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Sample records for injection spectrophotometric determination

  1. 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...

  2. Sequential injection spectrophotometric determination of V(V) in ...

    African Journals Online (AJOL)

    2009-01-15

    Jan 15, 2009 ... The determination was based on the oxidation of dopamine (DP) by V(V) in acidic medium followed by ... To overcome some of these drawbacks some flow injec- ..... The analytical signal increased with the reactor length.

  3. 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...

  4. Spectrophotometric flow injection catalytic determination of molybdenum in plant digest using ion exchange resin

    International Nuclear Information System (INIS)

    Pessenda, L.C.R.

    1987-03-01

    A spectrophotometric flow injection analytical method based on the catalytic action of molybdenum on the oxidation of iodide by hydrogen peroxide in acidic medium is proposed for the molybdenum determination in plant digests. A cation exchange resin column is incorporated into a flow injection system for removal of interferents. The following system variables were investigated and optimized: reagent concentrations, sample injection volume, mixing and reaction coil lengths, temperature, sampling time, pumping rate and concentration of eluting agents. The effects of interfering species and of the acidity of samples on the molybdenum retention by the ion exchange resin column were investigated. The proposed method is characterized by good precision (r.s.d. (2.0%), a sampling rate of about 40 samples per hour, and permits the determination of molybdenum in plant digests in the range 1.0 to 40.0 μg/l. The results compare well with those obtained by graphite furnace atomic absorption spectrometry. (author) [pt

  5. 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

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

    Directory of Open Access Journals (Sweden)

    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.

  7. 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)

  8. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  10. 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)

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

    International Nuclear Information System (INIS)

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

    2011-01-01

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

  12. 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)

  13. CATALYTIC KINETIC SPECTROPHOTOMETRIC DETERMINATION ...

    African Journals Online (AJOL)

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    acetylchlorophosphonazo(CPApA) by hydrogen peroxide in 0.10 M phosphoric acid. A novel catalytic kinetic-spectrophotometric method is proposed for the determination of copper based on this principle. Copper(II) can be determined spectrophotometrically ...

  14. 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

  15. Spectrophotometric Determination of Ezetimibe

    Directory of Open Access Journals (Sweden)

    P. Baby Sudha Lakshmi

    2010-01-01

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

  16. Determination of uranium in organic phase by flow injection spectrophotometric analysis

    International Nuclear Information System (INIS)

    Yu Yiyun

    1998-01-01

    Based on the use of merging zone circuit and simulating a series of standard solution of uranium in organic phase, uranium in unknown organic phase sample was determined by flow injection spectrophotometry. A linear calibration graph was obtained with correlation coefficient of 0.999 for uranium concentration in organic phase over 10∼200 mg/L. Isopropyl alcohol was used as carrier solution. Mixing colour solution contains isopropyl alcohol, triethanolamine, masking reagent and Br-PADAP. The relative standard deviation of the method was better than +-5%. Determination of each sample can be completed in one minute. The method characteristic is: (1) using merging zone and simulating standard solution of uranium in organic phase, the method is sensitive and reliable; (2) even if the determined solution was in turbid condition, it can be quantitatively determined; (3) by means of solution replace technique, the tube of peristaltic pump can be used over a long period of time

  17. Flow injection spectrophotometric determination of low concentrations of orthosphate in natural waters employing ion exchange resin

    International Nuclear Information System (INIS)

    Pessenda, L.C.R.

    1981-01-01

    A simple and fast method for the determination of low concentrations of orthophosphate in natural waters is described. Ion exchange is incorporated into a flow injection system by usina a resin column in the sample loop of a proportion injector. Effects of sample aspiration rate, sampling time, eluting agent concentration, pumping rate of the sample carrier stream and interfaces, were investigated both using 32 PO 3- 4 or 31 PO 3- 4 with columns coupled to a gerger-muller detector and incorporated in a flow system with molybdenum blue colorinetry. (M.A.C.) [pt

  18. Reverse flow injection spectrophotometric determination of ciprofloxacin in pharmaceuticals using iron from soil as a green reagent

    Science.gov (United States)

    Palamy, Sysay; Ruengsitagoon, Wirat

    2018-02-01

    A novel reverse flow injection spectrophotometric method for the determination of ciprofloxacin was successfully combined with the on-line introduction of an iron solution extracted from soil as green reagent. The assay was optimized by a univariate method to select the optimum conditions for the highest absorbance and highest stability of the complex. Beer-Lambert's law (λmax = 440 nm) is obeyed in the range 0.5-50 μg mL- 1 with a correlation coefficient (r2) of 0.9976 and 0.9996 using soil as green reagent from Khon Kaen, Thailand and Vientiane, Laos, respectively. The average percentage recoveries were in the range of 98.55-102.14% and the precision was in the range of 0.80-1.73%. The limit of detection and the limit of quantitation were 0.20 and 0.69 μg mL- 1, respectively, with a sampling rate of over 46 samples h- 1. The method was successfully applied to the determination of ciprofloxacin in commercial pharmaceutical formulations. The results were in good agreement with those obtained by the reference HPLC method using a t-test at 95% of confidence level for comparison. This method is suitable for laboratories looking for alternative analytical methods using green reagents.

  19. Spectrophotometric flow-injection determination of sulphite in white wines involving gas diffusion through a concentric tubular membrane

    Directory of Open Access Journals (Sweden)

    Melo Denise

    2003-01-01

    Full Text Available A flow-injection system is proposed for the spectrophotometric determination of sulphite in white wines. The method involves analyte conversion to SO2, gas diffusion through a Teflon® semi-permeable membrane, collection into an alkaline stream (pH 8, reaction with Malachite green (MG and monitoring at 620 nm. With a concentric tubular membrane, the system design was simplified. Influence of reagent concentrations, pH of donor and acceptor streams, temperature, timing, surfactant addition and presence of potential interfering species of the wine matrix were investigated. A pronounced (ca. 100% enhancement in sensitivity was noted by adding cetylpyridinium chloride (CPC. The proposed system is robust and baseline drift is not observed during 4 h operating periods. Only 400 muL of sample and 0.32 mg MG are required per determination. The system handles 30 samples per hour, yielding precise results (r.s.d. < 0.015 for 1.0 - 20.0 mg L-1 SO2 in agreement with those obtained by an alternative procedure.

  20. 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.

  1. 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

  2. Flow injection spectrophotometric determination of Fe(III) and V(v)

    International Nuclear Information System (INIS)

    Elrahman, Azza Mohamed

    2000-01-01

    Phenylflourone was synthesized with the objective of developing a method for determining Fe(III) and V(V) in the pressence of micelles using flow injectoin technique. Phenylflourone showed a wavelength of maximum absorption at 412 nm which was not affected by the presence of miccelles i.e. n-hexadodecylpyridinum bromide and sodium n-dodecylsulphate, but they have different effects on the absorbance of PHF. The example of PHF-Fe(III) and PHF-V(V) showed the wavelength of the maximum absorption at 4428 nm and 412 nm, respectively. Presence of micelles shifted the wavelength of the two complexes to a lower one. Generally the addition of micelles increased the absorbance of phenylflourone metal ions complexes except for PHF-V(V) with hexadodecylpyridinum bromide. With flow injection technique two approaches were practiced the use of micelle as a carrier or water as a carrier. Sodium n-dodecylsulphate increased the absorbance of the two complexes when it was used as a carrier or added to the metal ions using water as carrier. On the other hand, the use of n-hexadodecylpyridinum bromide as carrieer increased the absorbance of the complexes but it decreased the absorbance when it was used in conjunction with metal ions and water as a carrier. After establishing the optimum FI conditions for PHF-Fe(III) and PHF-V(V) complexes, the calibration curves were construction and produced semiliner response in the concentration range studied. Ti(IV) III, Mo(VI) showed a positive interference in PHF-Fe(III) and PHF-V(V) complexes, respectively.(Author)

  3. Flow-Injection Solid Phase Partial Least-Squares Spectrophotometric Simultaneous Determination of Iron, Nickel and Zinc

    Directory of Open Access Journals (Sweden)

    Teixeira Leonardo S. G.

    2002-01-01

    Full Text Available A PLS-2 multivariate calibration method has been developed for the simultaneous determination of iron, nickel and zinc in ternary mixtures by solid phase spectrophotometry associated with flow injection analysis. Fe(II, Ni(II and Zn(II form color complexes with 1-(2-thiazolylazo-2-naphthol (TAN, immobilized on a C18 bonded silica support, at pH 6.4. The proposed procedure is based on the different reaction/retention ratios of the studied ions on the solid support. Bilinear spectrophotometric data of the analytes, fixed in the solid support, were recorded in the 400-800 nm wavelength range as a function of time and a partial least squares (PLS-2 algorithm was used to predict results of synthetic samples. The calibration set employed was integrated by 8 ternary mixture standards and a blank solution. Mixtures containing 0.040 to 0.20 mg L-1, of each species, were successfully resolved, using 3 factors for each analyte and a restricted number of absorbance data obtained in the wavelength range from 560 to 650 nm.

  4. Flow injection on-line spectrophotometric determination of thorium(IV) after preconcentration on XAD-4 resin impregnated with oxytetracycline

    Energy Technology Data Exchange (ETDEWEB)

    Shahida, Shabnam; Khan, Muhammad Haleem [Univ. of Azad Jammu and Kashmir, Muzaffarabad (Pakistan). Dept. of Chemistry; Ali, Akbar [Pakistan Institute of Nuclear Science and Technology, Islamabad (Pakistan). Chemistry Div.

    2014-02-15

    A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L{sup -1} levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min{sup -1}. The trapped complex was then eluted with 3.6 mol L{sup -1} HCl at a flow rate of 4.9 mL min{sup -1}. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L{sup -1} HCl stabilized with 1 % triton X-100, 4.9 mL min{sup -1}) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h{sup -1}, the enhancement factor was 97, the detection limit was 0.25 μg L{sup -1}, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L{sup -1}), whereas for 300 s of the preconcentration time and a sample frequency of 10 h{sup -1}, the enhancement factor of 357, the detection limit (3s) of 0.069 μg L{sup -1} and the precision of 1.32 % (at 10 μg L{sup -1}) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.

  5. Flow injection on-line spectrophotometric determination of thorium(IV) after preconcentration on XAD-4 resin impregnated with oxytetracycline

    International Nuclear Information System (INIS)

    Shahida, Shabnam; Khan, Muhammad Haleem; Ali, Akbar

    2014-01-01

    A very sensitive, selective and simple flow injection time-based method was developed for on-line preconcentration and determination of thorium(IV) at micro g L"-"1 levels in environmental samples. The system operation was based on thorium(IV) ion retention at pH 4.0 in the minicolumn at a flow rate of 15.2 mL min"-"1. The trapped complex was then eluted with 3.6 mol L"-"1 HCl at a flow rate of 4.9 mL min"-"1. The amount of thorium(IV) in the eluate was measured spectrophotometrically at 651 nm using arsenazo-III solution (0.05 % in 3.6 mol L"-"1 HCl stabilized with 1 % triton X-100, 4.9 mL min"-"1) as colorimetric reagent. All chemical, and flow injection variables were optimized for the quantitative preconcentration of metal and a study of interference level of various ions was also carried out. The system offered low backpressure and improved sensitivity and selectivity. At a preconcentration time of 60 s and a sample frequency of 40 h"-"1, the enhancement factor was 97, the detection limit was 0.25 μg L"-"1, and the precision expressed as relative standard deviation was 1.08 % (at 50 μg L"-"1), whereas for 300 s of the preconcentration time and a sample frequency of 10 h"-"1, the enhancement factor of 357, the detection limit (3s) of 0.069 μg L"-"1 and the precision of 1.32 % (at 10 μg L"-"1) was reported. The accuracy of the developed method was sufficient and evaluated by the analysis of certified reference material IAEA-SL-1 (Lake Sediment) and spiked water samples.

  6. 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.

  7. Flow injection determination of metronidazole through spectrophotometric measurement of the nitrite ion produced upon alkaline hydrolysis

    Directory of Open Access Journals (Sweden)

    Simões Simone S.

    2006-01-01

    Full Text Available A new method for metronidazole determination, based on spectrometric monitoring of a diazonium salt produced in-line by alkaline hydrolysis released nitrite ions, was developed and successfully applied to pharmaceutical tablets (r = 0.9993, 2.0-20.0 mg L-1, DL = 0.7 mg L-1 with no interference from common ingredients accompanying the drug.

  8. 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

  9. Rapid determination of chromium(VI) in electroplating waste water by use of a spectrophotometric flow injection system.

    Science.gov (United States)

    Yuan, Dong; Fu, Dayou; Wang, Rong; Yuan, Jigang

    2008-11-01

    A new rapid and sensitive FI method is reported for spectrophotometric determination of trace chromium(VI) in electroplating waste water. The method is based on the reaction of Cr(VI) with sodium diphenylamine sulfonate (DPH) in acidic medium to form a purple complex (lambda(max) = 550 nm). Under the optimized conditions, the calibration curve is linear in the range 0.04-3.8 microg ml(-1) at a sampling rate of 30 h(-1). The detection limit of the method is 0.0217 microg ml(-1), and the relative standard deviation is 1.1% for eight determinations of 2 microg ml(-1) Cr(VI). The proposed method was applied to the determination of chromium in electroplating waste water with satisfactory results.

  10. 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 ...

  11. 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 ...

  12. 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 ...

  13. 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.

  14. 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.

  15. 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.

  16. One-shot flow injection spectrophotometric simultaneous determination of copper, iron and zinc in patients' sera with newly developed multi-compartment flow cell

    International Nuclear Information System (INIS)

    Teshima, Norio; Gotoh, Shingo; Ida, Kazunori; Sakai, Tadao

    2006-01-01

    We propose here an affordable flow injection method for simultaneous spectrophotometric determination of copper, iron and zinc in patients' sera. The use of a newly designed multi-compartment flow cell allowed the simultaneous determination of the three metals with a single injection ('one-shot') and a double beam spectrophotometer. The chemistry relied on the reactions of these metals with 2-(5-nitro-2-pyridylazo)-5-[N-propyl-N-(3-sulfopropyl)amino]phenol (nitro-PAPS) to form corresponding colored complexes. At pH 3.8, only copper-nitro-PAPS complex was formed in the presence of pyrophosphate as a masking agent for iron, and then the copper and iron(II) complexes were formed in the presence of reductant (ascorbic acid) at the same pH, and finally all three metals reacted with nitro-PAPS at pH 8.6. The characteristics were introduced into the flow system to determine each metal selectively and sensitively. Under the optimum conditions, linear calibration curves for the three metals were obtained in the range of 0.01-1 mg L -1 with a sample throughput rate of 20 h -1 . The limits of detection (3σ) were 3.9 μg L -1 for copper, 4.1 μg L -1 for iron and 4.0 μg L -1 for zinc. The proposed method was applied to analysis of some patients' sera

  17. 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)

  18. Simultaneous Spectrophotometric Determination of Valsartan and ...

    African Journals Online (AJOL)

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

  19. 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 ...

  20. 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 ...

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

    International Nuclear Information System (INIS)

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

    2005-01-01

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

  2. 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...

  3. 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

  4. 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 ...

  5. 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.

  6. Spectrophotometric determination of copper with ascorbic acid

    Energy Technology Data Exchange (ETDEWEB)

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

    1996-06-01

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

  7. Spectrophotometric Determination of Nitrate in Vegetables Using ...

    African Journals Online (AJOL)

    DR. MIKE HORSFALL

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

  8. Spectrophotometric determination of copper with ascorbic acid

    International Nuclear Information System (INIS)

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

    1996-01-01

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

  9. 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 ...

  10. 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

  11. 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 ...

  12. 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), ...

  13. 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.

  14. 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

  15. Uranium hexafluoride. Bromine spectrophotometric determination

    International Nuclear Information System (INIS)

    Anon.

    Bromine determination in hydrolized uranium hexafluoride by reduction of bromates by ferrous sulfate, oxidation of bromides by potassium permanganate to give bromine which is extracted into carbon tetrachloride and transformed in eosine for spectrophotometry at 510 nm. The method is suitable for determining 5 to 150 ppm with respect to uranium [fr

  16. 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

  17. 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

  18. 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)

  19. 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 %.

  20. 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.

  1. Flow-injection spectrophotometric determination of captopril in pharmaceutical formulations using a new solid-phase reactor containing AgSCN immobilized in a polyurethane resin

    Directory of Open Access Journals (Sweden)

    Fernando Campanhã Vicentini

    2012-06-01

    Full Text Available A simple flow-injection analysis procedure was developed for determining captopril in pharmaceutical formulations employing a novel solid-phase reactor containing silver thiocyanate immobilized in a castor oil derivative polyurethane resin. The method was based on silver mercaptide formation between the captopril and Ag(I in the solid-phase reactor. During such a reaction, the SCN- anion was released and reacted with Fe3+, which generated the FeSCN2+ complex that was continuously monitored at 480 nm. The analytical curve was linear in the captopril concentration range from 3.0 × 10-4 mol L-1 to 1.1 × 10-3 mol L-1 with a detection limit of 8.0 × 10-5 mol L-1. Recoveries between 97.5% and 103% and a relative standard deviation of 2% for a solution containing 6.0 × 10-4 mol L-1 captopril (n = 12 were obtained. The sample throughput was 40 h-1 and the results obtained for captopril in pharmaceutical formulations using this procedure and those obtained using a pharmacopoeia procedure were in agreement at a 95% confidence level.Um procedimento simples de análise por injeção em fluxo foi desenvolvido para a determinação de captopril em formulações farmacêuticas empregando um novo reator em fase sólida contendo tiocianato de prata imobilizado em resina poliuretana obtida a partir de óleo de mamona. O método foi baseado na formação de um mercapto composto de prata, no reator em fase sólida, obtido entre o captopril e Ag (I imobilizada. Durante a reação, íons SCN- eram liberados e reagiam com Fe3+, gerando o complexo FeSCN2+, que foi continuamente monitorado em 480 nm. A curva analítica foi linear no intervalo de concentração de captopril entre 3,0 × 10-4 a 1,1 × 10-3 mol L-1 com um limite de detecção de 8,0 × 10-5 mol L-1. Recuperações entre 97,5-103% e desvio padrão relativo de 2% para uma solução contendo 6,0 × 10-4 mol L-1 de captopril (n = 12 foram obtidos. A frequência de amostragem foi de 40 h-1 e os resultados

  2. 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 ...

  3. Application of hydrocyanic acid vapor generation via focused microwave radiation to the preparation of industrial effluent samples prior to free and total cyanide determinations by spectrophotometric flow injection analysis.

    Science.gov (United States)

    Quaresma, Maria Cristina Baptista; de Carvalho, Maria de Fátima Batista; Meirelles, Francis Assis; Santiago, Vânia Maria Junqueira; Santelli, Ricardo Erthal

    2007-02-01

    A sample preparation procedure for the quantitative determination of free and total cyanides in industrial effluents has been developed that involves hydrocyanic acid vapor generation via focused microwave radiation. Hydrocyanic acid vapor was generated from free cyanides using only 5 min of irradiation time (90 W power) and a purge time of 5 min. The HCN generated was absorbed into an accepting NaOH solution using very simple glassware apparatus that was appropriate for the microwave oven cavity. After that, the cyanide concentration was determined within 90 s using a well-known spectrophotometric flow injection analysis system. Total cyanide analysis required 15 min irradiation time (90 W power), as well as chemical conditions such as the presence of EDTA-acetate buffer solution or ascorbic acid, depending on the effluent to be analyzed (petroleum refinery or electroplating effluents, respectively). The detection limit was 0.018 mg CN l(-1) (quantification limit of 0.05 mg CN l(-1)), and the measured RSD was better than 8% for ten independent analyses of effluent samples (1.4 mg l(-1) cyanide). The accuracy of the procedure was assessed via analyte spiking (with free and complex cyanides) and by performing an independent sample analysis based on the standard methodology recommended by the APHA for comparison. The sample preparation procedure takes only 10 min for free and 20 min for total cyanide, making this procedure much faster than traditional methodologies (conventional heating and distillation), which are time-consuming (they require at least 1 h). Samples from oil (sour and stripping tower bottom waters) and electroplating effluents were analyzed successfully.

  4. Flow Injection Spectrophotometric Determination of Glyphosate ...

    African Journals Online (AJOL)

    NICOLAAS

    limits and causes digestive tract irritation, eyes and skin irrita- tion, low blood ... techniques, mostly chromatographic, have been developed for ... enhanced photochemically induced fluorescence (MEPIF) .... with glyphosate on the same field or in the nearby fields. .... At 700 µL sample volume two peaks near to each.

  5. 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.

  6. Determinação espectrofotométrica de vitamina B2 (riboflavina) em formulações farmacêuticas empregando sistema de análises por injeção em fluxo Spectrophotometric determination of vitamin B2 (riboflavin) in pharmaceutical formulations using flow injection analysis

    OpenAIRE

    Clezio Aniceto; Larissa de Souza Canaes; Orlando Fatibello-Filho; Carla C. S. Cavalheiro

    2000-01-01

    A flow injection spectrophotometric procedure exploiting merging zones is proposed for determining vitamin B2 (riboflavin) in pharmaceutical preparations. The determination is based on the red-colored complex formation between vitamin B2 and silver(I) which was measured at 520 nm. Vitamin B2 was determined in four pharmaceutical preparations in the 1.0 to 50.0 mg L-1 concentration range, with a detection limit of 0.5 mg L-1. The recovery from three samples ranged from 98.0 to 104.0 %. The ana...

  7. Determination of loratadine in pharmaceuticals by a spectrophotometric method

    Directory of Open Access Journals (Sweden)

    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.

  8. 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 ...

  9. 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 ...

  10. 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)

  11. 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 ...

  12. 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)

  13. 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.

  14. 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

  15. 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...

  16. Enzymatic spectrophotometric reaction rate determination of aspartame

    Directory of Open Access Journals (Sweden)

    Trifković Kata T.

    2015-01-01

    Full Text Available Aspartame is an artificial sweetener of low caloric value (approximately 200 times sweeter than sucrose. Aspartame is currently permitted for use in food and beverage production in more than 90 countries. The application of aspartame in food products requires development of rapid, inexpensive and accurate method for its determination. The new assay for determination of aspartame was based on set of reactions that are catalyzed by three different enzymes: α-chymotrypsin, alcohol oxidase and horseradish peroxidase. Optimization of the proposed method was carried out for: (i α-chymotrypsin activity; (ii time allowed for α-chymotrypsin action, (iii temperature. Evaluation of the developed method was done by determining aspartame content in “diet” drinks, as well as in artificial sweetener pills. [Projekat Ministarstva nauke Republike Srbije, br. III46010

  17. Magnesium analysis. Spectrophotometric determination of chromium

    International Nuclear Information System (INIS)

    Anon.

    Chromium determination in magnesium used in uranium fabrication by magnesiothermics, applicable for chromium content between 2 to 10 ppm. Magnesium is dissolved in sulfuric acid, oxidized by potassium permanganate, the excess of permanganate is eliminated by sodium nitride. Spectrophotometry at 540 nm of the chromium (VI)-diphenylcarbazide complex [fr

  18. Spectrophotometric Determination of Nitrate and Phosphate Levels ...

    African Journals Online (AJOL)

    MBI

    2013-04-09

    Apr 9, 2013 ... may help in the growth of algae (Beavington,. 1977). Determination of phosphate ion in drinking water. 50cm3 of water sample was pipetted into a 500cm3 volumetric flask, 5cm3 of Ammonium molybdate solution and 3.0cm3 of ascorbic acid were added with swirling, the mixture was diluted to the mark with ...

  19. Spectrophotometric determination of chromium in geological samples

    International Nuclear Information System (INIS)

    Rathore, D.P.S.; Tarafder, P.K.

    1992-01-01

    A method for the determination of chromium is presented, based on the oxidation of hydroxylamine hydrochloride to nitrous acid by chromium(VI) in acetic acid medium followed by diazotization of the nitrite produced with p-aminophenylmercaptoacetic acid and subsequent coupling of the diazonium salt with N-(1-naphthyl)ethylenediamine di-hydrochloride in acidic medium to form a stable blueish azo dye. The method is suitable for the determination of chromium(VI) from 0.04 to 1.2 mg l -1 in a 1.0-cm cuvette. The molar absorptivity and Sandell's sensitivity are 3.65x10 4 l mol -1 cm -1 and 0.0014μg cm -2 , respectively. (author). 17 refs.; 3 figs

  20. Spectrophotometric determination of zinc in impure solutions

    International Nuclear Information System (INIS)

    Rodriguez Hernandez, B.; Reyes Tamaral, A.

    1972-01-01

    A dithizone colorimetric method is described for determining zinc concentrations of 0.001 to 5 g/l in aqueous solutions from Rio Tinto Mines, containing copper, iron and other impurities. Citrate, cyanide and bis-2hydroxyethyl)-dithiocarbamate are added to the aqueous sample of masking several metals, and zinc is extracted at pH 5 with a solution of dithizone in carbon tetrachloride. Excess of dithizone is removed with sodium sulphide, and optical density of zinc dithionate in organic solution is measured at 5.35 nm. Calibration curves obey Beer's law up to 0.5 micro Zn/ml. (Author) 5 refs

  1. 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)

  2. Spectrophotometric determination of caffeine using polyaniline films

    International Nuclear Information System (INIS)

    Monlinong, Jason Paul C.; Portilla, Ma. Cristina B.; Agustin, Katrina Jane D.; Pascual, Cherrie B.

    2015-01-01

    Polyaniline (PANI) films were fabricated by chemical oxidative polymerization of aniline monomers using ammonium persulfate (APS). The effects of varying oxidant concentration, oxidant solvent and washing solution in the PANI film deposition were first evaluated. 0.250 M APS in 0.200 M HCl and 0.200 M aniline in 0.200 M HCl were used to produce the emeraldine PANI (green) films which were deposited onto commercially available acctate films. The fabricated PANI film acts as an optical sensor baed on its redox-dependent switching of polyaniline from emeraldine (green) to pernigranilline (blue) form. The change in absorbance of blue PANI films immerse in caffeine-containing solution vs green fabricated PANI films were utilized in analysis of caffeine at 829 nm using a UV-VIS spectrophotometer. Repeatable results were obtained in intra-branch and inter-branch repeatability studies, with coefficient of variation (CV) values ranging rom 9.8-13.9% and 5.1-14.5%, respectively. Linear response was obtained over the concentration of 10.0-50.0 μg/mL. The limit of detection (LOD) and limit of quantitation (LOQ) were determined to be 2.5 and 8.5μg/mL, respectively. The obtained % recovery values of caffeine spiked in aqueous solution ranged from 84.9-107%. Three pharmaceutical formulations containing 20.0 or 25.0 μg/Ml caffeine where analyzed using PANI films by external calibration method. The obtained average caffeine values were 25.2 mg/tablet, 22.4 mg/tablet and 15.4 mg/capsule for Fevadol®, Fevergan® and Alaxan®FR, respectively. These values were 77.0% to 101% of the label claims. Human urine samples spiked with caffeine were also analyzed, after sample pre-treatment. Obtained percent recovery values ranged from 79.1 to 105%. This method demonstrated the potential of laboratory-fabricated PANI films as a low-cost rapid, reliable, simple and accurate method for caffeine quantification in pharmaceutical and clinical specimens. (author)

  3. 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

  4. 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.

  5. 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

  6. 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 %.

  7. 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 %

  8. 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

  9. Kinetic Spectrophotometric Determination of Certain Cephalosporins in Pharmaceutical Formulations

    Directory of Open Access Journals (Sweden)

    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.

  10. 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.

  11. 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.

  12. 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.

  13. 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

  14. 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.

  15. 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)

  16. 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.

  17. 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.

  18. 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 +/).

  19. 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)

  20. 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

  1. Determination of lisinopril in pharmaceuticals by a kinetic spectrophotometric method

    Directory of Open Access Journals (Sweden)

    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.

  2. 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.

  3. 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.

  4. Spectrophotometric determination of the sulfhydryl containing drug mesna

    Directory of Open Access Journals (Sweden)

    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.

  5. THE SPECTROPHOTOMETRIC DETERMINATION OF NITRITES WITH N,N-DIETHYLANILINE

    Directory of Open Access Journals (Sweden)

    O. S. Pogrebnyak

    2015-11-01

    Full Text Available A new spectrophotometric method for nitrite determination was proposed. The method is based on the measurement of absorbance of the N,N-diethylaniline nitrosation product at 475 nm in the hydrochloric acid medium. The optimum concentrations and the influence of various conditions on the determination sensitivity have been determined. The detection limit (blank + 3s for nitrite is 0.98 mg∙L–1 where sis the standard deviation of blank estimation. The linearity range of the calibration graph was over 1.0–100 mg∙L–1 of  nitrite (sr≤ 0.029, n = 8. The metrological characteristics of the procedure were checked by means of method of additives on the control samples and natural waters. The relative error did not exceed 0.06 for nitrite determination on the control samples. The effect of foreign ions in nitrite determination of 1,0∙10−3 mol∙L–1 has been studied. The proposed procedure is simple  and suitable for nitrite determination in various objects.

  6. 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)

  7. Spectrophotometric determination of total lactones in Andrographis paniculata Nees

    Directory of Open Access Journals (Sweden)

    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

  8. 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

  9. 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.)

  10. 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.

  11. 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)

  12. 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 ...

  13. 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)

  14. 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.

  15. 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%.

  16. 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.

  17. Spectrophotometric Determination of Lamivudine in Pure and Tablet Forms

    Directory of Open Access Journals (Sweden)

    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.

  18. Determinação espectrofotométrica de vitamina B2 (riboflavina em formulações farmacêuticas empregando sistema de análises por injeção em fluxo Spectrophotometric determination of vitamin B2 (riboflavin in pharmaceutical formulations using flow injection analysis

    Directory of Open Access Journals (Sweden)

    Clezio Aniceto

    2000-10-01

    Full Text Available A flow injection spectrophotometric procedure exploiting merging zones is proposed for determining vitamin B2 (riboflavin in pharmaceutical preparations. The determination is based on the red-colored complex formation between vitamin B2 and silver(I which was measured at 520 nm. Vitamin B2 was determined in four pharmaceutical preparations in the 1.0 to 50.0 mg L-1 concentration range, with a detection limit of 0.5 mg L-1. The recovery from three samples ranged from 98.0 to 104.0 %. The analytical frequency was 42 h-1 and r.s.d. were lower than 1% for solutions containing 10.0, 30.0 and 50.0 mg L-1 vitamin B2 (n= 10. The results obtained in commercial formulations using the FIA procedure were in good agreement with those obtained by using a conventional fluorimetric procedure (r=0.9998 and also with the label values (r= 0.9997.

  19. 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.

  20. 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...

  1. 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.

  2. 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...

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

    Directory of Open Access Journals (Sweden)

    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

  4. 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.

  5. 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)

  6. A Sensitive Validated Spectrophotometric Method for the Determination of Flucloxacillin Sodium

    Directory of Open Access Journals (Sweden)

    R. Singh Gujral

    2009-01-01

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

  7. 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.

  8. 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)

  9. 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)

  10. Extractive Spectrophotometric Methods for the Determination of Etoricoxib in Tablets

    Directory of Open Access Journals (Sweden)

    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.

  11. 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)

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

    Directory of Open Access Journals (Sweden)

    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.

  13. 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.

  14. 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)

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

    Directory of Open Access Journals (Sweden)

    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.

  16. 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

  17. Determination of uranium (IV) in cloride solutions of enrichment columns by spectrometry with flow injection

    International Nuclear Information System (INIS)

    Bastos, M.B.R.

    1988-01-01

    The utilization of Flow Injection Analysis for the U (IV) spectrophotometric determination in chloride solutions is described. The method has been shown reproducible in the range of concentrations and conditions employed with a standard deviation of about 0,3. (C.G.C.) [pt

  18. 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. ...

  19. 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.

  20. 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)

  1. 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)

  2. Optimized and validated flow-injection spectrophotometric analysis of topiramate, piracetam and levetiracetam in pharmaceutical formulations.

    Science.gov (United States)

    Hadad, Ghada M; Abdel-Salam, Randa A; Emara, Samy

    2011-12-01

    Application of a sensitive and rapid flow injection analysis (FIA) method for determination of topiramate, piracetam, and levetiracetam in pharmaceutical formulations has been investigated. The method is based on the reaction with ortho-phtalaldehyde and 2-mercaptoethanol in a basic buffer and measurement of absorbance at 295 nm under flow conditions. Variables affecting the determination such as sample injection volume, pH, ionic strength, reagent concentrations, flow rate of reagent and other FIA parameters were optimized to produce the most sensitive and reproducible results using a quarter-fraction factorial design, for five factors at two levels. Also, the method has been optimized and fully validated in terms of linearity and range, limit of detection and quantitation, precision, selectivity and accuracy. The method was successfully applied to the analysis of pharmaceutical preparations.

  3. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

  6. 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

  7. Sensitive spectrophotometric determination of metoclopramide hydrochloride in dosage forms and spiked human urine using vanillin

    Directory of Open Access Journals (Sweden)

    O. Zenita Devi

    2016-09-01

    Full Text Available A new spectrophotometric method which is simple, sensitive, selective and rapid is described for the determination of metoclopramide hydrochloride (MCP in bulk drug and in dosage forms using vanillin as the chromogenic agent. The method is based on the condensation reaction between primary aromatic amine group present in MCP with aromatic aldehyde, vanillin to produce an intense yellow colored product. The resulting Schiff’s base shows an absorption maximum at 410 nm and the reaction product is stable for more than one day. The reaction was carried out in acetic acid and perchloric acid medium. Beer’s law was obeyed in the concentration range 1.5–15.0 μg ml−1 MCP with a molar absorptivity of 1.89 × 104 l mol−1 cm−1. The limit of detection (LOD and limit of quantification (LOQ were found to be 0.51 and 1.55 μg ml−1, respectively. The method was statistically evaluated by calculating percent relative error (% RE for accuracy and percent relative standard deviation (% RSD for precision, and was applied successfully to the determination of MCP in tablets, in injection and also in spiked human urine. No interference was observed from common additives found in pharmaceutical preparations. The results obtained by the proposed method were validated statistically by comparing the results with those of the reference method by applying the Student’s t-test and F-test. The accuracy and reliability of the method were further ascertained by performing recovery tests via standard-addition technique.

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

    Directory of Open Access Journals (Sweden)

    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.

  9. 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)

  10. 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)

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

    Directory of Open Access Journals (Sweden)

    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

  12. 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)

  13. 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)

  14. 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.

  15. 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

  16. 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.)

  17. 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

  18. 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...

  19. 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.

  20. Spectrophotometric Determination of Carbon Disulphide in the Workplace Air

    Directory of Open Access Journals (Sweden)

    V. Pitschmann

    2013-01-01

    Full Text Available This papre describes a simple method of carbon disulphide determination in the air of working environment in the chemical companies and plants after its absorption into aprotic N,N-dimethylformamide solvent. Carbon disulphide absorbed into aprotic solvent was transformed by using ammonium hydroxide on sulphides which were determined by spectrophotometry. 5,5′-Dithiobis(2-nitrobenzoic acid and blue tetrazolium chloride were used as chromogenic sensing reagents. Colour-reducing products were measured at the wavelength of 500, respectively 520 nm. Detection limits for determination of carbon disulphide in the air are 0.2, respectively 0.4 mg·m−3.

  1. Spectrophotometric determination of silica in water with Hach equipment

    International Nuclear Information System (INIS)

    Acosta L, E.

    1992-06-01

    The 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 using the indicated technique in the operation manual of the Hach equipment with a DR/3 spectrophotometer is described. This method covers the determination of the silica element in the interval from 0 to 1.5 mg/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)

  2. New Spectrophotometric Methods for the Determination of p ...

    African Journals Online (AJOL)

    derivatizing reagents for the determination of p-aminosalicylic acid (PAS) in tablets. The derivatization was carried ... liquid chromatography (HPLC) [7,8], nuclear magnetic resonance ..... aminosalicylic acid and m-aminophenol by derivative.

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

    African Journals Online (AJOL)

    HP

    Purpose: To develop a simple and cost effective spectrophotometer method for the determination of. ACE inhibitor ramipril in dosage forms. Methods: UV spectrophotometry was used to develop and validate a simple method .... 2003 software.

  4. Spectrophotometric determination of tannins by phosphotungstic-phosphomolybdic reagent

    Energy Technology Data Exchange (ETDEWEB)

    Reicher, F; Sierakowski, M R; Correa, J B.C. [Parana Univ., Curitiba (Brazil). Dept. de Bioquimica

    1981-01-01

    There are several colorimetric techniques to determine tannins in plant extracts. One frequently used is the Folin method (phosphotungstic acid reagent) that procedures a blue color with phenolic compounds. However, this coloured complex is unstable. With the Folin-Ciocalteau reagent, used in protein determination (Lowry et al. J.B.C. 193: 265, 1951) good results were obtained, even in the absence of cooper solution. Using phosphotungstic-phosphomolybdic reagent (Folin-Denis), it was obtained maximum color with 1,0 ml of the reagent in 20 minutes, after the additon of 10 ml 20% sodium carbonate solution. Tannins samples containing 10 to 200 ..mu..g/ml were analysed. Absorbances are determined at 720 or 600 nm. Tannins of commercial preparations from Acacia negra were analysed by the phosphotungstic-phosphomolybdic reagent before (A) and after (B) treatment with chromate hyde powder. By this procedure hydrolysible tannins were determined (A-B).

  5. Spectrophotometric determination of tannins by phosphotungstic-phosphomolibdic reagent

    International Nuclear Information System (INIS)

    Reicher, F.; Sierakowski, M.R.; Correa, J.B.C.

    1981-01-01

    There are several colorimetric techniques to determine tannins in plant extracts. One frequently used is the Folin method (phosphotungstic acid reagent) that procedures a blue color with phenolic compounds. However, this coloured complex is unstable. With the Folin-Ciocalteau reagent, used in protein determination (Lowry et al. J.B.C. 193: 265, 1951) good results were obtained, even in the absence of cooper solution. Using phosphotungstic-phosphomolibdic reagent (Folin-Denis), it was obtained maximum color with 1,0 ml of the reagent in 20 minutes, after the adition of 10 ml 20% sodium carbonate solution. Tannins samples containing 10 to 200 μg/ml were analysed. Absorbances are determined at 720 or 600 nm. Tannins of commercial preparations from Acacia negra were analysed by the phosphotungstic-phosphomolibdic reagent before (A) and after (B) treatment with chromate hyde powder. By this procedure hydrolysible tannins were determined (A-B). (Author) [pt

  6. Spectrophotometric Determination of Boron in Environmental Water Samples

    International Nuclear Information System (INIS)

    San San; Khin Win Kyi; Kwaw Naing

    2002-02-01

    The present paper deals with the study on the methods for the determination of boron in the environmental water samples. The standard methods which are useful for this determination are discussed thoroughly in this work. Among the standard methods approved by American Public Health Association, the carmine method was selected for this study. Prior to the determination of boron in the water samples, the precision and accuracy of the methods of choice were examined by using standard boron solutions. The determination of Boron was carried out by using water samples, waste water from Aquaculture Research Centre, University of Yangon, the Ayeyarwady River water near Magway Myathalon Pagoda in Magway Division, ground water from Sanchaung Township, and tap water from Universities' Research Centre, University of Yangon. Analyses of these water samples were done and statistical treatment of the results was carried out. (author)

  7. Indirect Spectrophotometric Determination of Trace Quantities of Hydrazine

    Energy Technology Data Exchange (ETDEWEB)

    Shabani, A. M. Haji; Dadfarnia, S.; Dehghan, K. [Yazd University, Yazd (Iran, Islamic Republic of)

    2004-02-15

    An indirect, sensitive and accurate method for the determination of trace amounts of hydrazine is described. The method is based on the oxidation of hydrazine by a known excess of iodate in the presence of hydrochloric acid. The unreacted iodate is used in the oxidation of hydroxylamine to nitrite. Sulfanilic acid is diazotized by the nitrite formed. The resulting diazonium ion is coupled with N-(1-naphthyl)ethylenediamine to form a stable azo dye, which shows an absorption maximum at 540 nm. Hydrazine can be determined in the range of 20-400 ng mL{sup -1} with a detection limit of 3.1 ng mL{sup -1}. The relative standard deviation for 50, 200 and 400 ng mL{sup -1} of hydrazine is 2, 1.5 and 1.3%, respectively (n = 10). The method was applied to the determination of hydrazine in water samples

  8. Cloud-point extraction and spectrophotometric determination of ...

    African Journals Online (AJOL)

    Aneco-friendly, simple and very sensitive method was developed for preconcentration and determination of clonazepam (CLO) in pharmaceutical dosage forms using cloud point extraction (CPE) technique. The method is based on cloud point extraction of product from oxidative coupling between reduced CLO and ...

  9. A Simple UV Spectrophotometric Method for the Determination of ...

    African Journals Online (AJOL)

    The method was also used in the determination of the content of levofloxacin in two commercial brands of levofloxacin in the Nigerian market. Results: The regression data for the calibration plots exhibited good linear relationship (r = 0.999) over a concentration range of 0.25 – 12.0 ìg/ml and the linear regression equation ...

  10. 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)

  11. Hydrazine determination in presence of uranium by modified spectrophotometric method

    International Nuclear Information System (INIS)

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

    2011-01-01

    In the present work an indirect, sensitive and accurate method for the determination of hydrazine is described. The method is based on the formation of yellow coloured azine complex by post column derivatization of hydrazine with P-dimethylamino benzaldehyde. The formed yellow coloured complex is stable in acidic medium and has a maximum absorption at 460 nm. Interference due to uranium was studied and the method was applied for the determination of hydrazine in presence of uranium in aqueous stream of nuclear fuel reprocessing. A calibration graph was made for the concentration range of hydrazine from 0.05 ppm to 10 ppm with RSD 0.807% and correlation coefficient of 0.99996. (author)

  12. Spectrophotometric determination of sugars labelled with 14C

    International Nuclear Information System (INIS)

    Vatsikova, A.; Kralikova, M.; Vyskochilova, Z.

    1982-01-01

    Comparative analysis of methods for determination of microgram amounts of 14 C-labelled sugars has been carried out. The ferricyanide and Shomodyi-Nelson methods were approbated in experimental study. The relative error of the ferricyanide method was found to be smaller than that of the Shomodyi-Nelson method. Thus the ferricyanide method was used for obtaining calibration curves for 15 sugars. The accuracy for sugar amounts higher than 3 μg/10 ml was better than +, - 5% [ru

  13. Indirect spectrophotometric determination of trace cyanide with cationic porphyrins.

    Science.gov (United States)

    Ishii, H; Kohata, K

    1991-05-01

    Three highly sensitive methods for the determination of cyanide have been developed, based on the fact that the complexation of silver ions with three cationic porphyrins, 5,10,15,20-tetrakis-(1-methyl-2-pyridinio)porphine [T(2-MPy)P], 5,10,15,20-tetrakis(1-methyl-3-pyridinio)porphine [T(3-MPy)P] and 5,10,15,20-tetrakis(1-methyl-4-pyridinio)porphine [T(4-MPy)P], in alkaline media is inhibited by cyanide and the decrease in absorbance of the silver(II) complex is proportional to the cyanide concentration. Sensitivities of the procedures developed are 0.133, 0.126 and 0.234 ng/cm(2), respectively for an absorbance of 0.001. Cadmium(II), copper(II), mercury(II), zinc(II), iodide and sulfide interfere with the cyanide determination. One of the proposed methods was applied to the determination of cyanide in waste-water samples, with satisfactory results.

  14. Spectrophotometric determination of indium with chromazurol S and dimethyllaurylbenzylammonium bromide

    International Nuclear Information System (INIS)

    Kwapulinska, G.; Buhl, F.

    1988-01-01

    The ternary system: indium-chromazurol S (CHAS)-dimethyllaurylbenzylammonium bromide (ST) was applied for determination of microgramme amounts of indium. The addition of ST enhances the sensitivity of the method; at λ max =625 nm the molar absorptivity of In-CHAS-ST complex equals 1.74 x 10 5 . The system obeyes the Lambert-Beer law in the range of indium concentration from 0.04 to 0.48 ppm. The maximal absorbance was obtained at pH 6. The complex is formed immediately and is stable during 2 hours. 3 figs., 10 refs. (author)

  15. 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...

  16. Kinetic spectrophotometric determination of ethamsylate in dosage forms.

    Science.gov (United States)

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

    2007-01-01

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

  17. Spectrophotometric determination of boron in ammonium diuranate and interference studies

    International Nuclear Information System (INIS)

    Ramanjaneyulu, P.S.; Raman, V.A.; Sayi, Y.S.; Ramakumar, K.L.

    2005-01-01

    This paper describes determination of boron in ammonium diuranate by spectrophotometry employing curcumin as a complexing agent after extraction of boron with 2-ethyl hexane 1,3 diol. Two diluents namely ethyl alcohol (EtOH) and N,N-dimethyl formamide (DMF) were investigated for the preparation of final solution. It was observed that the blank is less with DMF presumably due to higher extent of deprotonation of uncomplexed curcumin. The detection limits of method for 25 and 10 ml dilution are 20 ng and 10 ng respectively. Interference studies for several cation and anion species like Al, Cr, Mg, Ca, Fe, Mn, Mo, F, W, NO, and different amount of 10% EHD in CHCl 3 are also discussed. (author)

  18. 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.

  19. Spectrophotometric determination of microamounts of boron in water

    International Nuclear Information System (INIS)

    Weber de D'Alessio, Ana; Guido, O.O.; Bandin, N.A.

    1980-01-01

    A fast method of boron in water determination has been studied for the 0.5 .- 2 μg ml -1 concentration range. The procedure is based on the formation of a coloured complex of the tetrafluoroborate of a thionine derivate cation, its extraction by an organic solvent and the further absorptiometric measurement in such media. Methylene blue and azur C were comparatively tested as organic reagents, with 1.2-dichloroethane as the extractant. The absorbance was measured at the maximum (658 nm). The tetrafluoroboric acid formation was reached in 20 min on a water-bath kept at 60 deg C. The sensitivity with methylene blue was higher than with azur C. The molar absorptivities were 65,000 and 38,000 (l mol -1 cm -1 ) respectively. For a boron concentration of 0.1 μg ml -1 the relative standard deviation was 9% for methylene blue and 7% for azur C. The procedure is applicable to the control of boron traces in heavy water of nuclear reactors refrigerating loops. (author) [es

  20. Spectrophotometric determination of rare earths in binary mixtures

    International Nuclear Information System (INIS)

    Krasnova, A.V.; Shvarev, V.S.

    1978-01-01

    The possibility was investigated of using the reaction with brompyrogallol red (BPR) (dibrompyrogallosulfophthalein) for analyzing binary mixtures of rare earth metals close in ordinal numbers (La-Y, La-Eu, La-Sm, La-Nd, Nd-Y, Nd-Eu). Heavy REM are masked by nitrile-acetic acid (NAA). The experimental design method was used to determine optimum conditions. The optimizing parameters were the optical density measured with respect to water and the amount of the component bound into the complex. It was found that optimum conditions for the analysis of investigated mixtures differ only in the amount of NAA necessary to mask the heavy element [NAA]/[Sm 3+ ]=4; [NAA]/[Eu 3+ ]=5; [NAA]/Nb 3+ ]=10; [NAA]/[Y 3+ ]=2.5. The optimum acidity and the amount of BPR are always the same: pH 6.5; [BPR]/[La 3+ ]=[BPR]/[Nd 3+ ]=4. The given method for analyzing binary mixtures of lanthanoids surpasses considerably in sensitivity the methods based on intrinsic absorption spectra, while retaining the same reproducibility

  1. 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

  2. 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)

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. The determination, by flow-injection analysis, of iron, sulphate, silver and cadmium

    International Nuclear Information System (INIS)

    Jones, E.A.

    1983-01-01

    This report describes the spectrophotometric determination by flow-injection analysis including, where necessary, liquid-liquid extraction of iron with 1,10-phenanthroline; of sulphate by its catalytic effect on the methylthymol blue-zirconium reaction; of silver with bromopyrogallol red and 1,10-phenanthroline; and of cadmium with dithizone. Optimum conditions for each system are established, and sensitivities and ranges of determination are given

  8. 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.

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

    Directory of Open Access Journals (Sweden)

    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

  10. 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.)

  11. 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.

  12. An automatic system for acidity determination based on sequential injection titration and the monosegmented flow approach.

    Science.gov (United States)

    Kozak, Joanna; Wójtowicz, Marzena; Gawenda, Nadzieja; Kościelniak, Paweł

    2011-06-15

    An automatic sequential injection system, combining monosegmented flow analysis, sequential injection analysis and sequential injection titration is proposed for acidity determination. The system enables controllable sample dilution and generation of standards of required concentration in a monosegmented sequential injection manner, sequential injection titration of the prepared solutions, data collecting, and handling. It has been tested on spectrophotometric determination of acetic, citric and phosphoric acids with sodium hydroxide used as a titrant and phenolphthalein or thymolphthalein (in the case of phosphoric acid determination) as indicators. Accuracy better than |4.4|% (RE) and repeatability better than 2.9% (RSD) have been obtained. It has been applied to the determination of total acidity in vinegars and various soft drinks. The system provides low sample (less than 0.3 mL) consumption. On average, analysis of a sample takes several minutes. Copyright © 2011 Elsevier B.V. All rights reserved.

  13. 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.)

  14. 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...

  15. 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

  16. 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.

  17. 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)

  18. 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...

  19. 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.

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

    Directory of Open Access Journals (Sweden)

    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

  1. 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.

  2. 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.

  3. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  5. 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.

  6. 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

  7. 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)

  8. 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

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    Jana Braniša

    2014-02-01

    Full Text Available Chlorophylls and carotenoids are abundant pigments in plants, algae and cyanobacteria. In this study we verified the applicability of two previously developed UV-vis spectrophotometric methods for simultaneous quantitative determination of chlorophylls (a, b and carotenoids (lycopene, β-carotene or total carotenoids. The pigments were extracted from the strawberries, apricots and raspberries in both the acetone-water and acetone-hexane mixtures. Based on the statistical evaluation of the results the combination of mechanical disruption and sonication of fruit samples seems to be a suitable way to improve the pigment extraction efficiency from fruits in both types of solvents. In the case of apricot and raspberry fruit extracts the amount of chlorophylls and carotenoids calculated from the proposed equations was comparable to those published by other authors. However, the spectrophotometric determination of β-carotene content in strawberry acetone-hexane extract appeared to be problematic mainly due to the fact that carotenoids exhibited overlapping chlorophyll absorption bands. Overlap of bands leads to the negative values calculated from the proposed equation for the β-carotene content. The results indicate the limitations in use of the proposed set of equations for plant samples with comparable amounts of studied pigments.

  11. 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)

  12. 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

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

    International Nuclear Information System (INIS)

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

    2009-01-01

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

  14. 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.

  15. 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.

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

    International Nuclear Information System (INIS)

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

    2006-01-01

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

  17. 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)

  18. 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.

  19. 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.

  20. 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 %.

  1. 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.

  2. 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.

  3. 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.

  4. 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)

  5. 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)

  6. 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)

  7. 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.

  8. 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

  9. [Studies on a sequential injection renewable surface reflectance spectrophotometric system using a microchip flow cell].

    Science.gov (United States)

    Wang, Jian-ya; Fang, Zhao-lun

    2002-02-01

    A microchip flow cell was developed for flow injection renewable surface assay by reflectance spectrophotometry. The flow cell was coupled to a sequential injection system and optical fiber photometric detection system. The flow cell featured a three-layer structure. The flow channel was cut into a silicone rubber membrance which formed the middle layer, and a porous filter was inlayed across a widened section of the channel to trap microbeads introduced into the flow cell. The area of the detection window of the flow cell was approximately 3.6 mm2, the volume of the bead trapped in the flow cell was 2.2 microL, the depth of the bead layer was 600 microns. A multistrand bifurcated optical fiber was coupled with incident light, detector and flow cell. The chromogenic reaction of Cr(VI) with 1,5-diphenylcarbohydrazide (DPC) which was adsorbed on trapped Polysorb C-18 beads was used as a model reaction to optimize the flow cell design and the experimental system. The reflectance of the renewable reaction surface was monitored at 540 nm. With 100 microL sample loaded and 1.0 mL.min-1 carrier flow rate, the linear response range was 0-0.6 microgram.mL-1 Cr(VI). A detection limit (3 sigma) of 6 ng.mL-1, precision of 1.5% RSD(n = 11), and a throughput of 64 samples per hour were achieved. Considerations in system and flow cell design, the influence of depth of the bead layer, weight of beads used, and the flow rates of carrier stream on the performance were discussed.

  10. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  12. 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

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

    Directory of Open Access Journals (Sweden)

    Ruba Fahmi Abbas

    2017-07-01

    Full Text Available A sensitive spectrophotometric method has been developed for the determination of Doxycycline hyclate (DCH as pure and  capsule forms. This method is based on diazotization of primary amine group of benzocaine with sodium nitrite in hydrochloric acid medium; the formed diazonium salt is then reacted with DCH in sodium hydroxide medium, to form yellow – orange Azo dye. Beer's law is obeyed in the concentration rang 16-34mg. ml-1 at 480 nm with detection limit LOD and molar absorptivity Є were found to be 0.418 mg.ml-1 and 2.214× 10+4 L.mol-1.cm-1, respectively.

  14. 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

  15. 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.

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

    Science.gov (United States)

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

    2011-12-01

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

  17. 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.

  18. Determination of free acidity in nuclear fuel reprocessing streams by fiber optic aided spectrophotometric technique

    International Nuclear Information System (INIS)

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

    2014-01-01

    A fiber optic aided spectrophotometric technique has been developed for the determination of free acidity in nuclear fuel reprocessing streams. The developed method is simple, accurate and applicable to all ranges of nitric acid and heavy metal concentrations relevant to the purex process. The method is based on the formation of yellow colour with an acid-sensitive indicator such as chrome azurol s, the intensity of yellow colour is proportional to the acid concentration. The system obeys Lambert-Beer's law at 455 nm in the range of acidity 1-10 M of nitric acid. The results obtained are reproducible with standard deviation 2% and relative error is less than 3%. The results obtained by the developed technique are in good agreement with those obtained by the standard procedure. This method is adaptable for remote operation and on-line monitoring. (author)

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

    Science.gov (United States)

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

    2015-02-01

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

  20. 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

  1. 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).

  2. 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)

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

    Directory of Open Access Journals (Sweden)

    Asad Raza

    2009-01-01

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

  4. 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.

  5. 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.

  6. 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)

  7. 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

  8. 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...

  9. 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%.

  10. 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.

  11. Spectrophotometric high-precision seawater pH determination for use in underway measuring systems

    Directory of Open Access Journals (Sweden)

    S. Aßmann

    2011-10-01

    Full Text Available Autonomous sensors are required for a comprehensive documentation of the changes in the marine carbon system and thus to differentiate between its natural variability and anthropogenic impacts. Spectrophotometric determination of pH – a key variable of the seawater carbon system – is particularly suited to achieve precise and drift-free measurements. However, available spectrophotometric instruments are not suitable for integration into automated measurement systems (e.g. FerryBox since they do not meet the major requirements of reliability, stability, robustness and moderate cost. Here we report on the development and testing of a~new indicator-based pH sensor that meets all of these requirements. This sensor can withstand the rough conditions during long-term deployments on ships of opportunity and is applicable to the open ocean as well as to coastal waters with a complex matrix and highly variable conditions. The sensor uses a high resolution CCD spectrometer as detector connected via optical fibers to a custom-made cuvette designed to reduce the impact of air bubbles. The sample temperature can be precisely adjusted (25 °C ± 0.006 °C using computer-controlled power supplies and Peltier elements thus avoiding the widely used water bath. The overall setup achieves a measurement frequency of 1 min−1 with a precision of ±0.0007 pH units, an average offset of +0.0005 pH units to a reference system, and an offset of +0.0081 pH units to a certified standard buffer. Application of this sensor allows monitoring of seawater pH in autonomous underway systems, providing a key variable for characterization and understanding of the marine carbon system.

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

    Science.gov (United States)

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

    2015-03-01

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

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    MAGDA A. AKL

    2010-03-01

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

  15. 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.

  16. 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.

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

    Science.gov (United States)

    Zhang, Meiyun; Zhang, Yan; Li, Quanmin

    2010-03-01

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

  18. Determination of vanadium in steel and geological samples by its extraction and spectrophotometric determination using 2,3-dihydroxynaphthalene

    International Nuclear Information System (INIS)

    Mondal, R.K.; Tarafder, P.K.; Rathore, D.P.S.

    2013-01-01

    A new and simple method for extraction and spectrophotometric determination of vanadium has been described. Iron has been removed from the sample solution by its prior extraction with MIBK from concentrated HCl medium (∼6 M). Vanadium has been determined in the form of a colored complex with 2,3-dihydroxynaphthalene after its extraction into MIBK. The method is at least 5 fold more sensitive to BPHA method. The molar absorptivity of the complex at 530 nm being 1.5 x 10 4 Lmol -1 cm -1 . For samples having >5 fold excess concentration of TiO 2 , a prior separation of TiO 2 as its (Ti (OH) (HND) 3 ) complex is a must. The method has been successfully applied to different rock, soil and steel samples. (author)

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

    Directory of Open Access Journals (Sweden)

    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%.

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

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    Hany W. Darwish

    2013-01-01

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

  1. Validated Spectrophotometric Methods for Simultaneous Determination of Food Colorants and Sweeteners

    Directory of Open Access Journals (Sweden)

    Fatma Turak

    2013-01-01

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

  2. 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.

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

    Directory of Open Access Journals (Sweden)

    Sunitha B. Mathew

    2007-04-01

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

  4. 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)

  5. 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.

  6. 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.

  7. A new system for the spectrophotometric determination of trace amounts of nitrite in environmental samples

    Directory of Open Access Journals (Sweden)

    Cherian Tom

    2006-01-01

    Full Text Available A selective and rapid spectrophotometric method for the determination of nitrite is presented. It is based on the reaction of nitrite with p-nitroaniline in acid medium to form diazonium ion, which is coupled with ethoxyethylenemaleic ester or ethylcyanoacetate in basic medium to form azo dyes, showing absorption maxima at 439 and 465 nm respectively. The method obeys Beer's law in the concentration range of 0.5-16 µg mL-1 of nitrite with ethoxyethylenemaleic ester and 0.2-18 µg mL-1 of nitrite with ethylcyanoacetate. The molar absorptivity and Sandell's sensitivity of p-nitroaniline-ethoxyethylenemaleic ester and p-nitroaniline-ethylcyanoacetate azo dyes are 5.04 X 10(4 L mol-1cm-1, 0.98 X 10-2 µg cm-2 and 1.21 X 10(4 L mol-1 cm-1, 0.98 X 10-2 µg cm-2 respectively. The optimum reaction conditions and other analytical parameters were evaluated. The method was successfully applied to the determination of nitrite in various water samples and soil samples.

  8. 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.

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

    Science.gov (United States)

    Shishehbore, Masoud Reza; Aghamiri, Zahra

    2014-01-01

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

  10. Dibenzazepin hydrochloride as a new spectrophotometric reagent for determination of hydrogen peroxide in plant extracts.

    Science.gov (United States)

    Nagaraja, P; Prakash, J S; Asha, S C; Bhaskara, B L; Kumar, S Anil

    2012-10-01

    A rapid, simple, accurate, and sensitive visible spectrophotometric method for the determination of trace amounts of hydrogen peroxide in acidic buffer medium is reported. The proposed method is based on the oxidative coupling of Ampyrone with dibenzazepin hydrochloride by hydrogen peroxide in the buffer medium of pH 4.0 which is catalyzed by ferrous iron. The blue-colored product formed with maximum absorption at 620 nm was found to be stable for 2 h. Beer's law is obeyed for hydrogen peroxide concentration in the range of 0.03-0.42 μg ml(-1). The optimum reaction conditions and other important optical parameters are reported. The molar absorptive and Sandell's sensitivity are found to be 5.89 × 10(4) mol(-1) cm(-1) and 0.57 g/cm(2), respectively. The interference due to diverse ions and complexing agents was studied. The method is successfully applied to the determination of hydrogen peroxide in green plants satisfactorily.

  11. 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.

  12. Spectrophotometric determination of mefenamic acid excreted as free drug in urine of human beings

    International Nuclear Information System (INIS)

    Naseer, M.M.; Nawaz, R.; Shafique, M.; Rehman, R.

    2007-01-01

    Urinary excretion of free mefenamic acid was investigated in 16 healthy human volunteers, eight males and eight females, following the oral administration of 500 mg tablet of mefenamic acid. Urine samples were collected at pre-determined schedule and drug concentration was determined by spectrophotometric method. The total recovery of free mefenamic acid was 1.526 +- 0.128 and 1.193 +- 0.112% in male and female volunteers respectively. The average +- S.E values for diuresis, pH and rate of excretion of mefenamic acid was 0.0160 +- 0.004 mL/min./kg of body weight, 6.22 +- 0.167, 0.077 +- 0.016 micro g min/sup -1/kg/sup -1/in male while 0.0084 +- 0.0023mL min/sup -1/kg-1 of body weight, 6.35 +- 0.164, 0.054 +- 0.008 micro g min/sup -1/kg/sup -1/respectively in female volunteers. The results obtained are different from the earlier studies due to variability in dose, gender variation, fluctuation in urine pH, environmental conditions and nutritional ingredients. (author)

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Directory of Open Access Journals (Sweden)

    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.

  15. Spectrophotometric determination of dissolved tri n-butyl phosphate in aqueous streams of Purex process

    International Nuclear Information System (INIS)

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

    2012-01-01

    A spectrophotometric method is developed for the determination of dissolved tri-n butyl phosphate (TBP) in aqueous streams of Purex process used in nuclear fuel reprocessing. The method is based on the formation of phosphomolybdate with added ammonium molybdate followed by reduction with hydrazine sulphate in acid medium. Orthophosphate and molybdate ions combine in acidic solution to give molybdophosphoric (phosphomolybdic) acid, which upon selective reduction (with hydrazinium sulphate) produces a blue colour, due to molybdenum blue. The intensity of blue colour is proportional to the amount of phosphate. If the acidity at the time of reduction is 0.5 M in sulphuric acid and hydrazinium sulphate is the reductant, the resulting blue complex exhibits maximum absorption at 810-840 nm. The system obeys Lambert-Beer's law at 830 nm in the concentration range of 0.1-1.0 μg/mol of phosphate. Molar Absorptivity was determined to be 3.1 x 10 4 L mol -1 cm -1 at 830 nm. The results obtained are reproducible with standard deviation of 1 % and relative error less than 2 % and are in good agreement with those obtained by ion chromatographic technique. (author)

  16. Spectrophotometric Determination of Rifampicin in Bulk Drug and Pharmaceutical Formulations Based on Redox and Complexation Reactions

    Science.gov (United States)

    Swamy, N.; Basavaiah, K.

    2017-09-01

    Two spectrophotometric methods were developed and validated for the determination of rifampicin (RIF) in bulk form, formulations, and spiked human urine. The first method is based on the reduction of the Folin-Ciocalteu (FC) reagent by RIF to form a blue colored chromogen with λmax at 760 nm (the FCR method). In the second method, iron(III) is reduced by RIF in a neutral medium, and the resulting iron(II) is complexed with ferricyanide to form a Prussian blue peaking at 750 nm (the FFC method). Under optimum conditions, Beer's law enabled the determination of the drug in the concentration ranges 1-35 and 2.5-50 μg/mL with apparent molar absorptivities of 2.72 × 104 and 1.63×104 L/(mol × cm) for the FCR and FFC methods, respectively. The Sandell sensitivity, limits of detection (LOD), and quantification (LOQ) values were also reported for both methods. The precision of the methods, with % RSD of human urine without interference from endogenous substances. A statistical analysis indicated that there was no significant difference between the results obtained by the developed methods and the official method.

  17. Simultaneous determination of caffeine, theophylline and theobromine in food samples by a kinetic spectrophotometric method.

    Science.gov (United States)

    Xia, Zhenzhen; Ni, Yongnian; Kokot, Serge

    2013-12-15

    A novel kinetic spectrophotometric method was developed for the simultaneous determination of caffeine, theobromine and theophylline in food samples. This method was based on the different kinetic characteristics between the reactions of analytes with cerium sulphate in sulphuric acid and the associated change in absorbance at 320 nm. Experimental conditions, the effects of sulphuric acid, cerium sulphate and temperature, were optimised. Linear ranges (0.4-8.4 μg mL(-1)) for all three analytes were established, and the limits of detection were: 0.30 μg mL(-1) (caffeine), 0.33 μg mL(-1) (theobromine) and 0.16 μg mL(-1) (theophylline). The recorded data were processed by partial least squares and artificial neural network, and the developed mathematical models were then used for prediction. The proposed, novel method was applied to determine the analytes in commercial food samples, and there were no significant differences between the results from the proposed method and those obtained by high-performance liquid chromatography. Copyright © 2013 Elsevier Ltd. All rights reserved.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  19. 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.

  20. 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.

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

    Directory of Open Access Journals (Sweden)

    M. Vamsi Krishna

    2007-01-01

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

  2. 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

  3. 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)

  4. Novel Spectrophotometric Method for the Determination of Pindolol in Pharmaceutical Samples

    Science.gov (United States)

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

    2011-10-01

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

  5. Spectrophotometric determination of tizanidine and orphenadrine via ion pair complex formation using eosin Y

    Directory of Open Access Journals (Sweden)

    Eid Manal I

    2011-10-01

    Full Text Available Abstract A simple, sensitive and rapid spectrophotometric method was developed and validated for the determination of two skeletal muscle relaxants namely, tizanidine hydrochloride (I and orphenadrine citrate (II in pharmaceutical formulations. The proposed method is based on the formation of a binary complex between the studied drugs and eosin Y in aqueous buffered medium (pH 3.5. Under the optimum conditions, the binary complex showed absorption maxima at 545 nm for tizanidine and 542 nm for orphenadrine. The calibration plots were rectilinear over concentration range of 0.5-8 μg/mL and 1-12 μg/mL with limits of detection of 0.1 μg/mL and 0.3 μg/mL for tizanidine and orphenadrine respectively. The different experimental parameters affecting the development and stability of the complex were studied and optimized. The method was successfully applied for determination of the studied drugs in their dosage forms; and to the content uniformity test of tizanidine in tablets.

  6. 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.

  7. 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.

  8. 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.

  9. Spectrophotometric Determination of Reboxetine through Condensation and Diazo-Coupling Reactions

    Directory of Open Access Journals (Sweden)

    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.

  10. New Diazo Coupling Reactions for Visible Spectrophotometric Determination of Alfuzosin in Pharmaceutical Preparations

    Directory of Open Access Journals (Sweden)

    M. Vamsi Krishna

    2007-01-01

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

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

    Directory of Open Access Journals (Sweden)

    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.

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

    Science.gov (United States)

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

    2018-01-01

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

  13. Spectrophotometric Determination of Aminoglycoside Antibiotics Based on their Oxidation by Potassium Permanganate

    International Nuclear Information System (INIS)

    El-Didamony, A. M.; Ghoneim, A. K.; Telebany, A. M.; Amin, A. S.

    2006-01-01

    A rapid, simple and sensitive validated spectrophotometric methods have been described for the assay of neomycin and streptomycin either in pure form or in pharmaceutical formulations. The proposed methods were based on the oxidation of the studied drugs by a known excess of potassium permanganate in acidic medium and estimating the unreacted permanganate with amaranth dye (method A), acid orange II (method B), indigocarmine (method C), and methylene blue (method D), in the same acid medium at a suitable λ max =521, 485, 610 and 664 nm, respectively. Beer's law is obeyed in the concentration range of 5-10 and 2-7 mg mL -1 for neomycin and streptomycin, respectively. The apparent molar absorptivity and sandell sensitivity values are in the range 5.47-6.20x10 4 , 2.35-2.91x10 5 L mol -1 cm -1 and 7.57-8.59, 5.01-6.2 ng cm -2 for neomycin and streptomycin, respectively. Different variables affecting the reaction were studied and optimized. The proposed methods were applied successfully to the determination of the examined drugs either in a pure or pharmaceutical dosage forms with good accuracy and precision. No interferences were observed from excipients and the results obtained were in good agreement with those obtained using the official methods

  14. Simultaneous spectrophotometric determination of trimethoprim and sulphamethoxazole following charge-transfer complexation with chloranilic acid

    Directory of Open Access Journals (Sweden)

    Olajire A. Adegoke

    2017-05-01

    Full Text Available A simple, accurate and precise simultaneous spectrophotometric method has been developed for the analysis of trimethoprim–sulphamethoxazole combination in pure and tablet dosage forms. The method involves direct charge transfer complexation of trimethoprim (TMP with chloranilic acid (CAA in acetonitrile–dioxane solvent mixture and complexation of sulphamethoxazole (SMZ after its hydrolysis in dilute H2SO4. Optimization of temperature and time revealed the superiority of room temperature and 20 and 30 min respectively for TMP and SMZ. Optimal detector responses were obtained at 520 and 440 nm and were therefore selected as working wavelength maxima for SMZ and TMP respectively. TMP and hydrolysed SMZ were combined with CAA at mole ratios of 1:1 and 1:3 respectively. Accuracies were generally less than 4% (estimated as degree of inaccuracy or error with a precision of the order of less than 2% on a three-day assessment. Physicochemical factors responsible for complex stability were estimated and related to the observed data. The method was successfully applied to the determination of TMP and SMZ in tablet dosage forms with accuracies comparable to the official BP method. There were no interferences from common tablet excipients and TMP complex did not interfere with the assay of SMZ. The developed method could find application in routine quality control of TMP–SMZ combination. It is the first reported full simultaneous colorimetric assay of TMP and SMZ using the same analytical reagent.

  15. Spectrophotometric Determination of Terbutaline Sulphate and Tetracycline Hydrochloride via ion pair Complex Formation Using Eosin Y

    Directory of Open Access Journals (Sweden)

    Mohamed Y. Dhamra

    2014-06-01

    Full Text Available A simple, sensitive and rapid spectrophotometric method was developed and validated for the determination of terbutaline sulphate and tetracycline hydrochloride drugs in pure form and pharmaceutical formulations. The proposed method is based on the formation of binary complexes between these drugs and eosin Y in aqueous acetate buffered medium. Under the optimum conditions, the binary complexes showed absorption maxima at 545 nm. Beer's law was rectilinear over concentration range of 0.5-10 and 5-45 μg/mL, R2 were 0.9984 and 0.9988, RSD were ≤ 0.72 and ≤ 0.19 (n=5 with average recovery % 101.42 % and 100.08 % and the average recovery values of pharmaceutical formulations 101.48 and 98.01 for above drugs respectively. The limit of detection (LOD were 0.030 and 0.613 μg/mL and limit of quantitation (LOQ were 0.103 and 2.00 μg/mL with molar absorptivity values 3.169  103 and 6.347  103 l. mol-1. cm-1 and the relative standard deviation values ≤0.720 and ≤ 0.19 for both drugs respectively. No interference was observed from the excipients that are commonly present in pharmaceutical formulations. The proposed method was successfully applied to the analysis of terbutaline sulphate tablet and tetracycline hydrochloride capsule in their dosage forms.

  16. Spectrophotometric determination of terbutaline sulphate and tetracycline hydrochloride via ion pair complex formation using eosin y

    International Nuclear Information System (INIS)

    Dhamra, M.Y.; Sabha, T.N.A.; Ghabsha, T.S.A.

    2014-01-01

    A simple, sensitive and rapid spectrophotometric method was developed and validated for the determination of terbutaline sulphate and tetracycline hydrochloride drugs in pure form and pharmaceutical formulations. The proposed method is based on the formation of binary complexes between these drugs and eosin Y in aqueous acetate buffered medium. Under the optimum conditions, the binary complexes showed absorption maxima at 545 nm. Beer's law was rectilinear over concentration range of 0.5-10 and 5-45 micro g/mL, R/sub 2/ were 0.9984 and 0.9988, RSD were 0.72 and 0.19 (n=5) with average recovery 101.42 % and 100.08 % and the average recovery values of pharmaceutical formulations 101.48 and 98.01 for above drugs respectively. The limit of detection (LOD) were 0.030 and 0.613 micro g/mL and limit of quantitation (LOQ) were 0.103 and 2.00 micro g/mL with molar absorptivity values 3.169 10/sup 3/ and 6.347 10/sup 3/l. mol/sup -1/. Cm/sup -1/ and the relative standard deviation values 0.720 and 0.19 for both drugs respectively. No interference was observed from the excipients that are commonly present in pharmaceutical formulations. The proposed method was successfully applied to the analysis of terbutaline sulphate tablet and tetracycline hydrochloride capsule in their dosage forms. (author)

  17. A sensitive spectrophotometric determination of nitrogen dioxide in the working atmosphere

    Directory of Open Access Journals (Sweden)

    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.

  18. On-line lab-in-syringe cloud point extraction for the spectrophotometric determination of antimony.

    Science.gov (United States)

    Frizzarin, Rejane M; Portugal, Lindomar A; Estela, José M; Rocha, Fábio R P; Cerdà, Victor

    2016-02-01

    Most of the procedures for antimony determination require time-consuming sample preparation (e.g. liquid-liquid extraction with organic solvents), which are harmful to the environment. Because of the high antimony toxicity, a rapid, sensitive and greener procedure for its determination becomes necessary. The goal of this work was to develop an analytical procedure exploiting for the first time the cloud point extraction on a lab-in-syringe flow system aiming at the spectrophotometric determination of antimony. The procedure was based on formation of an ion-pair between the antimony-iodide complex and H(+) followed by extraction with Triton X-114. The factorial design showed that the concentrations of ascorbic acid, H2SO4 and Triton X-114, as well as second and third order interactions were significant at the 95% confidence level. A Box-Behnken design was applied to obtain the response surfaces and to identify the critical values. System is robust at the 95% confidence level. A linear response was observed from 5 to 50 µg L(-1), described by the equation A=0.137+0.050C(Sb) (r=0.998). The detection limit (99.7% confidence level), the coefficient of variation (n=5; 15 µg L(-1)) and the sampling rate was estimated at 1.8 µg L(-1), 1.6% and 16 h(-1), respectively. The procedure allows quantification of antimony in the concentrations established by environmental legislation (6 µg L(-1)) and it was successfully applied to the determination of antimony in freshwater samples and antileishmanial drugs, yielding results in agreement with those obtained by HGFAAS at the 95% confidence level. Copyright © 2015 Elsevier B.V. All rights reserved.

  19. Cloud point extraction and spectrophotometric determination of mercury species at trace levels in environmental samples.

    Science.gov (United States)

    Ulusoy, Halil İbrahim; Gürkan, Ramazan; Ulusoy, Songül

    2012-01-15

    A new micelle-mediated separation and preconcentration method was developed for ultra-trace quantities of mercury ions prior to spectrophotometric determination. The method is based on cloud point extraction (CPE) of Hg(II) ions with polyethylene glycol tert-octylphenyl ether (Triton X-114) in the presence of chelating agents such as 1-(2-pyridylazo)-2-naphthol (PAN) and 4-(2-thiazolylazo) resorcinol (TAR). Hg(II) ions react with both PAN and TAR in a surfactant solution yielding a hydrophobic complex at pH 9.0 and 8.0, respectively. The phase separation was accomplished by centrifugation for 5 min at 3500 rpm. The calibration graphs obtained from Hg(II)-PAN and Hg(II)-TAR complexes were linear in the concentration ranges of 10-1000 μg L(-1) and 50-2500 μg L(-1) with detection limits of 1.65 and 14.5 μg L(-1), respectively. The relative standard deviations (RSDs) were 1.85% and 2.35% in determinations of 25 and 250 μg L(-1) Hg(II), respectively. The interference effect of several ions were studied and seen commonly present ions in water samples had no significantly effect on determination of Hg(II). The developed methods were successfully applied to determine mercury concentrations in environmental water samples. The accuracy and validity of the proposed methods were tested by means of five replicate analyses of the certified standard materials such as QC Metal LL3 (VWR, drinking water) and IAEA W-4 (NIST, simulated fresh water). Copyright © 2011 Elsevier B.V. All rights reserved.

  20. 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)

  1. 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.

  2. 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

  3. 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.

  4. 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

  5. The determination of uranium(VI) by flow-injection analysis

    International Nuclear Information System (INIS)

    Jones, E.A.

    1985-01-01

    A method is described for the direct determination of uranium(VI) in waste waters and acid leach liquors by use of a flow-injection procedure and spectrophotometric measurement with 2-(5-bromo-2-pyridylazo)-5-diethylaminophenol (bromo-PADAP). The interference effects of several commonly occurring elements were studied. The calibration curve is linear over concentrations of uranium(VI) from 0,5 to 20 mg/1, and the precision obtained on a synthetic leach liquor was 0,019 (relative standard deviation). The procedure is rapid and convenient, and up to 40 samples can be analysed in an hour

  6. 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).

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

    Science.gov (United States)

    Amin, Alaa S.; Kassem, Mohammed A.

    2012-01-01

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

  8. 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.)

  9. Spectrophotometric determination of metal complexes of 1-nitroso-2-naphthol in micellar medium

    International Nuclear Information System (INIS)

    Shar, G.A.; Bhanger, M.I.

    2002-01-01

    Spectrophotometric determination of iron(III), nickel(II) and cobalt(II) is carried out with 1-nitroso-2-naphthol as complexing reagent in aqueous phase using non-ionic surfactant Tween 40. This replaces a tedious and time consuming solvent extraction method, because these solvents are costly and also toxic. Beer's law was obeyed, for Fe(III), Ni(II) and Co(II) over the range 0.5 - 4.0, 0.5 - 4.0 and 0.12 - 3.0 micro g ml/sup -1/ with detection limit (2 sigma ) of 3.3, 5.8 and 3.1 ng ml/sup -1/ respectively. The lambda /sub max/ molar absorption, molar absorptivity and Sandell's sensitivity of Fe(III), Ni(II) and Co(II) were (lambda /sub max/ 446 nm), (lambda/sub max/ 483.5 nm) and (lambda/sub max/ 444.5 nm); sigma/sub max/ x 10/sp 4/ mol/sp -1/ cm/sup -1/) is 1.69, 1.0 and 1.86, 3.3, 5.8 and 3.1 ng cm/sup -2/, respectively. The pH at which the complex is formed for Fe(III), Ni(II) and Co(II) is 1, 8 and 5 respectively. The critical micelle concentration (cmc) of 1-nitroso-2-naphthol is 5% solution. The present method is compared with that of atomic absorption spectroscopy and no significant difference is noted between the two methods at 95% confidence level. The method has been applied to the determination of iron(III), nickel(II) and cobalt(II) in pharmaceutical and industrial wastewater samples. (author)

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

    Science.gov (United States)

    El-Saharty, Yasser Shaker Ibrahim

    2008-01-01

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

  11. Extraction and spectrophotometric determination of molybdenum with omicron-hydroxythiophenols and aromatic amines

    International Nuclear Information System (INIS)

    Zalov, A.Z.; Verdizade, N.A.

    2015-01-01

    The interaction of molybdenum (VI) with o-hydroxythiophenol derivatives (HTPDs) and aromatic amines (AAs) was studied. The following three HTPDs, which contain different halogen atoms at position 5, were used: 2-hydroxy-5-chlorothiophenol(HCTP), 2-hydroxy-5-bromothiophenol (HBTP), 2-hydroxy-5-iodothiophenol (HITP)). The examined AAs were aniline (An), Nmethylaniline (mAn) and N,N-dimethylaniline (dAn). The obtained ternary complexes have a composition of 1:2:2 (Mo(V):HBTP:AA). Optimal conditions for their liquid-liquid extraction (LLE) were found: organic solvent (chloroform), pH (4-6), concentration of the reagents 10-3moldm-3 (AA)) and 10-3moldm-3 (HTPD) and (1.2-1.5) ((1.3-1.5) extraction time(colour develops almost immediately after the reagents addition). The absorbance of the extracts is stable for at least 48 hours. The optimum shaking time is 10 min.). Under the optimal max) at 515-538 conditions, the complexes have absorption maxima ( 104dm3mol-1 cm-1. The max) between 3.1 nm and molar absorptivities ( 98.4%. The results suggested that linear degrees of extraction were max or relationships exist between the spectral characteristics ( max) and some fundamental properties of the halogen substituent in the HTPD (atomic mass and electronegativity). The effect of foreign ions on the LLE-spectrophotometric determination of molybdenum was examined and two sensitive, selective and precise procedures for molybdenum determination were proposed. The relative standard deviations for Mo 10-4 % were 4% (HCTP-An procedure) and 3% (HBTP-An content of (3-5) procedure). (author)

  12. Extraction spectrophotometric determination of rare earth with trioctylethylammonium bromide and Xylenol Orange

    International Nuclear Information System (INIS)

    Shijo, Yoshio

    1976-01-01

    A spectrophotometric method of determination of the rare earth was studied by the solvent extraction of rare earth-Xylenol Orange chelate into xylene solution of trioctylethylammonium bromide(TOEA). The rare earth-XO-TOEA complexes are extracted into aromatic hydrocarbons such as benzene, toluene, and xylene, but not into polar solvents such as n-butanol ethylacetate, methylisobutylketone, and nitrobenzene. The optimum pH range for the extraction were 6.3 -- 6.7, 6.3 -- 6.5, 5.8 -- 6.9, 5.7 -- 6.9, and 5.5 -- 6.8 for lanthanum, praseodymium, cerium, gadolinium, and dysprosium, respectively. The absorption maximum of the complexes extracted into xylene were found at 605 nm for lanthanum, praseodymium, and cerium, 596 nm for gadolinium, and 590 nm for dysprosium. Beer's law held for about 0 -- 4.5 μg of rare earth per 5 ml of xylene. The molar absorptivity of the extracted species were 1.53x10 5 , 1.42x10 5 , 1.35x10 5 , 8.5x10 4 , 8.2x10 4 cm -1 mol -1 l for lanthanum, praseodymium, cerium, gadolinium, and dysprosium, respectively. The composition of the ternary complexes were estimated to be M:XO:TOEA=1:1:2 for gadolinium and dysprosium, whereas 1:2:n for lanthanum, praseodymium and cerium. Combination ratio n of TOEA to metal-XO chelates in the latters could not be estimated by the commonly available methods. Thorium, vanadium, uranium, bismuth, aluminum, zirconium, chromium, nitrate, perchlorate and iodide interfered when triethylenetetramine and 1,10-phenanthroline were added as masking agent. (auth.)

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

    International Nuclear Information System (INIS)

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

    1999-01-01

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

  14. Simple Sensitive Spectrophotometric Determination of Vanadium in Biological and Environmental Samples

    Directory of Open Access Journals (Sweden)

    B. Krishna Priya

    2006-01-01

    Full Text Available Novel, rapid, highly sensitive and selective spectrophotometric method for the determination of traces of vanadium (V in environmental and biological samples, pharmaceutical and steel samples was studied. The method is based on oxidation of 2,4- dinitro phenyl hydrazine(2,4-DNPH by vanadium (V followed by coupling reaction with N-(1-naphthalene-1-ylethane-1,2-diamine-dihydrochloride (NEDA in acidic medium to give red colored derivative or on oxidation of 4-Amino Pyridine by vanadium (V followed by coupling reaction with NEDA in basic medium to give pink colored derivative. The red colored derivative having an λmax 495 nm which is stable for 8 days and the pink colored derivative with 525 nm is stable for more than 7 days at 350C. Beer's law is obeyed for vanadium (V in the concentration range of 0.02 - 3.5 μg mL–1 (red derivative and 0.03 – 4.5 μg mL–1 (pink derivative at the wave length of maximum absorption. The optimum reaction conditions and other analytical parameters were investigated to enhance the sensitivity of the present method. The detailed study of various interferences made the method more selective. The proposed method was successfully applied to the analysis of vanadium in natural water samples, plant material, soil samples, synthetic mixtures, pharmaceutical samples and biological samples. The results obtained were agreed with the reported methods at the 95 % confidence level. The performance of proposed method was evaluated in terms of Student's t-test and Variance ratio f-test which indicates the significance of proposed method over reported method.

  15. 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)

  16. 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.

  17. Facile and Sensitive Spectrophotometric Technique for the Determination of Carbofuran in its Formulations, Water and Grain Samples with Substituted Anilines

    Directory of Open Access Journals (Sweden)

    V. Harikishna

    2005-01-01

    Full Text Available Methods are described for the determination of carbofuran in its formulations, in water and grain samples by the diazotization coupling spectrophotometric technique, using substituted anilines such as 4-bromoaniline, 4-methylaniline and 4-aminobenzaldehyde as the coupling agents. The orange red colour formed with 4-bromoaniline shows maximum absorption at 478 nm, yellow colour obtained with 4-methylaniline have maximum absorption at 465 nm whereas a red colour derivative formed with 4-aminobenzaldehyde shows λmax at 472 nm. The methods could be successfully applied for the determination of carbofuran in its formulations, water and grain samples.

  18. Spectrophotometric Determination of Lamotrigine in Pharmaceutical Preparations and Urine Samples Using Bromothymol Blue and Bromophenol Blue

    International Nuclear Information System (INIS)

    Najib, F.M.; Aziz, K.H.H.

    2013-01-01

    Two simple and sensitive spectrophotometric methods have been developed for the determination of the antiepileptic drug lamotrigine (LMT) in pharmaceutical preparations and urine samples. The methods are based on the interaction of LMT with two sulphonphthalein dyes, namely, bromothymol blue (BTB) and bromophenol blue (BPB) in dichloromethane (DCM) medium to form stable and yellow-colored ion-pairs with λ max 410 and 413 nm respectively. The ion-pair LMT-BPB has been extracted from aqueous solutions at pH 3.25±0.25 using DCM; while LMT-BTB ion-pair was directly prepared in DCM. Interferences from the compounds of the urine samples, in case of LMT-BPB were removed using a suppressing solution (S.S.) prepared from the salts of the interfering ions. In LMT-BTB method, the urine of normal person not taking LMT, was used as a blank to remove the effect of interferences. Under optimum conditions, the calibration curve of LMT-BTB was linear over the range of 1-12 μg.ml -1 , ε=1.97x10 4 L.mole -1 .cm -1 , r 2 = 0.9983, and D.L of 0.13 μg.ml -1 . The corresponding values for (LMT-BPB) ion-pair were 0.5-12 μg.ml -1 linear range, ε=1.92x10 4 , r 2 = 0.9980, and D.L= 0.24 μg.ml -1 . The stoichiometry of the ion-pairs were found to be 1:1, based on Jobs, mole ratio and slope ratio methods. The recoveries (%R) for both methods were in the range of 97-101.8 % and 95-97.1 % with RSD≤1.68 and 3.1 % respectively. For LMT- spiked urine samples, the recoveries were 98.5-106.6 % with RSD≤1.66 %. Interferences from phenobarbital and carbamazepine were in the range of 25-40 folds. Statistical comparison of the results with a published method using F and t-tests showed no significant differences between each of the two methods and the reported one at 95 % confidence level. A standard addition method, gave high accuracy with LMT-BPB method. The proposed methods were successfully applied for the determination of LMT in pharmaceutical preparation and urine samples. (author)

  19. 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.

  20. 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

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

    Directory of Open Access Journals (Sweden)

    L. Yu. Klimenko

    2014-08-01

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

  2. 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

  3. Novel microwell-based spectrophotometric assay for determination of atorvastatin calcium in its pharmaceutical formulations

    Directory of Open Access Journals (Sweden)

    Abdel-Rahman Hamdy M

    2011-10-01

    Full Text Available Abstract The formation of a colored charge-transfer (CT complex between atorvastatin calcium (ATR-Ca as a n-electron donor and 2, 3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ as a π-electron acceptor was investigated, for the first time. The spectral characteristics of the CT complex have been described, and the reaction mechanism has been proved by computational molecular modeling. The reaction was employed in the development of a novel microwell-based spectrophotometric assay for determination of ATR-Ca in its pharmaceutical formulations. The proposed assay was carried out in 96-microwell plates. The absorbance of the colored-CT complex was measured at 460 nm by microwell-plate absorbance reader. The optimum conditions of the reaction and the analytical procedures of the assay were established. Under the optimum conditions, linear relationship with good correlation coefficient (0.9995 was found between the absorbance and the concentration of ATR-Ca in the range of 10-150 μg/well. The limits of detection and quantitation were 5.3 and 15.8 μg/well, respectively. No interference was observed from the additives that are present in the pharmaceutical formulation or from the drugs that are co-formulated with ATR-Ca in its combined formulations. The assay was successfully applied to the analysis of ATR-Ca in its pharmaceutical dosage forms with good accuracy and precision. The assay described herein has great practical value in the routine analysis of ATR-Ca in quality control laboratories, as it has high throughput property, consumes minimum volume of organic solvent thus it offers the reduction in the exposures of the analysts to the toxic effects of organic solvents, and reduction in the analysis cost by 50-fold. Although the proposed assay was validated for ATR-Ca, however, the same methodology could be used for any electron-donating analyte for which a CT reaction can be performed.

  4. 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...

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

    Directory of Open Access Journals (Sweden)

    HASSAN ZAVVAR MOUSAVI

    2009-08-01

    Full Text Available A highly selective and sensitive catalytic spectrophotometric method was developed for the determination of nitrite in water samples. The method is based on its catalytic effect on the nuclear fast red–potassium bromate redox reaction in acidic medium. The reaction was followed spectrophotometrically by measuring the change in the absorbance at 518 nm of nuclear fast red 5 min after initiation of the reaction. In this study, the experimental parameters were optimized and the effects of other cations and anions on the determination of nitrite were examined. The calibration graph was linear in the range 2.0–45 µg mL-1 of nitrite. The relative standard deviations for the determination of 15 and 30 µg mL-1 of nitrite were 3.1 and 1.75 %, respectively (n = 8. The detection limit calculated from three times the standard deviation of the blank 3Sb was 0.7 µg mL-1. The method was successfully applied to the determination of nitrite in spiked tap, natural and wastewater samples.

  6. 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)

  7. 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

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

    Directory of Open Access Journals (Sweden)

    Mohammad Hosein Soruraddin

    2011-01-01

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

  9. 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.

  10. Determining How Magnetic Helicity Injection Really Works

    International Nuclear Information System (INIS)

    Paul M Bellan

    2001-01-01

    OAK-B135 The goal of the Caltech program is to determine how helicity injection works by investigating the actual dynamics and topological evolution associated with magnetic relaxation. A new coaxial helicity injection source has been constructed and brought into operation. The key feature of this source is that it has maximum geometric simplicity. Besides being important for fusion research, this work also has astrophysical implications. Photos obtained using high-speed cameras show a clear sequence of events in the formation process. In particular, they show initial merging/reconnection processes, jet-like expansion, kinking, and separation of the plasma from the source. Various diagnostics have been developed, including laser induced fluorescence and soft x-ray detection using high speed diodes. Gas valves have been improved and a patent disclosure relating to puffed gas valves has been filed. Presentations on this work have been given in the form of invited talks at several university physics departments that were previously unfamiliar with laboratory plasma experiments

  11. 2,2',3,4-Tetrahydroxy-3'-sulpho-5'-nitroazobenzene for spectrophotometric determination of aluminium in pharmaceutical suspensions and granite

    International Nuclear Information System (INIS)

    Guray, Tufan; Uysal, Uelkue Dilek; Gedikbey, Tevfik; Huseyinli, A. Ali

    2005-01-01

    A selective and sensitive new spectrophotometric method has been developed for the determination of aluminium. 2,2',3,4-Tetrahydroxy-3'-sulpho-5'-nitroazobenzene (tetrahydroxyazon SN) formed an orange chelate with aluminium at pH 4. Molar absorptivity of the complex in 1:2 is 5.46 x 10 4 l mol -1 cm -1 at 479 nm. The method obeys Beer's law in the range of 0.005-1.079 μg ml -1 . The determination of aluminium is not interfered with by earth alkaline, alkaline elements, rare earth elements, halides, phosphates, sulphates, urea, ascorbic acid, Sn 2+ , Sr 2+ , Cr 3+ , Cd 2+ , Hg 2+ , or Mn 2+ . The proposed method is rapid and simple, and it has been successfully applied to the determination of aluminium in certified pharmaceutical suspension and granite

  12. 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.

  13. 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

  14. Exploiting an automated microfluidic hydrodynamic sequential injection system for determination of phosphate.

    Science.gov (United States)

    Khongpet, Wanpen; Pencharee, Somkid; Puangpila, Chanida; Kradtap Hartwell, Supaporn; Lapanantnoppakhun, Somchai; Jakmunee, Jaroon

    2018-01-15

    A microfluidic hydrodynamic sequential injection (μHSI) spectrophotometric system was designed and fabricated. The system was built by laser engraving a manifold pattern on an acrylic block and sealing with another flat acrylic plate to form a microfluidic channel platform. The platform was incorporated with small solenoid valves to obtain a portable setup for programmable control of the liquid flow into the channel according to the HSI principle. The system was demonstrated for the determination of phosphate using a molybdenum blue method. An ascorbic acid, standard or sample, and acidic molybdate solutions were sequentially aspirated to fill the channel forming a stack zone before flowing to the detector. Under the optimum condition, a linear calibration graph in the range of 0.1-6mg P L -1 was obtained. The detection limit was 0.1mgL -1 . The system is compact (5.0mm thick, 80mm wide × 140mm long), durable, portable, cost-effective, and consumes little amount of chemicals (83μL each of molybdate and ascorbic acid, 133μL of the sample solution and 1.7mL of water carrier/run). It was applied for the determination of phosphate content in extracted soil samples. The percent recoveries of the analysis were obtained in the range of 91.2-107.3. The results obtained agreed well with those of the batch spectrophotometric method. Copyright © 2017 Elsevier B.V. All rights reserved.

  15. 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.

  16. 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)

  17. 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)

  18. 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.

  19. 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

  20. 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.

  1. 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.

  2. Extractive and spectrophotometric determination of U (VI) using 5-(3-phenolyl azo)-2-hydroxy-4-ethoxy propiophenone oxime (PHEPO)

    International Nuclear Information System (INIS)

    Subrahmanyam, P.; Krishnapriya, B.; Rekha, D.; Reddy Prasad, P.; Chiranjeevi, P.

    2007-01-01

    A simple spectrophotometric method for the determination of U (VI) using 5-(3-phenolyl azo)-2-hydroxy-4-ethoxy propiophenone oxime (PHEPO) is developed. The reagent PHEPO was synthesized and used for extraction of uranium. At pH 8.5-10.0 uranium forms a purple colored complex with PHEPO which was then quantitatively extracted in chloroform showing maximum absorbance at wavelength of 380nm. The proposed method obeys Beer's law in the range of 1.2-19.0ppm. molar absorptivity and Sandelson's sensitivity of extracted species were calculated to be 1.750 x 104 lmol-1 cm-1 and 8.5 x 10-5 mg cm-2 respectively. The method was applied for the determination of uranium in synthetic and plant samples. It was found that the newly developed method is competent to those of standard methods. (author)

  3. 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.

  4. 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.

  5. 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.

  6. Extractive liquid-liquid spectrophotometric procedure for the determination of thiocyanate ions employing the ion pair reagent amiloride monohydrochloride

    International Nuclear Information System (INIS)

    Bashammakh, A.S.; Bahaffi, S.O.; Al-Sibaai, A.A.; Al-Wael, H.O.; El-Shahawi, M.S.

    2007-01-01

    An accurate, inexpensive and less laborious liquid-liquid extractive spectrophotometric procedure for the determination of thiocyanate ions in aqueous media has been developed. The method has been based upon the formation of a yellow colored complex ion associate of the ion-pairing reagent 1-(3, 5-diamino-6-chloropyrazinecarboxyl) guanidine hydrochloride monohydrate, namely amiloride hydrochloride, DPG + .Cl - and the thiocyanate ions in aqueous media containing HNO 3 (0.5 mol L -1 ) and subsequent extraction with 4-methyl-2-pentanone. The absorption electronic spectrum of the ion associate showed one well-defined peak at λ max 366 nm. The stoichiometric mole ratio of DPG + .Cl - to the thiocyanate ions is 1:1.The effective molar absorptivity (ε) of the ion associate at λ max 366 nm is 1.1 ± 0.1 x 10 4 L mol -1 cm -1 . The extraction constants (K d , K ex , and β) enabled a simple and convenient use of the developed binary ion associate for the extractive spectrophotometric determination of traces of thiocyanate ions in the aqueous media. Beer's law and Ringbom's plots are obeyed in the concentration range 0.05-10 and 0.1-7 μg mL -1 of the thiocyanate ions, respectively with a relative standard deviation of ±2.3%. The calculated lower limits of detection (LOD) and quantitation (LOQ) of the developed procedure for the thiocyanate ions were found equal to 0.02 and 0.066 μg mL -1 , respectively. The developed method has been applied for the determination of trace amounts of thicyanate ions in tap-, waste- and natural water samples and compared successfully with the reported methods at the 95% confidence level. The proposed method was also applied successfully for the determination of thiocyanate ions in saliva samples

  7. 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

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

    International Nuclear Information System (INIS)

    Xia Yuanxian; Qian Hesheng

    1986-01-01

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

  9. 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.

  10. 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)

  11. 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.

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

    Science.gov (United States)

    Ozyurt, Dilek; Demirata, Birsen; Apak, Resat

    2007-02-28

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

  13. Spectrophotometric Investigations of Macrolide Antibiotics: A Brief Review

    Directory of Open Access Journals (Sweden)

    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.

  14. 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.

  15. Flow injection analysis using carbon film resistor electrodes for amperometric determination of ambroxol.

    Science.gov (United States)

    Felix, Fabiana S; Brett, Christopher M A; Angnes, Lúcio

    2008-06-30

    Flow injection analysis (FIA) using a carbon film sensor for amperometric detection was explored for ambroxol analysis in pharmaceutical formulations. The specially designed flow cell designed in the lab generated sharp and reproducible current peaks, with a wide linear dynamic range from 5x10(-7) to 3.5x10(-4) mol L(-1), in 0.1 mol L(-1) sulfuric acid electrolyte, as well as high sensitivity, 0.110 Amol(-1) L cm(-2) at the optimized flow rate. A detection limit of 7.6x10(-8) mol L(-1) and a sampling frequency of 50 determinations per hour were achieved, employing injected volumes of 100 microL and a flow rate of 2.0 mL min(-1). The repeatability, expressed as R.S.D. for successive and alternated injections of 6.0x10(-6) and 6.0x10(-5) mol L(-1) ambroxol solutions, was 3.0 and 1.5%, respectively, without any noticeable memory effect between injections. The proposed method was applied to the analysis of ambroxol in pharmaceutical samples and the results obtained were compared with UV spectrophotometric and acid-base titrimetric methods. Good agreement between the results utilizing the three methods and the labeled values was achieved, corroborating the good performance of the proposed electrochemical methodology for ambroxol analysis.

  16. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  18. 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.

  19. Spectrophotometric Determination of Gemifloxacin Mesylate in Pharmaceutical Formulations Through Ion-Pair Complex Formation

    Directory of Open Access Journals (Sweden)

    Marothu Vamsi Krishna

    2008-01-01

    Full Text Available Four simple and sensitive ion-pairing spectrophotometric methods have been described for the assay of gemifloxacin mesylate (GFX either in pure form or in pharmaceutical formulations. The developed methods involve formation of colored chloroform extractable ion-pair complexes of the drug with safranin O (SFN O and methylene blue (MB in basic medium; Napthol blue 12BR (NB 12BR and azocaramine G (AG in acidic medium. The extracted complexes showed absorbance maxima at 525, 650, 620 and 540 nm for SFN O, MB, NB 12BR and AG, respectively.Beer's law is obeyed in the concentration ranges 3-15, 4-20, 2-10 and 2-10 μg/mL with molar absorptivity of 2.81 × 104, 2.20 x 104, 4.02 × 104 and 4.15 × 104 L mole−1 cm−1 and relative standard deviation of 0.077, 0.104, 0.080 and 0.103% for SFN O, MB, NB 12BR and AG, respectively. These methods have been successfully applied for the assay of drug in pharmaceutical formulations. No interference was observed from common pharmaceutical adjuvants. Results of analysis were validated statistically and through recovery studies.

  20. Spectrophotometric Method for the Determination of Atmospheric Cr Pollution as a Factor to Accelerated Corrosion

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    Dereje Homa

    2017-01-01

    Full Text Available The effect of Cr(VI pollution on the corrosion rate of corrugated iron roof samples collected from tanning industry areas was investigated through simulated laboratory exposure and spectrophotometric detection of Cr(III deposit as a product of the reaction. The total level of Cr detected in the samples ranged from 113.892 ± 0.17 ppm to 53.05 ± 0.243 ppm and showed increasing trend as sampling sites get closer to the tannery and in the direction of tannery effluent stream. The laboratory exposure of a newly manufactured material to a simulated condition showed a relatively faster corrosion rate in the presence of Cr(VI with concomitant deposition of Cr(III under pH control. A significant (P = 0.05 increase in the corrosion rate was also recorded when exposing scratched or stress cracked samples. A coupled redox process where Cr(VI is reduced to a stable, immobile, and insoluble Cr(III accompanying corrosion of the iron is proposed as a possible mechanism leading to the elevated deposition of the latter on the materials. In conclusion, the increased deposits of Cr detected in the corrugated iron roof samples collected from tanning industry zones suggested possible atmospheric Cr pollution as a factor to the accelerated corrosion of the materials.

  1. 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

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

    Science.gov (United States)

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

    2017-08-01

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

  3. Spectrophotometric Method for the Determination of Atmospheric Cr Pollution as a Factor to Accelerated Corrosion.

    Science.gov (United States)

    Homa, Dereje; Haile, Ermias; Washe, Alemayehu P

    2017-01-01

    The effect of Cr(VI) pollution on the corrosion rate of corrugated iron roof samples collected from tanning industry areas was investigated through simulated laboratory exposure and spectrophotometric detection of Cr(III) deposit as a product of the reaction. The total level of Cr detected in the samples ranged from 113.892 ± 0.17 ppm to 53.05 ± 0.243 ppm and showed increasing trend as sampling sites get closer to the tannery and in the direction of tannery effluent stream. The laboratory exposure of a newly manufactured material to a simulated condition showed a relatively faster corrosion rate in the presence of Cr(VI) with concomitant deposition of Cr(III) under pH control. A significant ( P = 0.05) increase in the corrosion rate was also recorded when exposing scratched or stress cracked samples. A coupled redox process where Cr(VI) is reduced to a stable, immobile, and insoluble Cr(III) accompanying corrosion of the iron is proposed as a possible mechanism leading to the elevated deposition of the latter on the materials. In conclusion, the increased deposits of Cr detected in the corrugated iron roof samples collected from tanning industry zones suggested possible atmospheric Cr pollution as a factor to the accelerated corrosion of the materials.

  4. 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.

  5. Spectrophotometric determination of cyclotrimethylenetrinitramine (RDX) in explosive mixtures and residues with the Berthelot reaction.

    Science.gov (United States)

    Uzer, A; Erçağ, E; Apak, R

    2008-03-31

    On-site colorimetric methods are a valuable, cost-effective tool to assess the nature and extent of contamination in remediated sites and to enable on-site screening for police criminology laboratories. The existing colorimetric method for cyclotrimethylenetrinitramine (RDX) based on a Griess reaction suffers from the non-quantitative reduction to nitrite and from the unstable character of HNO2 in acidic medium. Thus we propose a novel spectrophotometric RDX assay in explosive mixtures and residues, based on (Zn+HCl) reduction of RDX in a microwave oven, followed by neutralization of the reduction products to ammonia and low molecular-weight amines, and Berthelot reaction of these amine-compounds with phenol and hypochlorite in alkaline medium to give an intensely blue indophenol dye absorbing at 631nm. The molar absorptivity and limit of detection (LOD) for RDX were (1.08+/-0.04)x10(4) L mol(-1) cm(-1) and 0.18 mg L(-1), respectively. Application of the method to synthetic mixture solutions of RDX and trinitrotoluene (TNT) at varying proportions showed that there was minimal interference from TNT (which could be compensated for by dicyclohexylamine colorimetry), since the Berthelot reaction was essentially non-responsive to m-substituted anilines derived from TNT upon (Zn+HCl) reduction. The proposed method was successfully applied to military-purpose explosive mixtures of (RDX+inert matter) such as Comp A5, Comp C4, and Hexal P30, and to (RDX+TNT) mixtures such as Comp B. The molar absorptivity of RDX was much higher than that of either ammonium or nitrate; RDX could be effectively separated from ammonium and nitrate in soil mixtures, based on solubility differences. The Berthelot method for RDX was statistically validated using Comp B mixtures against standard HPLC equipped with a Hypersil C-18 column with (40% MeOH-60% H2O) mobile phase, and against gas chromatography-thermal energy analysis (GC-TEA) system.

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

    Directory of Open Access Journals (Sweden)

    Shipra Singh

    2012-01-01

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

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

    Directory of Open Access Journals (Sweden)

    S Singh

    2012-01-01

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

  8. 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.

  9. Validation of a spectrophotometric method to determine ciprofibrate content in tablets

    Directory of Open Access Journals (Sweden)

    Guilherme Nobre Lima do Nascimento

    2011-03-01

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

  10. Spectrophotometric titrations: Application to the determination of some elements in uranium solutions; Les titrages spectrophotometriques: Application a la determination de quelques elements dans les solutions d'uranium

    Energy Technology Data Exchange (ETDEWEB)

    L' Her, M [Commissariat a l' Energie Atomique, Fontenay-aux-Roses (France). Centre d' Etudes Nucleaires

    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) [French] Le but de ce travail est l'application des titrages spectrophotometriques a l'analyse des solutions uraniferes. Nous avons ete amenes a examiner les principes generaux de ces titrages, principes qu'il nous est apparu necessaire de rappeler. Dans une premiere partie nous traiterons donc d'une facon generale des titrages spectrophotometriques, en examinant leur principe fondamental, leur mise en oeuvre ainsi que les possibilites diverses de dosage. Nous examinerons aussi les avantages de la methode de titrage, en insistant notamment sur la possibilite de faire des dosages successifs. La possibilite d'application de ces titrages spectrophotometriques a l'analyse des solutions uraniferes sera le sujet de la deuxieme partie: nous y decrivons le dosage de quelques especes, dans les solutions d'uranium (VI). A cette deuxieme partie nous joindrons une annexe experimentale comportant une description de l'appareillage que

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

    Directory of Open Access Journals (Sweden)

    Masoud Reza Shishehbore

    2013-01-01

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

  12. Indirect spectrophotometric determination of small amounts of selenium(IV) and arsenic(V) by simple extraction using flotation columns.

    Science.gov (United States)

    Mostafa, G A; Ghazy, S E

    2001-10-01

    A simple, rapid and selective procedure for the indirect spectrophotometric determination of Se(IV) and As(V) has been developed. It is based on the reduction of Se(IV) to Se(0) and As(V) to As(III) with hydroiodic acid (KI + HCl). The liberated iodine, equivalent to each analyte, is quantitatively extracted with oleic acid (HOL) surfactant. The iodine-HOL system exhibits its maximum absorbance at 435 nm. The different analytical parameters affecting the extraction and determination processes have been examined. The calibration graphs were found to be linear over the ranges 5-120 and 0.25-20 ppm of Se(IV) and As(V), with lower detection limits of 2.5 and 0.15 ppm and molar absorptivities of 1 x 10(4) and 0.5 x 10(4) dm3 mol(-1) cm(-1), respectively. Sandell's sensitivity was calculated to be 0.0078 and 0.0149 microg/cm2 in the same order. The relative standard deviation for five replicate analyses of 40 ppm Se(IV) and 4 ppm As(V) were 1.0 and 0.9%, respectively. The proposed procedure in the presence of EDTA as a masking agent for foreign ions has been successfully applied to the determination of Se(IV) in a reference sample and As(V) in copper metal, in addition to their determination in spiked and polluted water samples.

  13. Spectrophotometric determination of ruthenium(III) and rhodium(III) after extraction of their cyclohexylthioglycolate complexes into chloroform

    International Nuclear Information System (INIS)

    Rao, A.L.J.; Gupta, Usha; Puri, B.K.

    1986-01-01

    Cyclohexylthioglycolate has been used as a reagent for the spectrophotometric determination of ruthenium(III) and rhodium(III) after the extraction of their complexes into chloroform. Various parameters involved in the extraction have been studied and the composition of the extracted complex has been established in each instance. Ruthenium and rhodium complexes are extracted into chloroform in the pH ranges 5.0-9.0 and 9.0-12.5, respectively. The ruthenium complex absorbs strongly at 365 nm, whereas the rhodium complex shows a maximum absorption at 345 nm. Beer's law is obeyed over the concentration range 6-96 μg for ruthenium and 2-41 μg for rhodium in 10 ml of the chloroform solution. The molar absorptivities are 5.02 x 10 3 l mol -1 cm -1 for ruthenium and 1.60 x 10 4 l mol -1 cm -1 for rhodium. Ten replicate determinations on a sample solution containing 60.3 μg of ruthenium or 20.6 μg of rhodium gave mean absorbances of 0.300 and 0.320 with standard deviations of 0.0021 and 0.0025 and relative standard deviations of 0.70% and 0.78%, respectively. The interference of various ions has been studied and the method has been applied to the determination of the metals in various synthetic samples. Conditions have also been developed for the simultaneous determination of ruthenium and rhodium. (author)

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

    Directory of Open Access Journals (Sweden)

    Shrikant H. Patil

    2012-12-01

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

  15. Spectrophotometric Determination of the Trace Amount of Thallium in Water and Urine Samples by Novel Oxidative Coupling Reaction

    Directory of Open Access Journals (Sweden)

    P. Nagaraja

    2009-01-01

    Full Text Available A novel, simple, rapid, sensitive and selective method has been proposed for the trace determination of thallium by spectrophotometric detection. This method is based on the oxidation of MBTH (3-methyl-2-benzothiazolinone hydrazone hydrochloride by thallium(III to form diazonium cation, which couples with IPH (Imipramine hydrochloride in phosphoric acid medium at room temperature giving a blue colored species having a maximum absorption at 635 nm. The reagents and manifold variables influences on the sensitivity were investigated and the optimum reaction conditions have been established. The calibration curve was found to be linear over the range 0.1-5 μg mL-1 with the molar absorptivity and Sandell’s sensitivity of 2.9x104 L mol-1 cm-1, 0.0071 μg cm-2 respectively. The tolerance limit of the method towards various ions usually associated with thallium has been detected. The relative standard deviation for five replicate determination of 2μg mL-1 thallium was 0.47%. The method has been successfully applied for the determination of thallium(ІΙΙ and thallium(I in synthetic, standard reference materials, water and urine samples with satisfactory results. The performance of the proposed method was evaluated in terms of student’s t-test and variance ratio F-test, to find out the significance of proposed method over the reported methods.

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

    Science.gov (United States)

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

    2015-03-15

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

  17. Spectrophotometric determination of uranium using 2-(2- Thiazolylazo-p-Cresol (TAC in the presence of surfactants

    Directory of Open Access Journals (Sweden)

    Teixeira Leonardo Sena Gomes

    1999-01-01

    Full Text Available A sensitive and selective spectrophotometric method is proposed for the rapid determination of uranium using 2-(2- Thiazolylazo-p-Cresol (TAC. The reaction between TAC and uranium (VI is instantaneous at pH 6.5 and the absorbance remains stable for over 3 h. N-cetyl-N,N,N-trimethylamonium bromide (CTAB and triton X-100 are used for increasing the sensitivity and solubility of the system respectively. The method allows the determination of uranium in the range from 0.30 to 12.0 mug mL-1 with a molar absorptivity of 1.31 x 10(4 L mol-1 cm-1 and features a detection limit of 26 ng mL-1 at 588 nm. The selectivity of the reagent was improved by the use of (1,2-cyclohexylenedinitrilo tetraacetic acid (CyDTA as masking agent. The proposed method has been successfully applied to the determination of uranium in mine drainage waters. The precision (R.S.D. < 2% and the accuracy obtained were satisfactory.

  18. Speciative determination of total V and dissolved inorganic vanadium species in environmental waters by catalytic–kinetic spectrophotometric method

    Directory of Open Access Journals (Sweden)

    Ramazan Gürkan

    2017-02-01

    Full Text Available A kinetic determination of V(V as a catalyst was spectrophotometrically performed by using the indicator reaction of Gallamine blue (GB+ and bromate at pH 2.0. The reaction was followed by measuring absorbance change for a fixed-time of 3 min at 537 nm. The variables such as reagent concentration, pH, buffer concentration, ionic strength and temperature were optimized to improve the selectivity and sensitivity. Under the optimized conditions, the determination of V(V was performed in the range 1–100 μg L−1 with limits of detection and quantification of 0.31 and 0.94 μg L−1. The developed kinetic method is sufficiently sensitive, selective and simple. It was successfully applied to the speciative determination of total V and inorganic dissolved vanadium species, V(V and V(IV in environmental water samples. The oxidizing property of permanganate is used to differentiate between V(IV and V(V species. The V(IV content was found by subtracting the V(V content from those of total V. The recovery is above 95% for V(V spiked samples. Additionally, the accuracy was validated by analysis of a certified water sample, CRM TMDA-53.3, and the results were in good agreement with the certified value.

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

    Directory of Open Access Journals (Sweden)

    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.

  20. Flotation-spectrophotometric determination of ruthenium in the Ru(IV)-chloride-rhodamine 6G-toluene system

    International Nuclear Information System (INIS)

    Balcerzak, M.

    1985-01-01

    The reduction of RuO 4 in hydrochloric acid has been examined. A sensitive flotation-spectrophotometric method of the determination of ruthenium based on the ion associate formed by the anionic chlorid complex of ruthenium RuCl 2- 6 with the basic dye Rhodamine 6G (R6G) has been developed. The solution of the ion associate obeys Beer's law up to the concentration of 0.25 μg Ru/ml. The ion associate precipitates when the aqueous solution is shaken with toluene. The separated compound is dissolved in acetone. The molar absorptivity (epsilon) at 530 nm is 5.1 x 10 5 l x mole -1 x cm -1 . The relative standard deviation is 3-7%. The mole ratio of Ru:R6G in the complex is 1:5. Osmium reacts similarly. The determination of ruthenium can be selective after the preliminary separation of osmium as OsO 4 . The method was applied to the determination of microgram amounts of ruthenium in crucible platinum. (Author)

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

    Directory of Open Access Journals (Sweden)

    Paulo Roberto da Silva Ribeiro

    2014-09-01

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

  2. 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

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2010-09-15

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

  4. Flow injection spectrophotometry using natural reagent from Morinda citrifolia root for determination of aluminium in tea.

    Science.gov (United States)

    Tontrong, Sopa; Khonyoung, Supada; Jakmunee, Jaroon

    2012-05-01

    A flow injection (FI) spectrophotometric method with using natural reagent extracted from Morinda citrifolia root has been developed for determination of aluminium. The extract contained anthraquinone compounds which could react with Al(3+) to form reddish complexes which had maximum absorption wavelength at 499.0nm. The extract could be used as a reagent in FI system without further purification to obtain pure compound. A sensitive method for determination of aluminium in concentration range of 0.1-1.0mgL(-1), with detection limit of 0.05mgL(-1) was achieved. Relative standard deviations of 1.2% and 1.7% were obtained for the determination of 0.1 and 0.6mgL(-1) Al(3+) (n=11). Sample throughput of 35h(-1) was achieved with the consumption of 3mL each of carrier and reagent solutions per injection. The developed method was successfully applied to tea samples, validated by the FAAS standard method. The method is simple, fast, economical and could be classified as a greener analytical method. Copyright © 2011 Elsevier Ltd. All rights reserved.

  5. A Course at the Master Level Demonstrating Quality Assurance by Spectrophotometric Determination of Iron in two experiments

    DEFF Research Database (Denmark)

    In two experiments, the first a batch determination of iron, and the second determination of iron by flow injection analysis, the students perform a number of repetitions. The measurements were repeated until it became possible to estimate which one of the two methods exhibited the better perform...

  6. 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)

  7. 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 %.

  8. Utility of Charge Transfer and Ion-Pair Complexation for Spectrophotometric Determination of Eletriptan Hydrobromide in Pure and Dosage Forms

    Directory of Open Access Journals (Sweden)

    Ayman A. Gouda

    2013-01-01

    Full Text Available Three simple, sensitive, and accurate spectrophotometric methods have been developed for the determination of eletriptan hydrobromide (ELT in pure and dosage forms. The first two methods are based on charge transfer complex formation between ELT and chromogenic reagents quinalizarin (Quinz and alizarin red S (ARS producing charge transfer complexes which showed an absorption maximum at 569 and 533 nm for Quinz and ARS, respectively. The third method is based on the formation of ion-pair complex between ELT with molybdenum(V-thiocyanate inorganic complex in hydrochloric acid medium followed by extraction of the colored ion-pair with dichloromethane and measured at 470 nm. Different variables affecting the reactions were studied and optimized. Beer's law is obeyed in the concentration ranges 2.0–18, 1.0–8.0, and 2.0–32 μg mL−1 for Quinz, ARS, and Mo(V-thiocyanate, respectively. The molar absorptivity, Sandell sensitivity, detection, and quantification limits are also calculated. The correlation coefficients were ≥0.9994 with a relative standard deviation (R.S.D%. of ≤0.925. The proposed methods were successfully applied for simultaneous determination of ELT in tablets with good accuracy and precision and without interferences from common additives, and the validity is assessed by applying the standard addition technique, which is compared with those obtained using the reported method.

  9. Spectrophotometric determination of palladium (II) with rubeanic acid (RA) in presence of pyridine, piperidine and 3-picoline

    International Nuclear Information System (INIS)

    Hassiruzzaman, M.; Hossain, M.A.; Rahman, G.M.M.; Kamal, A.S.M.; Kabir, M.H.; Mustafa, A.I.

    1999-01-01

    Unpretentious and exclusive methods for the spectrophotometric determination of trace amount of divalent palladium (II) have been developed with rubeanic acid (dithio-oxamide) in presence of secondary ligands like pyridine, piperidine and 3-picoline. Both direct and extraction spectrophotometry showed that coloured rubeanates are only stable in acidic medium. The violent yellow coloured products are formed below ph 5.0 with an absorption maxima at 416.0 and 422.0 (pyridine), 405.0 and 416.5 (piperidine) and 418.0 and 422.0 (3-picoline) both in direct and isoamyl alcohol (IAA) extracted system, respectively. Results indicate that the highest sensitivity and molar absorptivity of Pd-RA pyridine system in direct spectrophotometry were 0.01497 mu g Pd(II) cm/sup -2/ and 7107.89 L mol sup -1/ cm/sup -1/ respectively. IAA extracted Pd-RA-piperidine system was found to give a sensitivity of 0.01087 mu g(Pd(II) cm /sup -2/ and molar absorptivity of 9788.80 L mol /sup -1/ cm/sup -1/ which were the highest of all the system. The effects due to variation of pH, reagent concentrations, order of addition of reagents, time, temperature and solvent media on the absorption spectra have been investigated and the optimum conditions determined. The effects of diverse ions and their tolerance limit have also been studies. (author)

  10. 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.

  11. 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.

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

    Science.gov (United States)

    Heydari, Rouhollah; Hosseini, Mohammad; Zarabi, Sanaz

    2015-01-01

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

  13. First derivative spectrophotometric determination of granisetron hydrochloride in presence of its hydrolytic products and preservative and application to pharmaceutical preparations.

    Science.gov (United States)

    Hewala, Ismail I; Bedair, Mona M; Shousha, Sherif M

    2013-04-01

    Granisetron is a selective 5-HT3 receptor antagonist used in prevention and treatment of chemotherapy-induced nausea and vomiting. The drug is available in tablet dosage form and parenteral dosage form containing benzyl alcohol as a preservative. The main route of degradation of granisetron is through hydrolysis. The present work describes the development of a simple, rapid, and reliable first derivative spectrophotometric method for the determination of granisetron in presence of its hydrolytic products as well as the formulations adjuvant and benzyl alcohol. The method is based on the measurement of the first derivative response of granisetron at 290 nm where the interference of the hydrolytic products, the co-formulated adjuvant and benzyl alcohol is completely eliminated. The proposed method was validated with respect to specificity, linearity, selectivity, accuracy, precision, robustness, detection, and quantification limits. Regression analysis showed good correlation between the first derivative response and the concentration of granisetron over a range of 8-16 μg ml(-1) . Statistical analysis proved the accuracy of the proposed method compared with a reference stability indicating high performance liquid chromatography method. The described method was successfully applied to the determination of granisetron in different batches of tablets and ampoules. The assay results obtained in this study strongly encourage us to apply the validated method for the quality control and routine analysis of tablets and parenteral preparations containing granisetron. Copyright © 2012 John Wiley & Sons, Ltd.

  14. The determination of hyperoside in the flower and leaf of hawthorn (Crataegus oxycantha and Crataegus monogyna by the spectrophotometric method

    Directory of Open Access Journals (Sweden)

    Mihajlović Dušanka

    2006-01-01

    Full Text Available The flower and leaf of hawthorn contains many active components, used in the production of pharmaceutical preparations for cardiotonic, anti-hypertonic anti-hypotonic, artherosclerotic, anti-arithmic and anti-anemic groups. According to the ROTTE list (1996, 159 of 1800 pharmaceutical preparations contain components from hawthorn. Due to the remedial action of hyperoside and other flavonoids from hawthorn, their determination is important for the standardization of extract and preparation quality. The extraction of the flavonoids from a mixture of hawthorn (C. oxycantha and C. monogyna flower and leaf was carried out by percolation with 40% and 70% (v/v ethanol. In order to determine the content of total flavonoids calculated as hyperoside spectrophotometric method with aluminium(lll chloride as a colour reagent at 425 nm was applied. The total flavonoid content in the herbal material mixture was 0.483%, in 40% and 70% (v/v ethanolic liquid extract it was 138 mg/100 cm3 and 157 mg/100 cm, respectively. The extraction degree of total flavonoids with 40% and 70% (v/v ethanolic solutions was 57.14% and 65.01% respectively. The yield of total flavonoids in the dry extract was 63% in regard to the herbal mixure content.

  15. Determination of DPPH Radical Oxidation Caused by Methanolic Extracts of Some Microalgal Species by Linear Regression Analysis of Spectrophotometric Measurements

    Directory of Open Access Journals (Sweden)

    Ulf-Peter Hansen

    2007-10-01

    Full Text Available The demonstrated modified spectrophotometric method makes use of the 2,2-diphenyl-1-picrylhydrazyl (DPPH radical and its specific absorbance properties. Theabsorbance decreases when the radical is reduced by antioxidants. In contrast to otherinvestigations, the absorbance was measured at a wavelength of 550 nm. This wavelengthenabled the measurements of the stable free DPPH radical without interference frommicroalgal pigments. This approach was applied to methanolic microalgae extracts for twodifferent DPPH concentrations. The changes in absorbance measured vs. the concentrationof the methanolic extract resulted in curves with a linear decrease ending in a saturationregion. Linear regression analysis of the linear part of DPPH reduction versus extractconcentration enabled the determination of the microalgae’s methanolic extractsantioxidative potentials which was independent to the employed DPPH concentrations. Theresulting slopes showed significant differences (6 - 34 μmol DPPH g-1 extractconcentration between the single different species of microalgae (Anabaena sp.,Isochrysis galbana, Phaeodactylum tricornutum, Porphyridium purpureum, Synechocystissp. PCC6803 in their ability to reduce the DPPH radical. The independency of the signal on the DPPH concentration is a valuable advantage over the determination of the EC50 value.

  16. Application of a Lithium-ion Selective Metallacrown to Extraction-Spectrophotometric Determination of Lithium in Saline Water.

    Science.gov (United States)

    Katsuta, Shoichi; Saito, Yuki; Takahashi, Suguru

    2018-01-01

    The solvent-extraction behavior of Li + and Na + with a Li + selective metallacrown, [{Ru(η 6 -3,5-dimethylanisole)(2,3-pyridinediolate)} 3 ], was investigated in the presence of organic dye anions, 3',3″,5',5″-tetrabromophenolphthalein ethyl ester ([TBPE] - ), 2,6-dichloroindophenolate, and picrate ([pic] - ). Each alkali metal ion was extracted as a 1:1:1 ternary complex of the metal ion, metallacrown, and anion. The Li + /Na + extraction selectivity is anion dependent and highest with [pic] - . Therefore, we devised an extraction-spectrophotometric determination method for Li + in saline water based on the extraction of Li + using the metallacrown and [pic] - for high selectivity and subsequent replacement of [pic] - in the extracted species with [TBPE] - for high sensitivity. When applying this to artificial seawater samples containing known concentrations of Li + , a linear relationship was observed between the absorbance at 571 nm of the organic phase and the Li + concentration in the samples. By this method, the determination of Li + at the sub-ppm level in natural seawater is possible.

  17. Spectrophotometric determination of thorium with 2-(2-thiazolylazo)-5-dimethylaminophenol in the presence of cetylpyridinium chloride

    International Nuclear Information System (INIS)

    Tsurumi, Chikao; Furuya, Keiichi; Kamada, Hitoshi.

    1979-01-01

    The method of the spectrophotometric determination of thorium with 2-(2-thiazolylazo)-5-dimethylaminophenol (TAM) in the presence of cetylpyridinium chloride (CPC) and methanol was investigated. Thorium reacts with TAM in the presence of CPC and methanol to form reddish-violet ternary complex. The maximum adsorbance at 570 nm in constant in the pH range from 4.3 to 4.8 and stable for at least 90 min. Beer's law is obeyed up to 2.4 μg cm -3 of thorium. The molar extinction coefficient of this wavelength is 8.5 x 10 4 dm 3 mol -1 cm -1 and the absorption sensitivity for thorium was 2.7 x 10 -3 μg cm -2 per 0.001 of absorbance. The molar ratio of thorium to TAM in the complex was confirmed to be 1 : 3 by both the continuous variation and mole ratio methods. The conditional formation constant of the ternary complex is 2.8 9 x 10 18 . Ba (II), Be (II), Ce (III), La (III) and Sr (II) can be masked by the addition of 2.0 cm 3 of 1 x 10 -2 mol dm -3 thiosemicarbazide solution as a masking agent. Co (II), Fe (III), Ni (II), V (V) and Zr (IV) seriously interfere with the determination of Th (IV) and show positive errors, while Fe (II), Mo (VI), Ta (V) and W (VI) interfere with it and do negative errors. (author)

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

    Directory of Open Access Journals (Sweden)

    SOFIJA M. RANČIĆ

    2009-08-01

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

  19. Indirect flow injection determination of N-acetyl-L-cysteine using cerium(IV) and ferroin

    International Nuclear Information System (INIS)

    Vieira, Heberth Juliano; Fatibello-Filho, Orlando

    2005-01-01

    An indirect flow injection spectrophotometric procedure is proposed for the determination of N-acetyl-L-cysteine in pharmaceutical formulations. In this system, ferroin ([Fe(II)-(fen) 2 ] 2+ ) in excess, with a strong absorption at 500 nm, is oxidized by cerium(IV) yielding cerium(III) and [Fe(III)-(fen) 2 ] 3+ (colorless), thus producing a baseline. When N-acetyl-L-cysteine solution is introduced into the flow injection system, it reacts with cerium(IV) increasing the analytical signal in proportion to the drug concentration. Under optimal experimental conditions, the linearity of the analytical curve for N-acetyl-L-cysteine ranged from 6.5x10 -6 to 1.3x10 -4 mol L -1 . The detection limit was 5.0x10 -6 mol L -1 and recoveries between 98.0 and 106% were obtained. The sampling frequency was 60 determinations per hour and the RSD was smaller than 1.4% for 2.2x10 -5 mol L -1 N-acetyl-L-cysteine. (author)

  20. Stopped-flow injection method for determination of phosphate in soils and fertilisers

    Directory of Open Access Journals (Sweden)

    Jaroon Jakmunee

    2008-02-01

    Full Text Available A stopped-flow injection system for the determination of phosphate has been developed. It involves the phosphate-molybdate-ascorbic acid reactions in the molybdenum blue method. The system is controlled by a semi-automatic stopped-FI analyser with a light emitting diode (LED-colorimeter for monitoring the absorbance change relating to the concentration of a reaction product formed during the stopping period while the injected zone of a standard or sample is being in the flow cell. The slope of the FIAgram obtained is linearly proportional to the reaction rate, which depends on the phosphate concentration. Effects of concentration of reagents, viz. sodium molybdate, ascorbic acid and nitric acid, on the slope of the FIAgram were studied. The suitable concentration is 0.02 M, 0.25 %w/v and 0.15 M, respectively. A linear calibration graph in the range of 0.3-6.0 mg P L-1 was employed for the determination of phosphate in soil and fertiliser samples. The results obtained agree well with those from a standard spectrophotometric method.

  1. Spectrophotometric speciation of Fe(II) and Fe(III) using hydrazone-micelle systems and flow injections

    International Nuclear Information System (INIS)

    Khojali, Inas Osman

    1999-04-01

    Two hydrazones were synthesised, namely salicylhyrazone (SH) and trihydroxyacetophenone (THAPH) were synthesised with the objective of developing a method for determining of Fe(II) and Fe(III) in the presence of each other and hence the total iron.those hydrazones were selected so as to combine the ability of phenolic compounds to complex Fe(III) ions and the complexing characteristics of hydrazones. The complexes of Fe(II) S H and Fe(III) S H as well those of Fe(II)-THAPH and Fe(III)-THAPH had shown maximum absorbance at λ=412 nm which was not not modified by presence of micelles i.e. sodium n-dodecyl sulphate (SDS) and n-hexa dodecyl pyridinium bromide. The maximum absorbance for all complexes takes place around a neutral pH. Generally, in addition, of n-hexa dodecylpyridinium bromide to fe(II)-SH and Fe(III)-SH absorbance of the complexes increases with increasing the concentration of the micelle. The effects of the addition of sodium n-dodecyle sulphate (SDS) to Fe(III)-SH is also studied. Generally, increasing the concentration of the micelle decrease the absorbance of the complexes. To study the effect of the presence of Fe(II) and Fe(III) on the determination of each other,mixtures of Fe(II)-SH and Fe(III)-SH are studied. However, the use of ascorbic acid as a reducing reagent for Fe(III) did not produce the needed results but non reducible results, which may be due to the masking effect of ascorbic acid and thus making the metal not available to the ligand. However, conversion of Fe(II) to Fe(III) prior to the determination was avoided as this requires the use of oxidant, which will oxidise the ligand as well. To establish the condition for the maximum absorbance of THAPH complexes, the effect of the base was investigated by using sodium and ammonium hydroxide. Generally, increasing the concentration of the base decreases the abosrbance. as expected, ammonium hydroxide produced positive results than sodium hydroxide. After establishing the optimum Fi

  2. Liquid-liquid extraction of ruthenium(III) thiocyanate with hexamethylphosphoramide: direct spectrophotometric determination in the organic phase

    International Nuclear Information System (INIS)

    Mitra, B.K.; Pal, B.K.; Chowdhury, R.P.

    1982-01-01

    Ru(III) thiocyanate has been extracted with hexamethylphosphoramide(HMPA) in methyl isobutyl ketone (MIBK). Thus the extractability, sensitivity and selectivity are improved over the simple binary Ru(III) thiocyanate system in spectrophotometric determination of ruthenium in the organic phase. The maximum colour develops on the steam bath, at the acidity range of 1.5 - 2.5 M with HCl and ammonium thiocyanate concentration range of 0.25 - O.5 M. The colour is completely extractable in MIBK when 1.5 - 3.0 ml HMPA is used and show maximum absorbance at 570 nm. The colour system obeys Beer's law for 0.7 - 13 μg Ru/ml and the optimum concentration range is 2 - 13 μg/ml. The molar absorptivity and sensitivity are 6940 l . mole -1 cm -1 and 0.0145 μg/cm 2 respectively. The percent relative error is 2.72%. The method is very simple and does not require oxidation and subsequent distillation. The method can be applied in the presence of osmium. (Author)

  3. 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.

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

    Directory of Open Access Journals (Sweden)

    Mohamed A. El Hamd

    2013-01-01

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

  5. Spectrophotometric determination of pKa's of 1-hydroxybenzotriazole and oxime derivatives in 95% acetonitrile-water

    International Nuclear Information System (INIS)

    Fathallah, M.F.; Khattab, S.N.

    2011-01-01

    1-hydroxybenzotriazole derivatives are used with carbodiimide as additives to generate active esters during peptide bond formation. They are also used as additives during the peptide bond formation. Dissociation constants of the 1-hydroxybenzotriazole (HOBt) and its derivatives, 1-hydroxy-6-chloro benzotriazole, 1-hydroxy-6-trifluoro methylbenzotriazole, 1-hydroxy-6-nitrobenzo-triazole were determined spectrophotometrically in 95% acetonitrile-water. In addition, 7-aza-1-hydroxybenzotriazole (7-HOAt) and 4-aza-1-hydroxybenzotriazole (4-HOAt) were also studied. Recently, oxyma was reported as a good replacement for the benzotriazole derivatives. As alcoholic components of active esters, the oximes seem to be good leaving groups. Therefore it was expected, that the strongly acidic and nucleophilic oximes, which possess electron-withdrawing groups in the molecule, are suitable as additives during the peptide bond formation. The dissociation constant of some oximes, such as diethyl 2-(hydroxyimino)malonate, ethyl 2-cyano-2-(hydroxyimino)acetate (oxyma), hydroxycarbonimidoyl dicyanide and N-hydroxypicolinimidoyl cyanide in 95% acetonitrile-water are reported. (author)

  6. Spectrophotometric and chemometric methods for determination of imipenem, ciprofloxacin hydrochloride, dexamethasone sodium phosphate, paracetamol and cilastatin sodium in human urine

    Science.gov (United States)

    El-Kosasy, A. M.; Abdel-Aziz, Omar; Magdy, N.; El Zahar, N. M.

    2016-03-01

    New accurate, sensitive and selective spectrophotometric and chemometric methods were developed and subsequently validated for determination of Imipenem (IMP), ciprofloxacin hydrochloride (CIPRO), dexamethasone sodium phosphate (DEX), paracetamol (PAR) and cilastatin sodium (CIL) in human urine. These methods include a new derivative ratio method, namely extended derivative ratio (EDR), principal component regression (PCR) and partial least-squares (PLS) methods. A novel EDR method was developed for the determination of these drugs, where each component in the mixture was determined by using a mixture of the other four components as divisor. Peak amplitudes were recorded at 293.0 nm, 284.0 nm, 276.0 nm, 257.0 nm and 221.0 nm within linear concentration ranges 3.00-45.00, 1.00-15.00, 4.00-40.00, 1.50-25.00 and 4.00-50.00 μg mL- 1 for IMP, CIPRO, DEX, PAR and CIL, respectively. PCR and PLS-2 models were established for simultaneous determination of the studied drugs in the range of 3.00-15.00, 1.00-13.00, 4.00-12.00, 1.50-9.50, and 4.00-12.00 μg mL- 1 for IMP, CIPRO, DEX, PAR and CIL, respectively, by using eighteen mixtures as calibration set and seven mixtures as validation set. The suggested methods were validated according to the International Conference of Harmonization (ICH) guidelines and the results revealed that they were accurate, precise and reproducible. The obtained results were statistically compared with those of the published methods and there was no significant difference.

  7. 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.)

  8. 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.

  9. Spectrophotometric determination of phenylpropanolamine in dosage forms using dimethylaminobenzaldehyde as a derivatizing reagent

    International Nuclear Information System (INIS)

    Rind, F.M.A.; Khushawar, M.Y.

    2000-01-01

    Phenylpropanolamine (PPA) was extracted from slightly alkaline medium in chloroform, derivatized with dimethylaminobenzaldehyde (DAB) and determined by spectrophotometry at 377 nm. Beer's law was obeyed for 4.5-13.5 mu g. After the extraction of PPA in organic phase, paracetamole remaining in the aqueous phase could also be determined by spectrophotometry at 291 nm. The method was applied for the determination of PPA and paracetamole in the pharmaceutical preparations. Tavagyl-D, sinulab and Panadol labels with RSD within 0.4-0.8%. (author)

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

    International Nuclear Information System (INIS)

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

    1991-01-01

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

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

    Directory of Open Access Journals (Sweden)

    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.

  12. Indirect spectrophotometric determination of piroxicam and tenoxicam through oxidation with potassium permanganate

    OpenAIRE

    A.S. Amin; H.A. Dessouki; K.M. Khalil

    2010-01-01

    Three rapid, simple, accurate and selective validated spectrophtometric methods (A, B and C) for the determination of piroxicam (PX) and tenoxicam (TX) in bulk sample and in dosage forms are described. The methods are based on the oxidation of the studied drugs by a known excess of potassium permanganate in sulfuric acid medium and subsequent determination of unreacted oxidant by reacting it with Methylene Blue (Basic Blue 9) dye (method A), Acid Red 27 (Amaranth) dye (method B) and Acid Oran...

  13. Spectrophotometric simultaneous determination of Rabeprazole Sodium and Itopride Hydrochloride in capsule dosage form

    Science.gov (United States)

    Sabnis, Shweta S.; Dhavale, Nilesh D.; Jadhav, Vijay. Y.; Gandhi, Santosh V.

    2008-03-01

    A new simple, economical, rapid, precise and accurate method for simultaneous determination of rabeprazole sodium and itopride hydrochloride in capsule dosage form has been developed. The method is based on ratio spectra derivative spectrophotometry. The amplitudes in the first derivative of the corresponding ratio spectra at 231 nm (minima) and 260 nm were selected to determine rabeprazole sodium and itopride hydrochloride, respectively. The method was validated with respect to linearity, precision and accuracy.

  14. Spectrophotometric determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction.

    Science.gov (United States)

    Lemos, Valfredo Azevedo; dos Santos, Liz Oliveira; Silva, Eldevan dos Santos; Vieira, Emanuel Vitor dos Santos

    2012-01-01

    A simple method for the determination of mercury in water samples after preconcentration using dispersive liquid-liquid microextraction is described. The procedure is based on the extraction of mercury in the form of a complex and its subsequent determination by spectrophotometry. The complex is formed between Hg(II) and 2-(2-benzothiazolylazo)-p-cresol. The detection at 650 nm is performed directly in the metal-rich phase, which is spread on a triacetylcellulose membrane. The method eliminates the need to use a cuvet or large quantities of samples and reagents. The parameters that influence the preconcentration were studied, and the analytical characteristics were determined. The enrichment factor and the consumptive index for this method were 64 and 0.16 mL, respectively. The LOD (3.3 microg/L) and LOQ (11.1 microg/L) were also determined. The accuracy of the method was tested by the determination of mercury in certified reference materials BCR 397 (Human Hair) and SRM 2781 (Domestic Sludge). The method was applied to the determination of mercury in samples of drinking water, sea water, and river water.

  15. Spectrophotometric determination of Sc in eriochrome cyanine R(chrome azurol S) - phosphatidyl choline system

    International Nuclear Information System (INIS)

    Xu, Y.; Chen, X.; Hu, Z.

    1987-01-01

    Eriochrome cyanine R(chrome azurol S) is used as a color reagent to determine Sc in the presence of phosphatidyl choline, eta = 3.7 * 10 4 (4.5 * 10 4 ). This method has been connected to extraction separation to determine Sc in the presence of rare earth elements, and good results have been obtained. Phosphatidyl choline(PC) is a biochemical reagent, which can be used as a surfactant. It has been reported that chrome azurol S(CAS) can be used to determine Be in the presence of PC but it has not been reported that eriochrome cyanine R(ECR) and CAS can been used to determine Sc in the presence of PC. This paper has put forward a method by which Sc can be determined. ECR (CAS) has been used as a color reagent and PC as a surfactant. Conditional experiments have been made and this method has been connected to extraction separation. Tributyl phosphate (TBP) extracts Sc from rare earth elements to make a determination and good results have been obtained

  16. Determination of Boron in soils and plants samples using spectrophotometric method

    International Nuclear Information System (INIS)

    Stas, J.; Hariri, Z.

    2011-10-01

    In this work, the concentration of boron in soil and plant samples was determined with UV-vis spectrophotometer by using azomethine-H as a complex reagent. The calibration curve for boron determination in the range of (0μ3 g.mL - 1) was constructed by plotting the measured absorption of the yellow azomethine-H-B complex at λmax = 412.6 nm against boron concentration in the aqueous phase. The detection limit, repeatability limit, intermediate precision, accuracy, and recovery coefficient of this method were calculated and found to be 0.021 μg.mL - 1, 0.335% , 0.81%, 2.93%, (98.4-101.5)% respectively. The influence of some foreign ions on the determination of boron were also investigated in detail, most of the studied ions, like iron, iodide, and calcium can be tolerated within the ranges of (20-35μg.mL-1), (3000-5000μg.mL - 1) , (15000-30000μg.mL - 1) respectively. This is due to the fact, that ascorbic acid and EDTA in the buffer masking reagent reaction system can be very effective in masking these ions. This method was found to be economic and suitable for boron determination in standard and local samples (soil, plant) and requires small amount of sample (1g). This method can also be applied for boron determination in water samples (drinking and industrial waste water).(author)

  17. Simultaneous spectrophotometric determination of binary mixtures of surfactants using continuous wavelet transformation

    International Nuclear Information System (INIS)

    Afkhami, Abbas; Nematollahi, Davood; Madrakian, Tayyebeh; Abbasi-Tarighat, Maryam; Hajihadi, Mitra

    2009-01-01

    This work presents a simple, rapid, and novel method for simultaneous determination of binary mixtures of some surfactants using continuous wavelet transformation. The method is based on the difference in the effect of surfactants Cetyltrimethylammoniumbromide (CTAB), dodecyl trimethylammonium bromide (DTAB), cetylpyridinium bromide (CPB) and TritonX-100 (TX-100) on the absorption spectra of complex of Beryllium with Chrome Azurol S (CAS) at pH 5.4. Binary mixtures of CTAB-DTAB, DTAB-CPB and CTAB-TX-100 were analyzed without prior separation steps. Different mother wavelets from the family of continuous wavelet transforms were selected and applied under the optimal conditions for simultaneous determinations. The proposed methods, under the working conditions, were successfully applied to simultaneous determination of surfactants in hair conditioner and mouthwash samples.

  18. 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.

  19. Spectrophotometric determination of quetiapine fumarate in pharmaceuticals and human urine by two charge-transfer complexation reactions

    Directory of Open Access Journals (Sweden)

    Vinay K.B.

    2012-01-01

    Full Text Available Two simple, rapid and accurate spectrophotometric procedures are proposed for the determination of quetiapine fumarate (QTF in pharmaceuticals and in spiked human urine. The methods are based on charge transfer complexation reactions of free base form of the drug (quetiapine, QTP, as n-electron donor (D, with either p-chloranilic acid (p-CAA (method A or 2,3-dichloro-5,6-dicyanoquinone (DDQ (method B as π-acceptors (A. The coloured charge transfer complexes produced exhibit absorption maxima at 520 and 540 nm, in method A and method B, respectively. The experimental conditions such as reagent concentration, reaction solvent and time have been carefully optimized to achieve the maximum sensitivity. Beer’s law is obeyed over the concentration ranges of 8.0 - 160 and 4.0 - 80.0 μg ml-1, for method A and method B, respectively. The calculated molar absorptivity values are 1.77 × 103 and 4.59 × 103 l mol-1cm-1, respectively, for method A and method B. The Sandell sensitivity values, limits of detection (LOD and quantification (LOQ have also been reported. The stoichiometry of the reaction in both cases was accomplished adopting the limiting logarithmic method and was found to be 1: 2 (D: A. The accuracy and precision of the methods were evaluated on intra-day and inter-day basis. The proposed methods were successfully applied for the determination of QTF in pharmaceutical formulations and spiked human urine.

  20. Catalytic and kinetic spectrophotometric method for determination of vanadium(V by 2,3,4-trihydroxyacetophenonephenylhydrazone

    Directory of Open Access Journals (Sweden)

    P.V. Chalapathi

    2014-12-01

    Full Text Available A new catalytic and kinetic spectrophotometric method for the determination of vanadium(V was studied using 2,3,4-trihydroxyacetophenonephenylhydrazone (THAPPH as an analytical reagent. The present method was developed on the catalytic effect of vanadium on oxidation of THAPPH by hydrogen peroxide in hydrochloric acid–potassium chloride buffer (pH = 2.8 at the 20th minute. The metal ion has formed 1:2 (M:L complex with THAPPH. Beer’s law was obeyed in the range 20–120 ng/mL of V(V at λmax 390 nm. The sensitivity of the method was calculated in terms of molar absorptivity (1.999 × 105 L mol−1cm−1 and Sandell’s sensitivity (0.000254 μg cm−2, shows that this method is more sensitive. The standard deviation (0.0022, relative standard deviation (0.56%, confidence limit (±0.0015 and standard error (0.0007 revealed that the developed method has more precision and accuracy. The stability constant was calculated with the help of Asmu’s (9.411 × 10−11 and Edmond’s & Birnbaum’s (9.504 × 10−11 methods at room temperature. The interfering effect of various cations and anions was also studied. The present method was successfully applied for the determination of vanadium(V in environmental and alloy samples. The method’s validity was checked by comparing the results obtained with atomic-absorption spectrophotometry and also by evaluation of results using F-test.

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

    Science.gov (United States)

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

    2012-03-01

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

  2. Analytical applications of some macro-schiff's bases for spectrophotometric determination of some metal ions

    International Nuclear Information System (INIS)

    Ahmed, N. A. M.

    2005-06-01

    In this research three schiff's bases PAD, N, NBPAD and N, NBHPAD were synthesized by condensation of o-phenylenediamine with p-aminoacetophenone, to give an intermediate which then further condensed with benzil, and 2,5 hexanedione, respectively, in ethanol to give macro schiff's bases. These schiff's bases were identified using I.R spectra, UV/VIS spectrophotometer, elemental analyzer, and melting point. Their applications as analytical reagents were studied using UV/VIS spectrophotometer with Pb(II), Cr(VI), Cu(II), Cd(II), V(V), Ni(II), Hg(II), Zn(II), Co(II), Fe(II) and Fe(III). Various parameters were investigated in order to find their optimum conditions for the analytical application of these schiff's bases. These include the effect of solvent, the effect of micelle as well as the presence of foreign metal ions. Good results were obtained for determination of Cr(VI), and V(V) with N, NBPAD in terms of linearity detection limit, and interference, and for the determination of Fe(II) with N, NBHPAD. The stoichiometry of some these complexes was determined. The study also showed a good results for the determination of Hg(II), and Pb(II) (two serious environmental pollutants) if interference is removed.(Author)

  3. 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.

  4. 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

  5. Study of a spectrophotometric method of plutonium determination in the organic phase

    International Nuclear Information System (INIS)

    Brutus, Andre

    1971-03-01

    The aim of this paper is to study a method of determining plutonium in the 'Purex' process organic phase, the minimum concentrations to be measured being about 10 -5 M. Spectrophotometry, at 665 nm, of the plutonium arsenazo III complex was carried out directly in the organic phase. Several complexes can be formed between arsenazo III and plutonium; the conditions under which a single complex is obtained, and also those for which this latter follows Beer's law, were determined. The nature and stability of the complex formed were studied, after which it was possible to calculate the equilibrium constant and the standard free enthalpy variation. The field application of the method was established from calculation of the regression line, the confidence limits, the detection limit and the sensitivity. Finally the principle of the elimination of certain troublesome cations in the medium involved was considered. (author) [fr

  6. Derivative spectrophotometric method for simultaneous determination of zofenopril and fluvastatin in mixtures and pharmaceutical dosage forms.

    Science.gov (United States)

    Stolarczyk, Mariusz; Maślanka, Anna; Apola, Anna; Rybak, Wojciech; Krzek, Jan

    2015-09-05

    Fast, accurate and precise method for the determination of zofenopril and fluvastatin was developed using spectrophotometry of the first (D1), second (D2), and third (D3) order derivatives in two-component mixtures and in pharmaceutical preparations. It was shown, that the developed method allows for the determination of the tested components in a direct manner, despite the apparent interference of the absorption spectra in the UV range. For quantitative determinations, "zero-crossing" method was chosen, appropriate wavelengths for zofenopril were: D1 λ=270.85 nm, D2 λ=286.38 nm, D3 λ=253.90 nm. Fluvastatin was determined at wavelengths: D1 λ=339.03 nm, D2 λ=252.57 nm, D3 λ=258.50 nm, respectively. The method was characterized by high sensitivity and accuracy, for zofenopril LOD was in the range of 0.19-0.87 μg mL(-1), for fluvastatin 0.51-1.18 μg mL(-1), depending on the class of derivative, and for zofenopril and fluvastatin LOQ was 0.57-2.64 μg mL(-1) and 1.56-3.57 μg mL(-1), respectively. The recovery of individual components was within the range of 100±5%. For zofenopril, the linearity range was estimated between 7.65 μg mL(-1) and 22.94 μg mL(-1), and for fluvastatin between 5.60 μg mL(-1) and 28.00 μg mL(-1). Copyright © 2015 Elsevier B.V. All rights reserved.

  7. Spectrophotometric determination of various polyanions with polymeric film optodes using microtiter plate reader.

    Science.gov (United States)

    Dürüst, Nedime; Meyerhoff, Mark E; Unal, Nazangül; Naç, Sibel

    2011-08-05

    Polycation-sensitive membrane optodes based on the chromoionophore 2',7'-dichlorofluorescein octadecylester (DCFOE) have previously been developed and used for determination of heparin via a titrimetric method. In this study, it is shown that some other important polyanions such as PPS (pentosan polysulfate), DNA, xanthan, Na-alginate, and carrageenan (food additive) can also be readily determined by using DCFOE-based microtiter plate-format optodes (MPOs) and polycationic titrants that bind these polyanionic species. The optical sensors are prepared with poly(vinyl chloride) (PVC), polyurethane (PU), bis(2-ethylhexyl)sebacate (DOS), and 2',7'-dichlorofluorescein octadecylester (DCFOE) and exhibit reproducible and sensitive absorbance changes in response to the varying polycationic titrant concentrations. Three different polycations; protamine, poly-l-lysine and poly-l-arginine, are employed as titrants. The method has a detection limit of 1 μg mL(-1), and a dynamic range of 1-40 μg mL(-1). After the quantitative determinations are successfully demonstrated in buffered solutions, similar titrations are also performed in real samples. The method is validated by recovery studies in these samples. The average polyanion recoveries were quantitative [99.7(±1.3) % for pastry cream with vanillin (protamine titrant); 100.4 (±3.3) % for pastry gel with strawberry(PLA titrant), and 102.9(±2.0) % for pastry gel with strawberry (PLL titrant)]. Copyright © 2011 Elsevier B.V. All rights reserved.

  8. Extraction and atomic absorption spectrophotometric determination of iron and ruthenium by using potassium xanthates

    Energy Technology Data Exchange (ETDEWEB)

    Aihara, M; Kiboku, M [Kinki Univ., Higashi-Osaka, Osaka (Japan)

    1981-06-01

    Potassium xanthates (potassium o-alkyl dithiocarbonate; KRX) react with many metal ions, and so the complex formation with iron (II, III) ion and the extraction of their complexes has been studied to some extent, but those of ruthenium (III) have not been. Iron-xanthate and ruthenium-xanthate complexes can be extracted into methyl isobutyl ketone (MIBK) from weakly acidic solution to weakly alkaline solution. For quantitative extraction of iron (20 ..mu..g/40 ml), KRX concentration should be above 2.0 x 10/sup -2/ mol dm/sup -3/ of KEtX, 1.0 x 10/sup -2/ mol dm/sup -3/ of KPrX, and 5.0 x 10/sup -3/ mol dm/sup -3/ of KBtX and KPeX, and for that of ruthenium (202 ..mu..g/40 ml), it should be above 2.0 x 10/sup -1/ mol dm/sup -3/ of KEtX and KPrX. Formation constant of ruthenium-xanthate complexes is presumed to be small. A 100-fold excess of Ni(II), Co(II), Cu(II), WO/sub 4//sup 2 -/, PO/sub 4//sup 3 -/, CrO/sub 4//sup 2 -/, and Cr/sub 2/O/sub 7//sup 2 -/ interfered with the determination of iron, however, the interferences are eliminated by adding 5 ml of 0.1 mol dm/sup -3/ ascorbic acid solution. For the determination of ruthenium, a 50-fold excess of Ag(I), Hg(II), Pb(II), Zn(II), Mn(II), Cr(III), and Pt(II), or a 100-fold excess of NO/sub 2//sup -/, S/sub 2/O/sub 3//sup 2 -/, CrO/sub 4//sup 2 -/ and Cr/sub 2/O/sub 7//sup 2 -/, respectively, interfered. The coefficient of variation after each ten runs, ranges from 0.9% to 3.2% in the determination of 10 ..mu..g, 20 ..mu..g, and 30 ..mu..g of iron, and from 1.4% to 4.3% in the determination of 100 ..mu..g, 200 ..mu..g, and 300 ..mu..g of ruthenium. The determination limit in aqueous samples is 0.02 ppm for iron and 0.2 ppm for ruthenium, when the volume ratio of aqueous phase to organic phase (MIBK) is 10:1.

  9. Spectrophotometric determination of molybdenum with non-ionic surfactant and thiocyanate

    International Nuclear Information System (INIS)

    Hayashi, Kenjiro; Yamamoto, Atsuo; Fujimura, Yasue; Ito, Saburo.

    1980-01-01

    Although the molybdenum (V)-thiocyanate complex is quite stable in non-aqueous solvent such as ether, the complex in dilute acidic solution is unstable. However, this unstable complex was stabilized remarkably by addition of some non-ionic surfactant such as Triton X-100 (alkylphenolpolyoxyethylene ether). The application of this stabilizing effect of the surfactant to the photometric determination of trace amounts of molybdenum with thiocyanate resulted in an increase in the sensitivity. The rate of formation of the Mo(V)-SCN complex was affected by the presence of ferrous ion and its rate constant was proportional to the concentration of Fe(II). The stabilizing effect of the surfactant on the yellowish orange coloration can be understood if we assume that the Mo(V)-SCN complex is incorporated into the micelles of Triton X-100 as [H 2 + , MoO(CNS) 5 2- ]. The optimum condition for the determination of molybdenum is as follows: concentration of sulfuric acid, 0.22 mol dm -3 ; Triton X-100, 0.8%; ascorbic acid, 0.32 mol dm -3 ; thiocyanate, 0.30 mol dm -3 ; iron, 40 mg dm -3 ; standing time for coloration, 10 min and more. Beer's law was obeyed over the range (1 -- 233) μg/50 cm 3 . The molar absorption coefficient at 468 nm was 1.7 2 x 10 4 cm -1 mol -1 dm 3 . The maximum permissible limits of foreign ions (mg/50 cm 3 ) were as follows: Ni(30); Co(12); W(VI) (2); Cu, Zn, V(V) (3); Cr(VI) (5). Large amounts of iron interfered, but this interference was removed by addition of the same amount of iron to the reagent blank. Trace amounts of molybdenum in steel was determined by this method with satisfactory results. (author)

  10. Indirect spectrophotometric determination of piroxicam and tenoxicam through oxidation with potassium permanganate

    Directory of Open Access Journals (Sweden)

    A.S. Amin

    2010-04-01

    Full Text Available Three rapid, simple, accurate and selective validated spectrophtometric methods (A, B and C for the determination of piroxicam (PX and tenoxicam (TX in bulk sample and in dosage forms are described. The methods are based on the oxidation of the studied drugs by a known excess of potassium permanganate in sulfuric acid medium and subsequent determination of unreacted oxidant by reacting it with Methylene Blue (Basic Blue 9 dye (method A, Acid Red 27 (Amaranth dye (method B and Acid Orange 7 (orange II dye (method C, in the same medium at a suitable λmax = 660, 520 and 485 nm, respectively. The reacted oxidant was found to be corresponding to the drug content. Regression analysis of Beer-Lambert plots showed good correlations in the concentration ranges 1.0-8.0, 1.0-9.0 and 1.0-7.2 μg mL-1 using methods A, B and C, respectively, for PX and 0.3-7.0, 0.3-1.6 and 0.3-2.5 μg mL-1 using methods A, B and C, respectively, for TX. The stoichiometric ratios for the cited drugs to oxidant were studied. The optimum reaction conditions and other analytical parameters were evaluated. The proposed methods were applied successfully to determine the examined drugs either in pure form or pharmaceutical formulations with good accuracy and precision. The relative standard deviations were ≤ 0.33 with recoveries 98.9-101.7% for PX and ≤ 0.49 with recoveries 99.4-102.0% for TX.

  11. Analysis of uranium and of some of its compounds and alloys. Copper spectrophotometric determination

    International Nuclear Information System (INIS)

    Copper determination in uranium, uranium oxides (UO 2 , UO 3 , U 3 O 8 ), ammonium diuranate, U-Al-Fe alloy (700 ppm Al and 300 ppm Fe) and U-Mo alloy (1.1 percent Mo) by acid dissolution reduction of copper by hydroxylamine hydrochloride and formation of a complex with diquinolyle-2,2' amyl alcohol (pH value 6 to 7) and spectrophotometry at 550 nm. The method is applicable for copper content between 5 to 40 ppm in respect of uranium contained in the material [fr

  12. Solid-phase extraction-spectrophotometric determination of uranium(VI) in natural waters

    Energy Technology Data Exchange (ETDEWEB)

    Sadeghi, Susan; Mohammadzadeh, Darush [Department of Chemistry, University of Birjand, Birjand (Iran); Yamini, Yadollah [Department of Chemistry, Tarbiat Moddars University, Tehran (Iran)

    2003-03-01

    A method for the extraction and determination of uranyl ion in natural waters using octadecyl bonded silica membrane disks modified with piroxicam and spectrophotometry with arsenazo(III) is proposed. The perconcentration step was studied with regard to experimental parameters such as amount of extractant, type and amount of eluent, pH, flow rates and tolerance limit of diverse ions on the recovery of uranyl ion. The limit of detection of the proposed method is 0.4 {mu}g L{sup -1} of uranyl. The method was applied to the recovery of uranyl from different water samples. (orig.)

  13. Solid-phase extraction-spectrophotometric determination of uranium(VI) in natural waters

    International Nuclear Information System (INIS)

    Sadeghi, Susan; Mohammadzadeh, Darush; Yamini, Yadollah

    2003-01-01

    A method for the extraction and determination of uranyl ion in natural waters using octadecyl bonded silica membrane disks modified with piroxicam and spectrophotometry with arsenazo(III) is proposed. The perconcentration step was studied with regard to experimental parameters such as amount of extractant, type and amount of eluent, pH, flow rates and tolerance limit of diverse ions on the recovery of uranyl ion. The limit of detection of the proposed method is 0.4 μg L -1 of uranyl. The method was applied to the recovery of uranyl from different water samples. (orig.)

  14. Spectrophotometric determination of uranium traces in zircaloy-4 and zirconium sponge

    International Nuclear Information System (INIS)

    Correia, R.J.; Weber de D'Alessio, Ana; Zucal, R.H.

    1980-01-01

    The uranium contents of the zircaloy-4 which is used for the fabrication of the fuel cans for the PHWR Atucha and Embalse nuclear power stations must not exceed 3.ppM. A method was developed for performing that control, involving the separation of the uranium from its matrix by partition chromatography and its determination by spectrophotometry with Arsenazo (III). This method is applied within the range of 0.2 to 10 ppM, obtaining a relative standard deviation of 6% for U contents of 3 ppm. (M.E.L.) [es

  15. Study on Solid Phase Extraction and Spectrophotometric Determination of Nickel in Waters and Biological Samples

    International Nuclear Information System (INIS)

    Hu, Qiufen; Yang, Guangyu; Huang, Zhangjie; Yin, Jiayuan

    2004-01-01

    A sensitive, selective and rapid method for the determination of nickel based on the rapid reaction of nickel(II) with QADMAA and the solid phase extraction of the Ni(II)-QADMAA chelate with C 18 membrane disks has been developed. In the presence of pH 6.0 buffer solution and sodium dodecyl sulfonate (SDS) medium, QADMAA reacts with nickel to form a violet complex of a molar ratio of 1 : 2 (nickel to QADMAA). This chelate was enriched by solid phase extraction with C 18 membrane disks. An enrichment factor of 50 was obtained by elution of the chelates form the disks with the minimal amount of isopentyl alcohol. The molar absorptivity of the chelate was 1.32 x 10 5 L mol -1 cm -1 at 590 nm in the measured solution. Beer's law was obeyed in the range of 0.01-0.6 μg/mL. This method was applied to the determination of nickel in water and biological samples with good results

  16. Utilization of a Green Brominating Agent for the Spectrophotometric Determination of Pipazethate HCl in Pure Form and Pharmaceutical Preparations

    Directory of Open Access Journals (Sweden)

    Ayman A. Gouda

    2013-01-01

    Full Text Available Five simple, accurate, and sensitive spectrophotometric methods (A–E have been described for the indirect assay of pipazethate HCl (PZT either in pure form or in pharmaceutical preparations. The proposed methods are based on the bromination of pipazethate HCl with a solution of excess bromate-bromide mixture in hydrochloric acid medium and subsequent estimation of the residual bromine by different reaction schemes. In the first three methods (A–C, the determination of the residual bromine is based on its ability to bleach the color of methyl orange, indigo carmine, or thymol blue dyes and measuring the absorbance at 520, 610, and 550 nm for methods A, B, and C, respectively. Methods D and E 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 for method D and the resulting iron(III is complexed with thiocyanate and the absorbance is measured at 480 nm for method E. The different experimental parameters affecting the development and stability of the color are carefully studied and optimized. Regression analysis of the Beer-Lambert plots showed good correlation in the concentration ranges of 0.5–8.0 μg . The apparent molar absorptivity, Sandell's sensitivity, detection and quantitation limits were evaluated. The proposed methods have been applied and validated successfully for the analysis of the drug in its pure form and pharmaceutical formulations with mean recoveries of 99.94%–100.15% and relative standard deviation ≤1.53. No interference was observed from a common pharmaceutical adjuvant. Statistical comparison of the results with the reference method shows excellent agreement and indicates no significant difference in accuracy and precision.

  17. Spectrophotometric determination of sildenafil citrate in pure form and in pharmaceutical formulation using some chromotropic acid azo dyes

    Science.gov (United States)

    Issa, Y. M.; El-Hawary, W. F.; Youssef, A. F. A.; Senosy, A. R.

    2010-04-01

    Two simple and highly sensitive spectrophotometric methods were developed for the quantitative determination of the drug sildenafil citrate (SC), Viagra, in pure form and in pharmaceutical formulations, through ion-associate formation reactions (method A) with mono-chromotropic acid azo dyes, chromotrope 2B (I) and chromotrope 2R (II) and ion-pair reactions (method B) with bi-chromotropic acid azo dyes, 3-phenylazo-6-o-carboxyphenylazo-chromotropic acid (III), bis-3,6-(o-hydroxyphenylazo)-chromotropic acid (IV), bis-3,6-(p-N,N-dimethylphenylazo)-chromotropic acid (V) and 3-phenylazo-6-o-hydroxyphenylazo-chromotorpic acid (VI). The reaction products, extractable in methylene chloride, were quantitatively measured at 540, 520, 540, 570, 600 and 575 nm using reagents, I-VI, respectively. The reaction conditions were studied and optimized. Beer's plots were linear in the concentration ranges 3.3-87.0, 3.3-96.0, 5.0-115.0, 2.5-125.0, 8.3-166.7 and 0.8-15.0 μg mL -1 with corresponding molar absorptivities 1.02 × 10 4, 8.34 × 10 3, 6.86 × 10 3, 5.42 × 10 3, 3.35 × 10 3 and 2.32 × 10 4 L mol -1 cm -1 using reagents I-VI, respectively. The limits of detection and Sandell's sensitivities were calculated. The methods were successfully applied to the analysis of commercial tablets (Vigoran) and the recovery study reveals that there is no interference from the common excipients that are present in tablets. Statistical comparison of the results was performed with regard to accuracy and precision using Student's t- and F-tests at 95% confidence level. There is no significant difference between the reported and proposed methods with regard to accuracy and precision.

  18. Sequential injection redox or acid-base titration for determination of ascorbic acid or acetic acid.

    Science.gov (United States)

    Lenghor, Narong; Jakmunee, Jaroon; Vilen, Michael; Sara, Rolf; Christian, Gary D; Grudpan, Kate

    2002-12-06

    Two sequential injection titration systems with spectrophotometric detection have been developed. The first system for determination of ascorbic acid was based on redox reaction between ascorbic acid and permanganate in an acidic medium and lead to a decrease in color intensity of permanganate, monitored at 525 nm. A linear dependence of peak area obtained with ascorbic acid concentration up to 1200 mg l(-1) was achieved. The relative standard deviation for 11 replicate determinations of 400 mg l(-1) ascorbic acid was 2.9%. The second system, for acetic acid determination, was based on acid-base titration of acetic acid with sodium hydroxide using phenolphthalein as an indicator. The decrease in color intensity of the indicator was proportional to the acid content. A linear calibration graph in the range of 2-8% w v(-1) of acetic acid with a relative standard deviation of 4.8% (5.0% w v(-1) acetic acid, n=11) was obtained. Sample throughputs of 60 h(-1) were achieved for both systems. The systems were successfully applied for the assays of ascorbic acid in vitamin C tablets and acetic acid content in vinegars, respectively.

  19. Spectrophotometric determination of uranium (VI) with arsenazo III in a nitric medium

    International Nuclear Information System (INIS)

    Yamaura, Mitiko; Wada, Luciana Yukie; Ribeiro, Fernando Castilho

    2002-01-01

    Arsenazo III is an organic reagent usually used for the photometric determination of various elements, including the uranium, thorium, plutonium, barium, strontium, hafnium, bismuth and the rare earth elements. The reactions of arsenazo III with many elements are very sensitive and, consequently is not specific for any element. Arsenazo III with U(VI) gives a 1:1 coloured complex in diluted acid solution of pH 1 to 3, and in strong acid media forming 1:1, 1:2 and 1:3 species. In this work, a detailed study of the influence of pH is described. The stability of formed complex and the interference of Fe(III) ions were also studied. (author)

  20. New azo coupling reactions for visible spectrophotometric determination of salbutamol in bulk and pharmaceutical preparations

    International Nuclear Information System (INIS)

    Dhahir, S. A.

    2011-01-01

    The purpose of the present study was to develop a new, simple, cheap, fast, accurate, and sensitive colorimetric methods that can be used for the determination of salbutamol sulphate drug in pure from as well as in pharmaceutical formulations. The method is based on the reaction 2-chloro-4-nitroaniline with nitrite in acid medium to form diazonium ion, which is coupled with of salbutamol in basic medium to form azo dyes, showing yellow color and absorption maxima at 463 nm. Beer's law is obeyed in the concentration of 4-48μg/ml. The molar absorptivity and san dell's sensitivity are 5.27x103 L mole-1 cm-1, 0.015 μgcm-2, respectively. The optimum reaction conditions and other analytical parameters were evaluated. (author).

  1. Spectrophotometric method for quantitative determination of total anthocyanins and quality characteristics of roselle (Hibiscus sabdariffa).

    Science.gov (United States)

    Sukwattanasinit, Tasamaporn; Burana-Osot, Jankana; Sotanaphun, Uthai

    2007-11-01

    A simple, rapid and cost-saving method for the determination of total anthocyanins in roselle has been developed. The method was based on pH-differential spectrophotometry. The calibration curve of the major anthocyanin in roselle, delphinidin 3-sambubioside (Dp-3-sam), was constructed by using methyl orange and their correlation factor. The reliability of this developed method was comparable to the direct method using standard Dp-3-sam and the HPLC method. Quality characteristics of roselle produced in Thailand were also reported. Its physical quality met the required specifications. The overall chemical quality was herein surveyed for the first time and it was found to be the important parameter corresponded to the commercial grading of roselle. Total contents of anthocyanins and phenolics were proportional to the antiradical capacity.

  2. Selective floatation-spectrophotometric determination of tellurium (4) with papaverine and butyl rhodamine B

    International Nuclear Information System (INIS)

    Skripchuk, V.G.

    1981-01-01

    It is shown, that papaverine reacts with a bromide complex of tellurium (4) to form a compound readily floated by toluene. The floatation is carried out from an aqueous solution, 5.2 M in H 2 SO 4 , 0.2 M in KBr and 5.4x10 -3 M in papaverine. The absorbance is a function of tellurium (4) concentration over a range of 5-100 μg Te/5 ml. Such a highly sensitive reagent as butylrhodamine B can be effectively substituted for papaverine. The floatation results in better selectivity. The method makes it possible to determine tellurium in blister, anodic and cathodic copper without matrix preseparation [ru

  3. Spectrophotometric determination and thermodynamic studies of the charge transfer complexes of azelastine-HCl

    Directory of Open Access Journals (Sweden)

    Nahla N. Salama

    2011-06-01

    Full Text Available Three charge transfer complexes of azelastine as n-donor with π acceptors, dichloro-dicyanobenzoquinone (DDQ, chloranilic acid (CA and tetracyanoquinodimethane (TCNQ were prepared in acetonitrile. They yield a radical anions measured at 456, 520 and 841 nm within concentration ranges of 8.0–72, 40–320 and 1.6–14.4 μg mL−1 with good correlation coefficients (r = 0.9996–0.9998. The molar absorptivities and association constants for the colored products were evaluated using the Benesi–Hildebrand equation. The free energy change (ΔG0 and the enthalpy of formation (ΔH0 as well as the entropy (ΔS0 were determined for the reaction product with TCNQ. The methods were successfully applied to the analysis of azelastine in its pharmaceutical preparations, where no interferences could be observed from the additives commonly present in the eye drops or nasal spray as proved by good mean recoveries of 98.89 ± 1.06–99.54 ± 1.84%. The results were compared, favorably with the manufacturer method and validated according to ICH guidelines.

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

    Directory of Open Access Journals (Sweden)

    A. S. Amin

    2017-08-01

    formulations based on the formation of ion-pair complexes with sudun II (SII, sudan (IV (SIV and sudan black B (SBB. 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 SII, SIV and SBB 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 SII, SIV, and SBB 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.

  5. 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.

  6. Selective Precipitation of Thorium lodate from a Tartaric Acid-Hydrogen Peroxide Medium Application to Rapid Spectrophotometric Determination of Thorium in Silicate Rocks and in Ores

    Science.gov (United States)

    Grimaldi, F.S.

    1957-01-01

    This paper presents a selective iodate separation of thorium from nitric acid medium containing d-tartaric acid and hydrogen peroxide. The catalytic decomposition of hydrogen peroxide is prevented by the use of 8quinolinol. A few micrograms of thorium are separated sufficiently clean from 30 mg. of such oxides as cerium, zirconium, titanium, niobium, tantalum, scandium, or iron with one iodate precipitation to allow an accurate determination of thorium with the thoronmesotartaric acid spectrophotometric method. The method is successful for the determination of 0.001% or more of thorium dioxide in silicate rocks and for 0.01% or more in black sand, monazite, thorite, thorianite, eschynite, euxenite, and zircon.

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

    International Nuclear Information System (INIS)

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

    1980-01-01

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

  8. SPECTROPHOTOMETRIC DETERMINATION OF PIZOTEFIN ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    respectively. Different experimental conditions for the two methods were optimized. Beer's law was obeyed in the concentration ranges of .... mixed in various proportions and the volume was diluted in a 10-mL volumetric flask with acetonitrile. The absorbance of the resulting solutions was measured at optimum wavelengths.

  9. Extraction spectrophotometric analyzer

    International Nuclear Information System (INIS)

    Batik, J.; Vitha, F.

    1985-01-01

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

  10. STRATEGY DETERMINATION FOR DIESEL INJECTION USING AVL ESE DIESEL

    Directory of Open Access Journals (Sweden)

    Vrublevskiy, A.

    2012-06-01

    Full Text Available Based on the design of research AVL FIRE ESE DIESEL environment they proposed to reduce noise and NOx emissions in the exhaust gases of the automobile diesel engine using two-stage injection. The parameters of the fuel for idling are determined.

  11. Spectrofluorimetric determination of cerium by flow injection analysis

    International Nuclear Information System (INIS)

    Liu Shaorong; Meng Jian; Liu Wenhua

    1990-01-01

    A spectrofluorimetric method for the determination of cerium (λ ex/em:251/365 nm) in hydrochloric acid solution by flow injection analysis is presented. It has well developed the normal spectrofluorimetric method for determination of cerium and has made: 1, the determination procedure shortened; 2, the determination speed increased to about 180 samples per hour; 3, the determination range widened to 0.05-100.0 ppm CeO 2 , abouot two times as wide as the normal spectrofluorimetric method; and 4, the relative standard deviation lessened (about 0.47% for 0.1 ppm CeO 2 , n = 13)

  12. 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.

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

    Directory of Open Access Journals (Sweden)

    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.

  14. 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.

  15. General procedure for the determination of trace amounts of iodine in natural water samples of unknown composition by spectrophotometric titration

    International Nuclear Information System (INIS)

    Pesavento, M.; Profumo, A.

    1985-01-01

    Concentrated hydrochloric acid is added to samples of natural waters containing 2 x 10 -7 to 5 x 10 -5 M iodine and the solutions are then oxidised with hydrogen peroxide on a boiling water-bath. They are then reduced with sodium sulphite, which is subsequently removed by bubbling a stream of inert gas through the solution. All of the inorganic iodine, now present in the solution in the -1 oxidation state, can be titrated spectrophotometrically with standard potassium iodate solution, following a method previously described in which interferences from oxidants and reductants are eliminated. (author)

  16. General procedure for the determination of trace amounts of iodine in natural water samples of unknown composition by spectrophotometric titration

    Energy Technology Data Exchange (ETDEWEB)

    Pesavento, M.; Profumo, A. (Pavia Univ. (Italy). Dip. di Chimica Generale)

    1985-02-01

    Concentrated hydrochloric acid is added to samples of natural waters containing 2 x 10/sup -7/ to 5 x 10/sup -5/ M iodine and the solutions are then oxidised with hydrogen peroxide on a boiling water-bath. They are then reduced with sodium sulphite, which is subsequently removed by bubbling a stream of inert gas through the solution. All of the inorganic iodine, now present in the solution in the -1 oxidation state, can be titrated spectrophotometrically with standard potassium iodate solution, following a method previously described in which interferences from oxidants and reductants are eliminated.

  17. 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.

  18. Simultaneous spectrophotometric determination of trace copper, nickel, and cobalt ions in water samples using solid phase extraction coupled with partial least squares approaches

    Science.gov (United States)

    Guo, Yugao; Zhao, He; Han, Yelin; Liu, Xia; Guan, Shan; Zhang, Qingyin; Bian, Xihui

    2017-02-01

    A simultaneous spectrophotometric determination method for trace heavy metal ions based on solid-phase extraction coupled with partial least squares approaches was developed. In the proposed method, trace metal ions in aqueous samples were adsorbed by cation exchange fibers and desorbed by acidic solution from the fibers. After the ion preconcentration process, the enriched solution was detected by ultraviolet and visible spectrophotometer (UV-Vis). Then, the concentration of heavy metal ions were quantified by analyzing ultraviolet and visible spectrum with the help of partial least squares (PLS) approaches. Under the optimal conditions of operation time, flow rate and detection parameters, the overlapped absorption peaks of mixed ions were obtained. The experimental data showed that the concentration, which can be calculated through chemometrics method, of each metal ion increased significantly. The heavy metal ions can be enriched more than 80-fold. The limits of detection (LOD) for the target analytes of copper ions (Cu2 +), cobalt ions (Co2 +) and nickel ions (Ni2 +) mixture was 0.10 μg L- 1, 0.15 μg L- 1 and 0.13 μg L- 1, respectively. The relative standard deviations (RSD) were less than 5%. The performance of the solid-phase extraction can enrich the ions efficiently and the combined method of spectrophotometric detection and PLS can evaluate the ions concentration accurately. The work proposed here is an interesting and promising attempt for the trace ions determination in water samples and will have much more applied field.

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

    Directory of Open Access Journals (Sweden)

    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.

  20. New method for simultaneous determination of Fe(II) and Fe(III) in water using flow injection technique

    International Nuclear Information System (INIS)

    Kozak, J.; Gutowski, J.; Kozak, M.; Wieczorek, M.; Koscielniak, P.

    2010-01-01

    The method exploits the possibilities of flow injection gradient titration in a system of reversed flow with spectrophotometric detection. In the developed approach a small amount of titrant (EDTA) is injected into a stream of sample containing a mixture of indicators (sulfosalicylic acid and 1,10-phenanthroline). In acid environment sulfosalicylic acid forms a complex with Fe(III), whereas 1,10-phenanthroline forms a complex with Fe(II). Measurements are performed at wavelength λ = 530 nm when radiation is absorbed by both complexes. After injection EDTA replaces sulfosalicylic acid and forms with Fe(III) more stable colourless complex. As a result, a characteristic 'cut off' peak is registered with a width corresponding to the Fe(III) concentration and with a height corresponding to the Fe(II) concentration. Calibration was performed by titration of four two-component standard solutions of the Fe(II)/Fe(III) concentrations established in accordance with 2 2 factorial plan. The method was tested with the use of synthetic samples and then it was applied to the analysis of water samples taken from artesian wells. Under optimized experimental conditions Fe(II) and Fe(III) were determined with precision less than 0.8 and 2.5% (RSD) and accuracy less than 3.2 and 5.1% (relative error) within the concentration ranges of 0.1-3.0 and 0.9-3.5 mg L -1 of both analytes, respectively.

  1. Atomic absorption spectrophotometric determination of microgram levels of Co, Ni, Cu, Pb, and Zn in soil and sediment extracts containing large amounts of Mn and Fe

    Science.gov (United States)

    Chao, T.T.; Sanzolone, R.F.

    1973-01-01

    An atomic absorption spectrophotometric method has been developed for the determination of seven metal ions in the hydroxylamine extract of soils and sediments. Mn, Fe, and Zn are directly determined in the aqueous extract upon dilution. Co, Ni, Cu, and Pb in a separate aliquot of the extract are chelated with APDC (ammonium pyrrolidine dithiocarbamate) and extracted into MIBK (methyl isobutyl ketone) before determination. Data are presented to show the quantitative recovery of microgram levels of Co, Ni, Cu, and Pb by APDC-MIBK chelation-extraction from synthetic solutions containing as much as 2,000 ug/ml (micrograms per milliliter) Mn or 50 ug/ml Fe. Recovery of known amounts of the metal ions from sample solutions is equally satisfactory. Reproducible results are obtained by replicate analyses of two sediment samples for the seven metals.

  2. Simultaneous spectrophotometric determination of lycopene beta-carotene concentrations in carotenoid mixtures of the extracts from tomatoes, papaya and orange juice

    International Nuclear Information System (INIS)

    Hammed, M.A.; Bello, I.A.; Oladoye, S.O.

    2013-01-01

    A simple and inexpensive spectrophotometric equation model for the simultaneous determination of lycopene and Beta-carotene concentrations in a mixture of carotenoids is proposed. Lycopene could be exclusively determined (with the relative accuracy of more than 95%) using the absorbance data at 502 nm. Because quantifying the Beta-carotene concentration in a carotenoid minture using the sole absorbance at 450 nm is prone to error, an equation to determine the concentration of this compound from the absorbances data at two wavelengths was modeled. Using the modeled equations to re-check the molar absorptivity of lycopene at 472 nm, the value obtained was about 98% close to the value reported in literature. The relative accuracy of the predicted concentrations of two carotenoids using the modeled equations is a function of the ratio of these carotenoids in the samples. (author)

  3. 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.

  4. Image resolution influence on determination of resin injection rock mass

    Science.gov (United States)

    Wang, Weixing; Hakami, Eva

    2006-01-01

    In the context of nuclear waste repositories, an important approach to understanding brittle rock mass behavior to integrate new and powerful observational and numerical methods with multi-functional 3-D imaging and visualization techniques. Since 1994, Swedish Nuclear Fuel and Waste Management Company (SKB) have identified the need for a better understanding of radionuclide transport and retention processes in fractured rock. As a cooperation project between Sweden and China, we sampled a number of rock specimens for analyze rock fracture network by optical image technique. The samples are resin injected, in which way; opened fractures can be seen clearly by means of UV (Ultraviolet) light illumination. In the study period, we used different optical focuses to obtain the images from the same samples; we found that Image resolution influences on porosity determination of resin injected rock mass. This paper presents and discusses the six issues based on our research results: (1) Fracture porosity increases as camera focus distance decreases; (2) Porosity increases as illumination increases in resin injected fracture images; (3) To roughly estimate the porosity, the low resolution image can be used; (4) To collect more details of fracture information, the high resolution image is needed; (5) The resolution of image should be determined based on the aim of fracture analysis; (6) To acquire high resolution image, constructing a special illumination (standard) box maybe helpful to avoid light reflection and diffusion.

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

    Directory of Open Access Journals (Sweden)

    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.

  6. 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.

  7. A simple spectrophotometric method for the determination of arsenic in industrial and environmental samples using 2,4-Dihydroxy benzophenone-2-amino thiophenol.

    Science.gov (United States)

    Deepa, K; Lingappa, Y

    2014-04-24

    2,4-Dihydroxy benzophenone-2-amino thiophenol (BPBT) has been proposed as new analytical reagent for the direct non-extractive spectrophotometric determination of arsenic. The reagent reacts with arsenic in acidic medium (pH=6.0, sodium acetate-acetic acid buffer) to form light greenish yellow colored 1:1 (M:L) complex. Maximum absorbance was obtained at 343 nm and remains constant for over 24 h. The molar absorptivity and Sandell's sensitivity of BPBT are found to be 6.01×10(4) L mol(-1)cm(-1) and 0.0016 μg cm(-2) respectively. The system obeys Beer's law in the range of 0.125-2.637 μg/ml of As (III). Since BPBT method is more sensitive, it was applied for the determination of arsenic in some environmental water samples. Copyright © 2013 Elsevier B.V. All rights reserved.

  8. Simultaneous Spectrophotometric Determination of Copper, Nickel, and Zinc Using 1-(2-Thiazolylazo)-2-Naphthol in the Presence of Triton X-100 Using Chemometric Methods

    International Nuclear Information System (INIS)

    Low, Kah Hin; Zain, Sharifuddin Md; Abas, Mhd. Radzi; Misran, Misni; Mohd, Mustafa Ali

    2009-01-01

    Multivariate models were developed for the simultaneous spectrophotometric determination of copper (II), nickel (II) and zinc (II) in water with 1-(2-thiazolylazo)-2-naphthol as chromogenic reagent in the presence of Triton X-100. To overcome the drawback of spectral interferences, principal component regression (PCR) and partial least square (PLS) multivariate calibration approaches were applied. Performances were validated with several test sets, and their results were then compared. In general, no significant difference in analytical performance between PLS and PCR models. The root mean square error of prediction (RMSEP) using three components for Cu 2+ , Ni 2+ and Zn 2+ were 0.018, 0.010, 0.011 ppm, respectively. Figures of merit such as sensitivity, analytical sensitivity, limit of detection (LOD) were also estimated. High reliability was achieved when the proposed procedure was applied to simultaneous determination of Cu 2+ , Ni 2+ and Zn 2+ in synthetic mixture and tap water

  9. 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

  10. Spectrophotometric studies on the complexation equilibria of Ni and Pb with 2-carboxy-2-hydroxy-5'-sulfo-formazylbenzene. Simultaneous determination of trace amounts of Ni and Pb.

    Science.gov (United States)

    Hashem, Elham Y; Abu-Bakr, Mohamed S; Hussain, Sawsan M

    2004-01-01

    Spectrophotometric studies have been made to investigate the reaction of Nickel and Lead with 2-carboxy-2'-hydroxy-5'-sulfoformazyl-benzene (zincon) in 50%(v/v) ethanol-water at 25 degrees C and an ionic strength of 0.1 M NaClO4. A complete picture of the complexation equilibria in the pH range (4.2-12.0) for nickel and (1.9-11.5) for lead are presented. Simple, rapid, selective and sensitive methods for the spectro-photometric determination of nickel and lead has been developed based on the color reaction of their complexes with zincon. The methods allow the determination of 4.69 microg mL(-1) of nickel at pH = 6.3 (lambdamax = 665 nm) and 10.3 microg ml(-1) of lead at pH = 5.6 (lambdamax = 610 nm). The apparent molar absorptivities were epsilon = 1.3 x 10(4) L mol(-1) cm(-1) for nickel and epsilon = 0.6 x 10(4) L mol(-1) cm(-1) for lead. The interference of a large number of foreign ions and complexing agents has been studied. Thiosulphate, as masking agent allows the simultaneous determination of nickel and lead in the presence of high concentrations of copper. Ascorbic acid, sodium cyanide and or sodium fluoride provide the elimination of many other interferences. The methods have been applied successfully to the simultaneous determination of nickel and lead in an aluminium and non-ferrous alloy.

  11. 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.

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

    Directory of Open Access Journals (Sweden)

    M. Jamaluddin Ahmed

    2012-06-01

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

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

    Science.gov (United States)

    Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

    2015-01-01

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

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

    Science.gov (United States)

    Niazi, Ali; Khorshidi, Neda; Ghaemmaghami, Pegah

    2015-01-25

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

  15. Determination of trace elements in Egyptian cane sugar (Deshna Factories) by neutron activation, atomic absorption spectrophotometric and inductively coupled plasma-atomic emission spectrometric analysis

    International Nuclear Information System (INIS)

    Awadallah, R.M.; Sherif, M.K.; Mohamed, A.E.; Grass, F.

    1986-01-01

    Multielement instrumental neutron activation (INAA), inductively coupled plasma-atomic emission spectrometric (ICP-AES) and atomic absorption spectrophotometric (AAS) analyses were utilized for the determination of Ag, Al, As, Au, Ba, Be, Br, Ca, Cd, Ce, Cl, Co, Cr, Cu, Eu, Fe, Ga, Hf, K, La, Li, Lu, Mg, Mn, Na, Nb, Ni, P, Pb, Sb, Sc, Se, Sm, Sn, Sr, Ta, Th, Ti, U, V, W and Zn in sugar cane plant, raw juice, juice in different stages, syrup, deposits, molasses, A, B and C sugar, refinery 1 and 2 sugar, and in soil samples picked up from the immediate vicinity of the cane plant roots at surface, 30 and 60 cm depth, respectively. (author)

  16. Spectrophotometric Determination of the CuSO4 Soret Coefficient of a CuSO4-H2O Binary Solutions System

    Directory of Open Access Journals (Sweden)

    Ijang Rohman

    2010-06-01

    Full Text Available A spectrophotometric technique for the determination of the CuSO4 soret coefficient of a CuSO4-water binary solutions system is described. A short column of solutions is placed between horizontal metal plates that are held at different temperatures. The subsequent changes in composition due to thermal diffusion are followed by monitoring changes of transmittance near the end of the solutions column. In water, CuSO4 diffuses to the warm compartment of column. The soret coefficient of CuSO4 0.0254 molal in water agrees with the appropriate theory, i.e. 17.60x10-3 °C-1 on the average.

  17. A simple spectrophotometric determination of diclofenac sodium in commercial dosage forms using 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ)

    International Nuclear Information System (INIS)

    Raza, A.; Ansari, T.M.; Niazi, S.B.; Bukhari, S.I.H.

    2005-01-01

    A rapid, simple and sensitive spectrophotometric method has been developed for the determination of diclofenac sodium in pure and tablet formulations. The method depends on the charge-transfer complexation between diclofenac sodium as n-electron donor with 2,3-dichloro-,6-dicyano-1,4-benzoquinone (DDQ) in acetonitrile medium as pi-acceptor to give a colored complex which absorbs maximally at 545 nm. Beer's law has been obeyed in the concentration range of 13-275 micro gram ml/sup -1/ with molar absorptivity of 2.5 x 10/sup 3/L mole/sup -1/cm/sup -1/. The proposed method is precise, accurate and specific for routine quantitative analysis of the drug in bulk and dosage forms. (author)

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

    Science.gov (United States)

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

    2015-06-01

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

  19. Flow-injection determination of thorium and uranium after on-line ion-exchange preconcentration in Dowex 50-X8

    International Nuclear Information System (INIS)

    Perez Pavon, J.L.; Garcia Pinto, C.G.; Rodriguez Garcia, Estrella; Moreno Cordero, Bernardo

    1992-01-01

    The preconcentration of thorium and uranium on Dowex 50-X8 was studied as a method for the preconcentration of these cations prior to their determination by flow injection with spectrophotometric detection using Arsenazo III in 3.6 M HCl stabilized with Triton X-100 as chromogenic reagent. The preconcentration device is a minicolumn included in the sample loop of the injection valve. A second valve contains a reducing minicolumn filled with lead powder to reduce U(VI) to U(IV) before the confluence of the sample with the reagent stream. The method can be applied to samples containing 0.5-100 μg l -1 and was tested with different spiked water samples. (author). 15 refs.; 3 figs.; 3 tabs

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

    Directory of Open Access Journals (Sweden)

    Serpil Sevim

    2015-12-01

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

  1. 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.

  2. Flow injection spectrofluorimetric method for the determination of cadmium

    International Nuclear Information System (INIS)

    Bo Tang; Taixing Yue; Lili Zhang; Junsen Wu; Zhenzhen Chen

    2004-01-01

    A novel fluorescent reagent, o-vanillin furoylhydrazone (OVFH), was synthesized, and its infrared spectrum, elemental analysis and dissociation constant are reported. The reaction between Cd 2+ and OVFH produces an intensely fluorescent complex in ethanol-water medium of pH 10.00, and this finding has led to a simple, rapid, and sensitive flow injection (FI) spectrofluorimetric method for on-line determination of Cd 2+ . Under the optimum experimental conditions, the fluorescent complex had excitation and emission maxima at 393 and 494 nm, respectively. The linear range is from 0.025 to 8.0 μg mL -1 of Cd 2+ , the detection limit is 7.6 μg L -1 and the maximum sampling rate is 80 h -1 . The effect of interferences was studied. The method was successfully applied to the determination of cadmium in environmental samples. (author)

  3. Rapid and specific spectrophotometric and RP-HPLC methods for the determination of ascorbic acid in fruits juices and in human plasma

    International Nuclear Information System (INIS)

    Arayne, M.S.; Bibi, Z.; Sultana, N.

    2009-01-01

    Ascorbic acid (AA) is one of the most important water soluble vitamin in the human diet, present naturally in a wide range of foods, especially fruits and vegetables. The objective of this study was to develop a rapid, sensitive and specific method for the determination of ascorbic acid (vitamin C) from a variety of sources like fresh fruits or from human plasma using spectrophotometric technique or by RP-HPLC. Initially, estimation of vitamin C was carried out spectrophotometrically as UV spectroscopy is a trusted technique to monitor small quantities of drugs and vitamins. The assay was linear over the concentration range of 0.05-100 mi cro g/mL/sup -I/. In the second procedure, we attempted to separate and quantitate ascorbic acid from fruit juices as well as from human plasma by RP-HPLC with UV detection. This has been possible because of the diversity of columns and conditions of analysis available. Chromatographic separation was successfully achieved on a pre-packed Kromasil 100, C/sub 18/ (5 macro m 25 x 0.46) column using acetonitrile water (60:40; v/v) as mobile phase at a flow rate of 0.75 mL/sup -min/ and effluent monitored at 265 nm. The assay was also linear over the concentration range of 0.05-100 micro g/mL/sub -1/, with recovery ranging from 99.0-100.0 % and intra and inter day CV <3 % when applied to the analysis of ascorbic acid from fruit juice available in Pakistan at the time of study Grape fruit, malta, mosami, sweetlemon, fruiter, lemon, lime, custard apple, orange, lemon, guava and papaya juice were found to be very rich in as ascorbic acid, while chikoo, pear, apricot, peach, carrot and some other fruits were found to be poor sources of ascorbic acid. (author)

  4. Indirect spectrophotometric determination of sodium ceftriaxone with n-propyl alcohol-ammonium sulfate-water system by extraction flotation of copper(II).

    Science.gov (United States)

    Zhao, Wei; Zhang, Yan; Li, Quanmin

    2008-05-01

    Although the determination methods of sodium ceftriaxone has been increasingly reported, these methods have their inherent limits preventing them from being broadly applied in common laboratories. In order to circumvent this problem, a rapid and simple method for the indirect spectrophotometric determination of sodium ceftriaxone is reported. Sodium ceftriaxone was degraded completely in the presence of 0.20 mol/l sodium hydroxide in boiling water bath for 20 min. The thiol group (-SH) of the degradation product (I) of sodium ceftriaxone could reduce cupric to cuprous ions, and the resulting which was precipitated with the thiol group (-SH) of the degradation product (II) at pH 4.0. By determining the residual amount of copper (II), the indirect determination of sodium ceftriaxone can be achieved. Standard curve of sodium ceftriaxone versus the flotation yield of copper(II) showed that sodium ceftriaxone could be determined in low concentrations. The linear range of sodium ceftriaxone was 0.70-32 microg/ml and the detection limit evaluated by calibration curve (3sigma/k) was found to be 0.60 microg/ml. A simple and efficient method was developed and it has been successfully applied to the determination of sodium ceftriaxone in human serum and urine samples, respectively. It is expected that this method will find broad applications in the detection of cephalosporin derivatives with similar structure.

  5. Second-order Data by Flow Injection Analysis with Spectrophotometric Diode-array Detection and Incorporated Gel-filtration Chromatographic Column

    DEFF Research Database (Denmark)

    Bechmann, Iben Ellegaard

    1997-01-01

    A flow injection analysis (FIA) system furnished with a gel-filtration chromatographic column and with photodiode-array detection was used for the generation of second-order data. The system presented is a model system in which the analytes are blue dextran, potassium hexacyanoferrate(III) and he......A flow injection analysis (FIA) system furnished with a gel-filtration chromatographic column and with photodiode-array detection was used for the generation of second-order data. The system presented is a model system in which the analytes are blue dextran, potassium hexacyanoferrate...

  6. Determination of very low levels of 5-(hydroxymethyl)-2-furaldehyde (HMF) in natural honey: comparison between the HPLC technique and the spectrophotometric white method.

    Science.gov (United States)

    Truzzi, Cristina; Annibaldi, Anna; Illuminati, Silvia; Finale, Carolina; Rossetti, Monica; Scarponi, Giuseppe

    2012-07-01

    In this work we compared 2 official methods for the determination of HMF in honey, the spectrophotometric White method and the HPLC method (International Honey Commission) for the determination of HMF in unifloral honey and honeydew samples with a very low HMF content (5 mg/kg, the molar extinction coefficient is 15369, lower than the literature value of 16830, and should be used for HMF determination. For samples with HMF content in the range 1-4 mg/kg the accuracy of the 2 methods is comparable both for unifloral and honeydew samples, whereas as regards precision, the HPLC method gives better results (3.5% compared with 6.4% for the White method). So, in general, the HPLC method seems to be more appropriate for the determination of HMF in honey in the range 1-4 mg/kg thanks to its greater precision, but for samples with a HMF content of less than 1 mg/kg the analyses are inaccurate for both methods. This work can help governmental and private laboratories that perform food analyses to choose the best method for the determination of HMF at very low levels in unifloral honey and honeydew samples. © 2012 Institute of Food Technologists®

  7. Dodecylbenzene sulfonate-coated magnetite nanoparticles as a new adsorbent for solid phase extraction-spectrophotometric determination of ultra trace amounts of ammonium in water samples.

    Science.gov (United States)

    Eskandari, Habibollah; Shariati, Mohammad Reza

    2011-10-17

    A new method was proposed for the determination of ammonium based on the preconcentration with dodecylbenzene sulfonate modified magnetite nanoparticles. Ammonium was oxidized to nitrite by hypobromite and then the nitrite produced was determined spectrophotometrically, using sulfabenzamide and N-(1-naphthyl) ethylenediamine after solid phase extraction. The azo dye produced was desorbed by an appropriate small volume of sodium hydroxide prior to the absorbance measurement. The linear calibration graphs were obtained in the concentration range of 0.03-6.00 ng mL(-1) ammonium. The relative standard deviation and recovery percents were 1.0 and 99.0, respectively, for 1.0 ng mL(-1) ammonium, and the limit of detection was 3.2 ng L(-1) ammonium. The interfering effects of a large number of diverse ions on the determination of ammonium were studied. The method was applied to the determination of ammonium in various types of water resources. The results revealed a high efficiency for the recommended ammonium determination method. Copyright © 2011 Elsevier B.V. All rights reserved.

  8. Sequential injection titration method using second-order signals: determination of acidity in plant oils and biodiesel samples.

    Science.gov (United States)

    del Río, Vanessa; Larrechi, M Soledad; Callao, M Pilar

    2010-06-15

    A new concept of flow titration is proposed and demonstrated for the determination of total acidity in plant oils and biodiesel. We use sequential injection analysis (SIA) with a diode array spectrophotometric detector linked to chemometric tools such as multivariate curve resolution-alternating least squares (MCR-ALS). This system is based on the evolution of the basic specie of an acid-base indicator, alizarine, when it comes into contact with a sample that contains free fatty acids. The gradual pH change in the reactor coil due to diffusion and reaction phenomenona allows the sequential appearance of both species of the indicator in the detector coil, recording a data matrix for each sample. The SIA-MCR-ALS method helps to reduce the amounts of sample, the reagents and the time consumed. Each determination consumes 0.413ml of sample, 0.250ml of indicator and 3ml of carrier (ethanol) and generates 3.333ml of waste. The frequency of the analysis is high (12 samples h(-1) including all steps, i.e., cleaning, preparing and analysing). The utilized reagents are of common use in the laboratory and it is not necessary to use the reagents of perfect known concentration. The method was applied to determine acidity in plant oil and biodiesel samples. Results obtained by the proposed method compare well with those obtained by the official European Community method that is time consuming and uses large amounts of organic solvents.

  9. Spectrophotometric Determination of Nano Amounts of Gallium (III) using 2-(5-Bromo-2-Pyridylazo)-5-Diethyl aminophenol Reagent in Water Samples

    International Nuclear Information System (INIS)

    Kandil, A.T.; Abd El-Atty, N.; El-Naggar, W.S.A.; Hafez, W.S.; Lasheen, T.A.

    2014-01-01

    The aim of the present work is to develop a simple and sensitive spectrophotometric method for determination of nano amounts of Ga(III) using 2-(5-Bromo-2-Pyridylazo)-5-Diethyl aminophenol (5-Br-PADAP) reagent. The factors affecting the determination procedure including absorption spectra, ph value, surfactant type and dye reagent concentration were studied and optimized. Interferences had also been evaluated. Maximum absorbance was obtained at 573 nm at ph 2.75, after 5 minutes mixing time. The proposed method was valid for Ga(III) concentration determination ranging from 0.005 to 1.25 Μg ml -1 in aqueous solution. However, the detection limit was decreased up to 0.001 Μg ml-1 in the presence of methanol. The ratio between Ga(III) and 5-Br-PADAP was found to be 1:1 with apparent molar absorptivity 1.12 × 10 5 l mol -1 cm -1 and coefficient of variation 0.44%. The elucidation of the complex composition was proved using FTIR technique. The method was applied for the determination of Ga(III) in some polluted water samples from different sources.

  10. Spectrophotometric analysis of irradiated spices

    Energy Technology Data Exchange (ETDEWEB)

    Josimovic, L; Cudina, I

    1987-01-01

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

  11. Extractive spectrophotometric determination of five selected drugs by ion-pair complex formation with bromothymol blue in pure form and pharmaceutical preparations

    Directory of Open Access Journals (Sweden)

    Sneha G. Nair

    2015-12-01

    Full Text Available Simple, precise, selective, and expeditious spectrophotometric methods have been developed for the determination of itopride (ITO, midodrine (MID, diclofenac (DIC, mesalamine (MES, and sumatriptan (SUM in their pure form as well as in pharmaceutical preparations. The method was based on ion-pair complex formation between the drugs and anionic dye, bromothymol blue in an acidic medium (pH 2.0–4.0. The yellow colored complexes formed were quantitatively extracted into chloroform and measured at 411, 410, 413, 412, and 414 nm wavelength for ITO, MID, DIC, MES, and SUM, respectively. Beer’s law was obeyed in the concentration range of 3.0–30 µg/mL for ITO, 1.0–20 µg/mL for MID, 1.5–40 µg/mL for DIC, 1.2–12 µg/mL for MES, and 0.5–15 µg/mL for SUM. The stoichiometry of the complexes formed between the drugs and the dye was 1:1 as determined by Job’s method of continuous variation. The association constant (KIP of the ion-pair complexes formed was evaluated using Benesi–Hildebrand equation. Limit of detection, limit of quantification, and Sandell’s sensitivity of the methods were also estimated. The proposed methods were successfully employed for the determination of these drugs in their pharmaceutical dosage forms.

  12. The comparison of partial least squares and principal component regression in simultaneous spectrophotometric determination of ascorbic acid, dopamine and uric acid in real samples

    Directory of Open Access Journals (Sweden)

    Habiboallah Khajehsharifi

    2017-05-01

    Full Text Available Partial least squares (PLS1 and principal component regression (PCR are two multivariate calibration methods that allow simultaneous determination of several analytes in spite of their overlapping spectra. In this research, a spectrophotometric method using PLS1 is proposed for the simultaneous determination of ascorbic acid (AA, dopamine (DA and uric acid (UA. The linear concentration ranges for AA, DA and UA were 1.76–47.55, 0.57–22.76 and 1.68–28.58 (in μg mL−1, respectively. However, PLS1 and PCR were applied to design calibration set based on absorption spectra in the 250–320 nm range for 36 different mixtures of AA, DA and UA, in all cases, the PLS1 calibration method showed more quantitative prediction ability than PCR method. Cross validation method was used to select the optimum number of principal components (NPC. The NPC for AA, DA and UA was found to be 4 by PLS1 and 5, 12, 8 by PCR. Prediction error sum of squares (PRESS of AA, DA and UA were 1.2461, 1.1144, 2.3104 for PLS1 and 11.0563, 1.3819, 4.0956 for PCR, respectively. Satisfactory results were achieved for the simultaneous determination of AA, DA and UA in some real samples such as human urine, serum and pharmaceutical formulations.

  13. Flow injection kinetic spectrofluorimetric determination of trace amounts of osmium

    Science.gov (United States)

    Tang, Bo; Zhang, Hui; Wang, Yan

    2005-07-01

    A flow injection (FI) kinetic spectrofluorimetric method is described for the determination of osmium(IV) and the possible mechanism of catalytic reaction is discussed. The method is based on the fluorescence enhancing reaction of o-vanillin furfuralhydrazone (OVFH) with potassium bromate, which is catalyzed by Os(IV) in water medium at pH 6.10 and 45 °C. OVFH is newly synthesized and its ionization, IR and elemental analysis are established. Under these experimental conditions, the oxidized product of OVFH has excitation and emission maxima at 337 and 490 nm, respectively. The linear range of this method is 0-600 ng ml -1 with the R.S.D. of 1.2%. The detection limit is 1.0 ng ml -1 of Os(IV). A high analysis rate of 24 samples h -1 is obtained by the FI method. The proposed method is applied successfully to determine Os(IV) in synthetic mixture and mineral samples, and the results are well consistent with the standard values.

  14. Sequential determination of multi-nutrient elements in natural water samples with a reverse flow injection system.

    Science.gov (United States)

    Lin, Kunning; Ma, Jian; Yuan, Dongxing; Feng, Sichao; Su, Haitao; Huang, Yongming; Shangguan, Qipei

    2017-05-15

    An integrated system was developed for automatic and sequential determination of NO 2 - , NO 3 - , PO 4 3- , Fe 2+ , Fe 3+ and Mn 2+ in natural waters based on reverse flow injection analysis combined with spectrophotometric detection. The system operation was controlled by a single chip microcomputer and laboratory-programmed software written in LabVIEW. The experimental parameters for each nutrient element analysis were optimized based on a univariate experimental design, and interferences from common ions were evaluated. The upper limits of the linear range (along with detection limit, µmolL -1 ) of the proposed method was 20 (0.03), 200 (0.7), 12 (0.3), 5 (0.03), 5 (0.03), 9 (0.2) µmolL -1 , for NO 2 - , NO 3 - , PO 4 3- , Fe 2+ , Fe 3+ and Mn 2+ , respectively. The relative standard deviations were below 5% (n=9-13) and the recoveries varied from 88.0±1.0% to 104.5±1.0% for spiked water samples. The sample throughput was about 20h -1 . This system has been successfully applied for the determination of multi-nutrient elements in different kinds of water samples and showed good agreement with reference methods (slope 1.0260±0.0043, R 2 =0.9991, n=50). Copyright © 2017 Elsevier B.V. All rights reserved.

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

    Science.gov (United States)

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

    2007-11-01

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

  16. Simple spectrophotometric methods for determination of fluoxetine and clomipramine hydrochlorides in dosage forms and in some post-mortem biological fluids samples

    Directory of Open Access Journals (Sweden)

    Emam A. Ali

    2016-12-01

    Full Text Available Sensitive, simple and rapid spectrophotometric methods for micro determination of fluoxetine hydrochloride (FLU and clomipramine hydrochloride (CLO. The methods are based on the reaction between the examined drugs and acid dyes, namely; bromocresol green (BCG, phenol red (PhR and metanil yellow (MY producing yellow ion-pair complexes followed by their extraction with methylene chloride and measured at 412, 407 and 409 nm for FLU with BCG, PhR and MY, respectively; whereas for CLO at 409, 406 and 407 nm, respectively. All variables that affect the performance of the proposed methods were carefully studied and optimized. Beer’s law was obeyed in the concentration ranges 0.86–24.32 μg/mL, 8.64–41.30 μg/mL, 0.86–34.76 μg/mL for FLU and 1.75–24.55 μg/mL, 7.0–50 μg/mL, 1.65–34.78 μg/mL for CLO using BCG, PhR and MY respectively. The methods were validated in terms of accuracy and precision. The proposed methods were successfully applied to the determination of fluoxetine hydrochloride and clomipramine hydrochloride in pure samples, pharmaceutical formulations, spiked post-mortem urine and blood samples.

  17. Spectrophotometric determination of cobalt(II), nickel(II) and copper (II) with 1-(2 pyridylazo)-2-naphthol in micellar medium

    International Nuclear Information System (INIS)

    Shar, G.A.; Soomro, G.A.

    2004-01-01

    Spectrophotometric determination of cobalt(II), nickel(II) and copper(II) is carried out with 1-(2 pyridylazo)-2-naphthol as a complexing reagent in aqueous phase using non-ionic surfactant Tween 80. Beer's law is obeyed for Co(II), Ni(II) and Cu(II) over the range 0.5 - 4.0, 0.5 - 4.0 and 0.5 - 3.0 ngmL/sup -1/ with detection limit (2 σ) of 6.7, 3.2 and 3.9 ngmL/sup -1/. The max molar absorption, molar absorptivity, Sandell's sensitivity of Co(II), Ni(II) and Cu(II) are 580 nm, 570 nm and 555 nm; max (104 mol/sup -1/ cm /sup -1/) is 0.87, 1.8 and 1.6 and 6.8, 3.3 and 3.9 ng cm-2 respectively. The pH at which complex is formed for Co(II), Ni(II) and Cu(II) is 5, 5.5 and 6.5 respectively. The critical micelle concentration (CMC) of Tween 80 is 5%. The present method is compared with that of atomic absorption spectroscopy and no significant difference is noted between the two methods at 95% confidence level. The method has been applied to the determination of Co(II), Ni(II) and Cu(II) in industrial waste water and pharmaceutical samples. (author)

  18. 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.

  19. Spectrophotometric determination of thorium in standard samples and monazite sands based on the floated complex of thorium with N-hydroxy-N, N'-diphenylbenzamidine and thorin

    International Nuclear Information System (INIS)

    Nashine, N.; Deb, M.K.; Mishra, R.K.

    1996-01-01

    A selective and sensitive spectrophotometric method for the determination of Th(IV) has been based on the reaction with thorin and subsequent extraction of the red-orange coloured complex with N-hydroxy-N, N'-diphenylbenzamidine (HDPBA) in benzene as floated complex at pH 2.2. The complex in ethanol exhibits a maximum absorbance at 495 nm, with a molar absorptivity of 6.0 x 10 4 l mol -1 cm -1 , with a Sandell's sensitivity of 3.9 x 10 -3 μg cm -2 . The method follows Beer's law up to 3.0 μg Th(IV) ml -1 . None of the common cations and anions tested interfere. The detection limit of the method is 0.04 μg Th(IV) ml -1 , the RSD (n=10) is 1.4%. The method has been successfully employed for the determination of thorium in various standard and monazite samples. (orig.). With 2 tabs

  20. Selective flotation-spectrophotometric determination of trace copper(II) in natural waters, human blood and drug samples using phenanthraquinone monophenylthiosemicarbazone.

    Science.gov (United States)

    Khalifa, M E; Akl, M A; Ghazy, S E

    2001-06-01

    Copper(II) forms 1:1 and 1:2 intense red complexes with phenanthraquinone monophenylthiosemicarbazone (PPT) at pH 3-3.5 and > or =6.5, respectively. These complexes exhibit maximal absorbance at 545 and 517 nm, the molar absorptivity being 2.3 x 10(4) and 4.8 x 10(4) l mol(-1) cm(-1), respectively. However, the 1:1 complex was quantitatively floated with oleic acid (HOL) surfactant in the pH range 4.5-5.5, providing a highly selective and sensitive procedure for the spectrophotometric determination of CuII. The molar absorptivity of the floated Cu-PPT complex was 1.5 x 10(5) l mol)(-1) cm(-1). Beer's law was obeyed over the range 3-400 ppb at 545 nm. The analytical parameters affecting the flotation process and hence the determination of copper traces were reported. Also, the structure of the isolated solid complex and the mechanism of flotation were suggested. Moreover, the procedure was successfully applied to the analysis of CuII in natural waters, serum blood and some drug samples.