determination of disopyramide and irbesartan in bulk drugs and pharmaceutical formulations. The common excipients and additives did not interfere in their determination. The results obtained by the proposed methods have been statistically compared by means of student t-test and by the variance ratio F-test. The validity was assessed by applying the standard addition technique. The results were compared statistically with the official or reference methods showing a good agreement with high precision and accuracy.

Spectrophotometric Determination of Gemifloxacin Mesylate, Moxifloxacin Hydrochloride, and Enrofloxacin in Pharmaceutical Formulations Using Acid Dyes

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Ayman A. Gouda

2014-01-01

Full Text Available Simple, rapid, and extractive spectrophotometric methods were developed for the determination of some fluoroquinolones antibiotics: gemifloxacin mesylate (GMF, moxifloxacin hydrochloride (MXF, and enrofloxacin (ENF in pure forms and pharmaceutical formulations. These methods are based on the formation of ion-pair complexes between the basic drugs and acid dyes, namely, bromocresol green (BCG, bromocresol purple (BCP, bromophenol blue (BPB, bromothymol blue (BTB, and methyl orange (MO in acidic buffer solutions. The formed complexes were extracted with chloroform and measured at 420, 408, 416, 415, and 422 nm for BCG, BCP, BPB, BTB, and MO, respectively, for GMF; at 410, 415, 416, and 420 nm for BCP, BTB, BPB, and MO, respectively, for MXF; and at 419 and 414 nm for BCG and BTB, respectively, in case of ENF. The analytical parameters and their effects are investigated. Beer’s law was obeyed in the ranges 1.0–30, 1.0–20, and 2.0–24 μg mL−1 for GMF, MXF, and ENF, respectively. The proposed methods have been applied successfully for the analysis of the studied drugs in pure forms and pharmaceutical formulations. Statistical comparison of the results with the reference methods showed excellent agreement and indicated no significant difference in accuracy and precision.

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.

Spectrophotometric determination and thermodynamic studies of the charge transfer complexation of emedastine difumarate with some π-acceptors

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Abdel-Raeq A. Sawsan

2017-05-01

Full Text Available Spectrophotometric procedures were presented for the determination of antihistaminic drug, emedastine difumarate. The methods are based on the charge transfer complexation reaction of the drug with π-acceptors; 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ, chloranilic acid (CA and 7,7,8,8-tetracyanoquinodimethane (TCNQ. Different charge-transfer complexes and colored radical anions were obtained. The formations of the colored complexes were utilized in the development of simple, rapid and accurate spectrophotometric methods for the analysis of emedastine in drug substance and products. Under the optimum reaction conditions, linear relationships with good correlation coefficients (0.9996–0.9999 were found between the absorbance at the relevant maxima and the concentrations of emedastine in the range of 0.8–200 μg mL−1. The limits of detection ranged from 0.06 to 0.76 μg mL−1. The molar absorptivities and association constants for the colored complexes were evaluated using the Benesi–Hildebrand equation. The free energy change (ΔG° and the enthalpy of formation (ΔH° as well as the entropy (ΔS° were also determined. The methods were successfully applied to analyze the drug formulation with mean recovery percentages ± RSD% of 100.04 ± 0.59–100.22 ± 0.72. The results were compared favorably with the official and reported methods.

Decision Dissonance: Evaluating an Approach to Measuring the Quality of Surgical Decision Making

Science.gov (United States)

Fowler, Floyd J.; Gallagher, Patricia M.; Drake, Keith M.; Sepucha, Karen R.

2013-01-01

Background Good decision making has been increasingly cited as a core component of good medical care, and shared decision making is one means of achieving high decision quality. If it is to be a standard, good measures and protocols are needed for assessing the quality of decisions. Consistency with patient goals and concerns is one defining characteristic of a good decision. A new method for evaluating decision quality for major surgical decisions was examined, and a methodology for collecting the needed data was developed. Methods For a national probability sample of fee-for-service Medicare beneficiaries who had a coronary artery bypass graft (CABG), a lumpectomy or a mastectomy for breast cancer, or surgery for prostate cancer during the last half of 2008, a mail survey of selected patients was carried out about one year after the procedures. Patients’ goals and concerns, knowledge, key aspects of interactions with clinicians, and feelings about the decisions were assessed. A Decision Dissonance Score was created that measured the extent to which patient ratings of goals ran counter to the treatment received. The construct and predictive validity of the Decision Dissonance Score was then assessed. Results When data were averaged across all four procedures, patients with more knowledge and those who reported more involvement reported significantly lower Decision Dissonance Scores. Patients with lower Decision Dissonance Scores also reported more confidence in their decisions and feeling more positively about how the treatment turned out, and they were more likely to say that they would make the same decision again. Conclusions Surveying discharged surgery patients is a feasible way to evaluate decision making, and Decision Dissonance appears to be a promising approach to validly measuring decision quality. PMID:23516764

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 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.

Physics and Analysis at a Hadron Collider - Making Measurements (3/3)

CERN Multimedia

CERN. Geneva

2010-01-01

This is the third lecture of three which together discuss the physics of hadron colliders with an emphasis on experimental techniques used for data analysis. This third lecture discusses techniques important for analyses making a measurement (e.g. determining a cross section or a particle property such as its mass or lifetime) using some CDF top-quark analyses as specific examples. The lectures are aimed at graduate students.

Multi-wavelength spectrophotometric determination of acidity constant of some newly synthesized Schiff bases and their QSPR study

Science.gov (United States)

Hemmateenejad, Bahram; Emami, Leila; Sharghi, Hashem

2010-01-01

The acidity constants of some newly synthesized Schiff base derivatives were determined by hard-model based multivariate data analysis of the spectrophotometric data in the course of pH-metric titration in 50% (v/v) methanol-water binary solvent. The employed data analysis method was also able to extract the pure spectra and pH-dependent concentration profiles of the acid-base species. The molecules that possess different substituents (both electron donating and withdrawing) on the ortho-, meta- and para-positions of one of the phenyl ring showed variable acidity constants ranging from 8.77 to 11.07 whereas the parent molecule had an acidity constant of 10.25. To investigate the quantitative effects of changing of substitution pattern on the acidity constant, a quantitative structure-property relation analysis was conducted using substituent constants and molecular descriptor. Some models with high statistical quality (measured by cross-validation Q2) were obtained. It was found that the acidity constant of the studied molecules in the methanol-water mixed solvent not only is affected by electronic features of the solutes but also by the lipophilic interaction between methanol part of solvent and the deprotonated solutes.

Meta-Cresol Purple Reference Material® (RM) for Seawater pH Measurements

Science.gov (United States)

Easley, R. A.; Waters, J. F.; Place, B. J.; Pratt, K. W.

2016-02-01

The pH of seawater is a fundamental quantity that governs the carbon dioxide - carbonate system in the world's oceans. High quality pH measurements for long-term monitoring, shipboard studies, and shorter-term biological studies (mesocosm and field experiments) can be ensured through a reference material (RM) that is compatible with existing procedures and which is traceable to primary pH measurement metrology. High-precision spectrophotometric measurements of seawater pH using an indicator dye such as meta-cresol purple (mCP) are well established. However, traceability of these measurements to the International System of Units (SI) additionally requires characterizing the spectrophotometric pH response of the dye in multiple artificial seawater buffers that themselves are benchmarked via primary pH (Harned cell) measurements at a range of pH, salinity, and temperature. NIST is currently developing such a mCP pH RM using this approach. This material will also incorporate new procedures developed at NIST for assessing the purity and homogeneity of the mCP reagent itself. The resulting mCP will provide long-term (years) stability and ease of shipment compared to artificial seawater pH buffers. These efforts will provide the oceanographic user community with a NIST issued mCP (RM), characterized as to its molar absorptivity values and acid dissociation constants (pKa), with uncertainties that comply with the Guide to the Expression of Uncertainty in Measurement (GUM).

Emodin (1,3,8-trihydroxy-6-methylanthraquinone): a spectrophotometric reagent for the determination of beryllium(II), magnesium(II) and calcium(II)

International Nuclear Information System (INIS)

Pal, T.; Jana, N.R.

1993-01-01

The individual determination of Be II , Mg II or Ca II by conventional spectrophotometry and simultaneous determination of Mg II and Ca II in mixtures by first-derivative spectrophotometry are possible at trace levels, using emodin (1,3,8-trihydroxy-6-methylanthraquinone) as spectrophotometric reagent. Interference from other metal species, application of these methods to rock samples and statistical analysis of the results are discussed. (author)

2-Hydro-4-n-But oxypropiophenone Oxime as a spectrophotometric reagent for Fe (III)

International Nuclear Information System (INIS)

Purohit, K.; Desai, K.K.

2006-01-01

2-Hydro-4-n-But oxypropiophenone Oxime [Hipbone] has been synthesized and used for the spectrophotometric determination of Fe (III). The reagent gives purple coloured complex with Fe (III) in 50% alcoholic medium in pH range of 2.5-4.5. Beer's law is obeyed up to 23.1 ppm of Fe (III). Molar absorptivity and sandell's sensitivity at 500 nm of complex were found to be 7.062x 10 power2 lit.mol.cm and 0.079 ug of Fe (III)/cm respectively. Composition and stability constant have been determined. The reagent is successfully used for determination of Fe (III) in dolomite and in pharmaceutical sample. It is also used for the indirect determination of fluoride in tap water sample. (author)

Genetic algorithm-based wavelength selection in multicomponent spectrophotometric determination by PLS: Application on sulfamethoxazole and trimethoprim mixture in bovine milk

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Givianrad Hadi Mohammad

2013-01-01

Full Text Available The simultaneous determination of sulfamethoxazole (SMX and trimethoprim (TMP mixtures in bovine milk by spectrophotometric method is a difficult problem in analytical chemistry, due to spectral interferences. By means of multivariate calibration methods, such as partial least square (PLS regression, it is possible to obtain a model adjusted to the concentration values of the mixtures used in the calibration range. Genetic algorithm (GA is a suitable method for selecting wavelengths for PLS calibration of mixtures with almost identical spectra without loss of prediction capacity using the spectrophotometric method. In this study, the calibration model based on absorption spectra in the 200-400 nm range for 25 different mixtures of SMX and TMP Calibration matrices were formed form samples containing 0.25-20 and 0.3-21 μg mL-1 for SMX and TMP, at pH=10, respectively. The root mean squared error of deviation (RMSED for SMX and TMP with PLS and genetic algorithm partial least square (GAPLS were 0.242, 0.066 μgmL-1 and 0.074, 0.027 μg mL-1, respectively. This procedure was allowed the simultaneous determination of SMX and TMP in synthetic and real samples and good reliability of the determination was proved.

Human perception of dental porcelain translucency correlated to spectrophotometric measurements.

Science.gov (United States)

Liu, Min-Chieh; Aquilino, Steven A; Lund, Peter S; Vargas, Marcos A; Diaz-Arnold, Ana M; Gratton, David G; Qian, Fang

2010-04-01

This study evaluated the relationship between instrumental measurements and subjective visual assessment of differences in dental porcelain translucency. Unshaded feldspathic porcelain was used with controlled amounts of tin oxide to create two groups of 12-mm diameter disks with incremental changes in opacity. Contrast ratio (CR = Yb/Yw) was determined with a spectrophotometer, and used as a measure of porcelain translucency (Group A = 0.20 to 0.40; Group B = 0.6-0.8). Within each group, there were 14 specimens with 11 CRs. Three observer groups (first year dental students, residents, faculty with >10 years of shade matching experience) were recruited to assess the translucency between porcelain disks under two lighting conditions (reflected light, transmitted light). Each subject's ability to distinguish between specimens of differing translucency was determined. Descriptive statistics and three-way ANOVA followed by a post-hoc Tukey-Kramer test were used to evaluate the translucency perception threshold (TPT) of subjects (alpha= 0.05). The overall mean TPT (DeltaC) was 0.07, while 50% of the subjects could perceive a 0.06 CR difference between porcelain specimens. Three-way ANOVA revealed a significant difference in translucency perception among the observer groups (p or =10 years) significantly improved the ability to perceive differences in translucency; however, neither the viewing condition nor porcelain opacity affected the perceived translucency threshold.

Separation of zirconium through extraction in hydrochloric medium with tri-n-octilamine and its spectrophotometric determination with chloroanilic acid

International Nuclear Information System (INIS)

Floh, B.; Abrao, A.; Federgruen, L.

1976-01-01

A procedure is outlined for the spectrophotometric determination of zirconium using its complex with chloroanilic acid in HC10 4 2M. Interfering elements like Fe, Zn, U, Cy, Cd, Sb, Co, Pb, Hg, Tl, Pt, Au, Pd, Ga, In, Mo and W are previously extracted with tri-n-octylamine 7,5%-benzene from 4 M HCL. Then, the acid content of the solution is ascertained to 10 M HCL and zirconium is extracted with the amine. Nb is a strong interference, being extracted by the amine as well as zirconium and absorbing at the same region as zirconium chloroanilate. Zirconium is stripped from the organic phase with Na 2 CO 3 . The colour development is done with chloroanilic acid in 2 M HC10 4 and the measurements at 340 nm. The method allows the determination of 5 micrograms of Zr. The work curve covers the 0.2 - 2.0 μg Zr/mL range. The procedure is being applied to the determination of zirconium in several alloys and in samples containing zinc, magnesium, iron, aluminium, uranium and thorium [pt

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.

Spectrophotometric determination of U(vi) in 30% tbp using dibenzoyl methane (DBM) and methanol (abstract)

International Nuclear Information System (INIS)

Islam, N.; Naqvi, A.

2011-01-01

The Spectrophotometric method for the determination of trace amount of Uranium in aqueous and organic samples has been developed. The method is proved very accurate and precise for rapid determination of Uranium with Dibenzoyl Methane (DBM) in Methanol medium instead of Pyridine medium. The maximum absorbance occurs at 410 nm with a molar absorptivity of 4.5 x 104 L.mole/sup -1/.cm/sup -1/.The linear calibration curve through the point of origin was obtained up to 10 mu gm L/sup -1/ of Uranium (VI). The relative standard deviation is +- 2%. In case of aqueous samples extraction procedure is adopted to obtain organic phase while organic samples are treated as such. (author)

Indirect spectrophotometric determination of cyanide by means of the colour reaction of silver with cadion 2B in presence of triton X-100.

Science.gov (United States)

Yu-Rui, Z; Fu-Sheng, W; Fang, Y

1983-10-01

Silver gives a colour reaction with cadion 2B in the presence of the non-ionic surfactant Triton X-100, and the suppression of the colour by competitive complexation of the silver can be used for the spectrophotometric determination of cyanide. Cyanide in waste water can be separated by distillation from other ions that also interfere, and then determined.

Liquid-liquid microextraction in a multicommuted flow system for direct spectrophotometric determination of iodine value in biodiesel.

Science.gov (United States)

Pereira, Andréia C; Rocha, Fábio R P

2014-06-04

A flow-based procedure was developed for the direct spectrophotometric determination of the iodine value (IV) in biodiesel. The procedure was based on the microextraction/reaction of unsaturated compounds with triiodide ions in an aqueous medium by inserting the reagent solution between the aliquots of biodiesel without any pretreatment. The interaction occurred through the biodiesel film formed on the inner walls of the hydrophobic tube used as the reactor and at the aqueous/biodiesel interfaces. The spectrophotometric detection was based on the discoloration of the I3(-) reagent in the aqueous phase by using a glass tube coupled to a fiber-optic spectrophotometer as the detection cell. Reference solutions were prepared by dilution of biodiesel samples with previously determined IV in hexane. The analytical response was linear for IV from 13 to 135 g I2/100 g with a detection limit of 5 g I2/100 g. A coefficient of variation of 1.7% (n=10) and a sampling rate of 108 determinations per hour were achieved by consuming 224 μL of the sample and 200 μg of I2 per determination. The slopes of analytical curves obtained with three different biodiesel samples were in agreement (variations in slopes lower than 3.1%), thus indicating an absence of any matrix effects. Results for biodiesel samples from different sources agreed with the volumetric official procedure at the 95% confidence level. The proposed procedure is therefore a simple, fast, and reliable alternative for estimating the iodine value of biodiesel. Copyright © 2014. Published by Elsevier B.V.

Spectrophotometric Determination of Reboxetine through Condensation and Diazo-Coupling Reactions

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K. Srikanth

2011-01-01

Full Text Available In the present study, two simple, sensitive and reproducible visible spectrophotometric methods were developed for the determination of reboxetine in pure form and in pharmaceutical formulations. The methods involve acid hydrolysis of reboxetine methane sulphonate (Reboxetine as methane sulphonate and the product obtained was used for the estimation. Out of the two methods developed in the laboratory, the first method involves the condensation reaction of hydrolysed reboxetine methane sulphonate with ethyl acetoacetate in sulphuric acid medium and the second method involves the diazocoupling reaction of hydrolysed reboxetine methane sulphonate with diazotized p-sulphanilic acid in alkaline medium. They have absorption maxima at 400 nm and 430 nm respectively and obey Beer’s law in the concentration ranges of 0.5 - 0.3 μgmL-1 and 1.0 - 7.5 μgmL-1 respectively. Results of analysis were validated statistically and by recovery studies. The apparent molar absorptivity values (∈max obtained are 7.549 x 104 L mol-1 cm-11 and 2.656x104 Lmol-1cm-1 respectively. Both these have correlation coefficient value of 0.9999. The proposed methods have good precision and accuracy.

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.

Selective and non-extractive spectrophotometric determination of cefdinir in formulations based on donor-acceptor complex formation

Directory of Open Access Journals (Sweden)

Babita K. Singh

2010-01-01

Full Text Available Cefdinir has broad spectrum of activity and high prescription rates, hence its counterfeiting seems imminent. We have proposed a simple, fast, selective and non-extractive spectrophotometric method for the content assay of cefdinir in formulations. The method is based on complexation of cefdinir and Fe under reducing condition in a buffered medium (pH 11 to form a magenta colored donor-acceptor complex (λ max = 550 nm; apparent molar absorptivity = 3720 L mol-1 cm-1. No other cephalosporins, penicillins and common excipients interfere under the test conditions. The Beer's law is followed in the concentration range 8-160 µg mL-1.

Spectrophotometric and potentiometric studies of oxidation of Mo(III) by Mo(VI) in phosphoric acid medium

Energy Technology Data Exchange (ETDEWEB)

Kumar, A; Verma, G S.P. [Ranchi Coll. (India). Dept. of Chemistry

1975-12-01

Oxidation of Mo(III) (green) by Mo(VI) in an inert atmosphere and in orthophosphoric acid medium at various acid concentrations is reported. Potentiometric and spectrophotometric data suggest that oxidation of Mo(III) proceeds to Mo(V) through a binuclear species Mo(III) Mo(IV) absorbing at 400 nm. The formation of this species is facilitated at high acid concentrations. It is further found that quantitative conversion of Mo(III) into Mo(V) takes place at fairly high acid concentrations. In high phosphoric acid concentrations, solution of Mo(III) has been found to be oxidized to Mo(VI) by air and hence this can be used as a good oxygen absorber.

Measurement and behaviour of technetium in fast reactor fuel reprocessing

International Nuclear Information System (INIS)

Ferguson, C.; Kyffin, T.W.

1986-02-01

A method is described for the spectrophotometric measurement of technetium in plant solutions from the reprocessing of fast reactor fuel. The technetium is selectively extracted using tri-iso-octylamine. After back extraction, thiocyanate is added, in the presence of tetrabutyl-ammonium hydroxide, to form the red hexa-thiocyanato anionic complex in a chloroform medium. The concentration of the technetium is then calculated from the spectrophotometric measurement of this complex. This method was applied to bulk samples, collected during a PFR fuel reprocessing campaign, to identify the main routes followed by technetium through the reprocessing plant. In order to understand the probable behaviour of technetium in the process plant streams, an investigation into the influence of plutonium IV nitrate on the extraction of Tc (VII) into 20%v/v tributyl phosphate/odourless kerosene solution from nitric acid solutions, was initiated. The results of this investigation, along with the known distribution coefficient for the extraction of the uranyl/technetium complex U0 2 (N0 3 )(Tc0 4 ).2TBP and the redox chemistry of technetium, are used to predict the probable behaviour of technetium in the process plant streams. This predicted behaviour is compared with the experimental results and reasonable agreement is obtained between experiment and theory, considering the history of the samples analysed. (author)

Decision-making impairment in obsessive-compulsive disorder as measured by the Iowa Gambling Task

Directory of Open Access Journals (Sweden)

Felipe Filardi da Rocha

2011-08-01

Full Text Available OBJECTIVE: This study aims to evaluate the process of decision-making in patients with obsessive-compulsive disorder (OCD using the Iowa Gambling Task (IGT. In addition, we intend to expand the understanding of clinical and demographic characteristics that influence decision-making. METHOD: Our sample consisted of 214 subjects (107 diagnosed with OCD and 107 healthy controls who were evaluated on their clinical, demographic and neuropsychological features. Moreover, the Iowa Gambling Task (IGT, a task that detects and measures decision-making impairments, was used. RESULTS: We found that OCD patients performed significantly worse on the IGT. Furthermore, features such as symptoms of anxiety did not influence IGT performance. CONCLUSION: Impaired decision-making seems to be a key feature of OCD. Given that OCD is a complex heterogeneous disorder, homogeneous groups are necessary for an accurate characterization of our findings.

A study of the direct spectrophotometric determination of uranium (VI) in trialkylamine extracts with 2-(5-bromo- 2-pyridylazo)-5-diethylaminophenol

International Nuclear Information System (INIS)

Lyle, S.J.; Tamizi, M.

1979-01-01

A straightforward spectrophotometric method is described for the determination of uranium (VI) in trialkylamine sulphate extracts in kerosene diluent; 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (Br-PADAP) is used for colour formation without resort to back extraction into an aqueous phase. The method provides good tolerance to sulphate ion and rapid colour development and appears to be free from interference when applied to extracts from uranium sulphate leach liquors. (Auth.)

Spectrophotometric determination of fluorides in water with Hach equipment; Determinacion espectrofotometrica de fluoruros en aguas con equipo Hach

Energy Technology Data Exchange (ETDEWEB)

Acosta L, E. [ININ, 52045 Ocoyoacac, Estado de Mexico (Mexico)]. e-mail: eal@nuclear.inin.mx

1994-11-15

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)

Spectrophotometric assay of phenylephrine hydrochloride using 4-aminoantipyrine and copper (II)

International Nuclear Information System (INIS)

Theia'a, N.; Sabha, A.

2010-01-01

A new spectrophotometric method is proposed for determination of phenylephrine hydrochloride. The method is based on the coupling of 4-aminoantipyrine (4-AAP) with phenylephrine hydrochloride (PEH) to give a new ligand that reacts with copper (II) in the presence of sodium tetraborate buffer solution of pH 9.00 at 50 deg. C to give an intense red colored chelate having maximum absorption at 480 nm. The optimization of the experimental conditions is described. The method has been used for the determination of 2.0 - 50.0 mu g/ml of PEH. The molar absorptivity is 5.34 X 103 L. mol/sup -1/cm /sup- 1/ and the accuracy of the method is achieved by the value of average recovery (101.28 %) and the precision is supported by relative standard deviation (RSD=1.25 %) values. The results of the method was compared with those of the standard method. The interference of excipients was studied. The mechanism of the chemical reaction has been proposed. The proposed method was successfully applied for the determination of the PEH in pharmaceutical syrup formulations. (author)

A sensitive spectrophotometric determination of nitrogen dioxide in the working atmosphere

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Prachi Parmar

2009-12-01

Full Text Available In the present investigation, a simple and sensitive spectrophotometric method for the determination of nitrogen dioxide in various environmental samples is described. Nitrogen dioxide in air was fixed as nitrite ion in alkaline sodium arsenite absorbing solution. The nitrite formed was diazotized with p−aminoacetophenone in acidic medium which was subsequently coupled with phloroglucinol to give yellow−orange dye in alkaline medium having an absorption maximum at 420 nm. Beer’s law was obeyed in the range of 0.008 − 0.12 μg mL-1 of nitrogen dioxide and has a molar absorptivity of 2.875 x 105 L mol-1 cm-1. Optimum reaction conditions for diazotization, full colour development and the effect of variables like temperature, time and pH have been studied. Detailed studies to check the collection efficiency and NO2:NO2- stoichiometric ratio has been carried out. The reaction has been successfully applied for the detection of nitrogen dioxide in cigarette smoke, scooter exhaust, and workroom air.

Spectrophotometric Assay of Phenylephrine Hydrochloride Using 4-Aminoantipyrine and Copper (II

Directory of Open Access Journals (Sweden)

Theia'a N. Al-Sabha

2010-06-01

Full Text Available A new spectrophotometric method is proposed for determination of phenylephrine hydrochloride. The method is based on the coupling of 4-aminoantipyrine (4-AAP with phenylephrine hydrochloride (PEH to give a new ligand that reacts with copper (II in the presence of sodium tetraborate buffer solution of pH 9.00 at 50 °C to give an intense red colored chelate having maximum absorption at 480 nm. The optimization of the experimental conditions is described. The method has been used for the determination of 2.0–50.0 μg/ml of PEH. The molar absorptivity is 5.34×103 L.mol.-1cm.-1 and the accuracy of the method is achieved by the value of average recovery (101.28 % and the precision is supported by relative standard deviation (RSD=1.25 % values. The results of the method was compared with those of the standard method. The interference of excipients was studied. The mechanism of the chemical reaction has been proposed. The proposed method was successfully applied for the determination of the PEH in pharmaceutical syrup formulations.

Spectrophotometric readout for alanine dosimeter to be used for food irradiation applications

International Nuclear Information System (INIS)

Ebraheem, S.; Beshir, W.B.; Eid, S.

2002-01-01

The electron spin resonance (EPR) readout of radical concentration produced upon irradiation of L-alanine is well known as a transfer dosimetry system for high dose level. The highly cost of EPR/alanine dosimetry system is a serious handicap for large scale routine application to be used in irradiation facilities. In this study, the reaction between L-alanine and 1,4-phenyl diammonium dichloride (PAC) solution produces a complex has a purple color. This complex has a variable absorbance with applied doses in the range from 1-20 kGy. Spectrophotometric evaluation at 368 and 505 nm for the absorbance intensity of this color as well as fluorimetric emission wavelength 435 nm were investigated, as a function of dose. The used method is uncomplicated and very easy for routine application. Evaluation of the dye concentration and the suitable amount of alanine has been studied. Stability of the product complex, for long period of time after the reaction had taken place, was also investigated

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

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Gervasio Ana P. G.

2001-01-01

Full Text Available 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 0.25 to 6.00 mg L-1, a reagent consumption of 25 mg ammonium molybdate and 2 mg stannous chloride per determination, and a relative standard deviation < 1% (n = 10 for a typical sample with 2.20 mg L-1 P were achieved. Three different types of samples were used to evaluate system performance. Accuracy was assessed by comparing the results with certified values and no significant difference at 95 % confidence level was observed.

A Unified tool to estimate Distances, Ages, and Masses (UniDAM) from spectrophotometric data

Science.gov (United States)

Mints, Alexey; Hekker, Saskia

2017-08-01

Context. Galactic archaeology, the study of the formation and evolution of the Milky Way by reconstructing its past from its current constituents, requires precise and accurate knowledge of stellar parameters for as many stars as possible. To achieve this, a number of large spectroscopic surveys have been undertaken and are still ongoing. Aims: So far consortia carrying out the different spectroscopic surveys have used different tools to determine stellar parameters of stars from their derived effective temperatures (Teff), surface gravities (log g), and metallicities ([Fe/H]); the parameters can be combined with photometric, astrometric, interferometric, or asteroseismic information. Here we aim to homogenise the stellar characterisation by applying a unified tool to a large set of publicly available spectrophotometric data. Methods: We used spectroscopic data from a variety of large surveys combined with infrared photometry from 2MASS and AllWISE and compared these in a Bayesian manner with PARSEC isochrones to derive probability density functions (PDFs) for stellar masses, ages, and distances. We treated PDFs of pre-helium-core burning, helium-core burning, and post helium-core burning solutions as well as different peaks in multimodal PDFs (I.e. each unimodal sub-PDF) of the different evolutionary phases separately. Results: For over 2.5 million stars we report mass, age, and distance estimates for each evolutionary phase and unimodal sub-PDF. We report Gaussian, skewed, Gaussian, truncated Gaussian, modified truncated exponential distribution or truncated Student's t-distribution functions to represent each sub-PDF, allowing us to reconstruct detailed PDFs. Comparisons with stellar parameter estimates from the literature show good agreement within uncertainties. Conclusions: We present UniDAM, the unified tool applicable to spectrophotometric data of different surveys, to obtain a homogenised set of stellar parameters. The unified tool and the tables with

The Gaia spectrophotometric standard stars survey: II. Instrumental effects of six ground-based observing campaigns

Science.gov (United States)

Altavilla, G.; Marinoni, S.; Pancino, E.; Galleti, S.; Ragaini, S.; Bellazzini, M.; Cocozza, G.; Bragaglia, A.; Carrasco, J. M.; Castro, A.; Di Fabrizio, L.; Federici, L.; Figueras, F.; Gebran, M.; Jordi, C.; Masana, E.; Schuster, W.; Valentini, G.; Voss, H.

2015-08-01

The Gaia SpectroPhotometric Standard Stars (SPSS) survey started in 2006, was awarded almost 450 observing nights and accumulated almost 100 000 raw data frames with both photometric and spectroscopic observations. Such large observational effort requires careful, homogeneous, and automatic data reduction and quality control procedures. In this paper, we quantitatively evaluate instrumental effects that might have a significant (i.e., ≥ 1 %) impact on the Gaia SPSS flux calibration. The measurements involve six different instruments, monitored over the eight years of observations dedicated to the Gaia flux standards campaigns: DOLORES@TNG in La Palma, EFOSC2@NTT and ROSS@REM in La Silla, CAFOS@2.2 m in Calar Alto, BFOSC@Cassini in Loiano, and LaRuca@1.5 m in San Pedro Mártir. We examine and quantitatively evaluate the following effects: CCD linearity and shutter times, calibration frames stability, lamp flexures, second order contamination, light polarization, and fringing. We present methods to correct for the relevant effects which can be applied to a wide range of observational projects at similar instruments. Based on data obtained with BFOSC@Cassini in Loiano, Italy; EFOSC2@NTT in La Silla, Chile; DOLORES@TNG in La Palma, Spain; CAFOS@2.2 m in Calar Alto, Spain; LaRuca@1.5 m in San Pedro Mártir, Mexico (see acknowledgements for more details).

Spectrophotometric determination of boron in complex matrices by isothermal distillation of borate ester into curcumin

International Nuclear Information System (INIS)

Thangavel, S.; Dhavile, S.M.; Dash, K.; Chaurasia, S.C.

2004-01-01

In situ distillation of borate ester into the curcumin solution has been developed for the spectrophotometric determination of boron in a variety of complex matrixes. A polypropylene vessel containing the sample solution was placed inside a vessel (PP) containing 10 ml of curcumin solution and the distillation was carried out at room temperature/on a water bath. The borate ester collected in to the curcumin solution was evaporated to dryness on the water bath, taken in acetone and the absorbance was measured at 550 nm. In situ distillation of borate ester directly into the chromogenic reagent eliminates tedious sample treatment (before and/or after borate separation), use of methanol, complicated quartz set up, possible loss of boron and reduces the analysis time significantly. In situ dehydration of sample solution by ethanolic vapour in the absence of dehydrating acid prevents the formation of fluoborate and co-distillation of potential anionic interferents (nitrate and fluoride). This developed method has been applied for the determination of traces of boric acid in boron powder by the distillation of methyl borate at room temperature. For other matrixes (water, uranium oxide, uranyl nitrate, fluoride salt, etc.) distillation of ethyl borate was carried out on the water bath. LOD (3σ) was 5 ng g -1 for water and 30 ng g -1 for solid samples

In situ, rapid, and temporally resolved measurements of cellulase adsorption onto lignocellulosic substrates by UV-vis spectrophotometry

Science.gov (United States)

Hao Liu; J. Y. Zhu; X. S. Chai

2011-01-01

This study demonstrated two in situ UV-vis spectrophotometric methods for rapid and temporally resolved measurements of cellulase adsorption onto cellulosic and lignocellulosic substrates during enzymatic hydrolysis. The cellulase protein absorption peak at 280 nm was used for quantification. The spectral interferences from light scattering by small fibers (fines) and...

Spectrophotometric procedure using rhodamine B for determination of submicrogram quantities of antimony in rocks

Science.gov (United States)

Schnepfe, M.M.

1973-01-01

A spectrophotometric procedure using Rhodamine B is given for the determination of antimony in mineralized rocks after its separation as stibine. A study of the Rhodamine B reaction points to the importance of the order of addition of reagents in enhancing sensitivity and increasing the stability of the system. The tolerance of some 26 elements is established for the overall procedure. Although the limit of determination is approximately 0??5 ppm Sb in a 0??2-g sample, the procedure is intended primarily for screening samples containing more than 1 ppm Sb. In pure solutions 0??1 ??g of antimony can be determined with a relative standard deviation of 25%. For >0??2 ??g of antimony a relative standard deviation of 15% or less can be expected. ?? 1973.

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)

Multi-Attribute Decision Making Based on Several Trigonometric Hamming Similarity Measures under Interval Rough Neutrosophic Environment

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Surapati Pramanik

2018-03-01

Full Text Available In this paper, the sine, cosine and cotangent similarity measures of interval rough neutrosophic sets is proposed. Some properties of the proposed measures are discussed. We have proposed multi attribute decision making approaches based on proposed similarity measures. To demonstrate the applicability, a numerical example is solved.

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).

Mean centering of ratio spectra and successive derivative ratio spectrophotometric methods for determination of isopropamide iodide, trifluoperazine hydrochloride and trifluoperazine oxidative degradate

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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.

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)

Black Versus Gray T-Shirts: Comparison of Spectrophotometric and Other Biophysical Properties of Physical Fitness Uniforms and Modeled Heat Strain and Thermal Comfort

Science.gov (United States)

2016-09-01

PROPERTIES OF PHYSICAL FITNESS UNIFORMS AND MODELED HEAT STRAIN AND THERMAL COMFORT DISCLAIMER The opinions or assertions contained herein are the...SHIRTS: COMPARISON OF SPECTROPHOTOMETRIC AND OTHER BIOPHYSICAL PROPERTIES OF PHYSICAL FITNESS UNIFORMS AND MODELED HEAT STRAIN AND THERMAL COMFORT ...the impact of the environment on the wearer. To model these impacts on human thermal sensation (e.g., thermal comfort ) and thermoregulatory

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)

Developing model-making and model-breaking skills using direct measurement video-based activities

Science.gov (United States)

Vonk, Matthew; Bohacek, Peter; Militello, Cheryl; Iverson, Ellen

2017-12-01

This study focuses on student development of two important laboratory skills in the context of introductory college-level physics. The first skill, which we call model making, is the ability to analyze a phenomenon in a way that produces a quantitative multimodal model. The second skill, which we call model breaking, is the ability to critically evaluate if the behavior of a system is consistent with a given model. This study involved 116 introductory physics students in four different sections, each taught by a different instructor. All of the students within a given class section participated in the same instruction (including labs) with the exception of five activities performed throughout the semester. For those five activities, each class section was split into two groups; one group was scaffolded to focus on model-making skills and the other was scaffolded to focus on model-breaking skills. Both conditions involved direct measurement videos. In some cases, students could vary important experimental parameters within the video like mass, frequency, and tension. Data collected at the end of the semester indicate that students in the model-making treatment group significantly outperformed the other group on the model-making skill despite the fact that both groups shared a common physical lab experience. Likewise, the model-breaking treatment group significantly outperformed the other group on the model-breaking skill. This is important because it shows that direct measurement video-based instruction can help students acquire science-process skills, which are critical for scientists, and which are a key part of current science education approaches such as the Next Generation Science Standards and the Advanced Placement Physics 1 course.

Spectro-photometric determination of niobium in Nb-Ti alloy using in-situ separation of Ti by masking with H3PO4

International Nuclear Information System (INIS)

Ghosh, Prasun; Dutta, M.; Jat, J.R.; Reddy, G.B.; Balaji Rao, Y.; Subba Rao, Y.

2016-01-01

The present paper details a simple procedure for the determination of Nb content in Nb-Ti alloy. The method involves dissolution of alloy in mixture of HNO 3 and HF followed by fuming with H 2 SO 4 . Subsequently, solution is taken for UV-Vis Spectro-photometric measurement after addition of Conc. H 3 PO 4 and H 2 O 2 . Hydrogen peroxide is added as coloring agent. Hydrogen peroxide (H 2 O 2 ) is known to form yellow color peroxo complex with both Niobium and Titanium in sulfuric acid medium and thus Ti will interfere with Nb in absorbance measurement. In view of this practical difficulty, in-situ separation of Ti during measurement has been resorted by masking Ti using Conc. H 3 PO 4 . Standard synthetic sample solution of Nb-Ti was prepared having Niobium and titanium in the ratio of 60:40, 50:50 and 40:60. Quantitative measurement of Niobium was carried out by UV-Visible spectrophotometer at 365 nm. The interference of titanium is prominent from the obtained Niobium concentration. Different ratios of H 3 PO 4 and H 2 SO 4 tried to arrive at optimum ratio to eliminate titanium interference and results are as shown. Quantitative measurement of Niobium was carried out at 355 nm as absorption maxima shifted from 365 nm to 355 nm in presence of phosphoric acid. Results show a good agreement with synthetic standard at 80:20 sulfuric to phosphoric acid ratio

Spectrophotometric determination of titanium with ascorbic acid in aluminium alloys and other materials. Determinacion espectrofotometrica de titanio con acido ascorbico en aleaciones de base aluminio y otros materiales

Energy Technology Data Exchange (ETDEWEB)

Bosch Serrat, F. (Departamento de Quimica Analitica. Facultad de Qauimica. Valencia (Spain))

1994-01-01

A spectrophotometric determination of titanium with ascorbic acid in aluminium alloys and bauxite is described. The proposed procedures permit to determine levels of titanium down to 5.10 ''3% with a good accuracy and precision. (Author) 13 refs.

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.

The development of a new inhibition kinetic spectrophotometric method for determination of phenylhydrazine

Directory of Open Access Journals (Sweden)

VIOLETA D. MITIC

2005-07-01

Full Text Available Anew sensitive kinetic method has been developed for the determination of trace amounts of phenylhydrazine in the range of 1.08×10-7 to 1.08×10-6 g/cm3. The detection limit of this method is 0.008 mg/cm3, based on the 3Sb criterion. Themethod is based on the inhibitory effect of phenylhydrazine on the oxidation of Victoria Blue 4-R by KBrO3. The reaction was monitored spectrophotometrically at 596.3 nm. The method development includes the optimization of the reagent concentration and temperature. The kinetic parameters of the reaction are reported and a rate equation is suggested. The effects of certain foreign ions upon the reaction rate were determined for the assessment of the selectivity of the method. The new developedmethod was found to have fairly good selectivity, sensitivity, simplicity and rapidity.

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.

TOWARD A NETWORK OF FAINT DA WHITE DWARFS AS HIGH-PRECISION SPECTROPHOTOMETRIC STANDARDS

Energy Technology Data Exchange (ETDEWEB)

Narayan, G.; Matheson, T.; Saha, A.; Claver, J. [National Optical Astronomy Observatory, 950 North Cherry Avenue, Tucson, AZ 85719 (United States); Axelrod, T.; Olszewski, E. [University of Arizona, Steward Observatory, 933 North Cherry Avenue, Tucson, AZ 85721 (United States); Holberg, J. B. [University of Arizona, Lunar and Planetary Laboratory, 1629 East University Boulevard, Tucson, AZ 85721 (United States); Stubbs, C. W. [Department of Physics, Harvard University, 17 Oxford Street, Cambridge, MA 02138 (United States); Bohlin, R. C.; Deustua, S.; Rest, A., E-mail: gnarayan@noao.edu [Space Telescope Science Institute, 3700 San Martin Drive, Baltimore, MD 21218 (United States)

2016-05-10

We present the initial results from a program aimed at establishing a network of hot DA white dwarfs to serve as spectrophotometric standards for present and future wide-field surveys. These stars span the equatorial zone and are faint enough to be conveniently observed throughout the year with large-aperture telescopes. The spectra of these white dwarfs are analyzed in order to generate a non-local-thermodynamic-equilibrium model atmosphere normalized to Hubble Space Telescope colors, including adjustments for wavelength-dependent interstellar extinction. Once established, this standard star network will serve ground-based observatories in both hemispheres as well as space-based instrumentation from the UV to the near IR. We demonstrate the effectiveness of this concept and show how two different approaches to the problem using somewhat different assumptions produce equivalent results. We discuss the lessons learned and the resulting corrective actions applied to our program.

Study of Ascorbic Acid as Iron(III Reducing Agent for Spectrophotometric Iron Speciation

Directory of Open Access Journals (Sweden)

Antesar Elmagirbi

2012-10-01

Full Text Available The study of ascorbic acid as a reducing agent for iron(III has been investigated in order to obtain an alternative carcinogenic reducing agent, hydroxylamine, used in spectrophotometric standard method based on the formation of a red-orange complex of Fe(II-o-phenanthroline. The study was optimised with regards to ascorbic acid concentration as well as pH solution. The results showed that ascorbic acid showed maximum capacity as reducing agent of iron(III under concentration of 4.46.10-4 M and pH solution of 1-4.Under these conditions, ascorbic acid reduced iron(III proportionally and performed similarly to that of hydroxylamine.  The method gave result to linear calibration over the range of 0.2-2 mg/L withhigh accuracy of 97 % and relative standard deviation of less than 2 %. This method was successfully applied to assay iron speciation in water samples.

Spectrophotometric determination of metformin in pharmaceutical preparations, serum and urine using benzoin as derivatizing reagent

International Nuclear Information System (INIS)

Alamgir, M.; Hayat, A.

2014-01-01

A simple and selective spectrophotometric procedure is described for the determination of Metformin based on derivatization with benzoin. The Beers law was obeyed with 2.50-12.50 meu mol L-1 at 290 nm with coefficient of determination (r2) 0.997. The experimental conditions in term of pH, reaction time and temperature, and addition of derivatizing reagent were examined. The pure metformin-benzoin derivative was prepared and characterized by FT-IR and mass spectroscopic techniques. The method was applied for the determination of metformin from pharmaceutical preparations and serum and urine of volunteers after spiking with metformin. The results were checked by standard addition method. A number of pharmaceutical additives and serum or urine matrix did not affect the determination of metformin. (author)

p-chloro- and p-bromo-benzoylacetoneoxime as the spectrophotometric reagents for palladium and ruthenium(III)

International Nuclear Information System (INIS)

Yeole, V.V.; Langade, A.D.; Shinde, V.M.

1980-01-01

A procedure is described for the extractive spectrophotometric determination of palladium or ruthenium(III) using p-chloro or p-bromobenzoylacetoneoxime as the reagent. The yellow palladium complexes which are extracted into chloroform from an aqueous solution of pH 3.5, absorb as 400 nm and conform to Beer's law in the range of 10 to 100 μg of Pd/10 ml of organic phase. The orange-red ruthenium complexes which are extracted into ethylacetate from an aqueous solution of pH 5.0, absorbs at 475 nm and conforms to Beer's law in the range of 20 to 200 μg of Ru/10 ml of organic phase. The molar absorptivities, Sandell's sensitivities and instability constants are reported. (author)

SHARDS: An Optical Spectro-photometric Survey of Distant Galaxies

Science.gov (United States)

Pérez-González, Pablo G.; Cava, Antonio; Barro, Guillermo; Villar, Víctor; Cardiel, Nicolás; Ferreras, Ignacio; Rodríguez-Espinosa, José Miguel; Alonso-Herrero, Almudena; Balcells, Marc; Cenarro, Javier; Cepa, Jordi; Charlot, Stéphane; Cimatti, Andrea; Conselice, Christopher J.; Daddi, Emmanuele; Donley, Jennifer; Elbaz, David; Espino, Néstor; Gallego, Jesús; Gobat, R.; González-Martín, Omaira; Guzmán, Rafael; Hernán-Caballero, Antonio; Muñoz-Tuñón, Casiana; Renzini, Alvio; Rodríguez-Zaurín, Javier; Tresse, Laurence; Trujillo, Ignacio; Zamorano, Jaime

2013-01-01

We present the Survey for High-z Absorption Red and Dead Sources (SHARDS), an ESO/GTC Large Program carried out using the OSIRIS instrument on the 10.4 m Gran Telescopio Canarias (GTC). SHARDS is an ultra-deep optical spectro-photometric survey of the GOODS-N field covering 130 arcmin2 at wavelengths between 500 and 950 nm with 24 contiguous medium-band filters (providing a spectral resolution R ~ 50). The data reach an AB magnitude of 26.5 (at least at a 3σ level) with sub-arcsec seeing in all bands. SHARDS' main goal is to obtain accurate physical properties of intermediate- and high-z galaxies using well-sampled optical spectral energy distributions (SEDs) with sufficient spectral resolution to measure absorption and emission features, whose analysis will provide reliable stellar population and active galactic nucleus (AGN) parameters. Among the different populations of high-z galaxies, SHARDS' principal targets are massive quiescent galaxies at z > 1, whose existence is one of the major challenges facing current hierarchical models of galaxy formation. In this paper, we outline the observational strategy and include a detailed discussion of the special reduction and calibration procedures which should be applied to the GTC/OSIRIS data. An assessment of the SHARDS data quality is also performed. We present science demonstration results on the detection and study of emission-line galaxies (star-forming objects and AGNs) at z = 0-5. We also analyze the SEDs for a sample of 27 quiescent massive galaxies with spectroscopic redshifts in the range 1.0 UV-to-MIR SEDs of the massive quiescent galaxies at z = 1.0-1.4 are well described by an exponentially decaying star formation history with scale τ = 100-200 Myr, age around 1.5-2.0 Gyr, solar or slightly sub-solar metallicity, and moderate extinction, A(V) ~ 0.5 mag. We also find that galaxies with masses above M* are typically older than lighter galaxies, as expected in a downsizing scenario of galaxy formation. This

Optical fiber couplers for spectrophotometry. Perspectives for in-situ on-line and remote measurements

International Nuclear Information System (INIS)

Boisde, G.; Linger, C.; Chevalier, G.; Perez, J.J.

1983-01-01

Optical fiber couplers have been developed specially for nuclear chemical spectrophotometric applications. Coupling devices are described for TELEPHOT industrial photometers and some commercial spectrophotometer, together with the probes and measurement cells employed. The value of optical multiplexing is mentioned. Non nuclear applications in medical analysis are also mentioned, together with the possibilities offered by these devices for uses other than spectrophotometry [fr

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.

Simultaneous spectrophotometric determination of overlapping spectra of paracetamol and caffeine in laboratory prepared mixtures and pharmaceutical preparations using continuous wavelet and derivative transform

Directory of Open Access Journals (Sweden)

Ahmed Ashour

2015-03-01

Full Text Available In the present paper, two spectrophotometric methods were used for the simultaneous analysis of paracetamol (PCT and caffeine (CAF in their laboratory prepared mixtures and pharmaceutical preparations. Simple spectrophotometric analysis of PCT and CAF is not possible due to their complete spectral overlap. The proposed methods are based on the application of continuous wavelet transform (CWT and derivative transform (using Savitsky–Golay filters on the ratio spectra to predict each of CAF and PCT. Several wavelet families were tested. Coif1 and Sym2 were found to give best results under optimum conditions. The transformed signals of ratio spectra were used to plot the calibration curves for both components. The predictability of the built calibrations was validated through their application on several synthetic mixtures of both drugs. The proposed methods were used for the prediction of CAF and PCT in pharmaceutical preparation. The obtained results were statistically compared to a reference HPLC method. No significant differences were found between the obtained results and those from the reference method. Being simple, rapid, cheap and sensitive, the proposed methods are recommended for the routine daily analysis of these two drugs in their mixtures in quality control laboratories.

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.

Spectrophotometric and potentiometric studies of oxidation of Mo(III) by Mo(VI) in phosphoric acid medium

International Nuclear Information System (INIS)

Kumar, Arvind; Verma, G.S.P.

1975-01-01

Oxidation of Mo(III) (green) by Mo(VI) in an inert atmosphere and in orthophosphoric acid medium at various acid concentrations is reported. Potentiometric and spectrophotometric data suggest that oxidation of Mo(III) proceeds to Mo(V) through a binuclear species Mo(III) Mo(IV) absorbing at 400 nm. The formation of this species is facilitated at high acid concentrations. It is further found that quantitative conversion of Mo(III) into Mo(V) takes place at fairly high acid concentrations. In high phosphoric acid concentrations, solution of Mo(III) has been found to be oxidized to Mo(VI) by air and hence this can be used as a good oxygen absorber. (author)

Simultaneous spectrophotometric determination of copper, cobalt, nickel and iron in foodstuffs and vegetables with a new bis thiosemicarbazone ligand using chemometric approaches.

Science.gov (United States)

Rohani Moghadam, Masoud; Poorakbarian Jahromi, Sayedeh Maria; Darehkordi, Ali

2016-02-01

A newly synthesized bis thiosemicarbazone ligand, (2Z,2'Z)-2,2'-((4S,5R)-4,5,6-trihydroxyhexane-1,2-diylidene)bis(N-phenylhydrazinecarbothioamide), was used to make a complex with Cu(2+), Ni(2+), Co(2+) and Fe(3+) for their simultaneous spectrophotometric determination using chemometric methods. By Job's method, the ratio of metal to ligand in Ni(2+) was found to be 1:2, whereas it was 1:4 for the others. The effect of pH on the sensitivity and selectivity of the formed complexes was studied according to the net analyte signal (NAS). Under optimum conditions, the calibration graphs were linear in the ranges of 0.10-3.83, 0.20-3.83, 0.23-5.23 and 0.32-8.12 mg L(-1) with the detection limits of 2, 3, 4 and 10 μg L(-1) for Cu(2+), Co(2+), Ni(2+) and Fe(3+) respectively. The OSC-PLS1 for Cu(2+) and Ni(2+), the PLS1 for Co(2+) and the PC-FFANN for Fe(3+) were selected as the best models. The selected models were successfully applied for the simultaneous determination of elements in some foodstuffs and vegetables. Copyright © 2015 Elsevier Ltd. All rights reserved.

Spectrophotometric determination of neodymium in mixture with lanthanum by eosin and 2,2'-dipyridyl

International Nuclear Information System (INIS)

Ovchar, L.A.; Poluehktov, N.S.

1980-01-01

The possibility of using rare earth complexes with eosin (EO) and 2.2-dipyridyl (DP) for spectrophotometric determination of some rare earths in the presence of the others. It has been out that the complexes are not extracted by organic solvents. The PH region of complex existence (approximately 6) and the relation of components in them (rare earths:DP:EO=1:2:3) are determined. The possibility has been shown of determining all the rare earts from praseodymium to lutetium and yttrium in a binary mixture with lanthanum based on different stability of the studied complexes. The method has been tested on the example of determining Nd 2 O 3 in a mixture with La 2 O 3 . The low limit of determined contents is 1-2%. The relative standard deviation is 0.035-0.17 [ru

Building-up a database of spectro-photometric standards from the UV to the NIR

Science.gov (United States)

Vernet, J.; Kerber, F.; Mainieri, V.; Rauch, T.; Saitta, F.; D'Odorico, S.; Bohlin, R.; Ivanov, V.; Lidman, C.; Mason, E.; Smette, A.; Walsh, J.; Fosbury, R.; Goldoni, P.; Groot, P.; Hammer, F.; Kaper, L.; Horrobin, M.; Kjaergaard-Rasmussen, P.; Royer, F.

2010-11-01

We present results of a project aimed at establishing a set of 12 spectro-photometric standards over a wide wavelength range from 320 to 2500 nm. Currently no such set of standard stars covering the near-IR is available. Our strategy is to extend the useful range of existing well-established optical flux standards (Oke 1990, Hamuy et al. 1992, 1994) into the near-IR by means of integral field spectroscopy with SINFONI at the VLT combined with state-of-the-art white dwarf stellar atmospheric models (TMAP, Holberg et al. 2008). As a solid reference, we use two primary HST standard white dwarfs GD71 and GD153 and one HST secondary standard BD+17 4708. The data were collected through an ESO “Observatory Programme” over ~40 nights between February 2007 and September 2008.

Spectrophotometric determination of uranium and thorium with arsenazo III in the flow injection system

International Nuclear Information System (INIS)

Andrade, M. das G.M. de.

1986-12-01

A simple system for flow injection analysis (FIA) with double confluence was built using a filter photocolorimeter, an analogic potentiometer, 'plexiglass' flow cuvettes, polyethylene colls and tubes, 'plexiglass' commuter and peristaltic pump to introduce solutions and gravity as flow source. The system was dimensioned and studied using only Arsenazo III solutions. Spectrophotometric methods for uranium and thorium using Arsenazo III were studied using a scanning spectrophotometer and after chosing adequate red filter, adapted to photocolorimetry using flow cuvettes and FIA. Synthetic samples, phosphate rock, and process samples from uranium recovery of dolomites were analysed. Rocks of Morro do Ferro (MG, Brazil), Caldasite (Baddeleyte + Zirconite), Zirconite, Monazite from a program for certification and certified rocks (Dunite DC-1, CANMET) were analysed without chemical separation of Th (IV) and with ion exchange separation in semi-micro columns of cation exchange resin (Dowex 50). (Author) [pt

The four principles: can they be measured and do they predict ethical decision making?

Science.gov (United States)

Page, Katie

2012-05-20

The four principles of Beauchamp and Childress--autonomy, non-maleficence, beneficence and justice--have been extremely influential in the field of medical ethics, and are fundamental for understanding the current approach to ethical assessment in health care. This study tests whether these principles can be quantitatively measured on an individual level, and then subsequently if they are used in the decision making process when individuals are faced with ethical dilemmas. The Analytic Hierarchy Process was used as a tool for the measurement of the principles. Four scenarios, which involved conflicts between the medical ethical principles, were presented to participants who then made judgments about the ethicality of the action in the scenario, and their intentions to act in the same manner if they were in the situation. Individual preferences for these medical ethical principles can be measured using the Analytic Hierarchy Process. This technique provides a useful tool in which to highlight individual medical ethical values. On average, individuals have a significant preference for non-maleficence over the other principles, however, and perhaps counter-intuitively, this preference does not seem to relate to applied ethical judgements in specific ethical dilemmas. People state they value these medical ethical principles but they do not actually seem to use them directly in the decision making process. The reasons for this are explained through the lack of a behavioural model to account for the relevant situational factors not captured by the principles. The limitations of the principles in predicting ethical decision making are discussed.

The four principles: Can they be measured and do they predict ethical decision making?

Directory of Open Access Journals (Sweden)

Page Katie

2012-05-01

Full Text Available Abstract Background The four principles of Beauchamp and Childress - autonomy, non-maleficence, beneficence and justice - have been extremely influential in the field of medical ethics, and are fundamental for understanding the current approach to ethical assessment in health care. This study tests whether these principles can be quantitatively measured on an individual level, and then subsequently if they are used in the decision making process when individuals are faced with ethical dilemmas. Methods The Analytic Hierarchy Process was used as a tool for the measurement of the principles. Four scenarios, which involved conflicts between the medical ethical principles, were presented to participants who then made judgments about the ethicality of the action in the scenario, and their intentions to act in the same manner if they were in the situation. Results Individual preferences for these medical ethical principles can be measured using the Analytic Hierarchy Process. This technique provides a useful tool in which to highlight individual medical ethical values. On average, individuals have a significant preference for non-maleficence over the other principles, however, and perhaps counter-intuitively, this preference does not seem to relate to applied ethical judgements in specific ethical dilemmas. Conclusions People state they value these medical ethical principles but they do not actually seem to use them directly in the decision making process. The reasons for this are explained through the lack of a behavioural model to account for the relevant situational factors not captured by the principles. The limitations of the principles in predicting ethical decision making are discussed.

The four principles: Can they be measured and do they predict ethical decision making?

Science.gov (United States)

2012-01-01

Background The four principles of Beauchamp and Childress - autonomy, non-maleficence, beneficence and justice - have been extremely influential in the field of medical ethics, and are fundamental for understanding the current approach to ethical assessment in health care. This study tests whether these principles can be quantitatively measured on an individual level, and then subsequently if they are used in the decision making process when individuals are faced with ethical dilemmas. Methods The Analytic Hierarchy Process was used as a tool for the measurement of the principles. Four scenarios, which involved conflicts between the medical ethical principles, were presented to participants who then made judgments about the ethicality of the action in the scenario, and their intentions to act in the same manner if they were in the situation. Results Individual preferences for these medical ethical principles can be measured using the Analytic Hierarchy Process. This technique provides a useful tool in which to highlight individual medical ethical values. On average, individuals have a significant preference for non-maleficence over the other principles, however, and perhaps counter-intuitively, this preference does not seem to relate to applied ethical judgements in specific ethical dilemmas. Conclusions People state they value these medical ethical principles but they do not actually seem to use them directly in the decision making process. The reasons for this are explained through the lack of a behavioural model to account for the relevant situational factors not captured by the principles. The limitations of the principles in predicting ethical decision making are discussed. PMID:22606995

Spectrophotometric study of Saturn's main rings by means of Monte Carlo ray-tracing and Hapke's theory

Science.gov (United States)

Ciarniello, Mauro; Filacchione, Gianrico; D'Aversa, Emiliano; Cuzzi, Jeffrey N.; Capaccioni, Fabrizio; Hedman, Matthew M.; Dalle Ore, Cristina M.; Nicholson, Philip D.; Clark, Roger Nelson; Brown, Robert H.; Cerroni, Priscilla; Spilker, Linda

2017-10-01

This work is devoted to the investigation of the spectrophotometric properties of Saturn's rings from Cassini-VIMS (Visible and Infrared Mapping Spectrometer) observations. The dataset used for this analysis is represented by ten radial spectrograms of the rings which have been derived in Filacchione et al. (2014) by radial mosaics produced by VIMS. Spectrograms report the measured radiance factor of the main Saturn's rings as a function of both radial distance (from 73.500 to 141.375 km) and wavelength (0.35-5.1 µm) for different observation geometries (phase angle ranging in the 1.9°-132.2° interval). We take advantage of a Monte Carlo ray-tracing routine to characterize the photometric behavior of the rings at each wavelength and derive the spectral Bond albedo of rings particles. This quantity is used to infer the composition of the regolith covering rings particles by applying Hapke's theory. Four different regions, characterized by different optical depths, and respectively located in the C ring, inner B ring, mid B ring and A ring, have been investigated. Results from spectral modeling indicate that rings spectrum can be described by water ice with minimal inclusion of organic materials (tholin, exogenous material, which is more effective in the less dense regions of the rings because of their lower content of pure water ice.

Spectrophotometric flow-injection analysis assay of tetracycline antibiotics using a dual light-emitting diode based detector

Directory of Open Access Journals (Sweden)

Prinya Masawat

2008-02-01

Full Text Available In this paper, a small dual light-emitting diode (LED-based detector for FIA process analyser has been designed. The detector’s optical parts comprise a flow-through cell, a dual-blue LED and a photodiode. Neither mirrors nor lenses are used. The optical path for the first LED detects the blank, while the other LED detects the sample. The detector’s electronic components including a signal amplifier and an A/D converter are integrated on one small board connected to a PC for measuring the results. The designed spectrophotometric detector was used for the determination of tetracycline antibiotics. Uranyl acetate was used as a reagent forming orange-red complexes with the drugs in N,N– dimethylformamide. The complexes show absorption maxima at 410, 416 and 408 nm for tetracycline hydrochloride (TCH, chlortetracycline hydrochloride (CTCH, and doxycycline hydrochloride (DCH, respectively. The detection limit was found to be 0.38, 0.75, 1.44 µg mL-1 and the linear range was obtained at 1.0-3.0, 3.0-5.0, and 3.0-10.0 µg mL-1 for TCH, CTCH and DCH, respectively. The proposed method has been successfully applied to the determination of tetracycline antibiotic residues in milk samples. Moreover, this method is an environmentally friendly approach and suitable for routine analysis.

A spectrophotometric study of cerium IV and chromium VI species in nuclear fuel reprocessing process streams

International Nuclear Information System (INIS)

Nickson, I D; Boxall, C; Jackson, A; Whillock, G O H

2010-01-01

Nuclear fuel reprocessing schemes such as PUREX and UREX utilise HNO 3 media. An understanding of the corrosion of process engineering materials such as stainless steel in such media is a major concern for the nuclear industry. Two key species are cerium and chromium which, as Ce(IV), Cr(VI), may act as corrosion accelerants. An on-line analytical technique for these quantities would be useful for determining the relationship between corrosion rate and [Ce(IV)] and [Cr(VI)]. Consequently, a strategy for simultaneous quantification of Ce(IV), Cr(VI) and Cr(III) in the presence of other ions found in average burn-up Magnox / PWR fuel reprocessing stream (Fe, Mg, Nd, Al) is being developed. This involves simultaneous UV-vis absorbance measurement at 620, 540, 450 nm, wavelengths where Ce and Cr absorb but other ions do not. Mixed solutions of Cr(VI) and Ce(IV) are found to present higher absorbance values at 540 nm than those predicted from absorbances recorded from single component solutions of those ions. This is attributed to the formation of a 3:1 Cr(VI)-Ce(IV) complex and we report on the complexation and UV-visible spectrophotometric characteristics of this species. To the best of our knowledge this is the first experimental study of this complex in aqueous nitric acid solution systems.

Spectrophotometric determination of β-adrenergic antagonists drugs via ion-pair complex formation using MO and EBT

Science.gov (United States)

El-Didamony, A. M.; Shehata, A. M.

2014-09-01

Two simple, rapid and sensitive spectrophotometric methods have been proposed for the assay of bisoprolol fumarate (BSF), propranolol hydrochloride (PRH), and timolol maleate (TIM) either in bulk or in pharmaceutical formulations. The methods are based on the reaction of the selected drugs with methyl orange (MO) and eriochrome black T in acidic buffers, after extracting in dichloromethane and measured quantitatively with maximum absorption at 428 and 518 nm for MO and EBT, respectively. The analytical parameters and their effects on the reported systems are investigated. The extracts are intensely colored and very stable at room temperature. The calibration graphs were linear over the concentration range of 0.8-6.4, 0.4-3.6, 0.8-5.6 μg/mL for BSF, PRH, and TIM, respectively, with MO and 0.8-6.4, 0.4-3.2, and 0.8-8.0 μg/mL for BSF, PRH, and TIM, respectively, with EBT. The stoichiometry of the complexes was found to be 1 : 1 in all cases. The proposed methods were successfully extended to pharmaceutical preparations. Excipients used as additive in commercial formulations did not interfere in the analysis. The proposed methods can be recommended for quality control and routine analysis where time, cost effectiveness and high specificity of analytical technique are of great importance.

Indirect spectrophotometric determination of sulfadiazine based on localized surface plasmon resonance peak of silver nanoparticles after cloud point extraction.

Science.gov (United States)

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Fattahi, Mohammad Reza; Khodaveisi, Javad

2017-12-05

A novel, efficient, easy to use, environmentally friendly and cost-effective methodology is developed for the indirect spectrophotometric determination of sulfadiazine in different samples. The method is based on the micelle-mediated extraction of silver sulfadiazine and converting the silver content of the resultant surfactant-rich phase to the silver nanoparticles via generation of [Ag(NH 3 ) 2 ] + followed by its chemical reduction using ascorbic acid. The changes in the amplitude of localized surface plasmon resonance peak of silver nanoparticles as a function of sulfadiazine concentration in the sample solution was monitored using fiber optic linear array spectrophotometry at 457nm. The experimental conditions were thoroughly investigated and optimized. Under the optimized condition, the developed procedure showed dynamic linear calibration within the range of 10.0-800.0μgL -1 with a detection limit of 2.8μgL -1 for sulfadiazine. The relative standard deviation of the method for six replicate measurements at 150.0μgL -1 of sulfadiazine was 4.7%. The developed method was successfully applied to the determination of sulfadiazine in different samples including well water, human urine, milk and pharmaceutical formulation. Copyright © 2017. Published by Elsevier B.V.

Indirect spectrophotometric determination of sulfadiazine based on localized surface plasmon resonance peak of silver nanoparticles after cloud point extraction

Science.gov (United States)

Kazemi, Elahe; Dadfarnia, Shayessteh; Haji Shabani, Ali Mohammad; Fattahi, Mohammad Reza; Khodaveisi, Javad

2017-12-01

A novel, efficient, easy to use, environmentally friendly and cost-effective methodology is developed for the indirect spectrophotometric determination of sulfadiazine in different samples. The method is based on the micelle-mediated extraction of silver sulfadiazine and converting the silver content of the resultant surfactant-rich phase to the silver nanoparticles via generation of [Ag(NH3)2]+ followed by its chemical reduction using ascorbic acid. The changes in the amplitude of localized surface plasmon resonance peak of silver nanoparticles as a function of sulfadiazine concentration in the sample solution was monitored using fiber optic linear array spectrophotometry at 457 nm. The experimental conditions were thoroughly investigated and optimized. Under the optimized condition, the developed procedure showed dynamic linear calibration within the range of 10.0-800.0 μg L- 1 with a detection limit of 2.8 μg L- 1 for sulfadiazine. The relative standard deviation of the method for six replicate measurements at 150.0 μg L- 1 of sulfadiazine was 4.7%. The developed method was successfully applied to the determination of sulfadiazine in different samples including well water, human urine, milk and pharmaceutical formulation.

Spectrophotometric readout for alanine dosimeter to be used for food irradiation applications

International Nuclear Information System (INIS)

Ebraheem, S.; Beshir, W.B.; Sobhy, R.; Kovacs, A.; Wojnarovits, L.

2002-01-01

Complete text of publication follows. The electron spin resonance (EPR) readout of radical concentration produced upon irradiation of L-alanine is well known as a transfer dosimetry system for high dose range. The high cost of EPR/alanine dosimetry system is a serious handicap for large-scale routine application for use in irradiation facilities. In this study the irradiated L-alanine was dissolved in 1,4 -phenyl diammonium dichloride (PAC) solution resulting a complex of a purple colour. This complex has a variable absorbance with applied dose in the range from 1 - 20 kGy. The absorbance of this complex using spectrophotometric evaluation was investigated at 401 and 478 nm with increasing dose. The fluorimetric emission was also studied at the wavelength of 475 nm as a function of dose. This methos for dose evaluation is uncomplicated and very easy for routine application. The effect of the dye concentration as well as the suitable amount of alanine has been studied with respect to practical use. The stability of the complex for long period of time was also investigated

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)

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

Directory of Open Access Journals (Sweden)

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.

Spectrophotometric analysis of discoloration and internal bleaching after use of different antibiotic pastes.

Science.gov (United States)

Fundaoğlu Küçükekenci, Funda; Çakici, Fatih; Küçükekenci, Ahmet Serkan

2018-04-14

To investigate teeth's antibiotic-induced color differences after bleaching using two different techniques. One hundred twenty extracted maxillar human incisors were examined. The specimens were randomly divided into six groups, each receiving one of six antibiotic paste fillings: (1) triple antibiotic paste (TAP) with minocycline, (2) double antibiotic paste (DAP), (3) TAP with amoxicillin, (4) TAP with cefaclor, (5) TAP with doxycycline, and (6) no filling (control group). Spectrophotometric measurements were obtained at baseline and then during the first, second, and third weeks after paste placement. The specimens discolored by antibiotics pastes were randomly divided into two subgroups: (1) internal bleaching with hydrogen peroxide (H 2 O 2) and (2) internal bleaching with H 2 O 2 plus Nd-YAG laser irradiation. The ∆E value was calculated and analyzed using a two-way analysis of variance and post-hoc Tukey's test (α = 0.05). The ∆E for all groups showed color differences exceeding the perceptibility threshold (∆E ˃ 3.7) at all time points except in the control and DAP groups. Minocycline-induced TAP showed the most severe coronal discoloration (32.42). When the ∆E was examined, thermo/photo bleaching (22.01 ± 8.23) caused more bleaching than walking bleaching (19.73 ± 5.73) at every time point (P = 0.19). No group returned to the original color after bleaching (P bleaching with Nd-YAG laser can be useful for bleaching/removing this discoloration. For clinically successful final appearances, understanding the effects of bleaching procedures on antibiotic paste discoloration is important.

Quantitative Analysis of Mixtures of Monoprotic Acids Applying Modified Model-Based Rank Annihilation Factor Analysis on Variation Matrices of Spectrophotometric Acid-Base Titrations

Directory of Open Access Journals (Sweden)

Ebrahim Ghorbani-Kalhor

2015-04-01

Full Text Available In the current work, a new version of rank annihilation factor analysis was developedto circumvent the rank deficiency problem in multivariate data measurements.Simultaneous determination of dissociation constant and concentration of monoprotic acids was performed by applying model-based rank annihilation factor analysis on variation matrices of spectrophotometric acid-base titrations data. Variation matrices can be obtained by subtracting first row of data matrix from all rows of the main data matrix. This method uses variation matrices instead of multivariate spectrophotometric acid-base titrations matrices to circumvent the rank deficiency problem in the rank quantitation step. The applicability of this approach was evaluated by simulated data at first stage, then the binary mixtures of ascorbic and sorbic acids as model compounds were investigated by the proposed method. At the end, the proposed method was successfully applied for resolving the ascorbic and sorbic acid in an orange juice real sample. Therefore, unique results were achieved by applying rank annihilation factor analysis on variation matrix and using hard soft model combination advantage without any problem and difficulty in rank determination. Normal 0 false false false EN-US X-NONE AR-SA /* Style Definitions */ table.MsoNormalTable {mso-style-name:"Table Normal"; mso-tstyle-rowband-size:0; mso-tstyle-colband-size:0; mso-style-noshow:yes; mso-style-priority:99; mso-style-parent:""; mso-padding-alt:0cm 5.4pt 0cm 5.4pt; mso-para-margin-top:0cm; mso-para-margin-right:0cm; mso-para-margin-bottom:10.0pt; mso-para-margin-left:0cm; line-height:115%; mso-pagination:widow-orphan; font-size:11.0pt; font-family:"Calibri","sans-serif"; mso-ascii-font-family:Calibri; mso-ascii-theme-font:minor-latin; mso-hansi-font-family:Calibri; mso-hansi-theme-font:minor-latin; mso-bidi-font-family:Arial; mso-bidi-theme-font:minor-bidi; mso-bidi-language:AR-SA;}    

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)

Cross Entropy Measures of Bipolar and Interval Bipolar Neutrosophic Sets and Their Application for Multi-Attribute Decision-Making

Directory of Open Access Journals (Sweden)

Surapati Pramanik

2018-03-01

Full Text Available The bipolar neutrosophic set is an important extension of the bipolar fuzzy set. The bipolar neutrosophic set is a hybridization of the bipolar fuzzy set and neutrosophic set. Every element of a bipolar neutrosophic set consists of three independent positive membership functions and three independent negative membership functions. In this paper, we develop cross entropy measures of bipolar neutrosophic sets and prove their basic properties. We also define cross entropy measures of interval bipolar neutrosophic sets and prove their basic properties. Thereafter, we develop two novel multi-attribute decision-making strategies based on the proposed cross entropy measures. In the decision-making framework, we calculate the weighted cross entropy measures between each alternative and the ideal alternative to rank the alternatives and choose the best one. We solve two illustrative examples of multi-attribute decision-making problems and compare the obtained result with the results of other existing strategies to show the applicability and effectiveness of the developed strategies. At the end, the main conclusion and future scope of research are summarized.

Spectrophotometric determination of nicradipine and isradipine in pharmaceutical formulations

Directory of Open Access Journals (Sweden)

S. M. Al-Ghannam

2009-05-01

Full Text Available A sensitive spectrophotometric method was developed for the determination of some 1,4-dihydropyridine compounds namely, nicardipine and isradipine either in pure form or in pharmaceutical preparations. The method is based on the reduction of nicardipine and isradipine with zinc powder and calcium chloride followed by further reduction with sodium pentacyanoaminoferrate (II to give violet and red products having the absorbance maximum at 546 and 539 nm with nicardipine and isradipine, respectively. Beer’s law was obeyed over the concentration range 8.0–180 μg/ml with the detection limit of 1.67 μg/ml for nicardipine and 8.0–110 μg/ml with the detection limit of 1.748 μg/ml for isradipine. The analytical parameters and their effects on the reported methods were investigated. The molar absorptivity, quantization limit, standard deviation of intercept (Sa, standard deviation of slope (Sb and standard deviation of the residuals (Sy/x were calculated. The composition of the result compounds were found 1:1 for nicardipine and 1:2 for isradipine by Job’s method and the conditional stability constant (Kf and the free energy changes (ΔG were calculated for compounds formed. The proposed method was applied successfully for the determination of nicardipine and isradipine in their dosage forms. The results obtained were in good agreement with those obtained using the reference or official methods. A proposal of the reaction pathway was presented.

Analysis of ionic channels by a flash spectrophotometric technique applicable to thylakoid membranes : CF0, the proton channel of the chloroplast ATP synthase, and, for comparison, gramicidin

NARCIS (Netherlands)

Lill, H.; Althoff, Gerd; Junge, Wolfgang

We previously introduced a flash spectrophotometric method to analyze proton conduction by CF0 in vesicles derived from thylakoid membranes (H. Lill, S. Engelbrecht, G. Schönknecht & W. Junge, 1986, Eur. J. Biochem.160:627-634). The unit conductance of CF0, as revealed by this technique, was orders

Spectrophotometric determination of ethionamide in pharmaceuticals using Folin–Ciocalteu reagent and iron(III-ferricyanide as chromogenic agents

Directory of Open Access Journals (Sweden)

Nagib A.S. Qarah

2017-09-01

Full Text Available Two simple and sensitive spectrophotometric methods are described for the determination of ethionamide (ETM in pure drug and tablets. The first method is based on the reduction of Folin–Ciocalteu (F–C reagent by ETM in sodium carbonate medium to form a blue coloured complex, which was measured at 760 nm (Molybdenum–tungsten blue method. In the second method (Prussian blue method, iron(III was reduced to iron(II by ETM in HCl medium, in which iron(II was complexed with ferricyanide, and the resulting Prussian blue was also measured at 760 nm. The absorbance measured in each case was related to the ETM concentration. The experimental conditions were carefully studied and optimised. Beer's law was obeyed in concentration ranges of 1–40 μg/ml and 0.2–4.0 μg/ml with the Molybdenum-tungsten blue method and the Prussian blue method, respectively, with corresponding molar absorptivity values of 5.72 × 103 and 3.18 × 104 l/(mol·cm. The limits of detection (LOD and quantification (LOQ were 0.09 and 0.27 μg/ml for the Molybdenum-tungsten blue method and 0.01 and 0.04 μg/ml for the Prussian blue method. Within-day and between-day relative standard deviations (%RSD at three different concentration levels were <3%, and the respective relative errors (%RE were ≤2%, implying good accuracy and precision of the methods. The proposed methods were successfully applied to the determination of ETM in bulk powder and tablets, and the results demonstrated that the methods were as accurate and precise as the official method.

Reaction of UO/sub 2//sup 2 +/ with Chromazurol S and the spectrophotometric determination of uranium in the presence of Septonex

Energy Technology Data Exchange (ETDEWEB)

Kanicky, V [Geological Survey Ostrava, Establishment Brno (Czechoslovakia); Havel, J; Sommer, L [Universita J.E. Purkyne, Brno (Czechoslovakia). Prirodovedecka Fakulta

1980-05-01

A detailed study is described of the reaction of UO/sub 2//sup 2 +/ with chromazurol S in the presence of cationic surfactant Septonex which was found to be very promising of the group of cationic surfactants. A number of conclusions were drawn regarding the effect of the cationic surfactant on the reaction of triphenylmethane dyes with salicylic acid groups with metal cations. The optimum conditions for the spectrophotometric determination of uranium with chromazurol S in the presence of Septonex were found.

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)

Liquid–liquid microextraction in a multicommuted flow system for direct spectrophotometric determination of iodine value in biodiesel

Energy Technology Data Exchange (ETDEWEB)

Pereira, Andréia C.; Rocha, Fábio R.P., E-mail: frprocha@cena.usp.br

2014-06-01

Highlights: • First flow-based procedure for iodine value determination in biodiesel. • Simple, fast and reliable procedure. • Detection without sample pretreatment or phase separation. • Liquid–liquid microextraction with low sample and reagent volumes. • Avoid toxic reagents and organic solvent used in the reference procedure. Abstract: A flow-based procedure was developed for the direct spectrophotometric determination of the iodine value (IV) in biodiesel. The procedure was based on the microextraction/reaction of unsaturated compounds with triiodide ions in an aqueous medium by inserting the reagent solution between the aliquots of biodiesel without any pretreatment. The interaction occurred through the biodiesel film formed on the inner walls of the hydrophobic tube used as the reactor and at the aqueous/biodiesel interfaces. The spectrophotometric detection was based on the discoloration of the I₃⁻ reagent in the aqueous phase by using a glass tube coupled to a fiber-optic spectrophotometer as the detection cell. Reference solutions were prepared by dilution of biodiesel samples with previously determined IV in hexane. The analytical response was linear for IV from 13 to 135 g I₂/100 g with a detection limit of 5 g I₂/100 g. A coefficient of variation of 1.7% (n = 10) and a sampling rate of 108 determinations per hour were achieved by consuming 224 μL of the sample and 200 μg of I₂ per determination. The slopes of analytical curves obtained with three different biodiesel samples were in agreement (variations in slopes lower than 3.1%), thus indicating an absence of any matrix effects. Results for biodiesel samples from different sources agreed with the volumetric official procedure at the 95% confidence level. The proposed procedure is therefore a simple, fast, and reliable alternative for estimating the iodine value of biodiesel.

Liquid–liquid microextraction in a multicommuted flow system for direct spectrophotometric determination of iodine value in biodiesel

International Nuclear Information System (INIS)

Pereira, Andréia C.; Rocha, Fábio R.P.

2014-01-01

Highlights: • First flow-based procedure for iodine value determination in biodiesel. • Simple, fast and reliable procedure. • Detection without sample pretreatment or phase separation. • Liquid–liquid microextraction with low sample and reagent volumes. • Avoid toxic reagents and organic solvent used in the reference procedure. - Abstract: A flow-based procedure was developed for the direct spectrophotometric determination of the iodine value (IV) in biodiesel. The procedure was based on the microextraction/reaction of unsaturated compounds with triiodide ions in an aqueous medium by inserting the reagent solution between the aliquots of biodiesel without any pretreatment. The interaction occurred through the biodiesel film formed on the inner walls of the hydrophobic tube used as the reactor and at the aqueous/biodiesel interfaces. The spectrophotometric detection was based on the discoloration of the I 3 − reagent in the aqueous phase by using a glass tube coupled to a fiber-optic spectrophotometer as the detection cell. Reference solutions were prepared by dilution of biodiesel samples with previously determined IV in hexane. The analytical response was linear for IV from 13 to 135 g I 2 /100 g with a detection limit of 5 g I 2 /100 g. A coefficient of variation of 1.7% (n = 10) and a sampling rate of 108 determinations per hour were achieved by consuming 224 μL of the sample and 200 μg of I 2 per determination. The slopes of analytical curves obtained with three different biodiesel samples were in agreement (variations in slopes lower than 3.1%), thus indicating an absence of any matrix effects. Results for biodiesel samples from different sources agreed with the volumetric official procedure at the 95% confidence level. The proposed procedure is therefore a simple, fast, and reliable alternative for estimating the iodine value of biodiesel

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)

Repurification and characterization of extractant mixture (isobutyl acetate-methyl isobutyl ketone) used in spectrophotometric analytical methods

International Nuclear Information System (INIS)

Al-Merey, R.; Al-Hameish, M.

2001-01-01

Isobutyl acetate (IBA) -methyl isobutyl ketone (MIBK) mixture used in analytical laboratories was re-purified by fractional distillation. The used mixture was washed with 0.5 M Na 2 CO 3 solution for the removal of inorganic substances. The range of fractional distillation was between 111-114 Centigrade which gave an azeotropic mixture that consists of 70% of IBA, 20% of MIBK and 10% of isobutanol (IBL). Gas chromatography (GC) analysis showed that isobutanol was increased by about 10% on the expense of IBA. This study suggests that MIBK could be determined in organic mixture spectrophotometrically. The analytical function of the re-purified mixture is found to be better than the unused mixture. Finally the distillation recovery was 93%. (author)

Effort-Based Decision Making in Schizophrenia: Evaluation of Paradigms to Measure Motivational Deficits.

Science.gov (United States)

Green, Michael F; Horan, William P

2015-09-01

Effort-based decision making requires one to decide how much effort to expend for a certain amount of reward. As the amount of reward goes up most people are willing to exert more effort. This relationship between reward level and effort expenditure can be measured in specialized performance-based tasks that have only recently been applied to schizophrenia. Such tasks provide a way to measure objectively motivational deficits in schizophrenia, which now are only assessed with clinical interviews of negative symptoms. The articles in this theme provide reviews of the relevant animal and human literatures (first 2 articles), and then a psychometric evaluation of 5 effort-based decision making paradigms (last 2 articles). This theme section is intended to stimulate interest in this emerging area among basic scientists developing paradigms for preclinical studies, human experimentalists trying to disentangle factors that contribute to performance on effort-based tasks, and investigators looking for objective endpoints for clinical trials of negative symptoms in schizophrenia. © The Author 2015. Published by Oxford University Press on behalf of the Maryland Psychiatric Research Center. All rights reserved. For permissions, please email: journals.permissions@oup.com.

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)

Cloud point extraction, preconcentration and spectrophotometric determination of nickel in water samples using dimethylglyoxime

Directory of Open Access Journals (Sweden)

Morteza Bahram

2013-01-01

Full Text Available A new and simple method for the preconcentration and spectrophotometric determination of trace amounts of nickel was developed by cloud point extraction (CPE. In the proposed work, dimethylglyoxime (DMG was used as the chelating agent and Triton X-114 was selected as a non-ionic surfactant for CPE. The parameters affecting the cloud point extraction including the pH of sample solution, concentration of the chelating agent and surfactant, equilibration temperature and time were optimized. Under the optimum conditions, the calibration graph was linear in the range of 10-150 ng mL-1 with a detection limit of 4 ng mL-1. The relative standard deviation for 9 replicates of 100 ng mL-1 Ni(II was 1.04%. The interference effect of some anions and cations was studied. The method was applied to the determination of Ni(II in water samples with satisfactory results.

An experimental method for making spectral emittance and surface temperature measurements of opaque surfaces

International Nuclear Information System (INIS)

Moore, Travis J.; Jones, Matthew R.; Tree, Dale R.; Daniel Maynes, R.; Baxter, Larry L.

2011-01-01

An experimental procedure has been developed to make spectral emittance and temperature measurements. The spectral emittance of an object is calculated using measurements of the spectral emissive power and of the surface temperature of the object obtained using a Fourier transform infrared (FTIR) spectrometer. A calibration procedure is described in detail which accounts for the temperature dependence of the detector. The methods used to extract the spectral emissive power and surface temperature from measured infrared spectra were validated using a blackbody radiator at known temperatures. The average error in the measured spectral emittance was 2.1% and the average difference between the temperature inferred from the recorded spectra and the temperature indicated on the blackbody radiator was 1.2%. The method was used to measure the spectral emittance of oxidized copper at various temperatures.

Organophosphorous complexones. Pt. 4. Spectrophotometric titration of beryllium(2) with (N,N,N',N-ethylenediamine) tetramethanephosphonic acid

International Nuclear Information System (INIS)

Szczepaniak, W.; Staniewska, M.

1976-01-01

Spectrophotometric titration of Be 2+ with (N,N,N'-ethylenediamine) tetramethanephosphonic acid (EDTP) using Chromazurol S as indicator was carried out. Using a TiMi attachment of a Specol colorimeter it is possible to determine 1.6 μg - 14 μg Be in 2 ml of solution. Alkali metals, alkaline earth metals as well as common anions as chlorides, nitrates, sulphates and acetates do not interfere. Using EDTA as masking agent it is possible to determine beryllium in the presence of divalent cations of the transition metals (Zn 2+ , Cd 2+ , Cu 2+ , Ni 2+ , Co 2+ , Pb 2+ ) Al 3+ , Fe 3+ and lanthanides. Uranyl ion and tetravalent cations e.g. Th 4+ interfere. (author)

Cationic dyes as extraction and spectrophotometric reagents: extraction of thiocyanate complex of mercury (II) in association with malachite green

Energy Technology Data Exchange (ETDEWEB)

Iyer, N V; Murthy, T K.S.

1975-01-01

An extraction spectrophotometric method for the determination of Hg(II) is described. This is based on the extraction of Hg(CNS)/sub 3//sup -/ complex in association with the cation of malachite green into benzene. The benzene extract has lambda max at 640 mm. Maximal extraction takes place from an aqueous solution of pH 4.5. Although four extractions are needed for quantitative recovery of Hg(II), a single extraction with aqueous organic = 2.5 : 1 is recommended for analysis and the apparent molar absorptivity is 65,000. The interference from a number of anions and cations has also been studied. (auth)

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.

Moving towards tangible decision-making tools for policy makers: Measuring and monitoring energy access provision

International Nuclear Information System (INIS)

Bhanot, Jaya; Jha, Vivek

2012-01-01

Access to energy services has been recognised as central to achieving economic growth and sustainable development. However, almost 1.3 billion people in the world still lack access to electricity and 2.7 billion lack access to clean cooking facilities. In this backdrop, the issue of energy access is receiving more interest than ever before and this has brought to the fore, the need for a robust decision support tool for policy makers to measure the progress of energy access provision and also to provide direction for future policy making. The paper studies existing definitions of energy access and identifies the key requirements for an appropriate decision-making tool to measure and monitor energy access provision. In this context the paper assesses the strengths and weaknesses of the metrics currently being used to measure energy access in policy, as well as of contemporary monitoring and evaluation frameworks being used in other sectors. Based on these insights, a dashboard of indicators is proposed as an alternate decision support tool for policy makers to measure energy access. The paper concludes with a discussion on what is needed to operationalise this proposed framework. - Highlights: ► No one indicator or metric can successfully capture progress on energy access. ► A service oriented approach is necessary to measure energy access. ► Socio-economic and political contexts influence success of energy access policies.

Patients' and observers' perceptions of involvement differ. Validation study on inter-relating measures for shared decision making.

Directory of Open Access Journals (Sweden)

Jürgen Kasper

Full Text Available OBJECTIVE: Patient involvement into medical decisions as conceived in the shared decision making method (SDM is essential in evidence based medicine. However, it is not conclusively evident how best to define, realize and evaluate involvement to enable patients making informed choices. We aimed at investigating the ability of four measures to indicate patient involvement. While use and reporting of these instruments might imply wide overlap regarding the addressed constructs this assumption seems questionable with respect to the diversity of the perspectives from which the assessments are administered. METHODS: The study investigated a nested cohort (N = 79 of a randomized trial evaluating a patient decision aid on immunotherapy for multiple sclerosis. Convergent validities were calculated between observer ratings of videotaped physician-patient consultations (OPTION and patients' perceptions of the communication (Shared Decision Making Questionnaire, Control Preference Scale & Decisional Conflict Scale. RESULTS: OPTION reliability was high to excellent. Communication performance was low according to OPTION and high according to the three patient administered measures. No correlations were found between observer and patient judges, neither for means nor for single items. Patient report measures showed some moderate correlations. CONCLUSION: Existing SDM measures do not refer to a single construct. A gold standard is missing to decide whether any of these measures has the potential to indicate patient involvement. PRACTICE IMPLICATIONS: Pronounced heterogeneity of the underpinning constructs implies difficulties regarding the interpretation of existing evidence on the efficacy of SDM. Consideration of communication theory and basic definitions of SDM would recommend an inter-subjective focus of measurement. TRIAL REGISTRATION: Controlled-Trials.com ISRCTN25267500.

Patients' and observers' perceptions of involvement differ. Validation study on inter-relating measures for shared decision making.

Science.gov (United States)

Kasper, Jürgen; Heesen, Christoph; Köpke, Sascha; Fulcher, Gary; Geiger, Friedemann

2011-01-01

Patient involvement into medical decisions as conceived in the shared decision making method (SDM) is essential in evidence based medicine. However, it is not conclusively evident how best to define, realize and evaluate involvement to enable patients making informed choices. We aimed at investigating the ability of four measures to indicate patient involvement. While use and reporting of these instruments might imply wide overlap regarding the addressed constructs this assumption seems questionable with respect to the diversity of the perspectives from which the assessments are administered. The study investigated a nested cohort (N = 79) of a randomized trial evaluating a patient decision aid on immunotherapy for multiple sclerosis. Convergent validities were calculated between observer ratings of videotaped physician-patient consultations (OPTION) and patients' perceptions of the communication (Shared Decision Making Questionnaire, Control Preference Scale & Decisional Conflict Scale). OPTION reliability was high to excellent. Communication performance was low according to OPTION and high according to the three patient administered measures. No correlations were found between observer and patient judges, neither for means nor for single items. Patient report measures showed some moderate correlations. Existing SDM measures do not refer to a single construct. A gold standard is missing to decide whether any of these measures has the potential to indicate patient involvement. Pronounced heterogeneity of the underpinning constructs implies difficulties regarding the interpretation of existing evidence on the efficacy of SDM. Consideration of communication theory and basic definitions of SDM would recommend an inter-subjective focus of measurement. Controlled-Trials.com ISRCTN25267500.

The making of pressure measurement device on heating-02 based realtime

International Nuclear Information System (INIS)

Giarno; Kussigit Santosa; Agus Nur Rachman; G B Heru K

2013-01-01

In order to modify the installation strand BETA Test Section Test integrated with heating-02 into a closed loop, it would require an additional system that can measure pressure changes in the closed-loop system. By making the measurement device to test the system pressure at the heating-expected 02 researchers can monitor the pressure changes that occur in the system. The pressure gauge device fabrication using manufacturing simulation methodology, the preparation of the hardware and software and test functions. Manufacturing simulation using measuring devices HIOKI DC current source Signal Source, preparation of pressure measurement devices require hardware such as pressure transducers, NI cRIO-9074, NI 9203 analog module, Computer and software LabVIEW 2011 as programming. In the test process function method is used to provide flow simulation module that is connected to the 9203 NI NI cRIO-9074. Current provision tailored to the specifics pressure transducer is 4 mA s/d 20 mA. Based on the test results obtained function value of the lowest current is 4.00 mA = 0.001 bar, and the highest current value of 20.00 mA = 4995 bar. From the results of calculations using the linear equations obtained correlation coefficient (R 2 ) of 0.999, so it is evident that the pressure changes in LabVIEW is affected by changes in flow. The results obtained from this activity is a device that can measure the pressure in the heating-02 test. (author)

Spectrophotometric Determination of Metoprolol Tartrate in Pharmaceutical Dosage Forms on Complex Formation with Cu(II

Directory of Open Access Journals (Sweden)

Mustafa Cesme

2011-06-01

Full Text Available A new, simple, sensitive and accurate spectrophotometric method has been developed for the assay of metoprolol tartrate (MPT, which is based on the complexation of drug with copper(II [Cu(II] at pH 6.0, using Britton-Robinson buffer solution, to produce a blue adduct. The latter has a maximum absorbance at 675 nm and obeys Beer’s law within the concentration range 8.5-70 mg/mL. Regression analysis of the calibration data showed a good correlation coefficient (r = 0.998 with a limit of detection of 5.56 mg/mL. The proposed procedure has been successfully applied to the determination of this drug in its tablets. In addition, the spectral data and stability constant for the binuclear copper(II complex of MPT (Cu2MPT2Cl2 have been reported.

Spectrophotometric determination of zirconium with Chrome Azurol s in aqueous streams of nuclear fuel reprocessing

International Nuclear Information System (INIS)

Ganesh, S.; Velavendan, P.; Pandey, N.K.; Kamachi Mudali, U.; Natarajan, R.

2014-01-01

A sensitive and reproducible spectrophotometric method for the determination of zirconium is developed. The method is based on the formation of stable bluish violet colour complex with Chrome Azurol S (CAS) with maximum absorption at 598 nm. The complex formed obeys Beer's law in the range of 1-7 μg/mL. Under optimum conditions, the sensitivity of the proposed method, (i.e. the detection limit), molar absorptivity and Sandell's sensitivity values are 2.42 μg/mL, 3.93 x10 3 L.Mol -1 .cm -1 and 2.54 x 10 -4 μg/cm 2 respectively. Relative standard deviation is less than 2% and correlation coefficient is 0.997. The present method is highly sensitive, selective, rapid and simple. It can be applied for the direct determination of zirconium in environmental, industrial, water and nuclear reprocessing samples. (author)