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Sample records for absorption spectrophotometric method

  1. Simultaneous spectrophotometric determination of Celecoxib and Diacerein in bulk and capsule by absorption correction method and chemometric methods

    NASA Astrophysics Data System (ADS)

    Patel, N. S.; Nandurbarkar, V. P.; Patel, A. J.; Patel, S. G.

    Two methods, absorption correction and multivariate spectrophotometric methods were developed for simultaneous estimation of Celecoxib (CEL) and Diacerein (DIA) in combined dosage form. Absorption correction method involves direct estimation of DIA at wavelength 341 nm in which CEL has zero absorbance and shows no interference. For estimation of CEL, corrected absorbance was calculated at 253 nm due to the interference of DIA at this wavelength. Linearity was observed in the range of 6-22 μg mL-1 for CEL and 3-11 μg mL-1 for DIA. The method was validated as per ICH guidelines. Chemometric methods including classical least square (CLS), inverse least square (ILS), principal component regression (PCR) and partial least square (PLS) were studied for simultaneous determination of CEL and DIA in capsule using spectrophotometry. A set of 25 standard mixtures containing both drugs were prepared in range of 5-25 μg mL-1 for CEL and 3-15 μg mL-1 for DIA. Analytical figure of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of detection and limit of quantitation were determined for chemometric methods. The proposed methods were applied for determination of two components from combined dosage form.

  2. Simultaneous spectrophotometric determination of celecoxib and diacerein in bulk and capsule by absorption correction method and chemometric methods.

    PubMed

    Patel, N S; Nandurbarkar, V P; Patel, A J; Patel, S G

    2014-05-01

    Two methods, absorption correction and multivariate spectrophotometric methods were developed for simultaneous estimation of Celecoxib (CEL) and Diacerein (DIA) in combined dosage form. Absorption correction method involves direct estimation of DIA at wavelength 341 nm in which CEL has zero absorbance and shows no interference. For estimation of CEL, corrected absorbance was calculated at 253 nm due to the interference of DIA at this wavelength. Linearity was observed in the range of 6-22 μg mL(-1) for CEL and 3-11 μg mL(-1) for DIA. The method was validated as per ICH guidelines. Chemometric methods including classical least square (CLS), inverse least square (ILS), principal component regression (PCR) and partial least square (PLS) were studied for simultaneous determination of CEL and DIA in capsule using spectrophotometry. A set of 25 standard mixtures containing both drugs were prepared in range of 5-25 μg mL(-1) for CEL and 3-15 μg mL(-1) for DIA. Analytical figure of merit (FOM), such as sensitivity, selectivity, analytical sensitivity, limit of detection and limit of quantitation were determined for chemometric methods. The proposed methods were applied for determination of two components from combined dosage form.

  3. Novel ratio difference at coabsorptive point spectrophotometric method for determination of components with wide variation in their absorptivities

    NASA Astrophysics Data System (ADS)

    Saad, Ahmed S.; Abo-Talib, Nisreen F.; El-Ghobashy, Mohamed R.

    2016-01-01

    Different methods have been introduced to enhance selectivity of UV-spectrophotometry thus enabling accurate determination of co-formulated components, however mixtures whose components exhibit wide variation in absorptivities has been an obstacle against application of UV-spectrophotometry. The developed ratio difference at coabsorptive point method (RDC) represents a simple effective solution for the mentioned problem, where the additive property of light absorbance enabled the consideration of the two components as multiples of the lower absorptivity component at certain wavelength (coabsorptive point), at which their total concentration multiples could be determined, whereas the other component was selectively determined by applying the ratio difference method in a single step. Mixture of perindopril arginine (PA) and amlodipine besylate (AM) figures that problem, where the low absorptivity of PA relative to AM hinders selective spectrophotometric determination of PA. The developed method successfully determined both components in the overlapped region of their spectra with accuracy 99.39 ± 1.60 and 100.51 ± 1.21, for PA and AM, respectively. The method was validated as per the USP guidelines and showed no significant difference upon statistical comparison with reported chromatographic method.

  4. Novel ratio difference at coabsorptive point spectrophotometric method for determination of components with wide variation in their absorptivities.

    PubMed

    Saad, Ahmed S; Abo-Talib, Nisreen F; El-Ghobashy, Mohamed R

    2016-01-01

    Different methods have been introduced to enhance selectivity of UV-spectrophotometry thus enabling accurate determination of co-formulated components, however mixtures whose components exhibit wide variation in absorptivities has been an obstacle against application of UV-spectrophotometry. The developed ratio difference at coabsorptive point method (RDC) represents a simple effective solution for the mentioned problem, where the additive property of light absorbance enabled the consideration of the two components as multiples of the lower absorptivity component at certain wavelength (coabsorptive point), at which their total concentration multiples could be determined, whereas the other component was selectively determined by applying the ratio difference method in a single step. Mixture of perindopril arginine (PA) and amlodipine besylate (AM) figures that problem, where the low absorptivity of PA relative to AM hinders selective spectrophotometric determination of PA. The developed method successfully determined both components in the overlapped region of their spectra with accuracy 99.39±1.60 and 100.51±1.21, for PA and AM, respectively. The method was validated as per the USP guidelines and showed no significant difference upon statistical comparison with reported chromatographic method. PMID:26253440

  5. Supramolecular fullerene/porphyrin charge transfer interaction studied by absorption spectrophotometric method

    NASA Astrophysics Data System (ADS)

    Mukherjee, Partha; Bhattacharya (Banerjee), Shrabanti; Nayak, Sandip K.; Chattopadhyay, Subrata; Bhattacharya, Sumanta

    2009-06-01

    A detailed UV-Vis spectrometric and thermodynamic studies were done to look insight into the nature of molecular interactions of the electron donor-acceptor complexes of C60 and C70 with 5,10,15,20-tetrakis(octadecyloxyphenyl)-21H,23H-porphyrin (1) in chloroform and toluene. Charge transfer (CT) absorption bands were located in the visible region and vertical ionization potential of 1 was determined utilizing CT transition energy. Low values of oscillator and transition dipole strengths suggested that the complexes were almost of neutral character in ground states. The high binding constant value for the C70-1 complex indicated high selectivity of 1 molecule towards C70. Experimental as well as theoretically determined of enthalpies of formation value substantiated the trend in K values for fullerene-1 complexes.

  6. On-line spectrophotometric method for monitoring weak residual absorption of CaMoO{sub 4} single crystals near the intrinsic luminescence peak

    SciTech Connect

    Buzanov, O. A.; Kanevskii, V. M.; Kornoukhov, V. N.; Nabatov, B. V.; Nabatov, V. V.; Fedorov, V. A.

    2013-11-15

    The optical and spectral characteristics of isotopically enriched Czochralski-grown {sup 40}Ca{sup 100}MoO{sub 4} single crystals have been investigated. This material is promising for detecting double neutrinoless {beta} decay. The possibility and the technique of spectrophotometric monitoring of weak residual absorption near the intrinsic luminescence peak of this scintillation material, which is designed for developing new-generation detectors of elementary particles, are considered.

  7. Extension of dry ash atomic absorption and spectrophotometric methods to determination of minerals and phosphorus in soy-based, whey-based, and enteral formulae (modification of AOAC Official Methods 985.35 and 986.24): collaborative study.

    PubMed

    Cook, K K

    1997-01-01

    Eight laboratories participated in a collaborative study of AOAC Official Method 985.35, Minerals in Ready-to-Feed Milk-Based infant Formula and Pet Foods, Atomic Absorption Spectrophotometric Method; and 7 laboratories participated in a study of AOAC Official Method 986.24, Phosphorus in Milk-Based infant Formula, Spectrophotometric Method, to extend these methods to infant formulae (other than milk-based) and enteral products. Three ready-to-feed soy-based formulae and 2 soy-based powder formulae were chosen to represent the plant matrix. A whey-based formula and a casein-based enteral formula were also included in the study. Soy formulae containing nearly identical concentrations of particular elements were matched, and an application of the Youden "closely matched pair" approach was used to estimate repeatability parameters. Average reproducibility values were as follows: calcium, 9.3%; copper, 9.7%; Iron, 5.5%; potassium, 4.0%; magnesium, 5.2%; manganese, 10.6%; sodium, 4.7%; phosphorus, 10.5%; and zinc, 7.3%. At similar analyte concentrations, the between-laboratory variabilities compared well with those reported for the official methods. Most repeatability and reproducibility parameters compared well with the original collaborative study. AOAC Official Methods 985.35 and 966.24 have been modified to extend their applicability to infant formulae (other than milk-based) and enteral products.

  8. Extractive spectrophotometric methods for determination of lercanidipine.

    PubMed

    Erk, Nevin

    2003-11-01

    Extractive spectrophotometric methods are described for the determination of lercanidipine (LER) either in pure form or in pharmaceutical formulations. The methods involve formation of coloured chloroform extractable ion-pair complexes with bromothymol blue (BTB) and bromocresol green (BCG) in acidic medium. The extracted complexes showed absorbance maxima at 417 and 416 nm for BTB and BCG, respectively. The optimization of the reaction conditions was investigated. Beer's law is obeyed in the concentration ranges 6.0-42.0 microg x ml(-1) or 7.1-43.8 microg x ml(-1) with BTB or BCG, respectively. The composition of the ion-pairs was found to be 1:1 by Job's method. The specific absorptivities, molar absorptivities, Sandell sensitivities, standard deviations and percent recoveries were evaluated. Also, LER was determined by measurement of its first derivative signals at 245 nm. Calibration graph was established for 4.2-58.0 microg x ml(-1) of LER. The methods have been applied to the determination of drug in commercial tablets. Results of analysis were validated. No interferences were observed from common pharmaceutical adjuvants.

  9. Atomic absorption spectrophotometric determination of microgram quantities of copper in tea after solvent extraction.

    PubMed

    Aziz-Alrahman, A M

    1985-01-01

    An atomic absorption spectrophotometric method is described for determining trace amounts of copper in tea. The method is based on the solvent extraction of the metal as tetraiodocuprate (I), from 2 M HCl solutions of tea samples which contain 12% (w/v) KI, into methylisobutyl ketone. The organic extracts, containing the ion-association complex of copper are atomized into an air-acetylene flame. The limit of detection is 1.14 micrograms g-1 Cu. PMID:4077371

  10. Spectrophotometric method for determination of phosphine residues in cashew kernels.

    PubMed

    Rangaswamy, J R

    1988-01-01

    A spectrophotometric method reported for determination of phosphine (PH3) residues in wheat has been extended for determination of these residues in cashew kernels. Unlike the spectrum for wheat, the spectrum of PH3 residue-AgNO3 chromophore from cashew kernels does not show an absorption maximum at 400 nm; nevertheless, reading the absorbance at 400 nm afforded good recoveries of 90-98%. No interference occurred from crop materials, and crop controls showed low absorbance; the method can be applied for determinations as low as 0.01 ppm PH3 residue in cashew kernels.

  11. Evaluation of Perrhenate Spectrophotometric Methods in Bicarbonate and Nitrate Media.

    PubMed

    Lenell, Brian A; Arai, Yuji

    2016-04-01

    2-pyridyl thiourea and methyl-2-pyridyl ketoxime based perrhenate, Re(VII), UV-vis spectrophotometric methods were evaluated in nitrate and bicarbonate solutions ranging from 0.001 M to 0.5 M. Standard curves at [Re]=2.5-50 mg L(-1) for the Re(IV)-thiourea and the Re ketoxime complexes were constructed at 405 nm and 490 nm, respectively. Detection of limits for N-(2-pyridyl) thiourea and methyl-2-pyridyl ketoxime methods in ultrapure water are 3.06 mg/L and 4.03 mg/L, respectively. Influences of NaHCO3 and NaNO3 concentration on absorbance spectra, absorptivity, and linearity were documented. For both methods, samples in ultrapure water and NaHCO3 have an R(2) value>0.99, indicating strong linear relationships. Statistical analysis supports that NaHCO3 does not affect linearity between standards for either method. NaNO3 causes major interference with the ketoxime method above 0.001 M NaNO3. Data provides information for practical use of Re spectrophotometric methods in environmental media that is high in bicarbonate and nitrate. PMID:26838460

  12. Liquid-liquid extraction, photometric and atomic absorption spectrophotometric determination of mercury

    SciTech Connect

    Agrawal, Y.K.; Desai, T.A.

    1985-01-01

    A selective and sensitive spectrophotometric and atomic absorption spectrophotometric method is developed for the determination of traces of mercury with N-phenylcinnamohydroxamic acid (PCHA) in the environment. Mercury is extracted into a chloroform solution of PCHA at pH 8.5-10.0 and determined by AAS. The mercury hydroxamate binary complex is yellow in color having a maximum absorbance at 390 nm and molar absorptivity 4.3 x 10/sup 3/ l mol/sup -1/ cm/sup -1/, sandell sensitivity 0.0466 ..mu..g/cm/sup 2/. The ternary system using 1-(2-pyridylazo) 2-naphthol has molar absorptivity 8.82 x 10/sup 3/ l mol/sup -1/ cm/sup -1/ at 550 nm, sandell sensitivity 0.0228 ..mu..g/cm/sup 2/. Beer's law is obeyed in the concentration range of 2.37-38.0 ppm and 0.80-19.5 ppm of mercury for binary and ternary system, respectively. The extraction of Hg-PCHA binary system is studied with a liquid cation exchanger, bis-(2-ethyl hexyl) phosphoric acid (HDEHP) and found to have better selectivity than Hg-PCHA-PAN system. The molar absorptivity of the Hg-PCHA-HDEHP system is 8.82 x 10/sup 3/ l mol/sup -1/ cm/sup -1/ at 390 nm and Beer's law is obeyed in the concentration range of 0.47-20 ppm of mercury. The present method is applied to the determination of mercury in eye drops, aurvedic drugs and environmental samples. 24 references, 3 tables.

  13. Extraction, spectrophotometric and atomic absorption spectrophotometric determination of molybdenum with caffeic acid and application in high purity grade steel and environmental samples

    SciTech Connect

    Shah, N.; Desai, M.N. ); Menon, S.K.; Agrawal, Y.K. )

    1989-06-01

    A new selective and sensitive method for extraction of yellow Mo(VI)-caffeic acid complex with a liquid ion exchanger, Aliquat 336 from 4.0 pH, and spectrophotometric determination of molybdenum in trace amounts is described. The molar absorptivity of the complex is 1.1 {times} 10{sup 5} 1 mol{sup {minus}1} cm{sup {minus}1} at 340 nm and the color system obeys Beers law in the range 0.04-0.99 ppm of Mo(VI). The molybdenum is also determined with AAS and the method is applied for its determination in steel and environmental samples.

  14. A simple UV spectrophotometric method for theophylline serum level determination.

    PubMed

    Plavsić, F

    1978-09-15

    A brief, simple and unexpensive UV spectrophotometric method for theophylline serum level determination is described. Charcoal extraction was performed for theophylline isolation from biological fluids. Coefficients of variation and recovery are similar to other parallel methods.

  15. Graphite furnace-atomic absorption spectrophotometric determination of palladium in soil.

    PubMed

    Patel, K S; Sharma, P C; Hoffmann, P

    2000-08-01

    A new and sensitive procedure for the graphite furnace-atomic absorption spectrophotometric (GF-AAS) determination of Pd in soil at nanogram level is described. The method is based on prior separation and enrichment of the metal as Pd(II)-SnCl3- -N-butylacetamide (BAA) complex into 1-pentanol (PN) by solvent extraction method. The value of the molar absorptivity of the complex in three solvents, i.e. ethyl acetate, 1-pentanol, chloroform, lie in the range of (0.70-2.75) x 10(4) L mol(-1) cm(-1) at lambda(max) 360-440 nm. The metal could be enriched into organic solvent, i.e. PN, up to 10-folds. The sensitivity (A = 0.0044) of the method in the term of the peak height was 0.5 ng Pd/mL of the aqueous solution at an enrichment factor (EF) of 5. Optimization of analytical variables during enrichment and GF-AAS determination of the metal are discussed. The method has been applied for the analysis of Pd to soil samples derived from roads and highways in Germany. PMID:11220609

  16. Spectrophotometric and high performance liquid chromatographic methods for sensitive determination of bisphenol A.

    PubMed

    Zhuang, Yafeng; Zhou, Meng; Gu, Jia; Li, Xiangmei

    2014-03-25

    A new spectrophotometric method for the determination of trace amounts of bisphenol A based on a diazotization-coupling reaction was developed. In acidic solution, clenbuterol was first diazotized with sodium nitrite, then coupled with bisphenol A to from an azo-compound [I] in NH3-NH4Cl buffer, which shows a maximum absorption at 410 nm. The effects of the amount of sodium nitrite, diazo reaction time, the amount of clenbuterol, coupling reaction time and coupling reaction temperature have been examined. Under the optional conditions, the determination of the linear range of bisphenol A is 0.24-8.4 μg/mL, correlation coefficient is 0.9905 and detection limit of this method is 0.15 μg/mL. The spectrophotometric method is simple, rapid, high sensitivity with better accuracy. High performance liquid chromatography (HPLC) technique combined with this new spectrophotometric method has been also developed for the measurement of bisphenol A. The analysis was achieved on a C18 column using water and methanol as a mobile phase and the detection was done spectrophotometrically at 410 nm. These reported methods were applied to the determination of bisphenol A in hot water in contact with commercially available table-water bottle samples.

  17. Spectrophotometric and high performance liquid chromatographic methods for sensitive determination of bisphenol A

    NASA Astrophysics Data System (ADS)

    Zhuang, Yafeng; Zhou, Meng; Gu, Jia; Li, Xiangmei

    2014-03-01

    A new spectrophotometric method for the determination of trace amounts of bisphenol A based on a diazotization-coupling reaction was developed. In acidic solution, clenbuterol was first diazotized with sodium nitrite, then coupled with bisphenol A to from an azo-compound [I] in NH3-NH4Cl buffer, which shows a maximum absorption at 410 nm. The effects of the amount of sodium nitrite, diazo reaction time, the amount of clenbuterol, coupling reaction time and coupling reaction temperature have been examined. Under the optional conditions, the determination of the linear range of bisphenol A is 0.24-8.4 μg/mL, correlation coefficient is 0.9905 and detection limit of this method is 0.15 μg/mL. The spectrophotometric method is simple, rapid, high sensitivity with better accuracy. High performance liquid chromatography (HPLC) technique combined with this new spectrophotometric method has been also developed for the measurement of bisphenol A. The analysis was achieved on a C18 column using water and methanol as a mobile phase and the detection was done spectrophotometrically at 410 nm. These reported methods were applied to the determination of bisphenol A in hot water in contact with commercially available table-water bottle samples.

  18. Simultaneous determination of some cholesterol-lowering drugs in their binary mixture by novel spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Lotfy, Hayam Mahmoud; Hegazy, Maha Abdel Monem

    2013-09-01

    Four simple, specific, accurate and precise spectrophotometric methods manipulating ratio spectra were developed and validated for simultaneous determination of simvastatin (SM) and ezetimibe (EZ) namely; extended ratio subtraction (EXRSM), simultaneous ratio subtraction (SRSM), ratio difference (RDSM) and absorption factor (AFM). The proposed spectrophotometric procedures do not require any preliminary separation step. The accuracy, precision and linearity ranges of the proposed methods were determined, and the methods were validated and the specificity was assessed by analyzing synthetic mixtures containing the cited drugs. The four methods were applied for the determination of the cited drugs in tablets and the obtained results were statistically compared with each other and with those of a reported HPLC method. The comparison showed that there is no significant difference between the proposed methods and the reported method regarding both accuracy and precision.

  19. Validation of spectrophotometric method for lactulose assay in syrup preparation

    NASA Astrophysics Data System (ADS)

    Mahardhika, Andhika Bintang; Novelynda, Yoshella; Damayanti, Sophi

    2015-09-01

    Lactulose is a synthetic disaccharide widely used in food and pharmaceutical fields. In the pharmaceutical field, lactulose is used as osmotic laxative in a syrup dosage form. This research was aimed to validate the spectrophotometric method to determine the levels of lactulose in syrup preparation and the commercial sample. Lactulose is hydrolyzed by hydrochloric acid to form fructose and galactose. The fructose was reacted with resorcinol reagent, forming compounds that give absorption peak at 485 nm. Analytical methods was validated, hereafter lactulose content in syrup preparation were determined. The calibration curve was linear in the range of 30-100 μg/mL with a correlation coefficient (r) of 0.9996, coefficient of variance (Vxo) of 1.1 %, limit of detection of 2.32 μg/mL, and limit of quantitation of 7.04 μg/mL. The result of accuracy test for the lactulose assay in the syrup preparation showed recoveries of 96.6 to 100.8 %. Repeatability test of lactulose assay in standard solution of lactulose and sample preparation syrup showed the coefficient of variation (CV) of 0.75 % and 0.7 %. Intermediate precision (interday) test resulted in coefficient of variation 1.06 % on the first day, the second day by 0.99 %, and 0.95 % for the third day. This research gave a valid analysis method and levels of lactulose in syrup preparations of samples A, B, C were 101.6, 100.5, and 100.6 %, respectively.

  20. Direct spectrophotometric method for analysis of food supplements containing synthetic polyhydroquinones

    NASA Astrophysics Data System (ADS)

    Vasilevsky, A. M.; Konoplev, G. A.; Stepanova, O. S.; Toropov, D. K.; Zagorsky, A. L.

    2016-04-01

    A novel direct spectrophotometric method for quantitative determination of Oxiphore® drug substance (synthetic polyhydroquinone complex) in food supplements is developed. Absorption spectra of Oxiphore® water solutions in the ultraviolet region are presented. Samples preparation procedures and mathematical methods of spectra post-analytical procession are discussed. Basic characteristics of the automatic CCD-based UV spectrophotometer and special software implementing the developed method are described. The results of the trials of the developed method and software are analyzed: the error of determination for Oxiphore® concentration in water solutions of the isolated substance and singlecomponent food supplements did not exceed 15% (average error was 7…10%).

  1. Novel spectrophotometric method for detection and estimation of butanol in acetone-butanol-ethanol fermenter.

    PubMed

    Maiti, Sampa; Sarma, Saurabh Jyoti; Brar, Satinder Kaur; Bihan, Yann Le; Drogui, Patrick; Buelna, Gerardo; Verma, Mausam; Soccol, Carlos Ricardo

    2015-08-15

    A new, simple, rapid and selective spectrophotometric method has been developed for detection and estimation of butanol in fermentation broth. The red colored compound, produced during reduction of diquat-dibromide-monohydrate with 2-mercaptoethanol in aqueous solution at high pH (>13), becomes purple on phase transfer to butanol and gives distinct absorption at λ520nm. Estimation of butanol in the fermentation broth has been performed by salting out extraction (SOE) using saturated K3PO4 solution at high pH (>13) followed by absorbance measurement using diquat reagent. Compatibility and optimization of diquat reagent concentration for detection and estimation of butanol concentration in the fermentation broth range was verified by central composite design. A standard curve was constructed to estimate butanol in acetone-ethanol-butanol (ABE) mixture under optimized conditions. The spectrophotometric results for butanol estimation, was found to have 87.5% concordance with the data from gas chromatographic analysis.

  2. Novel spectrophotometric method for detection and estimation of butanol in acetone-butanol-ethanol fermenter.

    PubMed

    Maiti, Sampa; Sarma, Saurabh Jyoti; Brar, Satinder Kaur; Bihan, Yann Le; Drogui, Patrick; Buelna, Gerardo; Verma, Mausam; Soccol, Carlos Ricardo

    2015-08-15

    A new, simple, rapid and selective spectrophotometric method has been developed for detection and estimation of butanol in fermentation broth. The red colored compound, produced during reduction of diquat-dibromide-monohydrate with 2-mercaptoethanol in aqueous solution at high pH (>13), becomes purple on phase transfer to butanol and gives distinct absorption at λ520nm. Estimation of butanol in the fermentation broth has been performed by salting out extraction (SOE) using saturated K3PO4 solution at high pH (>13) followed by absorbance measurement using diquat reagent. Compatibility and optimization of diquat reagent concentration for detection and estimation of butanol concentration in the fermentation broth range was verified by central composite design. A standard curve was constructed to estimate butanol in acetone-ethanol-butanol (ABE) mixture under optimized conditions. The spectrophotometric results for butanol estimation, was found to have 87.5% concordance with the data from gas chromatographic analysis. PMID:25966390

  3. Enzymic method for the spectrophotometric determination of aspartame in beverages.

    PubMed

    Hamano, T; Mitsuhashi, Y; Aoki, N; Yamamoto, S; Tsuji, S; Ito, Y; Oji, Y

    1990-04-01

    A sensitive spectrophotometric method for the determination of aspartame in beverages is described. The method involves the enzymic conversion of aspartame into formaldehyde by the alpha-chymotrypsin-alcohol oxidase system, followed by the formation of a chromophore with 4-aminopent-3-en-2-one. The calibration graph was linear in the range 2.0-30.0 micrograms ml-1 of aspartame. Many common ingredients of beverages do not interfere with the proposed method. The method was applied to the determination of the aspartame content of various real samples, and the results obtained were compared with those given by high-performance liquid chromatography.

  4. Spectrophotometric method for determining gibberellic acid in fermentation broths.

    PubMed

    Berríos, Julio; Illanes, Andrés; Aroca, Germán

    2004-01-01

    A novel method for the quantitative determination of gibberellic acid in fermentation broths has been developed. It is based on the kinetic of the reaction of conversion of gibberellic acid to gibberellenic acid. The method is simple, reliable, faster than most of methods known, and free of the interferences which commonly affect spectrophotometric methods currently in use. Its threshold sensitivity is 0.1 g and its accuracy is greater than 97% for concentrations of gibberellic acid ranging from 0.1 to 1 g l(-1).

  5. Visual vs. Spectrophotometric Methods for Shade Selection.

    PubMed

    Glockner, Karl; Glockner, Karl; Haiderer, Bernd

    2015-09-01

    The differences in tooth colour are important factors in the esthetic dentistry. The aim of this study was to determine the tooth colour using visual methods under natural light and "Easy Shade" device. Five hundred patients of Dental Clinic Graz Austria were selected for this study. The results of this study showed that the shade matching using "Easy Shade" device were not better than shade matching with visual methods under natural light. No difference was found between visual and digital methods in the selection of a tooth shade.

  6. Resolution of overlapped spectra for the determination of ternary mixture using different and modified spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Moussa, Bahia Abbas; El-Zaher, Asmaa Ahmed; Mahrouse, Marianne Alphonse; Ahmed, Maha Said

    2016-08-01

    Four new spectrophotometric methods were developed, applied to resolve the overlapped spectra of a ternary mixture of [aliskiren hemifumarate (ALS)-amlodipine besylate (AM)-hydrochlorothiazide (HCT)] and to determine the three drugs in pure form and in combined dosage form. Method A depends on simultaneous determination of ALS, AM and HCT using principal component regression and partial least squares chemometric methods. In Method B, a modified isosbestic spectrophotometric method was applied for the determination of the total concentration of ALS and HCT by measuring the absorbance at 274.5 nm (isosbestic point, Aiso). On the other hand, the concentration of HCT in ternary mixture with ALS and AM could be calculated without interference using first derivative spectrophotometric method by measuring the amplitude at 279 nm (zero crossing of ALS and zero value of AM). Thus, the content of ALS was calculated by subtraction. Method C, double divisor first derivative ratio spectrophotometry (double divisor 1DD method), was based on that for the determination of one drug, the ratio spectra were obtained by dividing the absorption spectra of its different concentrations by the sum of the absorption spectra of the other two drugs as a double divisor. The first derivative of the obtained ratio spectra were then recorded using the appropriate smoothing factor. The amplitudes at 291 nm, 380 nm and 274.5 nm were selected for the determination of ALS, AM and HCT in their ternary mixture, respectively. Method D was based on mean centering of ratio spectra. The mean centered values at 287, 295.5 and 269 nm were recorded and used for the determination of ALS, AM and HCT, respectively. The developed methods were validated according to ICH guidelines and proved to be accurate, precise and selective. Satisfactory results were obtained by applying the proposed methods to the analysis of pharmaceutical dosage form.

  7. Resolution of overlapped spectra for the determination of ternary mixture using different and modified spectrophotometric methods.

    PubMed

    Moussa, Bahia Abbas; El-Zaher, Asmaa Ahmed; Mahrouse, Marianne Alphonse; Ahmed, Maha Said

    2016-08-01

    Four new spectrophotometric methods were developed, applied to resolve the overlapped spectra of a ternary mixture of [aliskiren hemifumarate (ALS)-amlodipine besylate (AM)-hydrochlorothiazide (HCT)] and to determine the three drugs in pure form and in combined dosage form. Method A depends on simultaneous determination of ALS, AM and HCT using principal component regression and partial least squares chemometric methods. In Method B, a modified isosbestic spectrophotometric method was applied for the determination of the total concentration of ALS and HCT by measuring the absorbance at 274.5nm (isosbestic point, Aiso). On the other hand, the concentration of HCT in ternary mixture with ALS and AM could be calculated without interference using first derivative spectrophotometric method by measuring the amplitude at 279nm (zero crossing of ALS and zero value of AM). Thus, the content of ALS was calculated by subtraction. Method C, double divisor first derivative ratio spectrophotometry (double divisor (1)DD method), was based on that for the determination of one drug, the ratio spectra were obtained by dividing the absorption spectra of its different concentrations by the sum of the absorption spectra of the other two drugs as a double divisor. The first derivative of the obtained ratio spectra were then recorded using the appropriate smoothing factor. The amplitudes at 291nm, 380nm and 274.5nm were selected for the determination of ALS, AM and HCT in their ternary mixture, respectively. Method D was based on mean centering of ratio spectra. The mean centered values at 287, 295.5 and 269nm were recorded and used for the determination of ALS, AM and HCT, respectively. The developed methods were validated according to ICH guidelines and proved to be accurate, precise and selective. Satisfactory results were obtained by applying the proposed methods to the analysis of pharmaceutical dosage form. PMID:27128521

  8. Spectrophotometric method for the determination of chromium (VI) in water samples.

    PubMed

    Nagaraj, P; Aradhana, N; Shivakumar, Anantharaman; Shrestha, Ashwinee Kumar; Gowda, Avinash K

    2009-10-01

    A simple and sensitive spectrophotometric method for the determination of chromium has been developed. The method is based on the diazotization of Dapsone in hydroxylamine hydrochloride medium and coupling with N-(1-Napthyl) Ethylene Diamine Dihydrochloride by electrophilic substitution to produce an intense pink azo-dye, which has absorption maximum at 540 nm. The Beer's law is obeyed from 0.02-1.0 microg mL(-1) and the molar absorptivity is 3.4854 L mol(-1) cm(-1). The Limits of quantification and Limit of detection of the proposed method are 0.0012 microg mL(-1) and 0.0039 microg mL(-1) respectively. The method has been successfully applied for the determination of chromium in water samples and the results were statistically evaluated with that of the reference method.

  9. [Spectrophotometric determination of protein content in THP-1 monocytes/macrophages - description of the method].

    PubMed

    Wolska, Jolanta; Janda, Katarzyna; Gutowska, Izabela

    2015-01-01

    Proteins are the basic building block of tissue, and are part of enzymes and hormones regulating many important life processes. Changes in their concentration control the metabolic processes of the cell. Quantitative determination of the protein content is divided into indirect methods (e.g. Kjeldahl method) and direct methods (buret method, Lowry, immunoenzymatic, formol method, based on incorporation of dye in the range of ultraviolet spectrophotometry, and based on the phenomenon of selective absorption of radiation in the infrared range). One of the methods for the determination of protein content is the spectrophotometric method described by Bradford. The protein concentration assay procedure utilizes the phenomenon of formation of the dye (Coomassie Brillant Blue G-250)-protein and colour intensity is proportional to the protein content in the solution. The aim of this study was to verify the usefulness of this method for determining the protein content in THP-1 cells cultured with extracts of nettle fruit stalks (Urtica dioica L.). Aqueous and alcohol extracts at two concentrations were used. It has been shown that the spectrophotometric determination of protein content by the Bradford method is an effective and accurate method for determining the concentration of protein in THP-1 macrophages. The results indicate that this method can be recommended for the determination of the protein content in other cell cultures. PMID:27116861

  10. [Spectrophotometric determination of protein content in THP-1 monocytes/macrophages - description of the method].

    PubMed

    Wolska, Jolanta; Janda, Katarzyna; Gutowska, Izabela

    2015-01-01

    Proteins are the basic building block of tissue, and are part of enzymes and hormones regulating many important life processes. Changes in their concentration control the metabolic processes of the cell. Quantitative determination of the protein content is divided into indirect methods (e.g. Kjeldahl method) and direct methods (buret method, Lowry, immunoenzymatic, formol method, based on incorporation of dye in the range of ultraviolet spectrophotometry, and based on the phenomenon of selective absorption of radiation in the infrared range). One of the methods for the determination of protein content is the spectrophotometric method described by Bradford. The protein concentration assay procedure utilizes the phenomenon of formation of the dye (Coomassie Brillant Blue G-250)-protein and colour intensity is proportional to the protein content in the solution. The aim of this study was to verify the usefulness of this method for determining the protein content in THP-1 cells cultured with extracts of nettle fruit stalks (Urtica dioica L.). Aqueous and alcohol extracts at two concentrations were used. It has been shown that the spectrophotometric determination of protein content by the Bradford method is an effective and accurate method for determining the concentration of protein in THP-1 macrophages. The results indicate that this method can be recommended for the determination of the protein content in other cell cultures.

  11. Absorption spectrophotometric, fluorescence, transient absorption and quantum chemical investigations on fullerene/phthalocyanine supramolecular complexes.

    PubMed

    Ray, Anamika; Santhosh, Kotni; Bhattacharya, Sumanta

    2011-05-01

    The present paper reports the photophysical investigations on supramolecular interaction of a phthalocyanine derivative, namely, 2,9,16,23-tetra-tert-butyl-29H,31H-Pc (1) with C(60) and C(70) in toluene. The binding constants of the C(60) and C(70) complexes of 1 are estimated to be 27,360 and 25,205 dm(3), respectively. Transient absorption measurements in the visible region establishes that energy transfer from C60*T (and C70*T) to 1 occurs predominantly in toluene which is subsequently confirmed by the consecutive appearance of the triplet states of 1. Quantum chemical calculations at DFT level of theory explore the geometry and electronic structure of the supramolecules and testify the significant redistribution of charge between fullerenes and 1.

  12. A sensitive spectrophotometric method for the determination of sulfonamides in pharmaceutical preparations.

    PubMed

    Nagaraja, Padmarajaiah; Naik, Shailendra D; Shrestha, Ashwinee Kumar; Shivakumar, Anantharaman

    2007-09-01

    A new, simple and sensitive spectrophotometric method for the determination of some sulfonamide drugs has been developed. The method is based on the diazotization of sulfacetamide, sulfadiazine, sulfaguanidine, sulfamerazine, sulfamethazine, sulfamethoxazole, and their coupling with 8-hydroxyquinoline in alkaline media to yield red coloured products with absorption maxima at 500 nm. Beer's law is obeyed from 0.1-7.0 microg mL-1. The limits of quantification and limits of detection were 0.11-0.18 and 0.03-0.05 microg mL-1, respectively. Intraday precision (RSD 0.1-0.5%) and accuracy (recovery 97.3--100.8%) of the developed method were evaluated. No interference was observed from common adjuvants. The method has been successfully applied to the assay of sulpha drug in pharmaceutical formulations.

  13. Spectrophotometric method for the determination of amlodipine besylate with ninhydrin in drug formulations.

    PubMed

    Rahman, N; Azmi, S N

    2001-10-01

    A spectrophotometric method has been developed for the determination of amlodipine besylate in pure form and in pharmaceutical preparations. The method is based on the reaction of the primary amino group of the drug with ninhydrin in N,N'-dimethylformamide (DMF) medium producing a coloured complex which absorbs maximally at 595 nm. Beer's law is obeyed in the concentration range of 10-60 microg ml(-1) with RSD of 0.66% and molar absorptivity of 6.52 x 10(3) l mol(-1) cm(-1). All variables were studied in order to optimize the reaction conditions. The proposed method has been applied successfully to the analysis of the bulk drug and its dosage forms. No interference was observed from common pharmaceutical adjuvants. Statistical comparison of the results with the reference method shows excellent agreement and indicates no significant difference in accuracy and precision.

  14. Determination of ametryn in sugarcane and ametryn-atrazine herbicide formulations using spectrophotometric method.

    PubMed

    Shah, Jasmin; Jan, M Rasul; Ara, Behisht; Shehzad, Farhat-Un-Nisa

    2012-06-01

    A sensitive spectrophotometric method has been developed for determination of ametryn in agricultural samples. The proposed method was based on reaction with pyridine and further coupling with sulfanilic acid to form a colored product. The absorbance was measured at 400 nm with a molar absorptivity of 2.1 x 10(5) L mol(-1) cm(-1). The method shows a linear range from 0.2-20 μg mL(-1) with limit of detection and limit of quantification 0.16 and 0.54 μg mL(-1), respectively. The method has been successfully applied to the determination of ametryn in sugarcane juice and commercial formulations after separation of ametryn from triazine herbicides based on solvent extraction. Recovery values were found to be in the range of 96.0 ± 0.2% to 98.4  ±  0.1%.

  15. Spectrophotometric estimation of tamsulosin hydrochloride by acid-dye method

    PubMed Central

    Shrivastava, Alankar; Saxena, Prachi; Gupta, Vipin B.

    2011-01-01

    A new spectrophotometric method for the estimation of tamsulosin hydrochloride in pharmaceutical dosage forms has been developed and validated. The method is based on reaction between drug and bromophenol blue and complex was measured at 421 nm. The slope, intercept and correlation coefficient was found to be 0.054, -0.020 and 0.999, respectively. Method was validated in terms of specificity, linearity, range, precision and accuracy. The developed method can be used to determine drug in both tablet and capsule formulations. Reaction was optimized using three parameters i.e., concentration of the dye, pH of the buffer, volume of the buffer and shaking time. Maximum stability of the chromophore was achieved by using pH 2 and 2 ml volume of buffer. Shaking time kept was 2 min and concentration of the dye used was 2 ml of 0.05% w/v solution. Method was validated in terms of linearity, precision, range, accuracy, LOD and LOQ and stochiometry of the method was also established using Mole ratio and Job's method of continuous variation. The dye benzonoid form (blue color) of dye ionized into quinonoid form (purple color) in presence of buffer and reacts with protonated form of drug in 1:1 ratio and forms an ion-pair complex (yellow color). PMID:23781431

  16. Investigation of combustion in a gasoline engine using spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Hunicz, Jacek; Piernikarski, Dariusz

    2001-08-01

    Spectrophotometric methods provide many new possibilities of investigation of combustion process in the automotive engine with spark ignition. Emission spectrum of the flames from the combustion chamber provides valuable information, which is difficult or even not accessible with the aid of other measurement methods. Spectral analysis allows to evaluate concentration of active compounds present in flames, which do not constitute final products of combustion. Concentration of radicals depends on some combustion parameters such as air-fuel ratio. The paper describes an engine test stand equipped with fiber-optic measurement system. The measurement system consists of an optical sensor mounted in the engine head, fiber-optic bundle for signal transmission, grating monochromator and photodetector. Voltage signal from the photodetector is recorded by the PC- based data acquisition system. The main aim of research was to verify usability of the designed fiber-optic measurement system in combustion diagnosis and to develop a method of evaluation of the air-fuel ratio on the base of simplified spectral analysis of the emission during combustion process in an automotive gasoline engine.

  17. Determination of berkelium by the method of spectrophotometric titration

    SciTech Connect

    Frolova, L.M.; Vityutnev, V.M.; Vasil'ev, V.M.

    1987-01-01

    The method that the authors propose consists of the following: berkelium is oxidized electrochemically, spectrophotometric titration of berkelium(IV) by a solution of the reducing agent is performed, and the amount of berkelium(IV) is determined according to the volume of the titrant, and considering the degree of oxidation of berkelium(III) to berkelium(IV), the total berkelium content in the sample is also determined. In this case the necessity for preliminary determination of the molar extinction coefficient of berkelium(IV) under the experimental conditions falls away. Moreover, the radiometric method of determining the berkelium content is not used. Successful titration requires selection of a reagent which, on the one hand, would rapidly reduce berkelium(VI), but on the other hand, neither itself nor the reaction products would interfere with the measurement of the optical density of berkelium(IV). As is well known, berkelium(IV) is quantitatively and rapidly reduced by hydrogen peroxide (10, 11), hydroxylamine (11), and nitrous acid (9). After preliminary experiments, they selected hydrogen peroxide and sodium nitrite as the titrants.

  18. Development and validation of spectrophotometric methods for estimating amisulpride in pharmaceutical preparations.

    PubMed

    Sharma, Sangita; Neog, Madhurjya; Prajapati, Vipul; Patel, Hiren; Dabhi, Dipti

    2010-01-01

    Five simple, sensitive, accurate and rapid visible spectrophotometric methods (A, B, C, D and E) have been developed for estimating Amisulpride in pharmaceutical preparations. These are based on the diazotization of Amisulpride with sodium nitrite and hydrochloric acid, followed by coupling with N-(1-naphthyl)ethylenediamine dihydrochloride (Method A), diphenylamine (Method B), beta-naphthol in an alkaline medium (Method C), resorcinol in an alkaline medium (Method D) and chromotropic acid in an alkaline medium (Method E) to form a colored chromogen. The absorption maxima, lambda(max), are at 523 nm for Method A, 382 and 490 nm for Method B, 527 nm for Method C, 521 nm for Method D and 486 nm for Method E. Beer's law was obeyed in the concentration range of 2.5-12.5 microg mL(-1) in Method A, 5-25 and 10-50 microg mL(-1) in Method B, 4-20 microg mL(-1) in Method C, 2.5-12.5 microg mL(-1) in Method D and 5-15 microg mL(-1) in Method E. The results obtained for the proposed methods are in good agreement with labeled amounts, when marketed pharmaceutical preparations were analyzed.

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

    PubMed

    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.

  20. Derivative-ratio spectrophotometric method for the determination of ternary mixture of aspirin, paracetamol and salicylic acid.

    PubMed

    El-Yazbi, Fawzi A; Hammud, Hassan H; Assi, Sulaf A

    2007-10-01

    A derivative spectrophotometric method was developed for the assay of a ternary mixture of aspirin (ASP), paracetamol (PAR) and salicylic acid (SAL). The method is based on the use of the first and second derivatives of the ratio spectra and measurement at zero-crossing wavelengths. The ratio spectra were obtained by dividing the absorption spectrum of the mixture by that of one of the components. The concentration of the other components are then determined from their respective calibration curves treated similarly. The described method was applied for the determination of these combinations in synthetic mixtures and dosage forms. The results obtained were accurate and precise.

  1. Derivative-ratio spectrophotometric method for the determination of ternary mixture of aspirin, paracetamol and salicylic acid

    NASA Astrophysics Data System (ADS)

    El-Yazbi, Fawzi A.; Hammud, Hassan H.; Assi, Sulaf A.

    2007-10-01

    A derivative spectrophotometric method was developed for the assay of a ternary mixture of aspirin (ASP), paracetamol (PAR) and salicylic acid (SAL). The method is based on the use of the first and second derivatives of the ratio spectra and measurement at zero-crossing wavelengths. The ratio spectra were obtained by dividing the absorption spectrum of the mixture by that of one of the components. The concentration of the other components are then determined from their respective calibration curves treated similarly. The described method was applied for the determination of these combinations in synthetic mixtures and dosage forms. The results obtained were accurate and precise.

  2. Development and validation of sensitive spectrophotometric method for determination of two antiepileptics in pharmaceutical formulations

    NASA Astrophysics Data System (ADS)

    Gouda, Ayman A.; Malah, Zakia Al

    2013-03-01

    Rapid, sensitive and validated spectrophotometric methods for the determination of two antiepileptics (gabapentin (GAB) and pregabalin (PRG)) in pure forms and in pharmaceutical formulations was developed. The method is based on the formation of charge transfer complex between drug and the chromogenic reagents quinalizarin (Quinz) and alizarin red S (ARS) producing charge transfer complexes in methanolic medium which showed an absorption maximum at 571 and 528 nm for GAB and 572 and 538 nm for PRG using Quinz and ARS, respectively. The optimization of the reaction conditions such as the type of solvent, reagent concentration and reaction time were investigated. Beer's law is obeyed in the concentration ranges 0.4-8.0 and 0.5-10 μg mL-1 for GAB and PRG using Quinz and ARS, respectively. The molar absorptivity, Sandell sensitivity, detection and quantification limits are also calculated. The correlation coefficients were ⩾0.9992 with a relative standard deviation (RSD%) of ⩽1.76. The methods are successfully applied to the determination of GAB and PRG in pharmaceutical formulations and the validity assesses by applying the standard addition technique, which compared with those obtained using the reported methods.

  3. Novel spectrophotometric methods for simultaneous determination of Amlodipine, Valsartan and Hydrochlorothiazide in their ternary mixture

    NASA Astrophysics Data System (ADS)

    Lotfy, Hayam M.; Hegazy, Maha A.; Mowaka, Shereen; Mohamed, Ekram Hany

    2015-04-01

    This work represents a comparative study of two smart spectrophotometric techniques namely; successive resolution and progressive resolution for the simultaneous determination of ternary mixtures of Amlodipine (AML), Hydrochlorothiazide (HCT) and Valsartan (VAL) without prior separation steps. These techniques consist of several consecutive steps utilizing zero and/or ratio and/or derivative spectra. By applying successive spectrum subtraction coupled with constant multiplication method, the proposed drugs were obtained in their zero order absorption spectra and determined at their maxima 237.6 nm, 270.5 nm and 250 nm for AML, HCT and VAL, respectively; while by applying successive derivative subtraction they were obtained in their first derivative spectra and determined at P230.8-246, P261.4-278.2, P233.7-246.8 for AML, HCT and VAL respectively. While in the progressive resolution, the concentrations of the components were determined progressively from the same zero order absorption spectrum using absorbance subtraction coupled with absorptivity factor methods or from the same ratio spectrum using only one divisor via amplitude modulation method can be used for the determination of ternary mixtures using only one divisor where the concentrations of the components are determined progressively. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulation containing the cited drugs. Moreover comparative study between spectrum addition technique as a novel enrichment technique and a well established one namely spiking technique was adopted for the analysis of pharmaceutical formulations containing low concentration of AML. The methods were validated as per ICH guidelines where accuracy, precision and specificity were found to be within their acceptable limits. The results obtained from the proposed methods were statistically compared with the reported one where no significant

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. A new, sensitive, and rapid spectrophotometric method for the determination of sulfa drugs.

    PubMed

    Nagaraja, Padmarajaiah; Yathirajan, Hemmige S; Sunitha, Kallanchira R; Vasantha, Ramanathapura A

    2002-01-01

    A sensitive, rapid, and simple spectrophotometric method is described for the determination of sulfa drugs. The method is based on the formation of a red-colored product by the diazotization of sulfonamides such as sulfathiazole (SFT), sulfadiazine (SFD), sulfacetamide (SFA), sulfamethoxazole (SFMx), sulfamerazine (SFMr), sulfaguanidine (SFG), and sulfamethazine (SFMt), followed by complexation with dopamine in the presence of molybdate ions in (1 + 1) H2SO4 medium. Absorbance of the resulting red product is measured at 490-510 nm, and the product is stable for 2 days at 27 degrees C. Beer's law is obeyed in the concentration range of 0.04-8.0 microg/mL at the wavelength of maximum absorption. The method was used successfully for the determination of some sulfonamides in tablets and eye drops. Common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method offers the advantages of simplicity, rapidity, and sensitivity without the need for extraction or heating. The limits of detection and quantitation were calculated for SFT, SFD, SFA, SFMx, SFMr, SFG, and SFMt.

  7. Simple spectrophotometric method for determination of phosphine residues in wheat.

    PubMed

    Rangaswamy, J R

    1984-01-01

    A method has been developed for determination of phosphine residues in wheat, based on the reaction of phosphine with silver nitrate in aqueous solution to form an egg-yellow chromophore with an absorption maximum at 400 nm. At this wavelength, there is a linear relationship between absorbance and concentration of phosphine in the range 10-100 ng/mL. Phosphine-fumigated wheat is soaked in a known volume of AgNO3 solution, and the absorbance of the filtrate is read against a blank at 400 nm. The method is sensitive, with lower detection and estimation limits of 0.008 and 0.01 micrograms PH3, respectively. Recovery of added phosphine from a closed system was 85-100%. Accuracy for this method has been compared with that for the gas chromatographic method.

  8. Development and Validation of UV-Visible Spectrophotometric Method for Simultaneous Determination of Eperisone and Paracetamol in Solid Dosage Form

    PubMed Central

    Khanage, Shantaram Gajanan; Mohite, Popat Baban; Jadhav, Sandeep

    2013-01-01

    Purpose: Eperisone Hydrochloride (EPE) is a potent new generation antispasmodic drug which is used in the treatment of moderate to severe pain in combination with Paracetamol (PAR). Both drugs are available in tablet dosage form in combination with a dose of 50 mg for EPE and 325 mg PAR respectively. Methods: The method is based upon Q-absorption ratio method for the simultaneous determination of the EPE and PAR. Absorption ratio method is used for the ratio of the absorption at two selected wavelength one of which is the iso-absorptive point and other being the λmax of one of the two components. EPE and PAR shows their iso-absorptive point at 260 nm in methanol, the second wavelength used is 249 nm which is the λmax of PAR in methanol. Results: The linearity was obtained in the concentration range of 5-25 μg/mL for EPE and 2-10 μg/mL for PAR. The proposed method was effectively applied to tablet dosage form for estimation of both drugs. The accuracy and reproducibility results are close to 100% with 2% RSD. Results of the analysis were validated statistically and found to be satisfactory. The results of proposed method have been validated as per ICH guidelines. Conclusion: A simple, precise and economical spectrophotometric method has been developed for the estimation of EPE and PAR in pharmaceutical formulation. PMID:24312876

  9. Spectrophotometric Method for Quantitative Determination of Cefixime in Bulk and Pharmaceutical Preparation Using Ferroin Complex

    NASA Astrophysics Data System (ADS)

    Naeem Khan, M.; Qayum, A.; Ur Rehman, U.; Gulab, H.; Idrees, M.

    2015-09-01

    A method was developed for the quantitative determination of cefixime in bulk and pharmaceutical preparations using ferroin complex. The method is based on the oxidation of the cefixime with Fe(III) in acidic medium. The formed Fe(II) reacts with 1,10-phenanthroline, and the ferroin complex is measured spectrophotometrically at 510 nm against reagent blank. Beer's law was obeyed in the concentration range 0.2-10 μg/ml with a good correlation of 0.993. The molar absorptivity was calculated and was found to be 1.375×105 L/mol × cm. The limit of detection (LOD) and limit of quantification (LOQ) were found to be 0.030 and 0.101 μg/ml respectively. The proposed method has reproducibility with a relative standard deviation of 5.28% (n = 6). The developed method was validated statistically by performing a recoveries study and successfully applied for the determination of cefixime in bulk powder and pharmaceutical formulations without interferences from common excipients. Percent recoveries were found to range from 98.00 to 102.05% for the pure form and 97.83 to 102.50% for pharmaceutical preparations.

  10. Simple spectrophotometric method for determination of melamine in liquid milks based on green Mannich reaction

    NASA Astrophysics Data System (ADS)

    Chansuvarn, Woravith; Panich, Sirirat; Imyim, Apichat

    2013-09-01

    A new and simple spectrophotometric method has been developed and validated for measuring the contamination of melamine in different milk products. The method is based upon measuring the absorption of the complex formed from melamine, 4-hydroxyacetophenone (Hap) and 1-pyrene carboxaldehyde (Pcd), which was adapted from the Mannich reaction. Quantitative analysis was done at a wavelength of 236 nm within a few minutes. The reaction was optimized by focusing on both obtaining high performance of the method and to concern the volatility and toxicity of used reagents. This method provided a linear dynamic range, limit of detection and limit of quantification of 0.100-3.78, 0.08 and 0.14 mg L-1, respectively. The relative standard deviation (RSD) was 3.6% (n = 10). The recoveries of melamine spiked liquid milk samples, with melamine concentrations of 0.63, 1.26, 1.89 and 2.52 mg L-1, were 87.7 ± 3.7%, 91.1 ± 8.8%, 89.2 ± 4.4% and 90.6 ± 3.6% (n = 3), respectively.

  11. Analysis of residual solvents in ampicillin powder by headspace spectrophotometric method.

    PubMed

    Farajzadeh, Mirali; Mardani, Alireza

    2002-02-01

    In this study a headspace spectrophotometric method is proposed for analysis of dichloromethane and isobutyl methyl keton (IBMK) residues in the ampicillin powder. Ampicillin is dissolved in 1 M NaOH in the vessel of an arsenic analyzer unit of an atomic absorption spectrophotometer. After 3-min stirring, the headspace has flowed by air into the flow-through cell and its absorbance is read at 196 nm, as emitted by a selenium hollow cathode lamp. The absorbance of the headspace is read in two cases (in the presence and absence of MnO4- ion). In the former case, the absorbance is only related to dichloromethane; in the latter, it is related to both solvents. By this method both solvents are determined in the ampicillin samples. The obtained results are compared with gas chromatography (GC) data. These results have good agreement. The proposed method is very rapid, selective and repeatable. Other solvents present, such as isopropyl alcohol, ethylacetate and triethylamine, are not interfering.

  12. Development and validation of sensitive kinetic spectrophotometric method for the determination of moxifloxacin antibiotic in pure and commercial tablets

    NASA Astrophysics Data System (ADS)

    Ashour, Safwan; Bayram, Roula

    2015-04-01

    New, accurate, sensitive and reliable kinetic spectrophotometric method for the assay of moxifloxacin hydrochloride (MOXF) in pure form and pharmaceutical formulations has been developed. The method involves the oxidative coupling reaction of MOXF with 3-methyl-2-benzothiazolinone hydrazone hydrochloride monohydrate (MBTH) in the presence of Ce(IV) in an acidic medium to form colored product with lambda max at 623 and 660 nm. The reaction is followed spectrophotometrically by measuring the increase in absorbance at 623 nm as a function of time. The initial rate and fixed time methods were adopted for constructing the calibration curves. The linearity range was found to be 1.89-40.0 μg mL-1 for initial rate and fixed time methods. The limit of detection for initial rate and fixed time methods is 0.644 and 0.043 μg mL-1, respectively. Molar absorptivity for the method was found to be 0.89 × 104 L mol-1 cm-1. Statistical treatment of the experimental results indicates that the methods are precise and accurate. The proposed method has been applied successfully for the estimation of moxifloxacin hydrochloride in tablet dosage form with no interference from the excipients. The results are compared with the official method.

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

    PubMed

    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 microg/mL (7.60x10(-7)-3.42x10(-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 microg/mL and 1.5%, respectively. And the molar absorption coefficient of the indirect determination of ethamsylate is 1.0x10(5)L/mol cm. The method is successfully applied to determine ethamsylate in pharmaceutical preparations and biological samples.

  14. 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

    USGS Publications Warehouse

    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.

  15. A comparative study of novel spectrophotometric methods based on isosbestic points; application on a pharmaceutical ternary mixture

    NASA Astrophysics Data System (ADS)

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

    This work represents the application of the isosbestic points present in different absorption spectra. Three novel spectrophotometric methods were developed, the first method is the absorption subtraction method (AS) utilizing the isosbestic point in zero-order absorption spectra; the second method is the amplitude modulation method (AM) utilizing the isosbestic point in ratio spectra; and third method is the amplitude summation method (A-Sum) utilizing the isosbestic point in derivative spectra. The three methods were applied for the analysis of the ternary mixture of chloramphenicol (CHL), dexamethasone sodium phosphate (DXM) and tetryzoline hydrochloride (TZH) in eye drops in the presence of benzalkonium chloride as a preservative. The components at the isosbestic point were determined using the corresponding unified regression equation at this point with no need for a complementary method. The obtained results were statistically compared to each other and to that of the developed PLS model. The specificity of the developed methods was investigated by analyzing laboratory prepared mixtures and the combined dosage form. The methods were validated as per ICH guidelines where accuracy, repeatability, inter-day precision and robustness were found to be within the acceptable limits. The results obtained from the proposed methods were statistically compared with official ones where no significant difference was observed.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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.

  18. Highly sensitive and selective spectrophotometric and spectrofluorimetric methods for the determination of ropinirole hydrochloride in tablets.

    PubMed

    Aydoğmuş, Zeynep

    2008-06-01

    Three sensitive, selective, accurate spectrophotometric and spectrofluorimetric methods have been developed for the determination of ropinirole hydrochloride in tablets. The first method was based on measuring the absorbance of drug solution in methanol at 250 nm. The Beer's law was obeyed in the concentration range 2.5-24 microg ml(-1). The second method was based on the charge transfer reaction of drug, as n-electron donor with 7,7,8,8-tetracyanoquinodimethane (TCNQ), as pi-acceptor in acetonitrile to give radical anions that are measured at 842 nm. The Beer's law was obeyed in the concentration range 0.6-8 microg ml(-1). The third method was based on derivatization reaction with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer of pH 8.5 followed by measuring the fluorescence intensity at 525 nm with excitation at 464 nm in chloroform. Beer's law was obeyed in the concentration range 0.01-1.3 microg ml(-1). The derivatization reaction product of drug with NBD-Cl was characterized by IR, 1H NMR and mass spectroscopy. The developed methods were validated. The following analytical parameters were investigated: the molar absorptivity (epsilon), limit of detection (LOD, microg ml(-1)) and limit of quantitation (LOQ, microg ml(-1)), precision, accuracy, recovery, and Sandell's sensitivity. Selectivity was validated by subjecting stock solution of ropinirole to acidic, basic, oxidative, and thermal degradation. No interference was observed from common excipients present in formulations. The proposed methods were successfully applied for determination of drug in tablets. The results of these proposed methods were compared with each other statistically. PMID:17719838

  19. Highly sensitive and selective spectrophotometric and spectrofluorimetric methods for the determination of ropinirole hydrochloride in tablets

    NASA Astrophysics Data System (ADS)

    Aydoğmuş, Zeynep

    2008-06-01

    Three sensitive, selective, accurate spectrophotometric and spectrofluorimetric methods have been developed for the determination of ropinirole hydrochloride in tablets. The first method was based on measuring the absorbance of drug solution in methanol at 250 nm. The Beer's law was obeyed in the concentration range 2.5-24 μg ml -1. The second method was based on the charge transfer reaction of drug, as n-electron donor with 7,7,8,8-tetracyanoquinodimethane (TCNQ), as π-acceptor in acetonitrile to give radical anions that are measured at 842 nm. The Beer's law was obeyed in the concentration range 0.6-8 μg ml -1. The third method was based on derivatization reaction with 4-chloro-7-nitrobenzofurazan (NBD-Cl) in borate buffer of pH 8.5 followed by measuring the fluorescence intensity at 525 nm with excitation at 464 nm in chloroform. Beer's law was obeyed in the concentration range 0.01-1.3 μg ml -1. The derivatization reaction product of drug with NBD-Cl was characterized by IR, 1H NMR and mass spectroscopy. The developed methods were validated. The following analytical parameters were investigated: the molar absorptivity ( ɛ), limit of detection (LOD, μg ml -1) and limit of quantitation (LOQ, μg ml -1), precision, accuracy, recovery, and Sandell's sensitivity. Selectivity was validated by subjecting stock solution of ropinirole to acidic, basic, oxidative, and thermal degradation. No interference was observed from common excipients present in formulations. The proposed methods were successfully applied for determination of drug in tablets. The results of these proposed methods were compared with each other statistically.

  20. A new spectrophotometric method for determination of selenium in cosmetic and pharmaceutical preparations after preconcentration with cloud point extraction.

    PubMed

    Soruraddin, Mohammad Hosein; Heydari, Rouhollah; Puladvand, Morteza; Zahedi, Mir Mehdi

    2011-01-01

    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. PMID:21647287

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

    PubMed Central

    Soruraddin, Mohammad Hosein; Heydari, Rouhollah; Puladvand, Morteza; Zahedi, Mir Mehdi

    2011-01-01

    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. PMID:21647287

  2. A new spectrophotometric method for determination of selenium in cosmetic and pharmaceutical preparations after preconcentration with cloud point extraction.

    PubMed

    Soruraddin, Mohammad Hosein; Heydari, Rouhollah; Puladvand, Morteza; Zahedi, Mir Mehdi

    2011-01-01

    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.

  3. Spectrophotometric methods for simultaneous determination of betamethasone valerate and fusidic acid in their binary mixture

    NASA Astrophysics Data System (ADS)

    Lotfy, Hayam Mahmoud; Salem, Hesham; Abdelkawy, Mohammad; Samir, Ahmed

    2015-04-01

    Five spectrophotometric methods were successfully developed and validated for the determination of betamethasone valerate and fusidic acid in their binary mixture. Those methods are isoabsorptive point method combined with the first derivative (ISO Point - D1) and the recently developed and well established methods namely ratio difference (RD) and constant center coupled with spectrum subtraction (CC) methods, in addition to derivative ratio (1DD) and mean centering of ratio spectra (MCR). New enrichment technique called spectrum addition technique was used instead of traditional spiking technique. The proposed spectrophotometric procedures do not require any separation steps. Accuracy, precision and linearity ranges of the proposed methods were determined and the specificity was assessed by analyzing synthetic mixtures of both drugs. They were applied to their pharmaceutical formulation and the results obtained were statistically compared to that of official methods. The statistical comparison showed that there is no significant difference between the proposed methods and the official ones regarding both accuracy and precision.

  4. Determination of Trace Amounts of Lead Using the Flotation-spectrophotometric method

    PubMed Central

    Shiri, Sabah; Delpisheh, Ali; Haeri, Ali; Poornajaf, Abdolhossein; Golzadeh, Babak; Shiri, Sina

    2011-01-01

    The present study describes a simple and highly selective method for separation, preconcentration and spectrophotometric determination of extremely low concentrations of lead. It is based on flotation of a complex of Pb2+ ions and Alizarin yellow between aqueous and n-hexane interface at pH = 6. The proposed procedure is also applied for determination of lead in both tap water and prepared sea water samples. Beer’s Law was obeyed over the concentration range of 3.86 × 10–8 To 8.20 × 10–7 molL−1 (8–170 ngmL−1) with an apparent molar absorptivity of 1.33 × 106 molL−1 cm−1 for a 100 mL aliquot of the water sample. The detection limit (n = 10) was 8.7 × 10–9 molL−1 (1.0 ngmL−1) and the Relative standard deviation (R.S.D), (n = 10) for 7.2 × 10–7 molL−1 (150 ngmL−1) of Pb (II) was 4.36%. A notable advantage of the method is that the determination of Pb (II) is free from the interference of almost all cations and ions found in the environment and waste water samples. The determination of Pb (II) in tap and synthetic seawater samples was also carried out by the present method. The results were satisfactorily comparable so that the applicability of the proposed method was confirmed to the real samples.

  5. Light absorption from particulate impurities in snow and ice determined by spectrophotometric analysis of filters.

    PubMed

    Grenfell, Thomas C; Doherty, Sarah J; Clarke, Antony D; Warren, Stephen G

    2011-05-10

    Light absorption by particulate impurities in snow and ice can affect the surface albedo and is important for the climate. The absorption properties of these particles can be determined by collecting and melting snow samples and extracting the particulate material by filtration of the meltwater. This paper describes the optical design and testing of a new instrument to measure the absorption spectrum from 400 to 750 nm wavelength of the particles collected on filters using an "integrating-sandwich" configuration. The measured absorption is shown to be unaffected by scattering of light from the deposited particulates. A set of calibration standards is used to derive an upper limit for the concentration of black carbon (BC) in the snow. The wavelength dependence of the absorption spectra from 450 to 600 nm is used to calculate an absorption Ångstrom exponent for the aerosol. This exponent is used to estimate the actual BC concentration in the snow samples as well as the relative contributions of BC and non-BC constituents to the absorption of solar radiation integrated over the wavelength band 300 to 750 nm. PMID:21556105

  6. Light absorption from particulate impurities in snow and ice determined by spectrophotometric analysis of filters

    SciTech Connect

    Grenfell, Thomas C.; Doherty, Sarah J.; Clarke, Antony D.; Warren, Stephen G.

    2011-05-10

    Light absorption by particulate impurities in snow and ice can affect the surface albedo and is important for the climate. The absorption properties of these particles can be determined by collecting and melting snow samples and extracting the particulate material by filtration of the meltwater. This paper describes the optical design and testing of a new instrument to measure the absorption spectrum from 400 to 750 nm wavelength of the particles collected on filters using an ''integrating-sandwich'' configuration. The measured absorption is shown to be unaffected by scattering of light from the deposited particulates. A set of calibration standards is used to derive an upper limit for the concentration of black carbon (BC) in the snow. The wavelength dependence of the absorption spectra from 450 to 600 nm is used to calculate an absorption Angstrom exponent for the aerosol. This exponent is used to estimate the actual BC concentration in the snow samples as well as the relative contributions of BC and non-BC constituents to the absorption of solar radiation integrated over the wavelength band 300 to 750 nm.

  7. Chromium speciation in environmental samples using a solid phase spectrophotometric method

    NASA Astrophysics Data System (ADS)

    Amin, Alaa S.; Kassem, Mohammed A.

    2012-10-01

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

  8. INVESTIGATION AND OPTIMIZATION OF TITRIMETRIC AND SPECTROPHOTOMETRIC METHODS FOR THE ASSAY OF FLUNARIZINE DIHYDROCHLORIDE USING IN SITU BROMINE.

    PubMed

    Prashanth, Kudige Nagaraj; Swamy, Nagaraju; Basavaiah, Kanakapura

    2016-01-01

    Three indirect methods for the assay of flunarizine dihydrochloride (FNH) in bulk drug and commercial formulation based on titrimetric and spectrophotometric techniques using bromate-bromide mixture are described. In titrimetry, a measured excess of bromate-bromide mixture is added to an acidified solution of FNH and the unreacted bromine is determined iodometrically (method A). Spectrophotometry involves the addition of a known excess of bromate-bromide mixture to FNH in acid medium followed by estimation of unreacted bromine by its reaction with excess iodide and the liberated iodine (I₃⁻) is either measured at 370 nm (method B) or liberated iodine reacted with starch followed by the measurement of the blue colored starch-iodide complex at 575 run (method C). Titrimetric method is applicable over the range 4.5-30.0 mg FNH (method A), and the reaction stoichiometry is found to be 1:2 (FNH:KBrO₃). The spectrophotometric methods are applicable over the concentration ranges 0.8-16.0 µg/mL and 0.4-8.0 µg/mL FNH for method B and method C, respectively. The molar absorptivities are calculated to be 2.83 x 10⁴ and 4.96 x 10⁴ L mol⁻¹cm⁻¹ for method B and method C, respectively, and the corresponding Sandell sensitivity values are 0.0168 and 0.0096 µg cm⁻². The proposed methods have been applied successfully for the determination of FNH in pure form and in its dosage form and the results were compared with those of a literature method by applying the Student's t-test and F-test. PMID:27008799

  9. INVESTIGATION AND OPTIMIZATION OF TITRIMETRIC AND SPECTROPHOTOMETRIC METHODS FOR THE ASSAY OF FLUNARIZINE DIHYDROCHLORIDE USING IN SITU BROMINE.

    PubMed

    Prashanth, Kudige Nagaraj; Swamy, Nagaraju; Basavaiah, Kanakapura

    2016-01-01

    Three indirect methods for the assay of flunarizine dihydrochloride (FNH) in bulk drug and commercial formulation based on titrimetric and spectrophotometric techniques using bromate-bromide mixture are described. In titrimetry, a measured excess of bromate-bromide mixture is added to an acidified solution of FNH and the unreacted bromine is determined iodometrically (method A). Spectrophotometry involves the addition of a known excess of bromate-bromide mixture to FNH in acid medium followed by estimation of unreacted bromine by its reaction with excess iodide and the liberated iodine (I₃⁻) is either measured at 370 nm (method B) or liberated iodine reacted with starch followed by the measurement of the blue colored starch-iodide complex at 575 run (method C). Titrimetric method is applicable over the range 4.5-30.0 mg FNH (method A), and the reaction stoichiometry is found to be 1:2 (FNH:KBrO₃). The spectrophotometric methods are applicable over the concentration ranges 0.8-16.0 µg/mL and 0.4-8.0 µg/mL FNH for method B and method C, respectively. The molar absorptivities are calculated to be 2.83 x 10⁴ and 4.96 x 10⁴ L mol⁻¹cm⁻¹ for method B and method C, respectively, and the corresponding Sandell sensitivity values are 0.0168 and 0.0096 µg cm⁻². The proposed methods have been applied successfully for the determination of FNH in pure form and in its dosage form and the results were compared with those of a literature method by applying the Student's t-test and F-test.

  10. Polymerization Evaluation by Spectrophotometric Measurements.

    ERIC Educational Resources Information Center

    Dunach, Jaume

    1985-01-01

    Discusses polymerization evaluation by spectrophotometric measurements by considering: (1) association degrees and molar absorptivities; (2) association degrees and equilibrium constants; and (3) absorbance and equilibrium constants. (JN)

  11. Spectrophotometric measurement of carboxyhaemoglobin: An evaluation of the method of Commins and Lawther

    PubMed Central

    Lily, R. E. C.; Cole, P. V.; Hawkins, L. H.

    1972-01-01

    Lily, R. E. C., Cole, P. V., and Hawkins, L. H. (1972).Brit. J. industr. Med.,29, 454-457. Spectrophotometric measurement of carboxyhaemoglobin. An evaluation of the method of Commins and Lawther. The spectrophotometric method of Commins and Lawther for the measurement of carboxyhaemoglobin (COHb) concentration was evaluated for both accuracy and sensitivity. The method was calibrated by equilibrating diluted blood samples with known concentrations of carbon monoxide (CO) in air and measuring the resultant COHb saturations. Over the range 0-40% COHb saturation the mean error was 0·67% COHb (SD 0·65). It is considered that the accuracy of the method is more than sufficient for measurement of both the high COHb levels found in clinical situations and the lower COHb saturation resulting from exposure to urban air and cigarette smoking. PMID:4636665

  12. Spectrophotometric and spectrofluorimetric methods for analysis of tramadol, acebutolol and dothiepin in pharmaceutical preparations

    NASA Astrophysics Data System (ADS)

    Abdellatef, Hisham E.; El-Henawee, Magda M.; El-Sayed, Heba M.; Ayad, Magda M.

    2006-12-01

    Sensitive spectrophotometric and spectrofluorimetric methods are described for the determination of tramadol, acebutolol and dothiepin (dosulepin) hydrochlorides. The two methods are based on the condensation of the cited drugs with the mixed anhydrides of malonic and acetic acids at 60 °C for 25-40 min. The coloured condensation products are suitable for the spectrophotometric and spectrofluorimetric determination at 329-333 and 431-434 nm (excitation at 389 nm), respectively. For the spectrophotometric method, Beer's law was obeyed from 0.5 to 2.5 μg ml -1 for tramadol, dothiepin and 5-25 μg ml -1 for acebutolol. Using the spectrofluorimetric method linearity ranged from 0.25 to 1.25 μg ml -1 for tramadol, dothiepin and 1-5 μg ml -1 for acebutolol. Mean percentage recoveries for the spectrophotometric method were 99.68 ± 1.00, 99.95 ± 1.11 and 99.72 ± 1.01 for tramadol, acebutolol and dothiepin, respectively and for the spectrofluorimetric method, recoveries were 99.5 ± 0.844, 100.32 ± 0.969 and 99.82 ± 1.15 for the three drugs, respectively. The optimum experimental parameters for the reaction has 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 were successfully applied for the determination of the selected drugs in their pharmaceutical preparations with good recoveries. The procedures were accurate, simple and suitable for quality control application.

  13. Simultaneous determination of mebeverine hydrochloride and chlordiazepoxide in their binary mixture using novel univariate spectrophotometric methods via different manipulation pathways

    NASA Astrophysics Data System (ADS)

    Lotfy, Hayam M.; Fayez, Yasmin M.; Michael, Adel M.; Nessim, Christine K.

    2016-02-01

    Smart, sensitive, simple and accurate spectrophotometric methods were developed and validated for the quantitative determination of a binary mixture of mebeverine hydrochloride (MVH) and chlordiazepoxide (CDZ) without prior separation steps via different manipulating pathways. These pathways were applied either on zero order absorption spectra namely, absorbance subtraction (AS) or based on the recovered zero order absorption spectra via a decoding technique namely, derivative transformation (DT) or via ratio spectra namely, ratio subtraction (RS) coupled with extended ratio subtraction (EXRS), spectrum subtraction (SS), constant multiplication (CM) and constant value (CV) methods. The manipulation steps applied on the ratio spectra are namely, ratio difference (RD) and amplitude modulation (AM) methods or applying a derivative to these ratio spectra namely, derivative ratio (DD1) or second derivative (D2). Finally, the pathway based on the ratio spectra of derivative spectra is namely, derivative subtraction (DS). The specificity of the developed methods was investigated by analyzing the laboratory mixtures and was successfully applied for their combined dosage form. The proposed methods were validated according to ICH guidelines. These methods exhibited linearity in the range of 2-28 μg/mL for mebeverine hydrochloride and 1-12 μg/mL for chlordiazepoxide. The obtained results were statistically compared with those of the official methods using Student t-test, F-test, and one way ANOVA, showing no significant difference with respect to accuracy and precision.

  14. A continuous spectrophotometric assay method for peptidylarginine deiminase type 4 activity.

    PubMed

    Liao, Ya-Fan; Hsieh, Hui-Chieh; Liu, Guang-Yaw; Hung, Hui-Chih

    2005-12-15

    A simple, continuous spectrophotometric assay for peptidylarginine deiminase (PAD) is described. Deimination of peptidylarginine results in the formation of peptidylcitrulline and ammonia. The ammonia released during peptidylarginine hydrolysis is coupled to the glutamate-dehydrogenase-catalyzed reductive amination of alpha-ketoglutarate to glutamate and reduced nicotinamide adenine dinucleotide (NADH) oxidation. The disappearance of absorbance at 340nm due to NADH oxidation is continuously measured. The specific activity obtained by this new protocol for highly purified human PAD is comparable to that obtained by a commonly used colorimetric procedure, which measures the ureido group of peptidylcitrulline by coupling with diacetyl monoxime. The present continuous spectrophotometric method is highly sensitive and accurate and is thus suitable for enzyme kinetic analysis of PAD. The Ca(2+) concentration for half-maximal activity of PAD obtained by this method is comparable to that previously obtained by the colorimetric procedure.

  15. Simple spectrophotometric method for estimation of disodium edetate in topical gel formulations

    PubMed Central

    Kamboj, Sunil; Sharma, Deepak; Nair, Anroop B.; Kamboj, Suman; Sharma, Rakesh Kumar; Ali, Javed; Pramod, K; Ansari, S. H.

    2011-01-01

    A simple, sensitive, cost-effective and reproducible UV-spectrophotometric method has been developed and validated for the estimation of disodium edetate in topical gel formulations. Solution of disodium edetate reacts with ferric chloride to form complex in 0.1 N HCl giving λmax at 270 nm. Beer's law was obeyed in the concentration range of 5–50 μg/mL (r2= 0.9997). The limit of detection and limit of quantitation were found to be 1.190 and 3.608 μg/mL, respectively. The results show that the procedure is accurate, precise, and reproducible (relative standard deviation < 1%), while being simple and less time consuming. The study concluded that the UV-spectrophotometric method could be used for the quantification of disodium edetate in pure form as well as in pharmaceutical formulations. PMID:23781446

  16. Two smart spectrophotometric methods for the simultaneous estimation of Simvastatin and Ezetimibe in combined dosage form.

    PubMed

    Magdy, Nancy; Ayad, Miriam F

    2015-02-25

    Two simple, accurate, precise, sensitive and economic spectrophotometric methods were developed for the simultaneous determination of Simvastatin and Ezetimibe in fixed dose combination products without prior separation. The first method depends on a new chemometrics-assisted ratio spectra derivative method using moving window polynomial least square fitting method (Savitzky-Golay filters). The second method is based on a simple modification for the ratio subtraction method. The suggested methods were validated according to USP guidelines and can be applied for routine quality control testing.

  17. Two smart spectrophotometric methods for the simultaneous estimation of Simvastatin and Ezetimibe in combined dosage form

    NASA Astrophysics Data System (ADS)

    Magdy, Nancy; Ayad, Miriam F.

    2015-02-01

    Two simple, accurate, precise, sensitive and economic spectrophotometric methods were developed for the simultaneous determination of Simvastatin and Ezetimibe in fixed dose combination products without prior separation. The first method depends on a new chemometrics-assisted ratio spectra derivative method using moving window polynomial least square fitting method (Savitzky-Golay filters). The second method is based on a simple modification for the ratio subtraction method. The suggested methods were validated according to USP guidelines and can be applied for routine quality control testing.

  18. Atomic absorption spectrophotometric and X-ray studies of respirable dusts in Indian coal mines

    SciTech Connect

    Rawat, N.S.; Sinha, J.D.; Sahoo, B.

    1982-01-01

    Quantitative determination of 10 minor and 8 trace elements in respirable coal dust by atomic absorption spectrophotometry is described herein. The coal dust samples were collected in the mine atmosphere during drilling in coal seams. A ''Hexhlet'' appratus specially designed and fitted with a horizontal elutriator was used to collect the respirable coal dust fraction. After destruction of organic matter by wet oxidation and filtering off the clay and silica, iron, calcium, magnesium, sodium, potassium, manganese, zinc, copper, cadmium, and nickel were determined directly in the resulting solution by atomic absorption spectrophotometry. The studies relate to a respiratoy disease-pneumoconiosis-affecting coal mine workers. X-Ray diffraction studies have shown the presence of kaolin, quartz, pirrsonite and beidellite clay minerals in the coal dust.

  19. [Determination of iodide ions content in the edible salts and medical preparations by spectrophotometric and voltamperometric methods].

    PubMed

    Rzeszutko, W; Stolarczyk, M; Apola, A

    1999-01-01

    In this paper the spectrophotometric and voltamperometric methods for the determination of the iodide ions content are presented. The conformity of the edible table salts iodisation to the Polish Standards and to the contests declared by the producer was verified.

  20. Handling of electronic absorption spectra with a desk-top computer-II: calculation of stability constants from spectrophotometric titrations.

    PubMed

    Zuberbühler, A D; Kaden, T A

    1979-12-01

    A fully automatic system for combined spectrophotometric and pH titrations was described in Part I. Its performance in the titration of weak acids and metal complexes is discussed, along with a computer program for numerical treatment of the data, based on Marquardt's modification of the Newton-Gauss non-linear least-squares method. The deprotonation of p-nitrophenol at concentrations of 4 x 10(-5) and 4 x 10(-6)M was studied in order to test the sensitivity. Results identical within the reproducibility of the pH-meter were obtained: pK(H) = 7.00 +/- 0.01 and 7.02 +/- 0.01, respectively. Three complexation reactions were studied: (1) the interaction of SCN(-) with the Co(2+) complex of 1,4,8,11-tetramethyl-1,4,8,11-tetra-azacyclotetradecane (TMC); five independent experiments gave pK [CoTMC (SCN)(+) right harpoon over left harpoon CoTMC(2+) + SCN(-)] = 3.099 +/- 0.003: (2) the deprotonation of the Cu(2+) complex of 3,7-diazanonanediamide (DANA); five experiments gave pK (CuDANA(2+) right harpoon over left harpoon CuDANAH(+)(-1) + H(+)) = 7.14 +/- 0.01 and pK (CuDANAH(+)(-1) right harpoon over left harpoon CuDANAH(-2) + H(+)) = 8.38 +/- 0.01: (3) for the reaction of Cu(2+) with 1,3,7-triazacyclodecane (L), data from different ligand: metal ratios had to be combined to obtain pK (CuL(2+) right harpoon over left harpoon Cu(2+) + L) = 16.19 +/- 0.01, pK (CuL(2+)(2) right harpoon over left harpoon CuL(2+) + L) = 10.30 +/- 0.01, and pK (Cu(2)L(2) (OH)(2+)(2) right harpoon over left harpoon 2 CuL(2+) + 2 OH(-)) = 14.58 +/- 0.03. Titration curves with a total change in absorbance of as little as 0.03 units could be analysed satisfactorily, extending considerably the useful range of concentrations for spectrophotometric titrations. In combined spectrophotometric/pH titrations the accuracy of the glass electrode is normally the limiting factor. Other equilibrium constants can easily be reproduced with standard errors of less than 0.01 log unit.

  1. Application of rapid cloud point extraction method for trace cobalt analysis coupled with spectrophotometric determination.

    PubMed

    Wen, Xiaodong; He, Lei; Shi, Chunsheng; Deng, Qingwen; Wang, Jiwei; Zhao, Xia

    2013-11-01

    In this work, the analytical performance of conventional spectrophotometer was improved through the coupling of effective preconcentration method with spectrophotometric determination. Rapidly synergistic cloud point extraction (RS-CPE) was used to pre-concentrate ultra trace cobalt and firstly coupled with spectrophotometric determination. The developed coupling was simple, rapid and efficient. The factors influencing RS-CPE and spectrophotometer were optimized. Under the optimal conditions, the limit of detection (LOD) was 0.6μgL(-1), with sensitivity enhancement factor of 23. The relative standard deviation (RSD) for seven replicate measurements of 50μgL(-1) of cobalt was 4.3%. The recoveries for the spiked samples were in the acceptable range of 93.8-105%.

  2. Application of rapid cloud point extraction method for trace cobalt analysis coupled with spectrophotometric determination

    NASA Astrophysics Data System (ADS)

    Wen, Xiaodong; He, Lei; Shi, Chunsheng; Deng, Qingwen; Wang, Jiwei; Zhao, Xia

    2013-11-01

    In this work, the analytical performance of conventional spectrophotometer was improved through the coupling of effective preconcentration method with spectrophotometric determination. Rapidly synergistic cloud point extraction (RS-CPE) was used to pre-concentrate ultra trace cobalt and firstly coupled with spectrophotometric determination. The developed coupling was simple, rapid and efficient. The factors influencing RS-CPE and spectrophotometer were optimized. Under the optimal conditions, the limit of detection (LOD) was 0.6 μg L-1, with sensitivity enhancement factor of 23. The relative standard deviation (RSD) for seven replicate measurements of 50 μg L-1 of cobalt was 4.3%. The recoveries for the spiked samples were in the acceptable range of 93.8-105%.

  3. Novel spectrophotometric method for determination of some macrolide antibiotics in pharmaceutical formulations using 1,2-naphthoquinone-4-sulphonate

    NASA Astrophysics Data System (ADS)

    Ashour, Safwan; Bayram, Roula

    2012-12-01

    New, simple and rapid spectrophotometric method has been developed and validated for the assay of two macrolide drugs, azithromycin (AZT) and erythromycin (ERY) in pure and pharmaceutical formulations. The proposed method was based on the reaction of AZT and ERY with sodium 1,2-naphthoquinone-4-sulphonate (NQS) in alkaline medium at 25 °C to form an orange-colored product of maximum absorption peak at 452 nm. All variables were studied to optimize the reaction conditions and the reaction mechanism was postulated. Beer's law was obeyed in the concentration range 1.5-33.0 and 0.92-8.0 μg mL-1 with limit of detection values of 0.026 and 0.063 μg mL-1 for AZT and ERY, respectively. The calculated molar absorptivity values are 4.3 × 104 and 12.3 × 104 L mol-1 cm-1 for AZT and ERY, respectively. The proposed methods were successfully applied to the determination of AZT and ERY in formulations and the results tallied well with the label claim. The results were statistically compared with those of an official method by applying the Student's t-test and F-test. No interference was observed from the concomitant substances normally added to preparations.

  4. Novel two wavelength spectrophotometric methods for simultaneous determination of binary mixtures with severely overlapping spectra

    NASA Astrophysics Data System (ADS)

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

    2015-02-01

    This work presents the application of different spectrophotometric techniques based on two wavelengths for the determination of severely overlapped spectral components in a binary mixture without prior separation. Four novel spectrophotometric methods were developed namely: induced dual wavelength method (IDW), dual wavelength resolution technique (DWRT), advanced amplitude modulation method (AAM) and induced amplitude modulation method (IAM). The results of the novel methods were compared to that of three well-established methods which were: dual wavelength method (DW), Vierordt's method (VD) and bivariate method (BV). The developed methods were applied for the analysis of the binary mixture of hydrocortisone acetate (HCA) and fusidic acid (FSA) formulated as topical cream accompanied by the determination of methyl paraben and propyl paraben present as preservatives. The specificity of the novel methods was investigated by analyzing laboratory prepared mixtures and the combined dosage form. The methods were validated as per ICH guidelines where accuracy, repeatability, inter-day precision and robustness were found to be within the acceptable limits. The results obtained from the proposed methods were statistically compared with official ones where no significant difference was observed. No difference was observed between the obtained results when compared to the reported HPLC method, which proved that the developed methods could be alternative to HPLC techniques in quality control laboratories.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. Four Derivative Spectrophotometric Methods for the Simultaneous Determination of Carmoisine and Ponceau 4R in Drinks and Comparison with High Performance Liquid Chromatography

    PubMed Central

    Turak, Fatma; Dinç, Mithat; Dülger, Öznur; Özgür, Mahmure Ustun

    2014-01-01

    Four simple, rapid, and accurate spectrophotometric methods were developed for the simultaneous determination of two food colorants, Carmoisine (E122) and Ponceau 4R (E124), in their binary mixtures and soft drinks. The first method is based on recording the first derivative curves and determining each component using the zero-crossing technique. The second method uses the first derivative of ratio spectra. The ratio spectra are obtained by dividing the absorption spectra of the binary mixture by that of one of the components. The third method, derivative differential procedure, is based on the measurement of difference absorptivities derivatized in first order of solution of drink samples in 0,1 N NaOH relative to that of an equimolar solution in 0,1 N HCl at wavelengths of 366 and 451 nm for Carmoisine and Ponceau 4R, respectively. The last method, based on the compensation method is presented for derivative spectrophotometric determination of E122 and E124 mixtures with overlapping spectra. By using ratios of the derivative maxima, the exact compensation of either component in the mixture can be achieved, followed by its determination. These proposed methods have been successfully applied to the binary mixtures and soft drinks and the results were statistically compared with the reference HPLC method (NMKL 130). PMID:24672549

  7. Spectrophotometric methods for simultaneous determination of ternary mixture of amlodipine besylate, olmesartan medoxomil and hydrochlorothiazide

    NASA Astrophysics Data System (ADS)

    Merey, Hanan A.; Ramadan, Nesrin K.; Diab, Sherine S.; Moustafa, Azza A.

    Four, accurate, precise, and sensitive spectrophotometric methods are developed for the simultaneous determination of a ternary mixture containing amlodipine besylate (AM), olmesartan medoxomil (OL) and hydrochlorothiazide (HZ), where AM is determined at its λmax 364.6 nm (0D), while (OL) and (HZ) are determined by different methods. Method (A) depends on determining OL and HZ by measuring the second derivative of the ratio spectra (2DD) at 254.4 and 338.6 nm, respectively. Method (B) is first derivative of the double divisor ratio spectra (D-1DD) at 260.4 and 273.0 nm for OL and HZ, respectively. Method (C) based on successive spectrophotometric resolution technique (SSRT). The technique starts with the ratio subtraction method then measuring OL and HZ at their isoabsorptive point at 260.0 nm, while HZ is measured using the amplitude of first derivative at 335.2 nm. Method (D) is mean centering of the ratio spectra (MCR) at 252.0 nm and 220.0 nm for OL and HZ, respectively. The specificity of the developed methods is investigated by analyzing laboratory prepared mixtures containing different ratios of the three drugs and their combined dosage form. The obtained results are statistically compared with those obtained by the official or reported methods, showing no significant difference with respect to accuracy and precision at p = 0.05.

  8. Determination of niobium in rocks by an isotope dilution spectrophotometric method

    USGS Publications Warehouse

    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.

  9. Development and validation of column high-performance liquid chromatographic and ultraviolet spectrophotometric methods for citalopram in tablets.

    PubMed

    Menegola, Júlia; Steppe, Martin; Schapoval, Elfrides E S

    2008-01-01

    Column high-performance liquid chromatographic (LC) and UV spectrophotometric methods for the quantitative determination of citalopram, a potent and selective serotonin reuptake inhibitor, in tablets were developed. 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 the reversed-phase technique on an ACE C18 column with a mobile phase composed of 0.30% triethylamine solution-acetonitrile (55 + 45, v/v) adjusted to pH 6.6 with 10% ortho-phosphoric acid at a flow rate of 1.0 mL/min and 25 degrees C. The UV spectrophotometric method was performed at 239 nm. The linearity of the LC method was in the range of 10.00-70.00 microg/mL, and 2.50-17.50 microg/mL for the UV spectrophotometric method. The interday and intraday assay precision was < 1.5% (relative standard deviation) for the LC and UV spectrophotometric methods. The recoveries were in the range 100.70-101.35% for the LC method and 98.48-98.65% for the UV spectrophotometric method. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the 2 methods. The proposed methods are highly sensitive, precise, and accurate and can be used for the reliable quantitation of citalopram in tablets. PMID:18376585

  10. Fluorescence quenching and spectrophotometric methods for the determination of daunorubicin with meso-tera (4-sulphophenyl) porphyrin as probe.

    PubMed

    Tian, Jing; Liu, Shaopu; Liu, Zhongfang; Yang, Jidong; Zhu, Jinghui; Qiao, Man; Hu, Xiaoli

    2014-01-01

    In this work, a synthetic meso-tera (4-sulfophenyl) porphyrin (TPPS4) was used as a probe to determine daunorubicin (DNR) by fluorescence quenching and spectrophotometric methods. At pH 4.6 potassium acid phthalate-NaOH buffer solution, a 1:1 complex of DNR interacted with TPPS4 formed via the electrostatic attractions and hydrophobic interactions, thus resulted in TPPS4 fluorescence quenching and absorption spectra change. The maximum excitation wavelength (λex) and the maximum emission wavelength (λem) are 435 nm and 672 nm, respectively. The fluorescence quenching values (ΔF) are the good linear relationship to the concentration of DNR in the range of 0.8-6.0 mgL(-1). The method exhibits high sensitivity with the detection limit (3σ) being 27.0 ng mL(-1). Meanwhile, a decrease of absorbance is detected at 433 nm with the appearance of a new absorption peak at 420 nm. The optimum reaction conditions, influencing factors and the effect of coexisting substances have been investigated in our experiment. The results showed that the method had a good selectivity and could be applied to determine DNR in serum and urine samples. In addition, the combine ratio between DNR and TPPS4 was measured and the charge distribution before and after reaction was calculated by quantum chemistry calculation AM1 method. The type of fluorescence quenching was discussed by the absorption spectra change, Stern-Volmer plots and fluorescence lifetime determination. PMID:24177862

  11. Development of normalized spectra manipulating spectrophotometric methods for simultaneous determination of Dimenhydrinate and Cinnarizine binary mixture.

    PubMed

    Lamie, Nesrine T; Yehia, Ali M

    2015-01-01

    Simultaneous determination of Dimenhydrinate (DIM) and Cinnarizine (CIN) binary mixture with simple procedures were applied. Three ratio manipulating spectrophotometric methods were proposed. Normalized spectrum was utilized as a divisor for simultaneous determination of both drugs with minimum manipulation steps. The proposed methods were simultaneous constant center (SCC), simultaneous derivative ratio spectrophotometry (S(1)DD) and ratio H-point standard addition method (RHPSAM). Peak amplitudes at isoabsorptive point in ratio spectra were measured for determination of total concentrations of DIM and CIN. For subsequent determination of DIM concentration, difference between peak amplitudes at 250 nm and 267 nm were used in SCC. While the peak amplitude at 275 nm of the first derivative ratio spectra were used in S(1)DD; then subtraction of DIM concentration from the total one provided the CIN concentration. The last RHPSAM was a dual wavelength method in which two calibrations were plotted at 220 nm and 230 nm. The coordinates of intersection point between the two calibration lines were corresponding to DIM and CIN concentrations. The proposed methods were successfully applied for combined dosage form analysis, Moreover statistical comparison between the proposed and reported spectrophotometric methods was applied. PMID:26037499

  12. Validation of UV spectrophotometric methods for the determination of dothiepin hydrochloride in pharmaceutical dosage form and stress degradation studies

    NASA Astrophysics Data System (ADS)

    Abdulrahman, Sameer A. M.; Basavaiah, K.; Cijo, M. X.; Vinay, K. B.

    2012-11-01

    Spectrophotometric methods have been developed for the determination of dothiepin hydrochloride (DOTH) in both pure and tablet dosage form and their limits of detection and quantification have been evaluated. The methods are based on the measurement of the absorbance of a DOTH solution either in 0.1 N HCl at 229 nm (method A) or in methanol at 231 nm (method B). Beer's law is obeyed over a concentration range of 1-16 μg/ml DOTH for both methods. Molar absorptivity values are calculated to be 2.48 × 104 and 2.42 × 104 l/(mol × cm) with Sandell sensitivity values of 0.0134 and 0.0137 μg/cm2 for methods A and B, respectively. The degradation behavior of DOTH was investigated under different stress conditions such as acid hydrolysis, alkaline hydrolysis, water hydrolysis, oxidation, dry heat treatment, and UV-degradation. The drug undergoes significant degradation under oxidative conditions only.

  13. Spectrophotometric determination of organic nitrogen by a modified Lassaigne method and its application to meat products and baby food.

    PubMed

    Demirata, Birsen; Apak, Resat; Afsar, Hüseyin; Tor, Izzet

    2002-01-01

    A modified Lassaigne method was developed for N determination based on fusion of the organic substance with metallic Na, conversion of the cyanide in the aqueous leachate to thiocyanate by ammonium polysulfide treatment, and colorimetric measurement of the thiocyanate formed by the addition of excessive ferric ions in acidic medium. The mean molar absorptivity of the Fe(NCS)2+ complex at 480 nm is 2.96 x 10(3) L/mol x cm, enabling quantitation of 0.25-7.72 ppm N (linear range) in the final solution. The relative amounts of Na, (NH4)2S2, and Fe(III) with respect to nitrogen in the analyte were optimized. The developed method was successfully applied to the determination of N in various brands of baby food, and it was compared statistically with the conventional Kjeldahl and elemental analysis methods. Protein nitrogen in a number of meat products was also precisely determined by the developed method. Thus, the total digestion time of the conventional Kjeldahl method was reduced considerably (e.g., to approximately 15 min for a dried sample) with a relatively simple spectrophotometric method requiring no sophisticated instrumentation.

  14. Development and Validation of Simultaneous Spectrophotometric Methods for Drotaverine Hydrochloride and Aceclofenac from Tablet Dosage Form

    PubMed Central

    Shah, S. A.; Shah, D. R.; Chauhan, R. S.; Jain, J. R.

    2011-01-01

    Two simple spectrophotometric methods have been developed for simultaneous estimation of drotaverine hydrochloride and aceclofenac from tablet dosage form. Method I is a simultaneous equation method (Vierodt's method), wavelengths selected are 306.5 and 276 nm. Method II is the absorbance ratio method (Q-Analysis), which employs 298.5 nm as λ1 and 276 nm as λ2 (λmax of AF) for formation of equations. Both the methods were found to be linear between the range of 8-32 μg/ml for drotaverine and 10-40 μg/ml for aceclofenac. The accuracy and precision were determined and found to comply with ICH guidelines. Both the methods showed good reproducibility and recovery with % RSD in the desired range. The methods were found to be rapid, specific, precise and accurate and can be successfully applied for the routine analysis of drotaverine and aceclofenac in their combined tablet dosage form. PMID:22457554

  15. Development and application of a shipboard method for spectrophotometric determination of trace dissolved manganese in estuarine and coastal waters

    NASA Astrophysics Data System (ADS)

    Feng, Sichao; Huang, Yongming; Yuan, Dongxing; Zhu, Yong; Zhou, Tingjin

    2015-01-01

    A shipboard method for the determination of trace dissolved manganese in estuarine and coastal waters was developed using a technique of reverse flow injection analysis, which adopted a 1-m liquid waveguide capillary cell and spectrophotometric detection of manganese derivation with 1-(2-pyridylazo)-2-naphthol (PAN). The design of dual-sample-carrier speeded up the sample throughput and eliminated the Schlieren effect. The salinity of estuarine and coastal waters caused a huge increase in the blank absorption value at the maximum absorption wavelength; therefore, a less sensitive detection wavelength was selected to achieve a low blank value while the method sensitivity was not significantly decreased. Method parameters were optimized. The salinity effect from estuarine and coastal waters was carefully investigated, and interference from iron was evaluated. The proposed method had high sensitivity with a detection limit of 3.0 nmol L-1 and a wide linear range of 10-1500 nmol L-1 for dissolved manganese in seawater (S=35). The analytical results of five water samples with different salinities obtained using the proposed method showed good agreement with those using a reference ICP-MS method. The sample throughput of the proposed method was 120 h-1, which was capable of obtaining high spatial and temporal resolution data in shipboard analysis. The proposed method had the advantages of convenient application in estuarine and coastal waters with different salinities, low detection limit, as well as high sample throughput. The proposed method was successfully applied to a 24 h on-line analysis and a shipboard underway analysis of dissolved manganese in the Jiulongjiang Estuary.

  16. Quantification of Rifaximin in Tablets by Spectrophotometric Method Ecofriendly in Ultraviolet Region

    PubMed Central

    2016-01-01

    Rifaximin is an oral nonabsorbable antibiotic that acts locally in the gastrointestinal tract with minimal systemic adverse effects. It does not have spectrophotometric method ecofriendly in the ultraviolet region described in official compendiums and literature. The analytical techniques for determination of rifaximin reported in the literature require large amount of time to release results and are significantly onerous. Furthermore, they use toxic reagents both for the operator and environment and, therefore, cannot be considered environmentally friendly analytical techniques. The objective of this study was to develop and validate an ecofriendly spectrophotometric method in the ultraviolet region to quantify rifaximin in tablets. The method was validated, showing linearity, selectivity, precision, accuracy, and robustness. It was linear over the concentration range of 10–30 mg L−1 with correlation coefficients greater than 0.9999 and limits of detection and quantification of 1.39 and 4.22 mg L−1, respectively. The validated method is useful and applied for the routine quality control of rifaximin, since it is simple with inexpensive conditions and fast in the release of results, optimizes analysts and equipment, and uses environmentally friendly solvents, being considered a green method, which does not prejudice either the operator or the environment. PMID:27429835

  17. Simultaneous determination of some anti-hypertensive drugs in their binary mixture by novel spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Fayez, Yasmin Mohammed

    2014-11-01

    Three simple, accurate and precise spectrophotometric methods manipulating ratio spectra were developed and validated for simultaneous determination of Irbesartan (IRB) and Hydrochlorothiazide (HCT) without prior separation namely; ratio subtraction coupled with constant multiplication (RS-CM), ratio difference (RD) and constant center (CC). The accuracy, precision and linearity ranges of the proposed methods were determined, and the methods were validated and the specificity was assessed by analyzing synthetic mixtures containing the cited drugs. The three methods were applied for the determination of the cited drugs in tablets and the obtained results were statistically compared with each other and with those of official methods. The comparison showed that there is no significant difference between the proposed methods and the official methods regarding both accuracy and precision.

  18. A Simple Spectrophotometric Method for the Determination of Thiobarbituric Acid Reactive Substances in Fried Fast Foods

    PubMed Central

    Zeb, Alam; Ullah, Fareed

    2016-01-01

    A simple and highly sensitive spectrophotometric method was developed for the determination of thiobarbituric acid reactive substances (TBARS) as a marker for lipid peroxidation in fried fast foods. The method uses the reaction of malondialdehyde (MDA) and TBA in the glacial acetic acid medium. The method was precise, sensitive, and highly reproducible for quantitative determination of TBARS. The precision of extractions and analytical procedure was very high as compared to the reported methods. The method was used to determine the TBARS contents in the fried fast foods such as Shami kebab, samosa, fried bread, and potato chips. Shami kebab, samosa, and potato chips have higher amount of TBARS in glacial acetic acid-water extraction system than their corresponding pure glacial acetic acid and vice versa in fried bread samples. The method can successfully be used for the determination of TBARS in other food matrices, especially in quality control of food industries. PMID:27123360

  19. A Simple Spectrophotometric Method for the Determination of Thiobarbituric Acid Reactive Substances in Fried Fast Foods.

    PubMed

    Zeb, Alam; Ullah, Fareed

    2016-01-01

    A simple and highly sensitive spectrophotometric method was developed for the determination of thiobarbituric acid reactive substances (TBARS) as a marker for lipid peroxidation in fried fast foods. The method uses the reaction of malondialdehyde (MDA) and TBA in the glacial acetic acid medium. The method was precise, sensitive, and highly reproducible for quantitative determination of TBARS. The precision of extractions and analytical procedure was very high as compared to the reported methods. The method was used to determine the TBARS contents in the fried fast foods such as Shami kebab, samosa, fried bread, and potato chips. Shami kebab, samosa, and potato chips have higher amount of TBARS in glacial acetic acid-water extraction system than their corresponding pure glacial acetic acid and vice versa in fried bread samples. The method can successfully be used for the determination of TBARS in other food matrices, especially in quality control of food industries. PMID:27123360

  20. A new spectrophotometric method for quantification of potassium solubilized by bacterial cultures.

    PubMed

    Rajawat, Mahendra Vikram Singh; Singh, Surender; Saxena, Anil Kumar

    2014-03-01

    A new spectrophotometric method was developed for the quantification of potassium in the culture broth supernatant of K-solubilizing bacteria. The standard curve of potassium with the new method, which is based on the measurement of cobalt, showed a regression coefficient (R2) of 0.998. The quantification values of potassium obtained with flame photometric method and the newly developed method showed a significant correlation (r) of 0.978. The new method depends on the precipitation of sodium cobaltinitrite with solubilized potassium in liquid medium as potassium sodium cobaltinitrite, which develops bluish green colour by the addition of conc. HCl. The intensity of developed colour can be recorded at 623 nm. This method involves less number of steps, is easy and time saving, and can be used for the reliable estimation of available potassium in culture broth supernatant of K-solubilizing bacteria. PMID:24669669

  1. Comparison of three spectrophotometric methods for analysis of egg yolk carotenoids.

    PubMed

    Islam, K M S; Schweigert, F J

    2015-04-01

    Carotenoids accumulated in the egg yolk are of importance for two reasons. Firstly they are important pigments influencing customer acceptance and secondly they are essential components with positive health effects either as antioxidants or as precursor of vitamin A. Different analytical methods are available to quantitatively identify carotenoids from egg yolk such as spectrophotometric methods described by AOAC (Association of Official Analytical Chemists) and HPLC (High Performance Liquid Chromatography). Both methods have in common that they are time consuming, need a laboratory environment and well trained technical operators. Recently, a rapid lab-independent spectrophotometric method (iCheck, BioAnalyt GmbH, Germany) has been introduced that claims to be less time consuming and easy to operate. The aim of the current study was therefore to compare the novel method with the two standard methods. Yolks of 80 eggs were analysed as aliquots by the three methods in parallel. While both spectrometric methods are only able measure total carotenoids as total ß-carotene, HPLC enables the determination of individual carotenoids such lutein, zeaxanthin, canthaxanthin, ß-carotene and β-apocarotenoic ester. In general, total carotenoids levels as obtained by AOAC were in average 27% higher than those obtained by HPLC. Carotenoid values obtained by the reference methods AOAC and HPLC are highly correlated with the iCheck method with r(2) of 0.99 and 0.94 for iCheck vs. AOAC and iCheck vs. HPLC, respectively (both p<0.001). Bland Altman analysis showed that the novel iCheck method is comparable to the reference methods. In conclusion, the novel rapid and portable iCheck method is a valid and effective tool to determine total carotenoid of egg yolk under laboratory-independent conditions with little trained personal.

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

    PubMed

    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 ((1)DD), 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.

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

    NASA Astrophysics Data System (ADS)

    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.

  4. Validated stability-indicating spectrophotometric methods for the determination of cefixime trihydrate in the presence of its acid and alkali degradation products.

    PubMed

    Mostafa, Nadia M; Abdel-Fattah, Laila; Weshahy, Soheir A; Hassan, Nagiba Y; Boltia, Shereen A

    2015-01-01

    Five simple, accurate, precise, and economical spectrophotometric methods have been developed for the determination of cefixime trihydrate (CFX) in the presence of its acid and alkali degradation products without prior separation. In the first method, second derivative (2D) and first derivative (1D) spectrophotometry was applied to the absorption spectra of CFX and its acid (2D) or alkali (1D) degradation products by measuring the amplitude at 289 and 308 nm, respectively. The second method was a first derivative (1DD) ratio spectrophotometric method where the peak amplitudes were measured at 311 nm in presence of the acid degradation product, and 273 and 306 nm in presence of its alkali degradation product. The third method was ratio subtraction spectrophotometry where the drug is determined at 286 nm in laboratory-prepared mixtures of CFX and its acid or alkali degradation product. The fourth method was based on dual wavelength analysis; two wavelengths were selected at which the absorbances of one component were the same, so wavelengths 209 and 252 nm were used to determine CFX in presence of its acid degradation product and 310 and 321 nm in presence of its alkali degradation product. The fifth method was bivariate spectrophotometric calibration based on four linear regression equations obtained at the wavelengths 231 and 290 nm, and 231 and 285 nm for the binary mixture of CFX with either its acid or alkali degradation product, respectively. The developed methods were successfully applied to the analysis of CFX in laboratory-prepared mixtures and pharmaceutical formulations with good recoveries, and their validation was carried out following the International Conference on Harmonization guidelines. The results obtained were statistically compared with each other and showed no significant difference with respect to accuracy and precision.

  5. Validated spectrophotometric methods for determination of sodium valproate based on charge transfer complexation reactions

    NASA Astrophysics Data System (ADS)

    Belal, Tarek S.; El-Kafrawy, Dina S.; Mahrous, Mohamed S.; Abdel-Khalek, Magdi M.; Abo-Gharam, Amira H.

    2016-02-01

    This work presents the development, validation and application of four simple and direct spectrophotometric methods for determination of sodium valproate (VP) through charge transfer complexation reactions. The first method is based on the reaction of the drug with p-chloranilic acid (p-CA) in acetone to give a purple colored product with maximum absorbance at 524 nm. The second method depends on the reaction of VP with dichlone (DC) in dimethylformamide forming a reddish orange product measured at 490 nm. The third method is based upon the interaction of VP and picric acid (PA) in chloroform resulting in the formation of a yellow complex measured at 415 nm. The fourth method involves the formation of a yellow complex peaking at 361 nm upon the reaction of the drug with iodine in chloroform. Experimental conditions affecting the color development were studied and optimized. Stoichiometry of the reactions was determined. The proposed spectrophotometric procedures were effectively validated with respect to linearity, ranges, precision, accuracy, specificity, robustness, detection and quantification limits. Calibration curves of the formed color products with p-CA, DC, PA and iodine showed good linear relationships over the concentration ranges 24-144, 40-200, 2-20 and 1-8 μg/mL respectively. The proposed methods were successfully applied to the assay of sodium valproate in tablets and oral solution dosage forms with good accuracy and precision. Assay results were statistically compared to a reference pharmacopoeial HPLC method where no significant differences were observed between the proposed methods and reference method.

  6. Kinetic spectrophotometric method for the determination of morphine in biological samples

    NASA Astrophysics Data System (ADS)

    Sheibani, A.; Shishehbore, M. Reza; Mirparizi, E.

    2010-10-01

    In this paper a simple, selective and inexpensive kinetic method was developed for the determination of morphine based on its inhibitory effect on the Janus green-bromate system in sulfuric acid media. The reaction was monitored spectrophotometrically at 618 nm by a fixed time method. The effect of different parameters such as concentration of reactants and temperature on the rate of reaction was investigated and optimum conditions were obtained. The calibration curve was linear in the concentration range 0.07-7.98 mg L -1 of morphine, and detection limit of the method was 3.0 × 10 -2 mg L -1. The relative standard deviation for five determinations of 3.74 mg L -1 of morphine was 0.57%. Finally, the proposed method was successfully applied to the determination of morphine in human urine and serum as real samples.

  7. Validated spectrophotometric methods for simultaneous determination of Omeprazole, Tinidazole and Doxycycline in their ternary mixture

    NASA Astrophysics Data System (ADS)

    Lotfy, Hayam M.; Hegazy, Maha A.; Mowaka, Shereen; Mohamed, Ekram Hany

    2016-01-01

    A comparative study of smart spectrophotometric techniques for the simultaneous determination of Omeprazole (OMP), Tinidazole (TIN) and Doxycycline (DOX) without prior separation steps is developed. These techniques consist of several consecutive steps utilizing zero/or ratio/or derivative spectra. The proposed techniques adopt nine simple different methods, namely direct spectrophotometry, dual wavelength, first derivative-zero crossing, amplitude factor, spectrum subtraction, ratio subtraction, derivative ratio-zero crossing, constant center, and successive derivative ratio method. The calibration graphs are linear over the concentration range of 1-20 μg/mL, 5-40 μg/mL and 2-30 μg/mL for OMP, TIN and DOX, respectively. These methods are tested by analyzing synthetic mixtures of the above drugs and successfully applied to commercial pharmaceutical preparation. The methods that are validated according to the ICH guidelines, accuracy, precision, and repeatability, were found to be within the acceptable limits.

  8. Validated spectrophotometric methods for simultaneous determination of Omeprazole, Tinidazole and Doxycycline in their ternary mixture.

    PubMed

    Lotfy, Hayam M; Hegazy, Maha A; Mowaka, Shereen; Mohamed, Ekram Hany

    2016-01-15

    A comparative study of smart spectrophotometric techniques for the simultaneous determination of Omeprazole (OMP), Tinidazole (TIN) and Doxycycline (DOX) without prior separation steps is developed. These techniques consist of several consecutive steps utilizing zero/or ratio/or derivative spectra. The proposed techniques adopt nine simple different methods, namely direct spectrophotometry, dual wavelength, first derivative-zero crossing, amplitude factor, spectrum subtraction, ratio subtraction, derivative ratio-zero crossing, constant center, and successive derivative ratio method. The calibration graphs are linear over the concentration range of 1-20 μg/mL, 5-40 μg/mL and 2-30 μg/mL for OMP, TIN and DOX, respectively. These methods are tested by analyzing synthetic mixtures of the above drugs and successfully applied to commercial pharmaceutical preparation. The methods that are validated according to the ICH guidelines, accuracy, precision, and repeatability, were found to be within the acceptable limits. PMID:26322842

  9. Study on the determination of trace Ni (II) by the catalytic kinetic spectrophotometric method

    NASA Astrophysics Data System (ADS)

    Ji, Hongwei; Cao, Hengxia; Xin, Huizhen; Li, Shuang

    2010-03-01

    A new kinetic spectrophotometric method has been developed for the determination of trace Ni (II) in natural water. The method is based on the catalytic effect of Ni (II) on the oxidation of weak acid brilliant blue dye (RAWL) by KIO4 in acid medium. The concentration of nickel (II) can be determined spectrophotometrically by measuring the decrease of absorbance of RAWL at λ = 626 nm using the fix-time method. The influencing factors are investigated by the orthogonal experimental design. The obtained optimum analytical conditions are: pH = 2.00, c RAWL = 5.00×10-5 mol L-1, c KIO 4 = 2.00×10-5 mol L -1, the reaction time t = 10 min and the temperature T = 25°C. Under the optimum conditions, the developed method allows the measurement of Ni (II) in a range of 0-40.0 ng mL-1. The standard deviation of eleven independent measurements of blank reaction is S = 3.08×10-3 and the limit of detection is 2.20 ng mL-1. The relative standard deviations (RSDs) in six replicate determinations of 5 ng mL-1 and 8 ng mL-1 Ni (II) are 2.87% and 1.11%, respectively. Moreover, the experiments show few cations and anions can interfere with the measurement of Ni (II). The recovery efficiencies of this method are in a range of 97.0%-102.5% in freshwater samples. But there is a decreasing effect, which is about 0.2 times the added Ni (II) in seawater medium. After reasonable calibration this processing method is used for the determination of Ni (II) in seawater samples successfully. The results show this developed method has high accuracy and precision, high sensitivity, large range of linearity and high speed. The method can, therefore, be employed at room temperature.

  10. Spectrophotometric method for the assay of steroid 5α-reductase activity of rat liver and prostate microsomes.

    PubMed

    Iwai, Atsushi; Yoshimura, Teruki; Wada, Keiji; Watabe, Satoshi; Sakamoto, Yuki; Ito, Etsuro; Miura, Toshiaki

    2013-01-01

    A simple spectrophotometric method for the assay of steroid 5α-reductase (5α-SR) was developed in which 5α-dihydrotestosterone (5α-DHT) and 5α-androstane-3α,17β-diol (5α-diol), metabolites formed in the NADPH-dependent reduction of testosterone with enzyme sources of 5α-SR, were measured by enzymatic cycling using 3α-hydroxysteroid dehydrogenase in the presence of excess thionicotinamide-adenine dinucleotide (thio-NAD) and NADH. It was found that 5α-SR activity was proportional to the accumulated thio-NADH having an absorption maximum at 400 nm. Because of the high cycling rate (> 600 cycle per min) and no interference from testosterone, enzymatic cycling can determine the sum of 5α-DHT and 5α-diol at the picomole level without separation from excess testosterone. The present method was readily applicable to the assay of 5α-SR activity of rat liver and prostate microsomes as well as to the assay of inhibitory activity of finasteride, a synthetic inhibitor of 5α-SR. PMID:23574674

  11. Simultaneous estimation of ramipril, acetylsalicylic acid and atorvastatin calcium by chemometrics assisted UV-spectrophotometric method in capsules.

    PubMed

    Sankar, A S Kamatchi; Vetrichelvan, Thangarasu; Venkappaya, Devashya

    2011-09-01

    In the present work, three different spectrophotometric methods for simultaneous estimation of ramipril, aspirin and atorvastatin calcium in raw materials and in formulations are described. Overlapped data was quantitatively resolved by using chemometric methods, viz. inverse least squares (ILS), principal component regression (PCR) and partial least squares (PLS). Calibrations were constructed using the absorption data matrix corresponding to the concentration data matrix. The linearity range was found to be 1-5, 10-50 and 2-10 μg mL-1 for ramipril, aspirin and atorvastatin calcium, respectively. The absorbance matrix was obtained by measuring the zero-order absorbance in the wavelength range between 210 and 320 nm. A training set design of the concentration data corresponding to the ramipril, aspirin and atorvastatin calcium mixtures was organized statistically to maximize the information content from the spectra and to minimize the error of multivariate calibrations. By applying the respective algorithms for PLS 1, PCR and ILS to the measured spectra of the calibration set, a suitable model was obtained. This model was selected on the basis of RMSECV and RMSEP values. The same was applied to the prediction set and capsule formulation. Mean recoveries of the commercial formulation set together with the figures of merit (calibration sensitivity, selectivity, limit of detection, limit of quantification and analytical sensitivity) were estimated. Validity of the proposed approaches was successfully assessed for analyses of drugs in the various prepared physical mixtures and formulations.

  12. Sensitive spectrophotometric method for the determination of superoxide dismutase activity in tissue extracts

    SciTech Connect

    Paoletti, F.; Aldinucci, D.; Mocali, A.; Caparrini, A.

    1986-05-01

    Superoxide dismutase (EC 1.15.1.1) has been assayed by a spectrophotometric method based on the inhibition of a superoxide-driven NADH oxidation. The assay consists of a purely chemical reaction sequence which involves EDTA. Mn(II), mercaptoethanol, and molecular oxygen, requiring neither auxiliary enzymes nor sophisticated equipment. The method is very flexible and rapid and is applicable with high sensitivity to the determination of both pure and crude superoxide dismutase preparations. The decrease of the rate of NADH oxidation is a function of enzyme concentration, and saturation levels are attainable. Fifty percent inhibition, corresponding to one unit of the enzyme, is produced by approximately 15 ng of pure superoxide dismutase. Experiments on rat liver cytosol have shown the specificity of the method for superoxide dismutase. Moreover, common cellular components do not interfere with the measurement, except for hemoglobin when present at relatively high concentrations. The assay is performed at physiological pH and is unaffected by catalase.

  13. Spectrophotometric method for determination parts per million levels of cyclohexylamine in water.

    PubMed

    Kumbhar, A G; Narasimhan, S V; Mathur, P K

    1998-10-01

    UV-vis spectrophotometric method for the analysis of cyclohexylamine (CHA) in aqueous medium in the range of 0.3-20 ppm was developed by coupling CHA with sodium 1,2-naphthaquinone-4-sulphonate (NQS). At 470 nm a calibration slope of 0.028 OD ppm(-1) was observed. Minimum detection limit was 0.3 ppm with standard deviation of 0.1 ppm. Reagent concentration and solution pH for the analysis are optimised by studying its effect on absorbance at 470 nm. The method was applied to analyse CHA for evaluating the performance of ion exchange resin used in condensate purification plant (CPP) of power station where, CHA is used as all volatile treatment (AVT) reagent to inhibit steam generator (SG) corrosion. Structure of the adduct formed by coupling CHA with NQS is elucidated using NMR ((1)H and (13)C) and IR spectra, CHN analysis and mole ratio variation method. PMID:18967343

  14. Development and Validation of Stability-Indicating Derivative Spectrophotometric Methods for Determination of Dronedarone Hydrochloride

    NASA Astrophysics Data System (ADS)

    Chadha, R.; Bali, A.

    2016-05-01

    Rapid, sensitive, cost effective and reproducible stability-indicating derivative spectrophotometric methods have been developed for the estimation of dronedarone HCl employing peak-zero (P-0) and peak-peak (P-P) techniques, and their stability-indicating potential assessed in forced degraded solutions of the drug. The methods were validated with respect to linearity, accuracy, precision and robustness. Excellent linearity was observed in concentrations 2-40 μg/ml ( r 2 = 0.9986). LOD and LOQ values for the proposed methods ranged from 0.42-0.46 μg/ml and 1.21-1.27 μg/ml, respectively, and excellent recovery of the drug was obtained in the tablet samples (99.70 ± 0.84%).

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

    PubMed

    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.

  16. Development of microwave assisted spectrophotometric method for the determination of glucose

    NASA Astrophysics Data System (ADS)

    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.

  17. Validated spectrophotometric method for the determination, spectroscopic characterization and thermal structural analysis of duloxetine with 1,2-naphthoquinone-4-sulphonate

    NASA Astrophysics Data System (ADS)

    Ulu, Sevgi Tatar; Elmali, Fikriye Tuncel

    2012-03-01

    A novel, selective, sensitive and simple spectrophotometric method was developed and validated for the determination of the antidepressant duloxetine hydrochloride in pharmaceutical preparation. The method was based on the reaction of duloxetine hydrochloride with 1,2-naphthoquinone-4-sulphonate (NQS) in alkaline media to yield orange colored product. The formation of this complex was also confirmed by UV-visible, FTIR, 1H NMR, Mass spectra techniques and thermal analysis. This method was validated for various parameters according to ICH guidelines. Beer's law is obeyed in a range of 5.0-60 μg/mL at the maximum absorption wavelength of 480 nm. The detection limit is 0.99 μg/mL and the recovery rate is in a range of 98.10-99.57%. The proposed methods was validated and applied to the determination of duloxetine hydrochloride in pharmaceutical preparation. The results were statistically analyzed and compared to those of a reference UV spectrophotometric method.

  18. Comparative study of novel versus conventional two-wavelength spectrophotometric methods for analysis of spectrally overlapping binary mixture

    NASA Astrophysics Data System (ADS)

    Lotfy, Hayam M.; Hegazy, Maha A.; Rezk, Mamdouh R.; Omran, Yasmin Rostom

    2015-09-01

    Smart spectrophotometric methods have been applied and validated for the simultaneous determination of a binary mixture of chloramphenicol (CPL) and prednisolone acetate (PA) without preliminary separation. Two novel methods have been developed; the first method depends upon advanced absorbance subtraction (AAS), while the other method relies on advanced amplitude modulation (AAM); in addition to the well established dual wavelength (DW), ratio difference (RD) and constant center coupled with spectrum subtraction (CC-SS) methods. Accuracy, precision and linearity ranges of these methods were determined. Moreover, selectivity was assessed by analyzing synthetic mixtures of both drugs. The proposed methods were successfully applied to the assay of drugs in their pharmaceutical formulations. No interference was observed from common additives and the validity of the methods was tested. The obtained results have been statistically compared to that of official spectrophotometric methods to give a conclusion that there is no significant difference between the proposed methods and the official ones with respect to accuracy and precision.

  19. Simultaneous determination of Cinnarizine and Domperidone by area under curve and dual wavelength spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Abdelrahman, Maha M.

    2013-09-01

    Accurate, selective and sensitive spectrophotometric methods have been developed and validated for simultaneous determination of Cinnarizine and Domperidone, a binary mixture with overlapping spectra, without preliminary separation. These methods include area under the curve (AUC) and dual wavelength spectrophotometry. For the AUC method, the area under curve of mixture solutions in the wavelength ranges 241-258 nm and 280-292 nm were selected for determination of Cinnarizine and Domperidone and by applying Cramer's rule, concentration of each drug was obtained. In dual wavelength method, two wavelengths were selected for each drug in a way so that the difference in absorbance is zero for another drug. Domperidone shows equal absorbance at 240.2 nm and 273.2 nm, where the differences in absorbance were measured for the determination of Cinnarizine. Similarly, differences in absorbance at 230.8 nm and 259.2 nm were measured for determination of Domperidone. The proposed methods were applied for determination of Cinnarizine and Domperidone over the concentration ranges of 2-20 and 2-22 μg mL-1, respectively. The suggested methods were validated as per USP guidelines and the results revealed that they are reliable, reproducible and precise for routine use with short analysis time. The results obtained by the proposed methods were statistically compared to the reported method, and there was no significant difference between them regarding both accuracy and precision.

  20. Simultaneous determination of Cinnarizine and Domperidone by area under curve and dual wavelength spectrophotometric methods.

    PubMed

    Abdelrahman, Maha M

    2013-09-01

    Accurate, selective and sensitive spectrophotometric methods have been developed and validated for simultaneous determination of Cinnarizine and Domperidone, a binary mixture with overlapping spectra, without preliminary separation. These methods include area under the curve (AUC) and dual wavelength spectrophotometry. For the AUC method, the area under curve of mixture solutions in the wavelength ranges 241-258 nm and 280-292 nm were selected for determination of Cinnarizine and Domperidone and by applying Cramer's rule, concentration of each drug was obtained. In dual wavelength method, two wavelengths were selected for each drug in a way so that the difference in absorbance is zero for another drug. Domperidone shows equal absorbance at 240.2 nm and 273.2 nm, where the differences in absorbance were measured for the determination of Cinnarizine. Similarly, differences in absorbance at 230.8 nm and 259.2 nm were measured for determination of Domperidone. The proposed methods were applied for determination of Cinnarizine and Domperidone over the concentration ranges of 2-20 and 2-22 μg mL(-1), respectively. The suggested methods were validated as per USP guidelines and the results revealed that they are reliable, reproducible and precise for routine use with short analysis time. The results obtained by the proposed methods were statistically compared to the reported method, and there was no significant difference between them regarding both accuracy and precision. PMID:23735208

  1. Mean centering of double divisor ratio spectra, a novel spectrophotometric method for analysis of ternary mixtures

    NASA Astrophysics Data System (ADS)

    Hassan, Said A.; Elzanfaly, Eman S.; Salem, Maissa Y.; El-Zeany, Badr A.

    2016-01-01

    A novel spectrophotometric method was developed for determination of ternary mixtures without previous separation, showing significant advantages over conventional methods. The new method is based on mean centering of double divisor ratio spectra. The mathematical explanation of the procedure is illustrated. The method was evaluated by determination of model ternary mixture and by the determination of Amlodipine (AML), Aliskiren (ALI) and Hydrochlorothiazide (HCT) in laboratory prepared mixtures and in a commercial pharmaceutical preparation. For proper presentation of the advantages and applicability of the new method, a comparative study was established between the new mean centering of double divisor ratio spectra (MCDD) and two similar methods used for analysis of ternary mixtures, namely mean centering (MC) and double divisor of ratio spectra-derivative spectrophotometry (DDRS-DS). The method was also compared with a reported one for analysis of the pharmaceutical preparation. The method was validated according to the ICH guidelines and accuracy, precision, repeatability and robustness were found to be within the acceptable limits.

  2. First-order derivative UV spectrophotometric method for simultaneous measurement of delapril and manidipine in tablets.

    PubMed

    Todeschini, Vítor; Barden, Amanda Thomas; Sfair, Leticia Lenz; da Silva Sangoi, Maximiliano; Volpato, Nadia Maria

    2013-01-01

    A first-order derivative spectrophotometric (1D-UV) method was developed and validated for simultaneous determination of delapril (DEL) and manidipine (MAN) in tablets. The 1D-UV spectra were obtained using change lambda = 4.0 nm and wavelength set at 228 nm for DEL and 246 nm for MAN. The method was validated in accordance with the ICH requirements, involving the specificity, linearity, precision, accuracy, robustness and limits of detection and quantitation. The method showed high specificity in the presence of two drugs and formulation excipients and was linear over the concentration range of 18-54 microg mL(-1) (r2 = 0.9994) for DEL and 6-18 microg mL(-1) (r2 = 0.9981) for MAN with adequate results for the precision (< or = 1.47%) and accuracy (98.98% for DEL and 100.50% for MAN). Moreover, the method proved to be robust by a Plackett-Burman experimental design evaluation. The proposed 'D-UV method was successfully applied for simultaneous analysis of DEL and MAN in tablets and can be used as alternative green method to separation techniques. The results were compared with the validated liquid chromatography, capillary electrophoresis and liquid chromatography-tandem mass spectrometry methods, showing non-significant difference.

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

    PubMed

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

    2015-03-15

    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 (D(1)) where TXN and CZM were determined at 294 and 483.5 nm, respectively. Method B is first derivative of ratio spectra (DD(1)) 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 D(1) 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.

  4. Validated spectrophotometric and chromatographic methods for simultaneous determination of ketorolac tromethamine and phenylephrine hydrochloride.

    PubMed

    Belal, T S; El-Kafrawy, D S; Mahrous, M S; Abdel-Khalek, M M; Abo-Gharam, A H

    2016-07-01

    This work describes five simple and reliable spectrophotometric and chromatographic methods for analysis of the binary mixture of ketorolac tromethamine (KTR) and phenylephrine hydrochloride (PHE). Method I is based on the use of conventional Amax and derivative spectrophotometry with the zero-crossing technique where KTR was determined using its Amax and (1)D amplitudes at 323 and 341nm respectively, while PHE was determined by measuring the (1)D amplitudes at 248.5nm. Method II involves the application of the ratio spectra derivative spectrophotometry. For KTR, 12μg/mL PHE was used as a divisor and the (1)DD amplitudes at 265nm were plotted against KTR concentrations; while - by using 4μg/mL KTR as divisor - the (1)DD amplitudes at 243.5nm were found proportional to PHE concentrations. Method III depends on ratio-difference measurement where the peak to trough amplitudes between 260 and 284nm were measured and correlated to KTR concentration. Similarly, the peak to trough amplitudes between 235 and 260nm in the PHE ratio spectra were recorded. For method IV, the two compounds were separated using Merck HPTLC sheets of silica gel 60 F254 and a mobile phase composed of chloroform/methanol/ammonia (70:30:2, by volume) followed by densitometric measurement of KTR and PHE spots at 320 and 278nm respectively. Method V depends on HPLC-DAD. Effective chromatographic separation was achieved using Zorbax eclipse plus C8 column (4.6×250mm, 5μm) with a mobile phase consisting of 0.05M o-phosphoric acid and acetonitrile (50:50, by volume) at a flow rate 1mL/min and detection at 313 and 274nm for KTR and PHE respectively. Analytical performance of the developed methods was statistically validated according to the ICH guidelines with respect to linearity, ranges, precision, accuracy, detection and quantification limits. The validated spectrophotometric and chromatographic methods were successfully applied to the simultaneous analysis of KTR and PHE in synthetic mixtures

  5. A new spectrophotometric method for the determination of tianeptine in tablets using ion-pair reagents.

    PubMed

    Ulu, Sevgi Tatar; Aydogmus, Zeynep

    2008-12-01

    A new rapid and sensitive procedure assay is proposed for the spectrophotometric determination of tianeptine. The developed method involves formation of colored chloroform extractable ion-pair complexes of tianeptine with bromophenol blue (BPB), bromocresol green (BCG), bromothymol blue (BTB) and methyl orange (MO) in acidic medium. Beer's law is obeyed in the concentration ranges 3.0-12.0, 4.0-16.0, 4.0-14.0 and 2.0-10.0 microg ml(-1) with BPB, BCG, BTB and MO, respectively. The detection limit of tianeptine was found to be 1.8 microg ml(-1) for BPB, 2.0 for BCG, 2.0 microg ml(-1) for BTB and 1.0 microg ml(-1) for MO. Validation of the method was performed in terms of linearity, limit of detection (LOD), quantification (LOQ), accuracy and precision. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed method. The proposed method has been applied to determination of the examined drugs in pharmaceutical formulations and the results demonstrated that the method is equally accurate, precise, and reproducible as the official method. The t-test showed no significant difference at 95% confidence level.

  6. Spectrophotometric method for the determination, validation, spectroscopic and thermal analysis of diphenhydramine in pharmaceutical preparation

    NASA Astrophysics Data System (ADS)

    Ulu, Sevgi Tatar; Elmali, Fikriye Tuncel

    2010-09-01

    A sensitive, simple and rapid spectrophotometric method was developed for the determination of diphenhydramine in pharmaceutical preparation. The method was based on the charge-transfer complex of the drug, as n-electron donor, with 2,3-dichloro-5,6-dicyano- p-benzoquinone (DDQ), as π-acceptor. The formation of this complex was also confirmed by UV-vis, FTIR and 1H NMR spectra techniques and thermal analysis. The proposed method was validated according to the ICH guidelines with respect to linearity, limit of detection, limit of quantification, accuracy, precision, recovery and robustness. The linearity range for concentrations of diphenhydramine was found to be 12.5-150 μg/mL with acceptable correlation coefficients. The detection and quantification limits were found to be 2.09 and 6.27 μg/mL, respectively. The proposed and references methods were applied to the determination of drug in syrup. This preparation were also analyzed with an reference method and statistical comparison by t- and F-tests revealed that there was no significant difference between the results of the two methods with respect to mean values and standard deviations at the 95% confidence level.

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

    PubMed

    Charoennit, P; Lourith, N

    2012-04-01

    A UV-spectrophotometric method for the analysis of makeup remover was developed and validated according to ICH guidelines. Three makeup removers for which the main ingredients consisted of vegetable oil (A), mineral oil and silicone (B) and mineral oil and water (C) were sampled in this study. Ethanol was the optimal solvent because it did not interfere with the maximum absorbance of the liquid foundation at 250 nm. The linearity was determined over a range of makeup concentrations from 0.540 to 1.412 mg mL⁻¹ (R² = 0.9977). The accuracy of this method was determined by analysing low, intermediate and high concentrations of the liquid foundation and gave 78.59-91.57% recoveries with a relative standard deviation of <2% (0.56-1.45%). This result demonstrates the validity and reliability of this method. The reproducibilities were 97.32 ± 1.79, 88.34 ± 2.69 and 95.63 ± 2.94 for preparations A, B and C respectively, which are within the acceptable limits set forth by the ASEAN analytical validation guidelines, which ensure the precision of the method under the same operating conditions over a short time interval and the inter-assay precision within the laboratory. The proposed method is therefore a simple, rapid, accurate, precise and inexpensive technique for the routine analysis of makeup remover efficacy.

  8. Determination of rapid chlorination rate constants by a stopped-flow spectrophotometric competition kinetics method.

    PubMed

    Song, Dean; Liu, Huijuan; Qiang, Zhimin; Qu, Jiuhui

    2014-05-15

    Free chlorine is extensively used for water and wastewater disinfection nowadays. However, it still remains a big challenge to determine the rate constants of rapid chlorination reactions although competition kinetics and stopped-flow spectrophotometric (SFS) methods have been employed individually to investigate fast reaction kinetics. In this work, we proposed an SFS competition kinetics method to determine the rapid chlorination rate constants by using a common colorimetric reagent, N,N-diethyl-p-phenylenediamine (DPD), as a reference probe. A kinetic equation was first derived to estimate the reaction rate constant of DPD towards chlorine under a given pH and temperature condition. Then, on that basis, an SFS competition kinetics method was proposed to determine directly the chlorination rate constants of several representative compounds including tetracycline, ammonia, and four α-amino acids. Although Cl2O is more reactive than HOCl, its contribution to the overall chlorination kinetics of the test compounds could be neglected in this study. Finally, the developed method was validated through comparing the experimentally measured chlorination rate constants of the selected compounds with those obtained or calculated from literature and analyzing with Taft's correlation as well. This study demonstrates that the SFS competition kinetics method can measure the chlorination rate constants of a test compound rapidly and accurately.

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

    PubMed

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

    2015-01-01

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

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

    PubMed

    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.

  11. Determination of vanadium in groundwater samples with an improved kinetic spectrophotometric method.

    PubMed

    Bağda, Esra

    2014-01-01

    A kinetic catalytic method has been developed for the determination of vanadium based on its catalytic effect on the redox reaction of azorubin S and bromate in the presence of a sulphuric and nitric acid mixture. The reaction is monitored spectrophotometrically by measuring the decrease in absorbance of the reaction mixture at 515 nm. The fixed-time method was used for 0.5-5 min. Optimization of the reaction conditions regarding concentrations of acids, dye, oxidant, masking agent, etc. was investigated. The rate of decrease in absorbance of azorubin S was proportional to the concentration of vanadium in the range of 2.0-1.05 x 10(3) ng mL(-1). 3Sb/m was 0.0129 ng mL(-1) and 10 Sb/m was 0.0432 ng mL(-1). The catalytic method based on the oxidation reaction of azorubin S and bromate shows a good selectivity for vanadium over a wide variety of interference cations and anions. The proposed method was successfully applied to the determination of vanadium in groundwater samples and spiked-water samples.

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

    NASA Astrophysics Data System (ADS)

    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.

  13. A rapid derivative spectrophotometric method for simultaneous determination of naphazoline and antazoline in eye drops.

    PubMed

    Souri, Effat; Amanlou, Massoud; Farsam, Hassan; Afshari, Alma

    2006-01-01

    A zero-crossing first-derivative spectrophotometric method is applied for the simultaneous determination of naphazoline hydrochloride and antazoline phosphate in eye drops. The measurements were carried out at wavelengths of 225 and 252 nm for naphazoline hydrochloride and antazoline phosphate, respectively. The method was found to be linear (r2>0.999) in the range of 0.2-1 microg/ml for naphazoline hydrochloride in the presence of 5 microg/ml antazoline phosphate at 225 nm. The same linear correlation (r2>0.999) was obtained in the range of 1-10 microg/ml of antazoline phosphate in the presence of 0.5 microg/ml of naphazoline hydrochloride at 252 nm. The limit of determination was 0.2 microg/ml and 1 microg/ml for naphazoline hydrochloride and antazoline phosphate, respectively. The method was successfully used for simultaneous analysis of naphazoline hydrochloride and antazoline phosphate in eye drops without any interference from excipients and prior separation before analysis.

  14. Validation of a spectrophotometric method for quantification of xanthone in biodegradable nanoparticles.

    PubMed

    Teixeira, M; Pinto, M M M; Barbosa, C M

    2004-04-01

    Xanthone has been incorporated for the first time in nanoparticles of poly(D,L-lactide-co-glycolide) (PLGA). For this purpose the estimation of xanthone content in the nanoparticles is a crucial tool for guaranteeing the reliability of the results. Thus, a simple spectrophotometric method was validated according to USP25 and ICH guidelines for its specificity, linearity, accuracy and precision. The method was found to be specific for xanthone in the presence of nanoparticle excipients. The calibration curve was linear over the concentration range of 0.5 to 4.0 microg/mL (r > 0.999). Recovery of xanthone from nanoparticles ranged from 86.5 to 95.9%. Repeatability (intra-assay precision) and intermediate precision were found to be acceptable with relative standard deviations values (RSD) ranging from 0.3 to 3.0% and from 1.4 to 3.1%, respectively. The method was found to be suitable for the evaluation of xanthone content in nanoparticles of PLGA.

  15. A Highly Sensitive Kinetic Spectrophotometric Method for the Determination of Ascorbic Acid in Pharmaceutical Samples

    PubMed Central

    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. PMID:25237333

  16. Spectrophotometric Methods for the Determination of Sitagliptin and Vildagliptin in Bulk and Dosage Forms

    PubMed Central

    El-Bagary, Ramzia I.; Elkady, Ehab F.; Ayoub, Bassam M.

    2011-01-01

    Simple, accurate and precise spectrophotometric methods have been developed for the determination of sitagliptin and vildagliptin in bulk and dosage forms. The proposed methods are based on the charge transfer complexes of sitagliptin phosphate and vildagliptin with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), 7,7,8,8-tetracyanoquinodimethane (TCNQ) and tetrachloro-1,4-benzoquinone (p-chloranil). All the variables were studied to optimize the reactions conditions. For sitagliptin, Beer’s law was obeyed in the concentration ranges of 50-300 μg/ml, 20-120 μg/ml and 100-900 μg/ml with DDQ, TCNQ and p-chloranil, respectively. For vildagliptin, Beer’s law was obeyed in the concentration ranges of 50-300 μg/ml, 10-85 μg/ml and 50-350 μg/ml with DDQ, TCNQ and p-chloranil, respectively. The developed methods were validated and proved to be specific and accurate for the quality control of the cited drugs in pharmaceutical dosage forms. PMID:23675221

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

    PubMed Central

    Akhoundi-Khalafi, Ali Mohammad; Shishehbore, Masoud Reza

    2015-01-01

    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. PMID:25737724

  18. Spectrophotometric study of complexation equilibria with H-point standard addition and H-point curve isolation methods.

    PubMed

    Abdollahi, H; Zeinali, S

    2004-01-01

    The use of H-point curve isolation (HPCIM) and H-point standard addition methods (HPSAM) for spectrophotometric studies of complex formation equilibria are proposed. One step complex formation, two successive stepwise and mononuclear complex formation systems, and competitive complexation systems are studied successfully by the proposed methods. HPCIM is used for extracting the spectrum of complex or sum of complex species and HPSAM is used for calculation of equilibrium concentrations of ligand for each sample. The outputs of these procedures are complete concentration profiles of equilibrium system, spectral profile of intermediate components, and good estimation of conditional formation constants. The reliability of the method is evaluated using model data. Spectrophotometric studies of murexide-calcium, dithizone-nickel, methyl thymol blue (MTB)-copper, and competition of murexide and sulfate ions for complexation with zinc, are used as experimental model systems with different complexation stoichiometries and spectral overlapping of involved components.

  19. Comparative study of spectrophotometric methods manipulating ratio spectra: an application on pharmaceutical binary mixture of cinnarizine and dimenhydrinate.

    PubMed

    Lamie, Nesrine T

    2015-04-15

    Four simple, specific, accurate and precise spectrophotometric methods are developed and validated for simultaneous determination of cinnarizine (CIN) and dimenhydrinate (DIM) in a binary mixture with overlapping spectra, without preliminary separation. The first method is dual wavelength spectrophotometry (DW), the second is a ratio difference spectrophotometric one (RD) which measures the difference in amplitudes between 250 and 270 nm of ratio spectrum, the third one is novel constant center spectrophotometric method (CC) and the fourth method is mean centering of ratio spectra (MCR). The calibration curve is linear over the concentration range of 4-20 and 10-45 μg/ml for CIN and DIM, 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. The validity of results was assessed by applying standard addition technique. The results obtained were found to agree statistically with those obtained by a reported method, showing no significant difference with respect to accuracy and precision. PMID:25677532

  20. Comparative study of spectrophotometric methods manipulating ratio spectra: An application on pharmaceutical binary mixture of cinnarizine and dimenhydrinate

    NASA Astrophysics Data System (ADS)

    Lamie, Nesrine T.

    2015-04-01

    Four simple, specific, accurate and precise spectrophotometric methods are developed and validated for simultaneous determination of cinnarizine (CIN) and dimenhydrinate (DIM) in a binary mixture with overlapping spectra, without preliminary separation. The first method is dual wavelength spectrophotometry (DW), the second is a ratio difference spectrophotometric one (RD) which measures the difference in amplitudes between 250 and 270 nm of ratio spectrum, the third one is novel constant center spectrophotometric method (CC) and the fourth method is mean centering of ratio spectra (MCR). The calibration curve is linear over the concentration range of 4-20 and 10-45 μg/ml for CIN and DIM, 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. The validity of results was assessed by applying standard addition technique. The results obtained were found to agree statistically with those obtained by a reported method, showing no significant difference with respect to accuracy and precision.

  1. Investigation on the interaction of Safranin T with anionic polyelectrolytes by spectrophotometric method.

    PubMed

    Fradj, Anouar Ben; Lafi, Ridha; Hamouda, Sofiane Ben; Gzara, Lassaad; Hamzaoui, Ahmed Hichem; Hafiane, Amor

    2014-10-15

    Understanding the role played by chemical additives such as NaCl salt, acid and Cetylpyridinium Chloride (CPC) surfactant on the interaction between dye and polyelectrolyte contributes to optimization of processes using polyelectrolytes in the removal of dye from aqueous solution. Herein we focus in the interaction between Safranin T, a cationic dye, with two anionic polyelectrolytes, poly(ammonium acrylate) and poly(acrylic acid) using spectrophotometric method and conductivity measurement. In aqueous solution, each of anionic polyelectrolytes forms a complex with the dye and induces a metachromasy indicated by the blue shift of the absorbance of the dye. The stoichiometry of complexes evaluated by the molar ratio method are 1:1 for Safranin T poly(ammonium acrylate) and 2:1 in the case of Safranin T poly(acrylic acid). The effect of additives on the stability of complexes has been studied by varying concentrations of the salt and the surfactant and pH of the solution. The thermodynamic parameters of interaction ΔG, ΔH and ΔS at different temperatures were evaluated to determine the stability constant of the complexes.

  2. Evaluation of spectrophotometric and HPLC methods for shikimic acid determination in plants: models in glyphosate-resistant and -susceptible crops.

    PubMed

    Zelaya, Ian A; Anderson, Jennifer A H; Owen, Micheal D K; Landes, Reid D

    2011-03-23

    Endogenous shikimic acid determinations are routinely used to assess the efficacy of glyphosate in plants. Numerous analytical methods exist in the public domain for the detection of shikimic acid, yet the most commonly cited comprise spectrophotometric and high-pressure liquid chromatography (HPLC) methods. This paper compares an HPLC and two spectrophotometric methods (Spec 1 and Spec 2) and assesses the effectiveness in the detection of shikimic acid in the tissues of glyphosate-treated plants. Furthermore, the study evaluates the versatility of two acid-based shikimic acid extraction methods and assesses the longevity of plant extract samples under different storage conditions. Finally, Spec 1 and Spec 2 are further characterized with respect to (1) the capacity to discern between shikimic acid and chemically related alicyclic hydroxy acids, (2) the stability of the chromophore (t1/2), (3) the detection limits, and (4) the cost and simplicity of undertaking the analytical procedure. Overall, spectrophotometric methods were more cost-effective and simpler to execute yet provided a narrower detection limit compared to HPLC. All three methods were specific to shikimic acid and detected the compound in the tissues of glyphosate-susceptible crops, increasing exponentially in concentration within 24 h of glyphosate application and plateauing at approximately 72 h. Spec 1 estimated more shikimic acid in identical plant extract samples compared to Spec 2 and, likewise, HPLC detection was more effective than spectrophotometric determinations. Given the unprecedented global adoption of glyphosate-resistant crops and concomitant use of glyphosate, an effective and accurate assessment of glyphosate efficacy is important. Endogenous shikimic acid determinations are instrumental in corroborating the efficacy of glyphosate and therefore have numerous applications in herbicide research and related areas of science as well as resolving many commercial issues as a consequence of

  3. Determination of trace vanadium (V) in seawater and fresh water by the catalytic kinetic spectrophotometric method

    NASA Astrophysics Data System (ADS)

    Ji, Hongwei; Sha, Yuanyuan; Xin, Huizhen; Li, Shuang

    2010-12-01

    A new kinetic spectrophotometric method has been developed for the determination of vanadium (V). The method is based on the catalytic effect of vanadium (V) on the oxidation of weak acid brilliant blue dye (RAWL) by KBrO3 using the citric acid as activation reagent. The obtained optimum conditions are: c (RAWL) = 1×10-4 molL-1, c (KBrO3) = 3×10-2 molL-1, c (citric acid) = 9×10-3 molL-1, pH = 2.50, the reaction time being 7.0 min and the temperature being 25.0°C. Under the optimum conditions, the proposed method allows the determination of vanadium (V) in the range of 0-70.0 ng mL-1 and the detection limit is down to 0.407 ng mL-1. For standard vanadium (V) solution determination, the recovery efficiency is in the range of 98.5%-102% and the RSD ranges from 0.76%-1.25%. Moreover, it is demonstrated that most cations and anions do not interfere with the determination of vanadium (V) under the analytical condition. The new method was successfully applied in the determination of vanadium (V) in fresh water and seawater samples with satisfactory results. Vanadium (V) in the seawater samples from Qingdao offshore was determined using the method and the distribution of vanadium (V) was mapped. Compared with other instrumental analytical methods, the proposed method shows good selectivity, sensitivity, simplicity, lower cost and rapidity. It can be employed on shipboard easily.

  4. A simple and highly sensitive spectrophotometric method for the determination of cyanide in equine blood.

    PubMed

    Hughes, Charlie; Lehner, Fritz; Dirikolu, Levent; Harkins, Dan; Boyles, Jeff; McDowell, Karen; Tobin, Thomas; Crutchfield, James; Sebastian, Manu; Harrison, Lenn; Baskin, Stephen I

    2003-01-01

    An epidemiological association among black cherry trees (Prunus serotina), eastern tent caterpillars (Malacosoma americana), and the spring 2001 episode of mare reproductive loss syndrome in central Kentucky focused attention on the potential role of environmental cyanogens in the causes of this syndrome. To evaluate the role of cyanide (CN (-)) in this syndrome, a simple, rapid, and highly sensitive method for determination of low parts per billion concentrations of CN (-) in equine blood and other biological fluids was developed. The analytical method is an adaptation of methods commonly in use and involves the evolution and trapping of gaseous hydrogen cyanide followed by spectrophotometric determination by autoanalyzer. The limit of quantitation of this method is 2 ng/mL in equine blood, and the standard curve shows a linear relationship between CN (-) concentration and absorbance (r >. 99). The method throughput is high, up to 100 samples per day. Normal blood CN (-) concentrations in horses at pasture in Kentucky in October 2001 ranged from 3-18 ng/mL, whereas hay-fed horses showed blood CN (-) levels of 2-7 ng/mL in January 2002. Blood samples from a small number of cattle at pasture showed broadly similar blood CN (-) concentrations. Intravenous administration of sodium cyanide and oral administration of mandelonitrile and amygdalin yielded readily detectable increases in blood CN (-) concentrations. This method is sufficiently sensitive and specific to allow the determination of normal blood CN (-) levels in horses, as well as the seasonal and pasture-dependent variations. The method should also be suitable for investigation of the toxicokinetics and disposition of subacutely toxic doses of CN (-) and its precursor cyanogens in the horse as well as in other species. PMID:20021191

  5. Studies on Tinospora cordifolia monosugars and correlation analysis of uronic acids by spectrophotometric methods and GLC.

    PubMed

    Kumar, Vineet; Nagar, Shipra

    2014-01-01

    Cold water-soluble (CWSP) and hot water soluble polysaccharides (HWSP) from Tinospora cordifolia stems were isolated and purified in 2.99% and 1.99% yield respectively. Complete hydrolysis followed by paper chromatography and GLC analysis indicated the presence of L-rhamnose, L-arabinose, D-xylose, D-mannose, D-galactose and D-glucose in molar ratio of 0.857, 1.106, 0.727, 0.526, 0.708 and 95.763 in CWSP and 0.697, 0.777, 2.048, 0.777, 0.292 and 95.408 in HWSP. The uronic acid content in the polysaccharide has been studied extensively using assorted approaches. It was quantitatively estimated by GLC analysis and spectrophotometric methods using carbazole, m-hydroxydiphenyl and 3,5-dimethylphenol as colorimetric reagents. GLC analyses indicated galacturonic acid content of 3.06% and 5.16% in CWSP and HWSP respectively. Estimation of uronic acid using 3,5-dimethylphenol corroborated the above analysis. The study resulted in composition of constituent monosugars of CWSP and HWSP and co-relation analysis of uronic acid content, leading to an unambiguous structural analysis. PMID:24274509

  6. Plasmon absorption modulator systems and methods

    DOEpatents

    Kekatpure, Rohan Deodatta; Davids, Paul

    2014-07-15

    Plasmon absorption modulator systems and methods are disclosed. A plasmon absorption modulator system includes a semiconductor substrate, a plurality of quantum well layers stacked on a top surface of the semiconductor substrate, and a metal layer formed on a top surface of the stack of quantum well layers. A method for modulating plasmonic current includes enabling propagation of the plasmonic current along a metal layer, and applying a voltage across the stack of quantum well layers to cause absorption of a portion of energy of the plasmonic current by the stack of quantum well layers. A metamaterial switching system includes a semiconductor substrate, a plurality of quantum well layers stacked on a top surface of the semiconductor substrate, and at least one metamaterial structure formed on a top surface of the stack of quantum well layers.

  7. Application of the bivariate spectrophotometric method for the determination of metronidazole, furazolidone and di-iodohydroxyquinoline in pharmaceutical formulations.

    PubMed

    López-de-Alba, P L; Wróbel, K; López-Martínez, L; Wróbel, K; Yepez-Murrieta, M L; Amador-Hernández, J

    1997-10-01

    The bivariate calibration algorithm was applied to the spectrophotometric determination of metronidazole, furazolidone and di-iodohydroxyquinoline in pharmaceutical dosage forms. The results obtained were compared with the results of derivative spectrophotometry. The statistical evaluation of method bias was carried out, and it was shown that the proposed procedure may be competitive with commonly used first-derivative spectrophotometry. The advantage of the bivariate calibration is its simplicity, and the fact that there is no need to use the derivatization procedures.

  8. Development of an reliable analytical method for synergistic extractive spectrophotometric determination of cobalt(II) from alloys and nano composite samples by using chromogenic chelating ligand.

    PubMed

    Kamble, Ganesh S; Ghare, Anita A; Kolekar, Sanjay S; Han, Sung H; Anuse, Mansing A

    2011-12-15

    A synergistic simple and selective spectrophotometric method was developed for the determination of cobalt(II) with 1-(2',4'-dinitro aminophenyl)-4,4,6-trimethyl-1,4-dihydropyrimidine-2-thiol [2',4'-dinitro APTPT] as a chromogenic reagent. The proposed method has been described on the basis of synergistic effective extraction of cobalt(II) in presence of pyridine at pH range 9.5-10.2, showed orange-red coloured ternary complex having molar ratio 1:2:2 (M:L:Py). The equilibrium time is 10 min for extraction of cobalt(III) from organic phase. The absorbance of coloured organic layer in chloroform is measured spectrophotometrically at 490 nm against reagent blank. The Beer's law was obeyed in the concentration range 2.5-15 μg mL(-1) of cobalt(II) and optimum concentration range was 5-12.5 μg mL(-1) of cobalt(II) and it was evaluated from Ringbom's plot. The molar absorptivity and Sandell's sensitivity of cobalt(II)-2',4'-dinitro APTPT-pyridine complex in chloroform are 1.109×10(3) L mol(-1) cm(-1) and 0.053 μg cm(-2), respectively while molar absorptivity and Sandell's sensitivity of cobalt(II)-2',4'-dinitro APTPT complex in chloroform are 6.22×10(2) L mol(-1) cm(-1) and 0.096 μg cm(-2), respectively. The composition of cobalt(II)-2',4'-dinitro APTPT-pyridine complex (1:2:2) was established by slope ratio method, mole ratio method and Job's method of continuous variation. The ternary complex was stable for more than 48 h. The interfering effects of various cations and anions were also studied, and use of suitable masking agents enhances the selectivity of the method. The method is successfully applied for the determination of cobalt(II) in binary, synthetic mixtures and real samples. A repetition of the method was checked by finding relative standard deviation (R.S.D.) for n=5 which was 0.15%. The reliability of the method is confirmed by comparison of experimental results with atomic absorption spectrophotometer. PMID:21978559

  9. Development of an reliable analytical method for synergistic extractive spectrophotometric determination of cobalt(II) from alloys and nano composite samples by using chromogenic chelating ligand

    NASA Astrophysics Data System (ADS)

    Kamble, Ganesh S.; Ghare, Anita A.; Kolekar, Sanjay S.; Han, Sung H.; Anuse, Mansing A.

    2011-12-01

    A synergistic simple and selective spectrophotometric method was developed for the determination of cobalt(II) with 1-(2',4'-dinitro aminophenyl)-4,4,6-trimethyl-1,4-dihydropyrimidine-2-thiol [2',4'-dinitro APTPT] as a chromogenic reagent. The proposed method has been described on the basis of synergistic effective extraction of cobalt(II) in presence of pyridine at pH range 9.5-10.2, showed orange-red coloured ternary complex having molar ratio 1:2:2 (M:L:Py). The equilibrium time is 10 min for extraction of cobalt(III) from organic phase. The absorbance of coloured organic layer in chloroform is measured spectrophotometrically at 490 nm against reagent blank. The Beer's law was obeyed in the concentration range 2.5-15 μg mL -1 of cobalt(II) and optimum concentration range was 5-12.5 μg mL -1 of cobalt(II) and it was evaluated from Ringbom's plot. The molar absorptivity and Sandell's sensitivity of cobalt(II)-2',4'-dinitro APTPT-pyridine complex in chloroform are 1.109 × 10 3 L mol -1 cm -1 and 0.053 μg cm -2, respectively while molar absorptivity and Sandell's sensitivity of cobalt(II)-2',4'-dinitro APTPT complex in chloroform are 6.22 × 10 2 L mol -1 cm -1 and 0.096 μg cm -2, respectively. The composition of cobalt(II)-2',4'-dinitro APTPT-pyridine complex (1:2:2) was established by slope ratio method, mole ratio method and Job's method of continuous variation. The ternary complex was stable for more than 48 h. The interfering effects of various cations and anions were also studied, and use of suitable masking agents enhances the selectivity of the method. The method is successfully applied for the determination of cobalt(II) in binary, synthetic mixtures and real samples. A repetition of the method was checked by finding relative standard deviation (R.S.D.) for n = 5 which was 0.15%. The reliability of the method is confirmed by comparison of experimental results with atomic absorption spectrophotometer.

  10. Flow injection spectrophotometric method for chloride determination in natural waters using Hg(SCN)(2) immobilized in epoxy resin.

    PubMed

    Silva, Claudineia R; Vieira, Heberth J; Canaes, Larissa S; Nóbrega, Joaquim A; Fatibello-Filho, Orlando

    2005-02-28

    A flow injection (FI) spectrophotometric method was proposed for the determination of chloride ion in natural waters. The determination of chloride was carried out by reaction with Hg(SCN)(2) immobilized in an epoxy resin bead in a solid-phase reactor (SPR) and the thiocyanate ions released were determined spectrophotometrically at 480nm after complexing reaction with Fe(III). The analytical curve for chloride was linear in the concentration range from 5.6 x 10(-5) to 2.2 x 10(-4)moll(-1) with a detection limit of 1.4 x 10(-5)moll(-1). The relative standard deviation (R.S.D.) was 2.2% for a solution containing 2.2 x 10(-4)moll(-1) (n = 10). The simple manifold allows a routine analytical frequency of 100 determinations per hour. The main advantage of the developed method is the 400% reduction of the Hg waste solution generated when compared to conventional methods for chloride determination based on the same spectrophotometric reaction. PMID:18969896

  11. Flow injection spectrophotometric method for chloride determination in natural waters using Hg(SCN)(2) immobilized in epoxy resin.

    PubMed

    Silva, Claudineia R; Vieira, Heberth J; Canaes, Larissa S; Nóbrega, Joaquim A; Fatibello-Filho, Orlando

    2005-02-28

    A flow injection (FI) spectrophotometric method was proposed for the determination of chloride ion in natural waters. The determination of chloride was carried out by reaction with Hg(SCN)(2) immobilized in an epoxy resin bead in a solid-phase reactor (SPR) and the thiocyanate ions released were determined spectrophotometrically at 480nm after complexing reaction with Fe(III). The analytical curve for chloride was linear in the concentration range from 5.6 x 10(-5) to 2.2 x 10(-4)moll(-1) with a detection limit of 1.4 x 10(-5)moll(-1). The relative standard deviation (R.S.D.) was 2.2% for a solution containing 2.2 x 10(-4)moll(-1) (n = 10). The simple manifold allows a routine analytical frequency of 100 determinations per hour. The main advantage of the developed method is the 400% reduction of the Hg waste solution generated when compared to conventional methods for chloride determination based on the same spectrophotometric reaction.

  12. Simple flow injection method for simultaneous spectrophotometric determination of Fe(II) and Fe(III).

    PubMed

    Kozak, J; Jodłowska, N; Kozak, M; Kościelniak, P

    2011-09-30

    The method is based on spectrophotometric determination of Fe(II) and Fe(III) at a single wavelength (530 nm) with the use of a dedicated reversed-flow injection system. In the system, EDTA solution is injected into a carrier stream (HNO(3)) and then merged with a sample stream containing a mixture of sulfosalicylic acid and 1,10-phenanthroline as indicators. In an acid environment (pH≅3) the indicators form complexes with both Fe(III) and Fe(II), but EDTA replaces sulfosalicylic acid, forming a more stable colourless complex with Fe(III), whereas Fe(II) remains in a complex with 1,10-phenenthroline. As a result, the area and minimum of the characteristic peak can be exploited as measures corresponding to the Fe(III) and Fe(II) concentrations, respectively. The analytes were not found to affect each other's signals, hence two analytical curves were constructed with the use of a set of standard solutions, each containing Fe(II) and Fe(III). Both analytes were determined in synthetic samples within the concentration ranges of 0.05-4.0 and 0.09-6.0 mg L(-1), respectively, with precision less than 1.5 and 2.6% (RSD) and with accuracy less than 4.3 and 5.6% (RE). The method was applied to determination of the analytes in water samples collected from artesian wells and the results of the determination were consistent with those obtained using the ICP-OES technique.

  13. Different spectrophotometric methods applied for the analysis of binary mixture of flucloxacillin and amoxicillin: A comparative study

    NASA Astrophysics Data System (ADS)

    Attia, Khalid A. M.; Nassar, Mohammed W. I.; El-Zeiny, Mohamed B.; Serag, Ahmed

    2016-05-01

    Three different spectrophotometric methods were applied for the quantitative analysis of flucloxacillin and amoxicillin in their binary mixture, namely, ratio subtraction, absorbance subtraction and amplitude modulation. A comparative study was done listing the advantages and the disadvantages of each method. All the methods were validated according to the ICH guidelines and the obtained accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of flucloxacillin and amoxicillin in their binary mixtures.

  14. Different spectrophotometric methods applied for the analysis of binary mixture of flucloxacillin and amoxicillin: A comparative study.

    PubMed

    Attia, Khalid A M; Nassar, Mohammed W I; El-Zeiny, Mohamed B; Serag, Ahmed

    2016-05-15

    Three different spectrophotometric methods were applied for the quantitative analysis of flucloxacillin and amoxicillin in their binary mixture, namely, ratio subtraction, absorbance subtraction and amplitude modulation. A comparative study was done listing the advantages and the disadvantages of each method. All the methods were validated according to the ICH guidelines and the obtained accuracy, precision and repeatability were found to be within the acceptable limits. The selectivity of the proposed methods was tested using laboratory prepared mixtures and assessed by applying the standard addition technique. So, they can be used for the routine analysis of flucloxacillin and amoxicillin in their binary mixtures.

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

    NASA Astrophysics Data System (ADS)

    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.

  16. Selective kinetic spectrophotometric method for determination of gatifloxacin based on formation of its N-vinyl chlorobenzoquinone derivative

    NASA Astrophysics Data System (ADS)

    Darwish, Ibrahim A.; Sultan, Maha A.; Al-Arfaj, Hessa A.

    2010-01-01

    A selective and simple kinetic spectrophotometric has been developed, for the first time, for the determination of gatifloxacin (GAT) in its dosage forms. The method was based on the formation of a colored N-vinyl chlorobenzoquinone derivative of GAT by its reaction with 2,3,5,6-tetrachloro-1,4-benzoquinone in presence of acetaldehyde. The formation of the colored product was monitored spectrophotometrically by measuring the absorbances at 655 nm. The factors affecting the reaction were studied and optimized. The stoichiometry of the reaction was determined, and the reaction pathway was postulated. Under the optimized conditions, the initial rate and fixed time (at 5 min) methods were utilized for constructing the calibration graphs. The graphs were linear in the concentration ranges of 2-100 and 10-140 μg ml -1 with limits of detection of 0.84 and 3.5 μg ml -1 for the initial rate and fixed time methods, respectively. The analytical performance of both methods was fully validated, and the results were satisfactory. The proposed methods were successfully applied to the determination of GAT in its commercial dosage forms. The label claim percentages were 99.7-100.5 and 98.2-99.5% for the initial rate and fixed time methods, respectively. Statistical comparison of the results with those of the reference method showed excellent agreement and proved that there was no significant difference in the accuracy and precision between the reference and the proposed methods. The proposed methods are superior to all the previously reported spectrophotometric methods in terms of the procedure simplicity and assay selectivity.

  17. Detector absorptivity measuring method and apparatus

    NASA Technical Reports Server (NTRS)

    Sheets, R. E. (Inventor)

    1976-01-01

    A method and apparatus for measuring the absorptivity of a radiation detector by making the detector an integral part of a cavity radiometer are described. By substituting the detector for the surface of the cavity upon which the radiation first impinges a comparison is made between the quantity of radiation incident upon the detector and the quantity reflected from the detector. The difference between the two is a measurement of the amount of radiation absorbed by the detector.

  18. Extractive spectrophotometric method for the determination of vanadium(V) in steels and titanium base alloy

    SciTech Connect

    Yerramilli, A.; Kavipurapu, C.S.; Manda, R.R.; Pillutla, C.M.

    1986-06-01

    Vanadium(V) forms anionic chelates with 4-(2-pyridylazo)-resorcinol (PAR) at pH 5.0-7.8, which can be quantitatively extracted into nitrobenzene as an ion pair with xylometazolonium cation (XMH). The ternary system has an absorption maximum at 540 nm and obeys Beer's law in the range 0-1.8 /sup +/g of vanadium/mL with a molar absorptivity 4.56 x 10/sup 4/ L mol/sup -1/ cm/sup -1/. The Job's method of continuous variations indicated a composition of 1:1:1 for vanadium: PAR:XMH for the extracting species. In the presence of 1,3-diaminocyclohexanetetraacetic acid as a masking agent, the extraction becomes highly selective, and this method can be applied for the determination of vanadium(V), in the presence of various metal ions in synthetic mixtures, in steels, and in titanium base alloy.

  19. Simultaneous determination of iron and manganese in water using artificial neural network catalytic spectrophotometric method

    NASA Astrophysics Data System (ADS)

    Ji, Hongwei; Xu, Yan; Li, Shuang; Xin, Huizhen; Cao, Hengxia

    2012-09-01

    A new analytical method using Back-Propagation (BP) artificial neural network and kinetic spectrophotometry for simultaneous determination of iron and magnesium in tap water, the Yellow River water and seawater is established. By conditional experiments, the optimum analytical conditions and parameters are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 15-16-2 (nodes). The initial value of gradient coefficient µ is fixed at 0.001 and the increase factor and reduction factor of µ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviation of the calculated results for iron and manganese is 2.30% and 2.67% respectively. The results of standard addition method show that for the tap water, the recoveries of iron and manganese are in the ranges of 98.0%-104.3% and 96.5%-104.5%, and the RSD is in the range of 0.23%-0.98%; for the Yellow River water (Lijin district of Shandong Province), the recoveries of iron and manganese are in the ranges of 96.0%-101.0% and 98.7%-104.2%, and the RSD is in the range of 0.13%-2.52%; for the seawater in Qingdao offshore, the recoveries of iron and manganese are in the ranges of 95.3%-104.8% and 95.3%-104.7%, and the RSD is in the range of 0.14%-2.66%. It is found that 21 common cations and anions do not interfere with the determination of iron and manganese under the optimum experimental conditions. This method exhibits good reproducibility and high accuracy in the determination of iron and manganese and can be used for the simultaneous determination of iron and manganese in tap water and natural water. By using the established ANN-catalytic spectrophotometric method, the iron and manganese concentrations of the surface seawater at 11 sites in Qingdao offshore are determined and the level distribution maps of iron and

  20. Absorption spectrophotometric, fluorescence and quantum chemical investigations on non-covalent interaction between PC₇₀BM and designed diporphyrin in solution.

    PubMed

    Ray, Anamika; Bauri, Ajoy; Bhattacharya, Sumanta

    2015-01-01

    Present work reports the photophysical insights on supramolecular interaction of a C₇₀ derivative, namely, [6,6]-phenyl C₇₁ butyric acid methyl ester (PC₇₀BM), with two designed diporphyrin molecules having dithiophene (1) and carbazole (2) spacer in toluene and benzonitrile. Both absorption spectrophotometric and steady state fluorescence investigations reveal efficient complexation of PC₇₀BM with 1 and 2 in both toluene and benzonitrile. The magnitude of average value of binding constant, viz., Kav, for the complexes of PC₇₀BM with 1 and 2 in toluene (benzonitrile) are estimated to be 2.185 × 10(3)dm(3)mol(-1) (3.215 × 10(3)dm(3)mol(-1)) and 10.180 × 10(3)dm(3)mol(-1) (25.405 × 10(3)dm(3)mol(-1)), respectively. Selectivity in binding for the complexation process of PC₇₀BM with 1 and 2 is estimated to be ∼4.6 and ∼7.90 as observed in toluene and benzonitrile, respectively. The complexation between PC₇₀BM and diporphyrin is well accounted by a theoretical model which takes into account the electronic subsystems of both acceptor and donor. Ab initio calculations in vacuo establish that size selective orientation pattern of PC₇₀BM towards the cavity of diporphyrin dictates the magnitude of binding and electronic structure of the PC₇₀BM/diporphyrin complexes. PMID:25138385

  1. Spectrophotometric Procedure for Fast Reactor Advanced Coolant Manufacture Control

    NASA Astrophysics Data System (ADS)

    Andrienko, O. S.; Egorov, N. B.; Zherin, I. I.; Indyk, D. V.

    2016-01-01

    The paper describes a spectrophotometric procedure for fast reactor advanced coolant manufacture control. The molar absorption coefficient of dimethyllead dibromide with dithizone was defined as equal to 68864 ± 795 l·mole-1·cm-1, limit of detection as equal to 0.583 · 10-6 g/ml. The spectrophotometric procedure application range was found to be equal to 37.88 - 196.3 g. of dimethyllead dibromide in the sample. The procedure was used within the framework of the development of the method of synthesis of the advanced coolant for fast reactors.

  2. Spectrophotometric Analysis of Caffeine

    PubMed Central

    Ahmad Bhawani, Showkat; Fong, Sim Siong; Mohamad Ibrahim, Mohamad Nasir

    2015-01-01

    The nature of caffeine reveals that it is a bitter white crystalline alkaloid. It is a common ingredient in a variety of drinks (soft and energy drinks) and is also used in combination with various medicines. In order to maintain the optimum level of caffeine, various spectrophotometric methods have been developed. The monitoring of caffeine is very important aspect because of its consumption in higher doses that can lead to various physiological disorders. This paper incorporates various spectrophotometric methods used in the analysis of caffeine in various environmental samples such as pharmaceuticals, soft and energy drinks, tea, and coffee. A range of spectrophotometric methodologies including chemometric techniques and derivatization of spectra have been used to analyse the caffeine. PMID:26604926

  3. Spectrophotometric Analysis of Caffeine.

    PubMed

    Ahmad Bhawani, Showkat; Fong, Sim Siong; Mohamad Ibrahim, Mohamad Nasir

    2015-01-01

    The nature of caffeine reveals that it is a bitter white crystalline alkaloid. It is a common ingredient in a variety of drinks (soft and energy drinks) and is also used in combination with various medicines. In order to maintain the optimum level of caffeine, various spectrophotometric methods have been developed. The monitoring of caffeine is very important aspect because of its consumption in higher doses that can lead to various physiological disorders. This paper incorporates various spectrophotometric methods used in the analysis of caffeine in various environmental samples such as pharmaceuticals, soft and energy drinks, tea, and coffee. A range of spectrophotometric methodologies including chemometric techniques and derivatization of spectra have been used to analyse the caffeine. PMID:26604926

  4. Raman and absorption spectrophotometric studies of selected lanthanide, californium-doped lanthanide, and actinide trihalides in the solid state

    SciTech Connect

    Wilmarth, W.R.

    1988-03-01

    The solid-state absorption spectra of Cf(III) ions as a dopant in lanthanide trihalide hosts (LnCl/sub 3/: Ln = Ce, Sm, and Y; LnBr/sub 3/: Ln = Ce, Sm, Tb, and Y; LnI/sub 3/: Ln = Ce and Y) have been recorded. The spectra of Cf(III) have been correlated with the various crystal structures. The phonon Raman spectra and solid-state absorption spectra of PmF/sub 3/, PmCl/sub 3/, PmBr/sub 3/, and two crystal modifications of PmI/sub 3/ have been recorded. Symmetry assignments have been made for the Raman-active bands for these trihalides and also the sesquioxide. The room-temperature absorption spectra have been correlated to crystal field effects. The symmetry assignments of the Raman-active phonon modes have been made based on polarized Raman spectra from single crystals of YF/sub 3/-type orthorhombic TbF/sub 3/ and PuBr/sub 3/-type orthorhombic NdBr/sub 3/. Raman spectra of other isostructural lanthanide compounds have been recorded and compared. Symmetry assignments for these compounds have been made by analogy to the single-crystal assignments. Raman spectra have been obtained and catalogued for a number of actinide compounds. Symmetry assignments have been made for the observed Raman-active phonon bands in this work based on the assignments made for isostructural lanthanide compounds. 29 figs., 22 tabs.

  5. Cisapride a green analytical reagent for rapid and sensitive determination of bromate in drinking water, bread and flour additives by oxidative coupling spectrophotometric methods.

    PubMed

    Al Okab, Riyad Ahmed

    2013-02-15

    Green analytical methods using Cisapride (CPE) as green analytical reagent was investigated in this work. Rapid, simple, and sensitive spectrophotometric methods for the determination of bromate in water sample, bread and flour additives were developed. The proposed methods based on the oxidative coupling between phenoxazine and Cisapride in the presence of bromate to form red colored product with max at 520 nm. Phenoxazine and Cisapride and its reaction products were found to be environmentally friendly under the optimum experimental condition. The method obeys beers law in concentration range 0.11-4.00 g ml(-1) and molar absorptivity 1.41 × 10(4) L mol(-1)cm(-1). All variables have been optimized and the presented reaction sequences were applied to the analysis of bromate in water, bread and flour additive samples. The performance of these method was evaluated in terms of Student's t-test and variance ratio F-test to find out the significance of proposed methods over the reference method. The combination of pharmaceutical drugs reagents with low concentration create some unique green chemical analyses.

  6. Cisapride a green analytical reagent for rapid and sensitive determination of bromate in drinking water, bread and flour additives by oxidative coupling spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Al Okab, Riyad Ahmed

    2013-02-01

    Green analytical methods using Cisapride (CPE) as green analytical reagent was investigated in this work. Rapid, simple, and sensitive spectrophotometric methods for the determination of bromate in water sample, bread and flour additives were developed. The proposed methods based on the oxidative coupling between phenoxazine and Cisapride in the presence of bromate to form red colored product with max at 520 nm. Phenoxazine and Cisapride and its reaction products were found to be environmentally friendly under the optimum experimental condition. The method obeys beers law in concentration range 0.11-4.00 g ml-1 and molar absorptivity 1.41 × 104 L mol-1 cm-1. All variables have been optimized and the presented reaction sequences were applied to the analysis of bromate in water, bread and flour additive samples. The performance of these method was evaluated in terms of Student's t-test and variance ratio F-test to find out the significance of proposed methods over the reference method. The combination of pharmaceutical drugs reagents with low concentration create some unique green chemical analyses.

  7. Is it possible to screen for milk or whey protein adulteration with melamine, urea and ammonium sulphate, combining Kjeldahl and classical spectrophotometric methods?

    PubMed

    Finete, Virgínia de Lourdes Mendes; Gouvêa, Marcos Martins; Marques, Flávia Ferreira de Carvalho; Netto, Annibal Duarte Pereira

    2013-12-15

    The Kjeldahl method and four classic spectrophotometric methods (Biuret, Lowry, Bradford and Markwell) were applied to evaluate the protein content of samples of UHT whole milk deliberately adulterated with melamine, ammonium sulphate or urea, which can be used to defraud milk protein and whey contents. Compared with the Kjeldahl method, the response of the spectrophotometric methods was unaffected by the addition of the nitrogen compounds to milk or whey. The methods of Bradford and Markwell were most robust and did not exhibit interference subject to composition. However, the simultaneous interpretation of results obtained using these methods with those obtained using the Kjeldahl method indicated the addition of nitrogen-rich compounds to milk and/or whey. Therefore, this work suggests a combination of results of Kjeldahl and spectrophotometric methods should be used to screen for milk adulteration by these compounds.

  8. Simultaneous estimation of Cefixime and Erdosteine in capsule dosage form by spectrophotometric method.

    PubMed

    Dhoka, Madhura V; Gawande, Vandana T; Joshi, Pranav P; Gandhi, Santosh V; Patil, Neelam G

    2009-01-01

    Two accurate, precise, rapid and economical methods viz. Absorption correction method and Dual wavelength method were developed for the estimation of Cefixime (CEF) and Erdosteine (ERDO) in capsule dosage form. In both the methods linearity was observed in the concentration range of 2-25 microg/ml for Cefixime and 3-37.5 microg/ml for Erdosteine. The results of the analysis have been validated statistically and by recovery studies. The percentage assay was found to be 100.03 +/- 0.68 for Cefixime and 99.5 +/- 1.0 for Erdosteine (Mean +/- S.D) by method A and 99.54 +/- 0.84 for Cefixime and 100.54 +/- 1.3 for Erdosteine (Mean +/- S.D) by method B respectively.

  9. A simple spectrophotometric method for the determination of trace levels of molybdenum using N,N‧-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane

    NASA Astrophysics Data System (ADS)

    Kara, Derya; Karadaş, Cennet

    2015-08-01

    The present work describes a selective, rapid and economical spectrophotometric method for the determination of molybdenum using N,N‧-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane. Molybdenum(VI) reacts with N,N‧-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane to form a stable 1:1 yellow complex with an absorption maximum at 342 nm. The reaction is completed within 10 min and the absorbance of the molybdenum complex remains stable for at least 1 week at room temperature. The effective molar absorption coefficient at 342 nm was 9.6 × 103 L mol-1 cm-1. Under optimal conditions, the complex obeys Beer's law from 0 to 9.9 μg mL-1. The relative standard deviation was 0.08% (for 11 samples, each containing 6 μg mL-1 molybdenum). Under the optimum conditions, the detection limit (3σ) was 17.7 μg L-1 for molybdenum without any preconcentration. The precision was determined from 30 results obtained for 4.80 μg mL-1 Mo(VI); the mean value of a molybdenum(VI) was 4.83 μg ml-1 with a standard derivation of 0.002 μg ml-1 molybdenum(VI).

  10. A simple spectrophotometric method for the determination of trace levels of molybdenum using N,N'-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane.

    PubMed

    Kara, Derya; Karadaş, Cennet

    2015-08-01

    The present work describes a selective, rapid and economical spectrophotometric method for the determination of molybdenum using N,N'-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane. Molybdenum(VI) reacts with N,N'-bis(2-hydroxy-5-bromo-benzyl)1,2 diaminopropane to form a stable 1:1 yellow complex with an absorption maximum at 342 nm. The reaction is completed within 10 min and the absorbance of the molybdenum complex remains stable for at least 1 week at room temperature. The effective molar absorption coefficient at 342 nm was 9.6 × 10(3)L mol(-1)cm(-1). Under optimal conditions, the complex obeys Beer's law from 0 to 9.9 μg mL(-1). The relative standard deviation was 0.08% (for 11 samples, each containing 6 μg mL(-1) molybdenum). Under the optimum conditions, the detection limit (3σ) was 17.7 μg L(-1) for molybdenum without any preconcentration. The precision was determined from 30 results obtained for 4.80 μg mL(-1) Mo(VI); the mean value of a molybdenum(VI) was 4.83 μg ml(-1) with a standard derivation of 0.002 μg ml(-1) molybdenum(VI).

  11. Successive ratio subtraction coupled with constant multiplication spectrophotometric method for determination of hydroquinone in complex mixture with its degradation products, tretinoin and methyl paraben

    NASA Astrophysics Data System (ADS)

    Elghobashy, Mohamed R.; Bebawy, Lories I.; Shokry, Rafeek F.; Abbas, Samah S.

    2016-03-01

    A sensitive and selective stability-indicating successive ratio subtraction coupled with constant multiplication (SRS-CM) spectrophotometric method was studied and developed for the spectrum resolution of five component mixture without prior separation. The components were hydroquinone in combination with tretinoin, the polymer formed from hydroquinone alkali degradation, 1,4 benzoquinone and the preservative methyl paraben. The proposed method was used for their determination in their pure form and in pharmaceutical formulation. The zero order absorption spectra of hydroquinone, tretinoin, 1,4 benzoquinone and methyl paraben were determined at 293, 357.5, 245 and 255.2 nm, respectively. The calibration curves were linear over the concentration ranges of 4.00-46.00, 1.00-7.00, 0.60-5.20, and 1.00-7.00 μg mL- 1 for hydroquinone, tretinoin, 1,4 benzoquinone and methyl paraben, respectively. The pharmaceutical formulation was subjected to mild alkali condition and measured by this method resulting in the polymerization of hydroquinone and the formation of toxic 1,4 benzoquinone. The proposed method was validated according to ICH guidelines. The results obtained were statistically analyzed and compared with those obtained by applying the reported method.

  12. Spectrophotometric method for the determination of manganese with phenylfluorone in the presence of Triton X-100 and cetylpyridinium chloride in pharmacological preparations and vegetable fertilizers.

    PubMed

    Winkler, Wanda; Buhl, Franciszek; Arenhövel-Pacuła, Agata; Hachuła, Urszula

    2003-07-01

    A simple and very sensitive method for the spectrophotometric determination of manganese in pharmacological preparations and vegetable fertilizers is proposed. The method is based on the formation of a blue coloured complex of Mn (II) with 9-phenyl-2,3,7-trihydroxy-6-fluorone (PF) in the presence of cetylpyridinium chloride (CP) and Triton X-100. Optimum concentrations of PF, CP, Triton X-100 and pH ensuring maximum absorbance were defined. The complex Mn(II)-PF-CP-Triton X-100 shows maximum absorbance at 591 nm with the molar absorptivity value 1.77x10(5 )L mol(-1 )cm(-1). The detection limit of the method is 0.004 microg mL(-1). The Beer's law is obeyed for manganese concentrations in the range 0.02-0.2 microg mL(-1). The effect of foreign ions was elucidated. The statistical evaluation of the method was carried out for six determination using 5 microg Mn and the following results were obtained: standard deviation 0.021, confidence interval 5.05+/-0.05 microg Mn. The method has been applied for the determination of manganese in pharmacological preparations (Biovital, Kinder Biovital) and vegetable fertilizers (Hydrovit 100, Florovit). PMID:12861432

  13. Successive ratio subtraction coupled with constant multiplication spectrophotometric method for determination of hydroquinone in complex mixture with its degradation products, tretinoin and methyl paraben.

    PubMed

    Elghobashy, Mohamed R; Bebawy, Lories I; Shokry, Rafeek F; Abbas, Samah S

    2016-03-15

    A sensitive and selective stability-indicating successive ratio subtraction coupled with constant multiplication (SRS-CM) spectrophotometric method was studied and developed for the spectrum resolution of five component mixture without prior separation. The components were hydroquinone in combination with tretinoin, the polymer formed from hydroquinone alkali degradation, 1,4 benzoquinone and the preservative methyl paraben. The proposed method was used for their determination in their pure form and in pharmaceutical formulation. The zero order absorption spectra of hydroquinone, tretinoin, 1,4 benzoquinone and methyl paraben were determined at 293, 357.5, 245 and 255.2 nm, respectively. The calibration curves were linear over the concentration ranges of 4.00-46.00, 1.00-7.00, 0.60-5.20, and 1.00-7.00 μg mL(-1) for hydroquinone, tretinoin, 1,4 benzoquinone and methyl paraben, respectively. The pharmaceutical formulation was subjected to mild alkali condition and measured by this method resulting in the polymerization of hydroquinone and the formation of toxic 1,4 benzoquinone. The proposed method was validated according to ICH guidelines. The results obtained were statistically analyzed and compared with those obtained by applying the reported method. PMID:26745510

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

    PubMed

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

    2016-12-01

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

  15. Blood cyanide determination in two cases of fatal intoxication: comparison between headspace gas chromatography and a spectrophotometric method.

    PubMed

    Gambaro, Veniero; Arnoldi, Sebastiano; Casagni, Eleonora; Dell'acqua, Lucia; Pecoraro, Chiara; Froldi, Rino

    2007-11-01

    Blood samples of two cases were analyzed preliminarily by a classical spectrophotometric method (VIS) and by an automated headspace gas chromatographic method with nitrogen-phosphorus detector (HS-GC/NPD). In the former, hydrogen cyanide (HCN) was quantitatively determined by measuring the absorbance of chromophores forming as a result of interaction with chloramine T. In the automated HS-GC/NPD method, blood was placed in a headspace vial, internal standard (acetonitrile) and acetic acid were then added. This resulted in cyanide being liberated as HCN. The spectrophotometric (VIS) and HS-GC/NPD methods were validated on postmortem blood samples fortified with potassium cyanide in the ranges 0.5-10 and 0.05-5 mug/mL, respectively. Detection limits were 0.2 mug/mL for VIS and 0.05 mug/mL for HS-GC/NPD. This work shows that results obtained by means of the two procedures were insignificantly different and that they compared favorably. They are suitable for rapid diagnosis of cyanide in postmortem cases.

  16. Generalized net analyte signal standard addition as a novel method for simultaneous determination: application in spectrophotometric determination of some pesticides.

    PubMed

    Asadpour-Zeynali, Karim; Saeb, Elhameh; Vallipour, Javad; Bamorowat, Mehdi

    2014-01-01

    Simultaneous spectrophotometric determination of three neonicotinoid insecticides (acetamiprid, imidacloprid, and thiamethoxam) by a novel method named generalized net analyte signal standard addition method (GNASSAM) in some binary and ternary synthetic mixtures was investigated. For this purpose, standard addition was performed using a single standard solution consisting of a mixture of standards of all analytes. Savings in time and amount of used materials are some of the advantages of this method. All determinations showed appropriate applicability of this method with less than 5% error. This method may be applied for linearly dependent data in the presence of known interferents. The GNASSAM combines the advantages of both the generalized standard addition method and net analyte signal; therefore, it may be a proper alternative for some other multivariate methods. PMID:24672886

  17. Application of the ratio difference spectrophotometry to the determination of ibuprofen and famotidine in their combined dosage form; Comparison with previously published spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Zaazaa, Hala E.; Elzanfaly, Eman S.; Soudi, Aya T.; Salem, Maissa Y.

    2015-05-01

    Ratio difference spectrophotometric method was developed for the determination of ibuprofen and famotidine in their mixture form. Ibuprofen and famotidine were determined in the presence of each other by the ratio difference spectrophotometric (RD) method where linearity was obtained from 50 to 600 μg/mL and 2.5 to 25 μg/mL for ibuprofen and famotidine, respectively. The suggested method was validated according to ICH guidelines and successfully applied for the analysis of ibuprofen and famotidine in their pharmaceutical dosage forms without interference from any additives or excipients.

  18. Application of the ratio difference spectrophotometry to the determination of ibuprofen and famotidine in their combined dosage form: comparison with previously published spectrophotometric methods.

    PubMed

    Zaazaa, Hala E; Elzanfaly, Eman S; Soudi, Aya T; Salem, Maissa Y

    2015-05-15

    Ratio difference spectrophotometric method was developed for the determination of ibuprofen and famotidine in their mixture form. Ibuprofen and famotidine were determined in the presence of each other by the ratio difference spectrophotometric (RD) method where linearity was obtained from 50 to 600μg/mL and 2.5 to 25μg/mL for ibuprofen and famotidine, respectively. The suggested method was validated according to ICH guidelines and successfully applied for the analysis of ibuprofen and famotidine in their pharmaceutical dosage forms without interference from any additives or excipients.

  19. Development and validation of simple spectrophotometric and chemometric methods for simultaneous determination of empagliflozin and metformin: Applied to recently approved pharmaceutical formulation

    NASA Astrophysics Data System (ADS)

    Ayoub, Bassam M.

    2016-11-01

    New univariate spectrophotometric method and multivariate chemometric approach were developed and compared for simultaneous determination of empagliflozin and metformin manipulating their zero order absorption spectra with application on their pharmaceutical preparation. Sample enrichment technique was used to increase concentration of empagliflozin after extraction from tablets to allow its simultaneous determination with metformin without prior separation. Validation parameters according to ICH guidelines were satisfactory over the concentration range of 2-12 μg mL- 1 for both drugs using simultaneous equation with LOD values equal to 0.20 μg mL- 1 and 0.19 μg mL- 1, LOQ values equal to 0.59 μg mL- 1 and 0.58 μg mL- 1 for empagliflozin and metformin, respectively. While the optimum results for the chemometric approach using partial least squares method (PLS-2) were obtained using concentration range of 2-10 μg mL- 1. The optimized validated methods are suitable for quality control laboratories enable fast and economic determination of the recently approved pharmaceutical combination Synjardy® tablets.

  20. Spectrophotometric system to develop a non-invasive method for monitoring of posidonia oceanica meadows

    NASA Astrophysics Data System (ADS)

    Menesatti, P.; Urbani, G.; Dolce, T.

    2007-09-01

    Posidonia oceanica (L.) is an endemic phanerogam of the Mediterranean Sea. It lives between 0.2 and 40 m depth and make up extensive meadows that play a fundamental role in the marine coast ecosystem. Near the coasts at higher anthropic pressure, Posidonia meadows present both quality and quantity damages (regression) due to the mechanical operations on the seabed (anchoring, drag netting, pipe lines) and the sea pollution. Nowadays, the seagrass regression is monitored by different systems: aereophotografic, side scan sonar, underwater television camera, direct underwater visual inspection. Scientific community is looking for to develop monitoring systems more reliable, rapid and non invasive. Aim of this study is to evaluate the application of a new spectrophotometric imaging system based on the acquisition of reflectance spectral images with a good optical (250 Kpixels) and spectral resolution (spectral range 400-970 nm, a total of 115 single wavelength, 5 nm step each one). First trials were made on Posidonia's leafs to evaluate the system capacity to recognize spectral differences between samples picked up at two different depths (0.3 - 4 m). High discrimination percentage (90%) were found between leaf samples as function of the different depths, analyzing the spectral data by Partial Least Squares model. Forward activities will stress the system capability also to evaluate different phenol concentrations on Posidonia leaves, an important index of physiologic vegetal damage, through direct underwater spectrophotometric monitoring.

  1. Stability-indicating spectrophotometric and spectrodensitometric methods for the determination of diacerein in the presence of its degradation product.

    PubMed

    Nebsen, Marianne; Abd El-Rahman, Mohamed K; Salem, Maissa Y; El-Kosasy, Amira M; El-Bardicy, Mohamed G

    2011-04-01

    Three sensitive, selective, and precise stability-indicating methods for the determination of the novel osteoarthritis drug, diacerein (DIA) in the presence of its alkaline degradation product (active metabolite, rhein) and in pharmaceutical formulation were developed and validated. The first method is a first derivative (D(1) ) spectrophotometric one, which allows the determination of DIA in the presence of its degradate at 322 nm (corresponding to zero crossing of the degradate) over a concentration range of 4-40 µg/mL with mean percentage recovery 100.21 ± 0.833. The second method is the first derivative of the ratio spectra (DD(1) ) by measuring the peak amplitude at 352 nm over the same concentration range as (D(1) ) spectrophotometric method, with mean percentage recovery 100.09 ± 0.912. The third method is a TLC-densitometric one, where DIA was separated from its degradate on silica gel plates using ethyl acetate:methanol:chloroform (8:1.5:0.5 v:v:v) as a developing system. This method depends on quantitative densitometric evaluation of thin layer chromatogram of DIA at 340 nm over a concentration range of 1-10 µg/spot, with mean percentage recovery 100.24 ± 1.412. The selectivity of the proposed methods was tested using laboratory-prepared mixtures. The proposed methods have been successfully applied to the analysis of DIA in pharmaceutical dosage forms without interference from other dosage form additives and the results were statistically compared with reference method. PMID:21500366

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    Mohamed, Heba M; Lamie, Nesrine T

    2016-02-15

    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 360nm. 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 306nm (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 278.5nm (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. Stability indicating spectrophotometric and spectrodensitometric methods for the determination of diatrizoate sodium in presence of its degradation product.

    PubMed

    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. PMID:25456658

  6. Extractive spectrophotometric methods for determination of diltiazem HCl in pharmaceutical formulations using bromothymol blue, bromophenol blue and bromocresol green.

    PubMed

    Rahman, N; Hejaz-Azmi, S N

    2000-12-01

    Three simple and sensitive extractive spectrophotometric methods have been described for the assay of diltiazem hydrochloride either in pure form or in pharmaceutical formulations. The developed methods involve formation of coloured chloroform extractable ion-pair complexes of the drug with bromothymol blue (BTB), bromophenol blue (BPB) and bromocresol green (BCG) in acidic medium. The extracted complexes showed absorbance maxima at 415 nm for all three methods. Beer's law is obeyed in the concentration ranges 2.5-20.0, 2.5-10.0 and 2.5-12.5 microg ml(-1) with BTB, BPB and BCG, respectively. The methods have been applied to the determination of drug in commercial tablets and capsules. Results of analysis were validated statistically and through recovery studies.

  7. Evaluation of flow injection analysis method with spectrophotometric detection for the determination of atrazine in soil extracts.

    PubMed

    Martins, Elisandra C; Melo, Vander De F; Abate, Gilberto

    2016-09-01

    A method for determining atrazine in soil extracts was evaluated by flow injection analysis with spectrophotometric detection. The method is based on the reaction of atrazine with pyridine in an acid medium followed by the reaction with NaOH and sulfanilic acid. Several analytical conditions were previously studied and optimized. Under the best conditions of analysis, the limits of detection and quantification were 0.15 and 0.45 mg L(-1), respectively, for a linear response between 0.50 and 2.50 mg L(-1), and a sampling throughput of 21 determinations per hour. Using the standard addition method, the maximum relative standard deviation of 17% and recovery values between 80 and 100% were observed for three extracts from soil samples with different composition. The proposed method is simple, low-cost and easy to use, and can be employed for studies involving atrazine in soil samples or for screening of atrazine in soils.

  8. Fourth-order derivative spectrophotometric method for simultaneous determination of pseudoephedrine and naproxen in pharmaceutical dosage forms

    PubMed Central

    Souri, Effat; Mosafer, Amir; Tehrani, Maliheh Barazandeh

    2016-01-01

    Combination dosage forms of naproxen sodium and pseudoephedrine hydrochloride are used for symptomatic treatment of cold and sinus disorders. In this study, fourth-order derivative spectrophotometric method was used for simultaneous determination of naproxen sodium and pseudoephedrine hydrochloride. The method was linear over the range of 2-28 μg/ml for pseudoephedrine hydrochloride and 4-200 μg/ml for naproxen sodium. The within-day and between-day coefficient of variation values were less than 5.8% and 2.5% for pseudoephedrine hydrochloride and naproxen sodium, respectively. The application of the proposed method for simultaneous determination of naproxen and pseudoephedrine in dosage forms was demonstrated without any special pretreatment. PMID:27168748

  9. Fourth-order derivative spectrophotometric method for simultaneous determination of pseudoephedrine and naproxen in pharmaceutical dosage forms.

    PubMed

    Souri, Effat; Mosafer, Amir; Tehrani, Maliheh Barazandeh

    2016-01-01

    Combination dosage forms of naproxen sodium and pseudoephedrine hydrochloride are used for symptomatic treatment of cold and sinus disorders. In this study, fourth-order derivative spectrophotometric method was used for simultaneous determination of naproxen sodium and pseudoephedrine hydrochloride. The method was linear over the range of 2-28 μg/ml for pseudoephedrine hydrochloride and 4-200 μg/ml for naproxen sodium. The within-day and between-day coefficient of variation values were less than 5.8% and 2.5% for pseudoephedrine hydrochloride and naproxen sodium, respectively. The application of the proposed method for simultaneous determination of naproxen and pseudoephedrine in dosage forms was demonstrated without any special pretreatment.

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

    PubMed

    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

  11. Development of a highly sensitive extractive spectrophotometric method for the determination of nickel(II) from environmental matrices using N-ethyl-3-carbazolecarboxaldehyde-3-thiosemicarbazone.

    PubMed

    Ramachandraiah, C; Rajesh Kumar, J; Janardhan Reddy, K; Lakshmi Narayana, S; Varada Reddy, A

    2008-09-01

    Nickel(II) reacts with N-ethyl-3-carbazolecarboxaldehyde-3-thiosemicarbazone (ECCT) and forms a yellow colored complex, which was extracted into n-butanol from sodium acetate and acetic acid buffer at pH 6.0. The absorbance value of the Ni(II)-ECCT complex was measured at different intervals of time at 400 nm, to ascertain the time stability of the complex. The extraction of the complex into the solvent was instantaneous and stable for more than 72 h. The system obeyed Beer's law in the concentration range of 1.2-5.6 microg ml(-1) of nickel(II), with an excellent linearity and a correlation coefficient of 0.999. The molar absorptivity and Sandell's sensitivity of the extracted species were found to be 1.114 x 10(4)L mol(-1)cm(-1) and 5.29 x 10(-3)microg cm(-2) at 400 nm, respectively. Hence, a detailed study of the extraction of nickel(II) with ECCT has been undertaken with a view to developing a rapid and sensitive extractive spectrophotometric method for the determination of nickel(II) when present alone or in the presence of diverse ions which are usually associated with nickel(II) in environmental matrices like soil and industrial effluents. Various standard alloy samples (CM 247 LC, IN 718, BCS 233, 266, 253 and 251) have been tested for the determination of nickel for the purpose of validation of the present method. The results of the proposed method are comparable with those from atomic absorption spectrometry and were found to be in good agreement.

  12. A simple spectrophotometric method for determination of zirconium or hafnium in selected molybdenum-base alloys

    NASA Technical Reports Server (NTRS)

    Dupraw, W. A.

    1972-01-01

    A simple analytical procedure is described for accurately and precisely determining the zirconium or hafnium content of molybdenum-base alloys. The procedure is based on the reaction of the reagent Arsenazo III with zirconium or hafnium in strong hydrochloric acid solution. The colored complexes of zirconium or hafnium are formed in the presence of molybdenum. Titanium or rhenium in the alloy have no adverse effect on the zirconium or hafnium complex at the following levels in the selected aliquot: Mo, 10 mg; Re, 10 mg; Ti, 1 mg. The spectrophotometric measurement of the zirconium or hafnium complex is accomplished without prior separation with a relative standard deviation of 1.3 to 2.7 percent.

  13. Graphite furnace atomic absorption spectrophotometry--a novel method to quantify blood volume in experimental models of intracerebral hemorrhage.

    PubMed

    Kashefiolasl, Sepide; Foerch, Christian; Pfeilschifter, Waltraud

    2013-02-15

    Intracerebral hemorrhage (ICH) accounts for 10% of all strokes and has a significantly higher mortality than cerebral ischemia. For decades, ICH has been neglected by experimental stroke researchers. Recently, however, clinical trials on acute blood pressure lowering or hyperacute supplementation of coagulation factors in ICH have spurred an interest to also design and improve translational animal models of spontaneous and anticoagulant-associated ICH. Hematoma volume is a substantial outcome parameter of most experimental ICH studies. We present graphite furnace atomic absorption spectrophotometric analysis (AAS) as a suitable method to precisely quantify hematoma volumes in rodent models of ICH.

  14. Ultraviolet and Light Absorption Spectrometry.

    ERIC Educational Resources Information Center

    Hargis, L. G.; Howell, J. A.

    1984-01-01

    Reviews developments in ultraviolet and light absorption spectrometry from December 1981 through November 1983, focusing on the chemistry involved in developing suitable reagents, absorbing systems, and methods of determination, and on physical aspects of the procedures. Includes lists of spectrophotometric methods for metals, non-metals, and…

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

    PubMed

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

    2015-09-01

    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). PMID:25863461

  16. Extraction-Spectrophotometric Method for Determination of Gallium(III) in the Form of Ion Associate with a Monotetrazolium Salt

    NASA Astrophysics Data System (ADS)

    Stojnova, K. T.; Divarov, V. V.; Racheva, P. V.; Lekova, V. D.

    2015-11-01

    The possibility of application of the ternary ion-association complex of gallium(III), 4-(2-pyridyl azo)resorcinol (PAR) and 2,3,5-triphenyl-2H-tetrazolium chloride (TTC) for extraction-spectrophotometric determination of gallium(III) was studied. The liquid-liquid extraction system Ga(III)-PAR-TTC-H2O-CHCl3 was applied for this purpose. The effect of the foreign ions on the extraction was investigated. Based on the obtained results, a sensitive, relatively simple, and inexpensive method for determination of gallium(III) in a model mixture was developed, which can be implemented in industrial, biological, medical, and pharmaceutical samples.

  17. A comparative study of validated spectrophotometric and TLC- spectrodensitometric methods for the determination of sodium cromoglicate and fluorometholone in ophthalmic solution

    PubMed Central

    Saleh, Sarah S.; Lotfy, Hayam M.; Hassan, Nagiba Y.; Elgizawy, Samia M.

    2013-01-01

    The determination of sodium cromoglicate (SCG) and fluorometholone (FLU) in ophthalmic solution was developed by simple, sensitive and precise methods. Three spectrophotometric methods were applied: absorptivity factor (a-Factor method), absorption factor (AFM) and mean centering of ratio spectra (MCR). The linearity ranges of SCG were found to be (2.5–35 μg/mL) for (a-Factor method) and (MCR); while for (AFM), it was found to be (7.5–50 μg/mL). The linearity ranges of FLU were found to be (4–16 μg/mL) for (a-Factor method) and (AFM); while for (MCR), it was found to be (2–16 μg/mL). The mean percentage recoveries/RSD for SCG were found to be 100.31/0.90, 100.23/0.57 and 100.43/1.21; while for FLU, they were found to be 100.11/0.56, 99.97/0.35 and 99.94/0.88 using (a-Factor method), (AFM) and (MCR), respectively. A TLC-spectrodensitometric method was developed by separation of SCG and FLU on silica gel 60 F254 using chloroform:methanol:toluene:triethylamine in the ratio of (5:2:4:1 v/v/v/v) as developing system, followed by spectrodensitometric measurement of the bands at 241 nm. The linearity ranges and the mean percentage recoveries/RSD were found to be (0.4–4.4 μg/band), 100.24/1.44 and (0.2–1.6 μg/band), 99.95/1.50 for SCG and FLU, respectively. A comparative study was conducted between the proposed methods to discuss the advantage of each method. The suggested methods were validated in compliance with the ICH guidelines and were successfully applied for the determination of SCG and FLU in their laboratory prepared mixtures and commercial ophthalmic solution in the presence of benzalkonium chloride as a preservative. These methods could be an alternative to different HPLC techniques in quality control laboratories lacking the required facilities for those expensive techniques. PMID:24227962

  18. A continuous spectrophotometric method based on enzymatic cycling for determining L-glutamate.

    PubMed

    Valero, E; Garcia-Carmona, F

    1998-06-01

    A continuous spectrophotometric assay for determining low levels of L-glutamate is described. The assay, which involves the enzymes L-glutamate oxidase and glutamic-pyruvic transaminase, is based on the recycling of L-glutamate into alpha-ketoglutarate, with the concomitant appearance of one molecule of hydrogen peroxide in each turn of the cycle. This is subsequently reduced by means of a peroxidase-coupled reaction, using 2, 2'-azinobis(3-ethylbenzthiazoline-6-sulfonic acid) as substrate. In this way the interference observed in the cyclic assay using glutamic-oxalacetic transaminase, which is due to the fact that L-aspartate is also a substrate of L-glutamate oxidase, is eliminated. A kinetic study of the system is presented, with the accumulation of chromophore being seen to undergo a transient phase, which is dependent both on the cycling rate and on the auxiliary enzyme concentration. The kinetic parameters characterizing the system have been determined, making it possible to optimize costs with respect to the enzymes involved in the cycle, since the minimum amount needed for a given rate constant of the cycle can be calculated.

  19. Spectrophotometric probe

    DOEpatents

    Prather, William S.; O'Rourke, Patrick E.

    1994-01-01

    A support structure bearing at least one probe for making spectrophotometric measurements of a fluid using a source of light and a spectrophotometer. The probe includes a housing with two optical fibers and a planoconvex lens. A sleeve bearing a mirror surrounds the housing. The lens is separated from the mirror by a fixed distance, defining an interior space for receiving a volume of the fluid sample. A plurality of throughholes extending through the sleeve communicate between the sample volume and the exterior of the probe, all but one hole bearing a screen. A protective jacket surrounds the probe. A hollow conduit bearing a tube is formed in the wall of the probe for venting any air in the interior space when fluid enters. The probe is held at an acute angle so the optic fibers carrying the light to and from the probe are not bent severely on emergence from the probe.

  20. Spectrophotometric probe

    DOEpatents

    Prather, W.S.; O'Rourke, P.E.

    1994-08-02

    A support structure is described bearing at least one probe for making spectrophotometric measurements of a fluid using a source of light and a spectrophotometer. The probe includes a housing with two optical fibers and a planoconvex lens. A sleeve bearing a mirror surrounds the housing. The lens is separated from the mirror by a fixed distance, defining an interior space for receiving a volume of the fluid sample. A plurality of throughholes extending through the sleeve communicate between the sample volume and the exterior of the probe, all but one hole bearing a screen. A protective jacket surrounds the probe. A hollow conduit bearing a tube is formed in the wall of the probe for venting any air in the interior space when fluid enters. The probe is held at an acute angle so the optic fibers carrying the light to and from the probe are not bent severely on emergence from the probe. 3 figs.

  1. A novel approach in dispersive liquid-liquid microextraction based on the use of an auxiliary solvent for adjustment of density UV-VIS spectrophotometric and graphite furnace atomic absorption spectrometric determination of gold based on ion pair formation.

    PubMed

    Kocúrová, Lívia; Balogh, Ioseph S; Skrlíková, Jana; Posta, József; Andruch, Vasil

    2010-10-15

    This paper presents a novel approach to dispersive liquid-liquid microextraction (DLLME), based on the use of an auxiliary solvent for the adjustment of density. The procedure utilises a solvent system consisting of a dispersive solvent, an extraction solvent and an auxiliary solvent, which allows for the use of solvents having a density lower than that of water as an extraction solvent while preserving simple phase separation by centrifugation. The suggested approach could be an alternative to procedures described in the literature in recent months and which have been devoted to solving the same problem. The efficiency of the suggested approach is demonstrated through the determination of gold based on the formation of the ion pair [Au(CN)(2)](-) anion with Astra Phloxine (R) reagent and its extraction using the DLLME procedure with subsequent UV-VIS spectrophotometric and graphite furnace atomic absorption spectrometric detection. The optimum conditions were found to be: pH 3; 0.8 mmol L(-1) K(4)[Fe(CN)(6)]; 0.12 mmol L(-1) R; dispersive solvent, methanol; extraction solvent, toluene; auxiliary solvent, tetrachloromethane. The calibration plots were linear in the ranges 0.39-4.7 mg L(-1) and 0.5-39.4 μg L(-1) for UV-VIS and GFAAS detection, respectively; thus enables the application of the developed method in two ranges differing from one from another by three orders of magnitude. The presented approach can be applied to the development of DLLME procedures for the determination of other compounds extractable by organic solvents with a density lower than that of water. PMID:20875602

  2. Spectrophotometric Determination of Certain Benzimidazole Proton Pump Inhibitors

    PubMed Central

    Syed, A. A.; Syeda, Ayesha

    2008-01-01

    Spectrophotometric method for the determination of certain proton pump inhibitors belonging to the benzimidazole class of compounds has been developed. The method is based on the reaction of omeprazole, lansoprazole, pantoprazole, rabeprazole and esomeprazole with iron (III) and subsequent reaction with ferricyanide under neutral condition which yields Prussian blue product with maximum absorption at 720–730 nm. The commonly encountered excipients and additives that often accompany pharmaceutical preparations did not interfere with the determination. The method was applied for the determination of omeprazole, lansoprazole, pantoprazole, rabeprazole and esomeprazole in pharmaceutical preparations and no difference was found statistically. Thus, the spectrophotometric method can be applied as inexpensive, rapid, easy, accurate and precise method for the routine analysis of the five proton pump inhibitors in pharmaceutical preparations. PMID:20046782

  3. A rapid and high-throughput microplate spectrophotometric method for field measurement of nitrate in seawater and freshwater

    PubMed Central

    Wu, Jiapeng; Hong, Yiguo; Guan, Fengjie; Wang, Yan; Tan, Yehui; Yue, Weizhong; Wu, Meilin; Bin, Liying; Wang, Jiaping; Wen, Jiali

    2016-01-01

    The well-known zinc-cadmium reduction method is frequently used for determination of nitrate. However, this method is seldom to be applied on field research of nitrate due to the long time consuming and large sample volume demand. Here, we reported a modified zinc-cadmium reduction method (MZCRM) for measurement of nitrate at natural-abundance level in both seawater and freshwater. The main improvements of MZCRM include using small volume disposable tubes for reaction, a vortex apparatus for shaking to increase reduction rate, and a microplate reader for high-throughput spectrophotometric measurements. Considering salt effect, two salinity sections (5~10 psu and 20~35 psu) were set up for more accurate determination of nitrate in low and high salinity condition respectively. Under optimized experimental conditions, the reduction rates were stabilized on 72% and 63% on the salinity of 5 and 20 psu respectively. The lowest detection limit for nitrate was 0.5 μM and was linear up to 100 μM (RSDs was 4.8%). Environmental samples assay demonstrated that MZCRM was well consistent with conventional zinc-cadmium reduction method. In total, this modified method improved accuracy and efficiency of operations greatly, and would be realized a rapid and high-throughput determination of nitrate in field analysis of nitrate with low cost. PMID:26832984

  4. A rapid and high-throughput microplate spectrophotometric method for field measurement of nitrate in seawater and freshwater

    NASA Astrophysics Data System (ADS)

    Wu, Jiapeng; Hong, Yiguo; Guan, Fengjie; Wang, Yan; Tan, Yehui; Yue, Weizhong; Wu, Meilin; Bin, Liying; Wang, Jiaping; Wen, Jiali

    2016-02-01

    The well-known zinc-cadmium reduction method is frequently used for determination of nitrate. However, this method is seldom to be applied on field research of nitrate due to the long time consuming and large sample volume demand. Here, we reported a modified zinc-cadmium reduction method (MZCRM) for measurement of nitrate at natural-abundance level in both seawater and freshwater. The main improvements of MZCRM include using small volume disposable tubes for reaction, a vortex apparatus for shaking to increase reduction rate, and a microplate reader for high-throughput spectrophotometric measurements. Considering salt effect, two salinity sections (5~10 psu and 20~35 psu) were set up for more accurate determination of nitrate in low and high salinity condition respectively. Under optimized experimental conditions, the reduction rates were stabilized on 72% and 63% on the salinity of 5 and 20 psu respectively. The lowest detection limit for nitrate was 0.5 μM and was linear up to 100 μM (RSDs was 4.8%). Environmental samples assay demonstrated that MZCRM was well consistent with conventional zinc-cadmium reduction method. In total, this modified method improved accuracy and efficiency of operations greatly, and would be realized a rapid and high-throughput determination of nitrate in field analysis of nitrate with low cost.

  5. Development of a spectrophotometric method for on-site analysis of peroxygens during in-situ chemical oxidation applications.

    PubMed

    Bennedsen, Lars Rønn; Søgaard, Erik Gydesen; Muff, Jens

    2014-01-01

    Activated peroxygens are frequently used as active agents in in-situ chemical oxidation (ISCO) contaminated site remediation applications, and fast and simple quantitative analysis of these species on site is necessary. In this work, the use of a spectrophotometric method based on classic iodometric titration is studied for quantitative analysis of S2O8(2-) and H2O2. Instead of a back-titration step, the absorbance of the yellow iodide colour was measured at 352 nm in the presence of a bicarbonate buffer. A linear calibration curve was obtained from 0 to 0.1 mM for both S2O8(2-) and H2O2. By dilution, the method can be used for all concentrations typically applied in the field. Concerning pH dependence, neutral pH levels caused no significant error whereas pH levels above 8 caused a 9% and 6% deviation from the theoretical peroxygen concentrations. Furthermore, the method showed little dependence on other matrix components, and absorbance was stable (<2% change) for more than a week. Overall, the method proved to be fast and simple, which are important features for a field method. PMID:25429454

  6. Spectrophotometric micro method for measurement of dialyzable calcium by use of cresolphthalein complexone and continuous-flow analysis.

    PubMed

    Toffaletti, J; Kirvan, K

    1980-10-01

    We adapted a method for dialyzable calcium from fluorometric detection by use of calcein to a more specific spectrophotometric determination with cresolphthalein complexone. The reagents are available commercially and perform satisfactorily with respect to noise level, drift, stability, and sensitivity. Construction of the continuous-flow manifold with commercially available components (injection blocks, coils, and dialyzer) and the use of a 9-mm pathlength flow cell in an AutoAnalyzer I colorimeter have permitted a sampling rate of 70/h, and decreased the volume of serum required to 130 microL. A comparison of 71 sera analyzed by the present and the calcein method gave means of 1.39 (SD 0.14) and 1.39 (SD 0.13) mmol/L, respectively. The regression equation was: present method = 1.016 calcein--0.022 mmol/L (r = 0.97). The CV for the new method, as determined from 46 randomized duplicate analyses, was < 1%. The reference interval, as evaluated from results for 93 different individuals, was 1.26-1.43 mmol/L. We conclude that our methods is an improvement with respect to noise level, drift, specificity, detectability, and more general availability of instrumentation. Moreover, the smaller sample volume required makes possible the routine measurement of dialyzable calcium in pediatric samples.

  7. Development and Validation of Different Ultraviolet-Spectrophotometric Methods for the Estimation of Besifloxacin in Different Simulated Body Fluids

    PubMed Central

    Singh, C. L.; Singh, A.; Kumar, S.; Kumar, M.; Sharma, P. K.; Majumdar, D. K.

    2015-01-01

    In the present study a simple, accurate, precise, economical and specific UV-spectrophotometric method for estimation of besifloxacin in bulk and in different pharmaceutical formulation has been developed. The drug shows maximum λmax289 nm in distilled water, simulated tears and phosphate buffer saline. The linearity range of developed methods were in the range of 3-30 μg/ml of drug with a correlation coefficient (r2) 0.9992, 0.9989 and 0.9984 with respect to distilled water, simulated tears and phosphate buffer saline, respectively. Reproducibility by repeating methods as %RSD were found to be less than 2%. The limit of detection in different media was found to be 0.62, 0.72 and 0.88 μg/ml, respectively. The limit of quantification was found to be 1.88, 2.10, 2.60 μg/ml, respectively. The proposed method was validated statically according to International Conference on Harmonization guidelines with respect to specificity, linearity, range, accuracy, precision and robustness. The proposed methods of validation were found to be accurate and highly specific for the estimation of besifloxacin in different pharmaceutical formulations. PMID:26664055

  8. Development and Validation of Different Ultraviolet-Spectrophotometric Methods for the Estimation of Besifloxacin in Different Simulated Body Fluids.

    PubMed

    Singh, C L; Singh, A; Kumar, S; Kumar, M; Sharma, P K; Majumdar, D K

    2015-01-01

    In the present study a simple, accurate, precise, economical and specific UV-spectrophotometric method for estimation of besifloxacin in bulk and in different pharmaceutical formulation has been developed. The drug shows maximum λmax289 nm in distilled water, simulated tears and phosphate buffer saline. The linearity range of developed methods were in the range of 3-30 μg/ml of drug with a correlation coefficient (r(2)) 0.9992, 0.9989 and 0.9984 with respect to distilled water, simulated tears and phosphate buffer saline, respectively. Reproducibility by repeating methods as %RSD were found to be less than 2%. The limit of detection in different media was found to be 0.62, 0.72 and 0.88 μg/ml, respectively. The limit of quantification was found to be 1.88, 2.10, 2.60 μg/ml, respectively. The proposed method was validated statically according to International Conference on Harmonization guidelines with respect to specificity, linearity, range, accuracy, precision and robustness. The proposed methods of validation were found to be accurate and highly specific for the estimation of besifloxacin in different pharmaceutical formulations. PMID:26664055

  9. A rapid and high-throughput microplate spectrophotometric method for field measurement of nitrate in seawater and freshwater.

    PubMed

    Wu, Jiapeng; Hong, Yiguo; Guan, Fengjie; Wang, Yan; Tan, Yehui; Yue, Weizhong; Wu, Meilin; Bin, Liying; Wang, Jiaping; Wen, Jiali

    2016-01-01

    The well-known zinc-cadmium reduction method is frequently used for determination of nitrate. However, this method is seldom to be applied on field research of nitrate due to the long time consuming and large sample volume demand. Here, we reported a modified zinc-cadmium reduction method (MZCRM) for measurement of nitrate at natural-abundance level in both seawater and freshwater. The main improvements of MZCRM include using small volume disposable tubes for reaction, a vortex apparatus for shaking to increase reduction rate, and a microplate reader for high-throughput spectrophotometric measurements. Considering salt effect, two salinity sections (5~10 psu and 20~35 psu) were set up for more accurate determination of nitrate in low and high salinity condition respectively. Under optimized experimental conditions, the reduction rates were stabilized on 72% and 63% on the salinity of 5 and 20 psu respectively. The lowest detection limit for nitrate was 0.5 μM and was linear up to 100 μM (RSDs was 4.8%). Environmental samples assay demonstrated that MZCRM was well consistent with conventional zinc-cadmium reduction method. In total, this modified method improved accuracy and efficiency of operations greatly, and would be realized a rapid and high-throughput determination of nitrate in field analysis of nitrate with low cost.

  10. Development of sensitive spectrofluorimetric and spectrophotometric methods for the determination of duloxetine in capsule and spiked human plasma.

    PubMed

    Sagirli, Olcay; Toker, Sıdıka Erturk; Önal, Armağan

    2014-12-01

    A new, sensitive and selective spectrofluorimetric method has been developed for the determination of duloxetine (DLX) in capsule and spiked human plasma. DLX, as a secondary amine compound, reacts with 7-chloro-4-nitrobenzofurazon (NBD-Cl), a highly sensitive fluorogenic and chromogenic reagent used in many investigations. The method is based on the reaction between the drug and NBD-Cl in borate buffer at pH 8.5 to yield a highly fluorescent derivative that is measured at 523 nm after excitation at 478 nm. The fluorescence intensity was directly proportional to the concentration over the range 50-250 ng/mL. The reaction product was also measured spectrophotometrically. The relation between the absorbance at 478 nm and the concentration is rectilinear over the range 1.0-12.0 µg/mL. The methods were successfully applied for the determination of this drug in pharmaceutical dosage form. The spectrofluorimetric method was also successfully applied to the determination of duloxetine in spiked human plasma. The suggested procedures could be used for the determination of DLX in pure form, capsules and human plasma being sensitive, simple and selective.

  11. Kinetic spectrophotometric method as a new strategy for the determination of vitamin B 9 in pharmaceutical and biological samples

    NASA Astrophysics Data System (ADS)

    Shishehbore, M. Reza; Sheibani, A.; Haghdost, A.

    2011-10-01

    In this study, a new method is proposed for the determination of trace amounts of folic acid (vitamin B 9). This method is based on the inhibitory effect of folic acid on the reaction of Thionine and bromate in sulfuric acid media. The reaction can be monitored spectrophotometrically by measuring the decrease in absorbance at 601 nm ( λmax). The effective variables on the reaction rate were investigated. Under optimum experimental conditions, the method allows to determine of the folic acid in a wide linear range with two linear segments. The limit of detection was 0.36 μg mL -1 of folic acid. Relative standard deviations of six replicate determinations of 5.0 and 50.0 μg mL -1 of folic acid were 1.18 and 1.02%, respectively. The interfering effect of the different species was also investigated. The method was evaluated by quantifying of folic acid in biological and pharmaceutical samples with satisfactory assay results.

  12. Different Spectrophotometric and TLC-Densitometric Methods for Determination of Mesalazine in Presence of Its Two Toxic Impurities.

    PubMed

    Morcoss, Martha Moheb; Abdelwahab, Nada Sayed; Ali, Nouruddin Wagieh; Elsaady, Mohammed Taha

    2016-01-01

    Two selective spectrophotometric and TLC-densitometric methods were developed for determination of mesalazine (ME) and its two toxic impurities, 4-amino phenol (4AP) and salicylic acid (SA) without preliminary separation. The proposed methods are: ratio difference in the subtracted spectra (RDSS) {Method 1}, area under the curve (AUC) {Method 2} and TLC-densitometric {Method 3}. In method {1} combination of measuring the amplitude of the constant at 350 nm (using standard spectrum of 10 µg/mL ME as a divisor) and ratio difference in the subtracted ratio spectrum for determination of 4AP and SA using the ratio difference at 221.4 and 242.2 nm, 230 and 241.2 nm, respectively. In method {2} ME was determined by direct measuring the AUC in the wavelength range of 350-370 nm while the impurities could be determined by dividing their spectra by standard spectrum of 10 µg/mL ME then interference from ME was eliminated by subtracting the amplitude of the constant at 350 nm then multiplying by the divisor. AUC in the range of 220-230 and 235-245 nm was used for measuring concentrations of 4AP and SA. On the other hand, the third method {3} is TLC-densitometric method at which chromatographic separation was achieved using ethyl acetate-methanol-triethylamine (8.5 : 2 : 0.7, v/v/v) as a developing system with UV scanning at 230 nm. The validation of the proposed methods was performed according to International Conference on Harmonization (ICH) guidelines. No significant difference was found when these methods were compared to the reported one. PMID:27581631

  13. Use of lignin extracted from different plant sources as standards in the spectrophotometric acetyl bromide lignin method.

    PubMed

    Fukushima, Romualdo S; Kerley, Monty S

    2011-04-27

    A nongravimetric acetyl bromide lignin (ABL) method was evaluated to quantify lignin concentration in a variety of plant materials. The traditional approach to lignin quantification required extraction of lignin with acidic dioxane and its isolation from each plant sample to construct a standard curve via spectrophotometric analysis. Lignin concentration was then measured in pre-extracted plant cell walls. However, this presented a methodological complexity because extraction and isolation procedures are lengthy and tedious, particularly if there are many samples involved. This work was targeted to simplify lignin quantification. Our hypothesis was that any lignin, regardless of its botanical origin, could be used to construct a standard curve for the purpose of determining lignin concentration in a variety of plants. To test our hypothesis, lignins were isolated from a range of diverse plants and, along with three commercial lignins, standard curves were built and compared among them. Slopes and intercepts derived from these standard curves were close enough to allow utilization of a mean extinction coefficient in the regression equation to estimate lignin concentration in any plant, independent of its botanical origin. Lignin quantification by use of a common regression equation obviates the steps of lignin extraction, isolation, and standard curve construction, which substantially expedites the ABL method. Acetyl bromide lignin method is a fast, convenient analytical procedure that may routinely be used to quantify lignin.

  14. Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

    PubMed

    Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

    2016-05-01

    Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples. PMID:27040110

  15. Development of a Rapid Derivative Spectrophotometric Method for Simultaneous Determination of Acetaminophen, Diphenhydramine and Pseudoephedrine in Tablets

    PubMed Central

    Souri, Effat; Rahimi, Aghil; Shabani Ravari, Nazanin; Barazandeh Tehrani, Maliheh

    2015-01-01

    A mixture of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride is used for the symptomatic treatment of common cold. In this study, a derivative spectrophotometric method based on zero-crossing technique was proposed for simultaneous determination of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride. Determination of these drugs was performed using the 1D value of acetaminophen at 281.5 nm, 2D value of diphenhydramine hydrochloride at 226.0 nm and 4D value of pseudoephedrine hydrochloride at 218.0 nm. The analysis method was linear over the range of 5-50, 0.25-4, and 0.5-5 µg/mL for acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride, respectively. The within-day and between-day CV and error values for all three compounds were within an acceptable range (CV<2.2% and error<3%). The developed method was used for simultaneous determination of these drugs in pharmaceutical dosage forms and no interference from excipients was observed. PMID:25901150

  16. Development of a rapid derivative spectrophotometric method for simultaneous determination of acetaminophen, diphenhydramine and pseudoephedrine in tablets.

    PubMed

    Souri, Effat; Rahimi, Aghil; Shabani Ravari, Nazanin; Barazandeh Tehrani, Maliheh

    2015-01-01

    A mixture of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride is used for the symptomatic treatment of common cold. In this study, a derivative spectrophotometric method based on zero-crossing technique was proposed for simultaneous determination of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride. Determination of these drugs was performed using the (1)D value of acetaminophen at 281.5 nm, (2)D value of diphenhydramine hydrochloride at 226.0 nm and (4)D value of pseudoephedrine hydrochloride at 218.0 nm. The analysis method was linear over the range of 5-50, 0.25-4, and 0.5-5 µg/mL for acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride, respectively. The within-day and between-day CV and error values for all three compounds were within an acceptable range (CV<2.2% and error<3%). The developed method was used for simultaneous determination of these drugs in pharmaceutical dosage forms and no interference from excipients was observed.

  17. Development of a rapid derivative spectrophotometric method for simultaneous determination of acetaminophen, diphenhydramine and pseudoephedrine in tablets.

    PubMed

    Souri, Effat; Rahimi, Aghil; Shabani Ravari, Nazanin; Barazandeh Tehrani, Maliheh

    2015-01-01

    A mixture of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride is used for the symptomatic treatment of common cold. In this study, a derivative spectrophotometric method based on zero-crossing technique was proposed for simultaneous determination of acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride. Determination of these drugs was performed using the (1)D value of acetaminophen at 281.5 nm, (2)D value of diphenhydramine hydrochloride at 226.0 nm and (4)D value of pseudoephedrine hydrochloride at 218.0 nm. The analysis method was linear over the range of 5-50, 0.25-4, and 0.5-5 µg/mL for acetaminophen, diphenhydramine hydrochloride and pseudoephedrine hydrochloride, respectively. The within-day and between-day CV and error values for all three compounds were within an acceptable range (CV<2.2% and error<3%). The developed method was used for simultaneous determination of these drugs in pharmaceutical dosage forms and no interference from excipients was observed. PMID:25901150

  18. Sensitive spectrophotometric determination of Co(II) using dispersive liquid-liquid micro-extraction method in soil samples.

    PubMed

    Hasanpour, Foroozan; Hadadzadeh, Hassan; Taei, Masoumeh; Nekouei, Mohsen; Mozafari, Elmira

    2016-05-01

    Analytical performance of conventional spectrophotometer was developed by coupling of effective dispersive liquid-liquid micro-extraction method with spectrophotometric determination for ultra-trace determination of cobalt. The method was based on the formation of Co(II)-alpha-benzoin oxime complex and its extraction using a dispersive liquid-liquid micro-extraction technique. During the present work, several important variables such as pH, ligand concentration, amount and type of dispersive, and extracting solvent were optimized. It was found that the crucial factor for the Co(II)-alpha benzoin oxime complex formation is the pH of the alkaline alcoholic medium. Under the optimized condition, the calibration graph was linear in the ranges of 1.0-110 μg L(-1) with the detection limit (S/N = 3) of 0.5 μg L(-1). The preconcentration operation of 25 mL of sample gave enhancement factor of 75. The proposed method was applied for determination of Co(II) in soil samples.

  19. Validated derivative and ratio derivative spectrophotometric methods for the simultaneous determination of levocetirizine dihydrochloride and ambroxol hydrochloride in pharmaceutical dosage form

    NASA Astrophysics Data System (ADS)

    Ali, Omnia I. M.; Ismail, Nahla S.; Elgohary, Rasha M.

    2016-01-01

    Three simple, precise, accurate and validated derivative spectrophotometric methods have been developed for the simultaneous determination of levocetirizine dihydrochloride (LCD) and ambroxol hydrochloride (ABH) in bulk powder and in pharmaceutical formulations. The first method is a first derivative spectrophotometric method (1D) using a zero-crossing technique of measurement at 210.4 nm for LCD and at 220.0 nm for ABH. The second method employs a second derivative spectrophotometry (2D) where the measurements were carried out at 242.0 and 224.4 nm for LCD and ABH, respectively. In the third method, the first derivative of the ratio spectra was calculated and the first derivative of the ratio amplitudes at 222.8 and 247.2 nm was selected for the determination of LCD and ABH, respectively. Calibration graphs were established in the ranges of 1.0-20.0 μg mL- 1 for LCD and 4.0-20.0 μg mL- 1 for ABH using derivative and ratio first derivative spectrophotometric methods with good correlation coefficients. The developed methods have been successfully applied to the simultaneous determination of both drugs in commercial tablet dosage form.

  20. Validated derivative and ratio derivative spectrophotometric methods for the simultaneous determination of levocetirizine dihydrochloride and ambroxol hydrochloride in pharmaceutical dosage form.

    PubMed

    Ali, Omnia I M; Ismail, Nahla S; Elgohary, Rasha M

    2016-01-15

    Three simple, precise, accurate and validated derivative spectrophotometric methods have been developed for the simultaneous determination of levocetirizine dihydrochloride (LCD) and ambroxol hydrochloride (ABH) in bulk powder and in pharmaceutical formulations. The first method is a first derivative spectrophotometric method ((1)D) using a zero-crossing technique of measurement at 210.4 nm for LCD and at 220.0 nm for ABH. The second method employs a second derivative spectrophotometry ((2)D) where the measurements were carried out at 242.0 and 224.4 nm for LCD and ABH, respectively. In the third method, the first derivative of the ratio spectra was calculated and the first derivative of the ratio amplitudes at 222.8 and 247.2 nm was selected for the determination of LCD and ABH, respectively. Calibration graphs were established in the ranges of 1.0-20.0 μg mL(-1) for LCD and 4.0-20.0 μg mL(-1) for ABH using derivative and ratio first derivative spectrophotometric methods with good correlation coefficients. The developed methods have been successfully applied to the simultaneous determination of both drugs in commercial tablet dosage form.

  1. Validated derivative and ratio derivative spectrophotometric methods for the simultaneous determination of levocetirizine dihydrochloride and ambroxol hydrochloride in pharmaceutical dosage form.

    PubMed

    Ali, Omnia I M; Ismail, Nahla S; Elgohary, Rasha M

    2016-01-15

    Three simple, precise, accurate and validated derivative spectrophotometric methods have been developed for the simultaneous determination of levocetirizine dihydrochloride (LCD) and ambroxol hydrochloride (ABH) in bulk powder and in pharmaceutical formulations. The first method is a first derivative spectrophotometric method ((1)D) using a zero-crossing technique of measurement at 210.4 nm for LCD and at 220.0 nm for ABH. The second method employs a second derivative spectrophotometry ((2)D) where the measurements were carried out at 242.0 and 224.4 nm for LCD and ABH, respectively. In the third method, the first derivative of the ratio spectra was calculated and the first derivative of the ratio amplitudes at 222.8 and 247.2 nm was selected for the determination of LCD and ABH, respectively. Calibration graphs were established in the ranges of 1.0-20.0 μg mL(-1) for LCD and 4.0-20.0 μg mL(-1) for ABH using derivative and ratio first derivative spectrophotometric methods with good correlation coefficients. The developed methods have been successfully applied to the simultaneous determination of both drugs in commercial tablet dosage form. PMID:26439526

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

    PubMed

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

    2014-07-15

    Three novel numerical methods were developed for the spectrophotometric multi-component analysis of capsules and synthetic mixtures of aspirin, atorvastatin and clopedogrel without any chemical separation. The subtraction method is based on the relationship between the difference in absorbance at four wavelengths and corresponding concentration of analyte. In this method, the linear determination ranges were 0.8-40 μg mL(-1) aspirin, 0.8-30 μg mL(-1) atorvastatin and 0.5-30 μg mL(-1) clopedogrel. In the quotient method, 0.8-40 μg mL(-1) aspirin, 0.8-30 μg mL(-1) atorvastatin and 1.0-30 μg mL(-1) clopedogrel were determine from spectral data at the wavelength pairs that show the same ratio of absorbance for other two species. Standard addition method was used for resolving ternary mixture of 1.0-40 μg mL(-1) aspirin, 0.8-30 μg mL(-1) atorvastatin and 2.0-30 μg mL(-1) clopedogrel. The proposed methods were validated. The reproducibility and repeatability were found satisfactory which evidence was by low values of relative standard deviation (<2%). Recovery was found to be in the range (99.6-100.8%). By adopting these methods, the time taken for analysis was reduced as these methods involve very limited steps. The developed methods were applied for simultaneous analysis of aspirin, atorvastatin and clopedogrel in capsule dosage forms and results were in good concordance with alternative liquid chromatography.

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

    NASA Astrophysics Data System (ADS)

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

    2014-07-01

    Three novel numerical methods were developed for the spectrophotometric multi-component analysis of capsules and synthetic mixtures of aspirin, atorvastatin and clopedogrel without any chemical separation. The subtraction method is based on the relationship between the difference in absorbance at four wavelengths and corresponding concentration of analyte. In this method, the linear determination ranges were 0.8-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 0.5-30 μg mL-1 clopedogrel. In the quotient method, 0.8-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 1.0-30 μg mL-1 clopedogrel were determine from spectral data at the wavelength pairs that show the same ratio of absorbance for other two species. Standard addition method was used for resolving ternary mixture of 1.0-40 μg mL-1 aspirin, 0.8-30 μg mL-1 atorvastatin and 2.0-30 μg mL-1 clopedogrel. The proposed methods were validated. The reproducibility and repeatability were found satisfactory which evidence was by low values of relative standard deviation (<2%). Recovery was found to be in the range (99.6-100.8%). By adopting these methods, the time taken for analysis was reduced as these methods involve very limited steps. The developed methods were applied for simultaneous analysis of aspirin, atorvastatin and clopedogrel in capsule dosage forms and results were in good concordance with alternative liquid chromatography.

  4. Spectrophotometric methods based on 2,6-dichloroindophenol acetate and indoxylacetate for butyrylcholinesterase activity assay in plasma.

    PubMed

    Pohanka, Miroslav; Drtinova, Lucie

    2013-03-15

    Butyrylcholinesterase (BChE) is an enzyme presented in quite high level in blood plasma where it participates in detoxification reactions. Due to fact that the enzyme is constituted in livers, it is a marker of liver parenchyma function. It can be used for diagnosis of poisoning for e.g., nerve agents or carbofuran and intoxication by some drugs such as rivastigmine. The present experiment is devoted for the creation of new spectrophotometric tests for assay of BChE activity in biological samples. Standard Ellman's method was compared with use of 2,6-dichloroindophenol acetate and indoxylacetate as chromogenic substrates. Maximal velocities and Michaelis constants were calculated for the substrates. Considering calibration, 2,6-dichloroindophenol acetate provided the lowest limit of detection: 1.20 × 10(-9)kat and a long linear range. All methods were verified using pooled human plasma samples and tested for potential interferents. 2,6-dichloroindophenol acetate is recommended as suitable substrate for BChE assay in clinical diagnostics.

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

    PubMed

    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.

  6. Developing a new micro cloud point extraction method for simultaneous preconcentration and spectrophotometric determination of uranium and vanadium in brine.

    PubMed

    Ghasemi, Elham; Kaykhaii, Massoud

    2015-01-01

    A fast, simple, and economical method was developed for simultaneous spectrophotometric determination of uranium(VI) and vanadium(V) in water samples based on micro cloud point extraction (MCPE) at room temperature. This is the first report on the simultaneous extraction and determination of U(VI) and V(V). In this method, Triton X114 was employed as a non-ionic surfactant for the cloud point procedure and 4-(2-pyridylazo) resorcinol (PAR) was used as the chelating agent for both analytes. To reach the cloud point at room temperature, the MCPE procedure was carried out in brine. The factors influencing the extraction efficiency were investigated and optimized. Under the optimized condition, the linear calibration curve was found to be in the concentration range between 100 - 750 and 50 - 600 μg L(-1) for U(VI) and V(V), respectively, with a limit of detection of 17.03 μg L(-1) (U) and 5.51 μg L(-1) (V). Total analysis time including microextraction was less than 5 min.

  7. Comparison of Adsorbed Mercury Screening Method With Cold-Vapor Atomic Absorption Spectrophotometry for Determination of Mercury in Soil

    NASA Technical Reports Server (NTRS)

    Easterling, Donald F.; Hovanitz, Edward S.; Street, Kenneth W.

    2000-01-01

    A field screening method for the determination of elemental mercury in environmental soil samples involves the thermal desorption of the mercury from the sample onto gold and then the thermal desorption from the gold to a gold-film mercury vapor analyzer. This field screening method contains a large number of conditions that could be optimized for the various types of soils encountered. In this study, the conditions were optimized for the determination of mercury in silty clay materials, and the results were comparable to the cold-vapor atomic absorption spectrophotometric method of determination. This paper discusses the benefits and disadvantages of employing the field screening method and provides the sequence of conditions that must be optimized to employ this method of determination on other soil types.

  8. Spectrophotometric measurement of calcium carbonate saturation states in seawater.

    PubMed

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

    2013-02-01

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

  9. Sensitive Spectrophotometric Method for Quantitation of Guaifenesin and Dropropizine in Their Dosage Forms

    PubMed Central

    Abdallah, Ola M.

    2010-01-01

    Guaifenesin and dropropizine were analyzed through oxidation with periodic acid to give formaldehyde which was allowed to condense with 4-Amino-5-hydrazino-4H [1,2,4]-triazole-3-thiol (AHTT). The condensation product was further oxidized to yield a purple colored compound with maximum absorption at 550 nm. Beer's law was obeyed in the range of 5–45 μg mL−1 for guaifenesin and 10–80 μg mL−1 for dropropizine. Both drugs were also successfully determined in their dosage forms. PMID:20671996

  10. Examination of the Measurement of Absorption Using the Reverberant Room Method for Highly Absorptive Acoustic Foam

    NASA Technical Reports Server (NTRS)

    Hughes, William O.; McNelis, Anne M.; Chris Nottoli; Eric Wolfram

    2015-01-01

    The absorption coefficient for material specimens are needed to quantify the expected acoustic performance of that material in its actual usage and environment. The ASTM C423-09a standard, "Standard Test Method for Sound Absorption and Sound Absorption Coefficients by the Reverberant Room Method" is often used to measure the absorption coefficient of material test specimens. This method has its basics in the Sabine formula. Although widely used, the interpretation of these measurements are a topic of interest. For example, in certain cases the measured Sabine absorption coefficients are greater than 1.0 for highly absorptive materials. This is often attributed to the diffraction edge effect phenomenon. An investigative test program to measure the absorption properties of highly absorbent melamine foam has been performed at the Riverbank Acoustical Laboratories. This paper will present and discuss the test results relating to the effect of the test materials' surface area, thickness and edge sealing conditions. A follow-on paper is envisioned that will present and discuss the results relating to the spacing between multiple piece specimens, and the mounting condition of the test specimen.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    NASA Astrophysics Data System (ADS)

    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.

  13. Spectrophotometric determination of ascorbic acid by the modified CUPRAC method with extractive separation of flavonoids-La(III) complexes.

    PubMed

    Ozyürek, Mustafa; Güçlü, Kubilay; Bektaşoğlu, Burcu; Apak, Reşat

    2007-04-01

    The proposed method for ascorbic acid: AA (Vitamin C) determination is based on the oxidation of AA to dehydroascorbic acid with the CUPRAC reagent of total antioxidant capacity assay, i.e., Cu(II)-neocuproine (Nc), in ammonium acetate-containing medium at pH 7, where the absorbance of the formed bis(Nc)-copper(I) chelate is measured at 450 nm. The flavonoids (essentially flavones and flavonols) normally interfering with the CUPRAC procedure were separated with preliminary extraction as their La(III) chelates into ethylacetate (EtAc). The Cu(I)-Nc chelate responsible for color development was formed immediately with AA oxidation. Beer's law was obeyed between 8.0 x 10(-6) and 8.0 x 10(-5) M concentration range, with the equation of the linear calibration curve: A(450 nm)=1.60 x 10(4)C (mol dm(-3))-0.0596. The relative standard deviation (R.S.D.) in the analysis of N=45 synthetic mixtures containing 1.25 x 10(-2) mM AA with flavonoids was 5.3%. The Cu(II)-Nc reagent is a lower redox-potential and therefore more selective oxidant than the Fe(III)-1,10-phenanthroline reagent conventionally used for the same assay. This feature makes the proposed method superior for real samples such as fruit juices containing weak reductants such as citrate, oxalate and tartarate that may otherwise produce positive errors in the Fe(III)-phen method when equilibrium is achieved. The developed method was applied to some commercial fruit juices and pharmaceutical preparations containing Vitamin C+bioflavonoids. The findings of the developed method for fruit juices and pharmaceuticals were statistically alike with those of HPLC. The proposed spectrophotometric method was practical, low-cost, rapid, and could reliably assay AA in the presence of flavonoids without enzymatic procedures open to interferences by enzyme inhibitors.

  14. In Situ Spectrophotometric Determination of pH under Geologic CO2 Sequestration Conditions: Method Development and Application

    SciTech Connect

    Shao, Hongbo; Thompson, Christopher J.; Qafoku, Odeta; Cantrell, Kirk J.

    2013-02-25

    Injecting massive amounts of CO2 into deep geologic formations will cause a range of coupled thermal, hydrodynamic, mechanical, and chemical changes. A significant perturbation in water-saturated formations is the pH drop in the reservoir fluids due to CO2 dissolution. Knowing the pH under geological CO2 sequestration conditions is important for a better understanding of the short- and long-term risks associated with geological CO2 sequestration and will help in the design of sustainable sequestration projects. Most previous studies on CO2-rock-brine interactions have utilized thermodynamic modeling to estimate the pH. In this work, a spectrophotometric method was developed to determine the in-situ pH in CO2-H2O-NaCl systems in the presence and absence of reservoir rock by observing the spectra of a pH indicator, bromophenol blue, with a UV-visible spectrophotometer. Effects of temperature, pressure, and ionic strength on the pH measurement were evaluated. Measured pH values in CO2-H2O-NaCl systems were compared with several thermodynamic models. Results indicate that bromophenol blue can be used to accurately determine the pH of brine in contact with supercritical CO2 under geologic CO2 sequestration conditions.

  15. Spectrophotometric methods for the simultaneous analysis of meclezine hydrochloride and pyridoxine hydrochloride in bulk drug and pharmaceutical formulations.

    PubMed

    Arayne, M Saeed; Sultana, Najma; Siddiqui, Farhan Ahmed; Zuberi, M Hashim; Mirza, Agha Zeeshan

    2007-04-01

    Three new spectrophotometric procedures for the simultaneous determination of pyridoxine hydrochloride and meclezine hydrochloride are described. The first method depends on the application of simultaneous equation to resolve the interference due to spectral overlapping. The analytical signals were measured at 231 and 220 nm. Calibration graphs were established for 1 to 20 microGmL(-1) for pyridoxine hydrochloride and 0.5 to 10 microGmL(-1) for meclezine hydrochloride in binary mixture. In the second method, the determination of pyridoxine hydrochloride and meclezine hydrochloride was performed by measuring the absorbances at 290 and 235 nm in the simple absorbance spectra of their mixture. In third method a yellowish orange complex of pyridoxine hydrochloride was formed with ferric chloride, which absorbs in the visible region with lambda(max) at 445 nm. Calibration curve of complex formation range was conducted in between 20 to 250 microGmL(-1). These methods were validated with respect to accuracy, precision, linearity, limit of detection and quantification. Regression analysis of Beer's plot showed good correlation in a general concentration range of 1 to 20 microGml(-1) with correlation coefficient (r = 0.9999 and 0.9999; CV < 0.858) for pyridoxine hydrochloride, whereas meclezine hydrochloride concentration range 0.5 to 10 microGmL(-1) with correlation coefficient (r = 0.9998 and 0.9998; CV < 0.826). These methods can be readily applied, without any interference from the excipients. The suggested procedures were successfully applied to the determination of these compounds in synthetic mixtures and in pharmaceutical preparations, with high percentage of recovery, good accuracy and precision. PMID:17416572

  16. Spectrophotometric, difference spectroscopic, and high-performance liquid chromatographic methods for the determination of cefixime in pharmaceutical formulations.

    PubMed

    Shah, Paresh B; Pundarikakshudu, Kilambi

    2006-01-01

    Three simple and sensitive spectrophotometric, difference spectroscopic, and liquid chromatographic (LC) methods are described for the determination of cefixime. The first method is based on the oxidative coupling reaction of cefixime with 3-methyl-2-benzothiazolinon hydrazone HCI in presence of ferric chloride. The absorbance of reaction product was measured at the maximum absorbance wavelength (wavelength(max)), 630 nm. The difference spectroscopic method is based on the measurement of absorbance of cefixime at the absorbance maximum, 268 nm, and minimum, 237 nm. The measured value was the amplitude of maxima and minima between 2 equimolar solutions of the analyte in different chemical forms, which exhibited different spectral characteristics. The conditions were optimized, and Beer's law was obeyed for cefixime at 1 to 16 microg/mL and 10 to 50 microg/mL, respectively. The third method, high-performance LC, was developed for the determination of cefixime using 50 mM potassium dihydrogen phosphate (pH 3.0)-methanol (78 + 22, v/v) as the mobile phase and measuring the response at wavelength(max) 286 nm. The analysis was performed on a Lichrospher RPC18 column. The calibration curve was obtained for cefixime at 5 to 250 microg/mL, and the mean recovery was 99.71 +/- 0.01%. The methods were validated according to the guidelines of the U.S. Pharmacopoeia and also assessed by applying the standard addition technique. The results obtained in the analysis of dosage forms agreed well with the contents stated on the labels.

  17. [Comparative Analysis of Spectrophotometric Methods of the Protein Measurement in the Pectic Polysaccharide Samples].

    PubMed

    Ponomareva, S A; Golovchenko, V V; Patova, O A; Vanchikova, E V; Ovodov, Y S

    2015-01-01

    For the assay to reliability of determination of the protein content in the pectic polysaccharide samples by absorbance in the ultraviolet and visible regions of the spectrum a comparison of the eleven techniques called Flores, Lovry, Bradford, Sedmak, Rueman (ninhydrin reaction) methods, the method of ultraviolet spectrophotometry, the method Benedict's reagent, the method Nessler's reagent, the method with amide black, the bicinchoninic reagent and the biuret method was carried out. The data obtained show that insufficient sensitivity of the seven methods from the listed techniques doesn't allow their usage for determination of protein content in pectic polysaccharide samples. But the Lowry, Bradford, Sedmak methods, and the method Nessler's reagent may be used for determination of protein content in pectic polysaccharide samples, and the Bradford method is advisable for protein contaminants content determination in pectic polysaccharide samples in case protein content is less than 15%, and the Lowry method--for samples is more than 15%. PMID:26165122

  18. Study report on a double isotope method of calcium absorption

    NASA Technical Reports Server (NTRS)

    1978-01-01

    Some of the pros and cons of three methods to study gastrointestinal calcium absorption are briefly discussed. The methods are: (1) a balance study; (2) a single isotope method; and (3) a double isotope method. A procedure for the double isotope method is also included.

  19. Sensitive indirect spectrophotometric determination of isoniazid

    NASA Astrophysics Data System (ADS)

    Safavi, A.; Karimi, M. A.; Hormozi Nezhad, M. R.; Kamali, R.; Saghir, N.

    2004-03-01

    A simple, rapid, sensitive and accurate indirect spectrophotometric method for the microdetermination of isoniazid (INH) in pure form and pharmaceutical formulations is developed. The procedure is based on the reaction of copper(II) with isoniazid in the presence of neocuproine (NC). In the presence of neocuproine, copper(II) is reduced easily by isoniazid to a Cu(I)-neocuproine complex, which shows an absorption maximum at 454 nm. By measuring the absorbance of the complex at this wavelength, isoniazid can be determined in the range 0.3-3.5 μg ml -1. This method was applied to the determination of isoniazid in pharmaceutical formulation and enabled the determination of the isoniazid in microgram quantities (0.3-3.5 μg ml -1). The results obtained for the assay of pharmaceutical preparations compared well with those obtained by the official method and demonstrated good accuracy and precision.

  20. Sensitive indirect spectrophotometric determination of isoniazid.

    PubMed

    Safavi, A; Karimi, M A; Hormozi Nezhad, M R; Kamali, R; Saghir, N

    2004-03-01

    A simple, rapid, sensitive and accurate indirect spectrophotometric method for the microdetermination of isoniazid (INH) in pure form and pharmaceutical formulations is developed. The procedure is based on the reaction of copper(II) with isoniazid in the presence of neocuproine (NC). In the presence of neocuproine, copper(II) is reduced easily by isoniazid to a Cu(I)-neocuproine complex, which shows an absorption maximum at 454 nm. By measuring the absorbance of the complex at this wavelength, isoniazid can be determined in the range 0.3-3.5 microgml-1. This method was applied to the determination of isoniazid in pharmaceutical formulation and enabled the determination of the isoniazid in microgram quantities (0.3-3.5 microgml-1). The results obtained for the assay of pharmaceutical preparations compared well with those obtained by the official method and demonstrated good accuracy and precision.

  1. Simultaneous Determination of Octinoxate, Oxybenzone, and Octocrylene in a Sunscreen Formulation Using Validated Spectrophotometric and Chemometric Methods.

    PubMed

    Abdel-Ghany, Maha F; Abdel-Aziz, Omar; Ayad, Miriam F; Mikawy, Neven N

    2015-01-01

    Accurate, reliable, and sensitive spectrophotometric and chemometric methods were developed for simultaneous determination of octinoxate (OMC), oxybenzone (OXY), and octocrylene (OCR) in a sunscreen formulation without prior separation steps, including derivative ratio spectra zero crossing (DRSZ), double divisor ratio spectra derivative (DDRD), mean centering ratio spectra (MCR), and partial least squares (PLS-2). With the DRSZ technique, the UV filters could be determined in the ranges of 0.5-13.0, 0.3-9.0, and 0.5-9.0 μg/mL at 265.2, 246.6, and 261.8 nm, respectively. By utilizing the DDRD technique, UV filters could be determined in the above ranges at 237.8, 241.0, and 254.2 nm, respectively. With the MCR technique, the UV filters could be determined in the above ranges at 381.7, 383.2, and 355.6 nm, respectively. The PLS-2 technique successfully quantified the examined UV filters in the ranges of 0.5-9.3, 0.3-7.1, and 0.5-6.9 μg/mL, respectively. All the methods were validated according to the International Conference on Harmonization guidelines and successfully applied to determine the UV filters in pure form, laboratory-prepared mixtures, and a sunscreen formulation. The obtained results were statistically compared with reference and reported methods of analysis for OXY, OMC, and OCR, and there were no significant differences with respect to accuracy and precision of the adopted techniques.

  2. Simultaneous Determination of Octinoxate, Oxybenzone, and Octocrylene in a Sunscreen Formulation Using Validated Spectrophotometric and Chemometric Methods.

    PubMed

    Abdel-Ghany, Maha F; Abdel-Aziz, Omar; Ayad, Miriam F; Mikawy, Neven N

    2015-01-01

    Accurate, reliable, and sensitive spectrophotometric and chemometric methods were developed for simultaneous determination of octinoxate (OMC), oxybenzone (OXY), and octocrylene (OCR) in a sunscreen formulation without prior separation steps, including derivative ratio spectra zero crossing (DRSZ), double divisor ratio spectra derivative (DDRD), mean centering ratio spectra (MCR), and partial least squares (PLS-2). With the DRSZ technique, the UV filters could be determined in the ranges of 0.5-13.0, 0.3-9.0, and 0.5-9.0 μg/mL at 265.2, 246.6, and 261.8 nm, respectively. By utilizing the DDRD technique, UV filters could be determined in the above ranges at 237.8, 241.0, and 254.2 nm, respectively. With the MCR technique, the UV filters could be determined in the above ranges at 381.7, 383.2, and 355.6 nm, respectively. The PLS-2 technique successfully quantified the examined UV filters in the ranges of 0.5-9.3, 0.3-7.1, and 0.5-6.9 μg/mL, respectively. All the methods were validated according to the International Conference on Harmonization guidelines and successfully applied to determine the UV filters in pure form, laboratory-prepared mixtures, and a sunscreen formulation. The obtained results were statistically compared with reference and reported methods of analysis for OXY, OMC, and OCR, and there were no significant differences with respect to accuracy and precision of the adopted techniques. PMID:26525239

  3. Comparative analysis of radical scavenging and antioxidant activity of phenolic compounds present in everyday use spice plants by means of spectrophotometric and chromatographic methods.

    PubMed

    Stankevičius, Mantas; Akuņeca, Ieva; Jãkobsone, Ida; Maruška, Audrius

    2011-06-01

    Comparative analysis of radical scavenging and antioxidant activities of phenolic compounds present in everyday use spice plants was carried out by means of spectrophotometric and chromatographic methods. Six spice plant samples, namely onion (Allium cepa), parsley (Petroselinum crispum) roots and leaves, celery (Apium graveolens) roots and leaves and leaves of dill (Anethum graveolens) were analyzed. Total amount of phenolic compounds and radical scavenging activity (RSA) was the highest in celery leaves and dill extracts and was the lowest in celery roots. Comparing commonly used spectrophotometric analysis of 2,2-diphenyl-1-picrylhydrazyl (DPPH) RSA of extracts with the results obtained using reversed-phase chromatographic separation with on-line post-column radical scavenging reaction detection, good correlation was obtained (R(2)=0.848). Studies using HPLC system with electrochemical detector showed that bioactive phytochemicals can be separated and antioxidant activities of individual compounds evaluated without the need of a complex HPLC system with reaction detector. The results obtained using electrochemical detection correlate with the RSA assayed using spectrophotometric method (R(2)=0.893).

  4. UV Spectrophotometric Method for Estimation of Polypeptide-K in Bulk and Tablet Dosage Forms

    NASA Astrophysics Data System (ADS)

    Kaur, P.; Singh, S. Kumar; Gulati, M.; Vaidya, Y.

    2016-01-01

    An analytical method for estimation of polypeptide-k using UV spectrophotometry has been developed and validated for bulk as well as tablet dosage form. The developed method was validated for linearity, precision, accuracy, specificity, robustness, detection, and quantitation limits. The method has shown good linearity over the range from 100.0 to 300.0 μg/ml with a correlation coefficient of 0.9943. The percentage recovery of 99.88% showed that the method was highly accurate. The precision demonstrated relative standard deviation of less than 2.0%. The LOD and LOQ of the method were found to be 4.4 and 13.33, respectively. The study established that the proposed method is reliable, specific, reproducible, and cost-effective for the determination of polypeptide-k.

  5. Data supporting the spectrophotometric method for the estimation of catalase activity

    PubMed Central

    Hadwan, Mahmoud Hussein; Abed, Hussein Najm

    2015-01-01

    Here we provide raw and processed data and methods for the estimation of catalase activities. The method for presenting a simple and accurate colorimetric assay for catalase activities is described. This method is based on the reaction of undecomposed hydrogen peroxide with ammonium molybdate to produce a yellowish color, which has a maximum absorbance at 374 nm. The method is characterized by adding a correction factor to exclude the interference that arises from the presence of amino acids and proteins in serum. The assay acts to keep out the interferences that arose from measurement of absorbance at unsuitable wavelengths. PMID:26862558

  6. Automation of a spectrophotometric method for measuring L -carnitine in human blood serum.

    PubMed

    Galan, A; Padros, A; Arambarri, M; Martin, S

    1998-01-01

    A spectrometric method for the determination of L-carnitine has been developed based on the reaction of the 5,5' dithiobis-(2-nitrobenzoic) acid (DTNB) and adapted to a Technicon RA-2000 automatic analyser Química Farmacéutica Bayer, S.A.). The detection limit of the method is 13.2 mumol/l, with a measurement interval ranging from 30 to 320 mumoll1. Imprecision and accuracy are good even at levels close to the detection limit (coeffcient of variation of 5.4% for within-run imprecision for a concentration of 35 mumol/l). A good correlation was observed between the method studied and the radiometric method. The method evaluated has suffcient analytical sensitivity to diagnose carnitine deficiencies. The short time period required for sample processing (30 samples in 40min), the simple methodology and apparatus, the ease of personnel training and the low cost of the reagents make this method a good alternative to the classical radiometric method for evaluating serum L-carnitine in clinical laboratories without radioactive installations.

  7. [Research into simultaneous spectrophotometric determination of components in cough syrup by principal component regression method].

    PubMed

    Zhang, Li-qing; Wu, Xiao-hua; Tang, Xi; Zhu, Xian-liang; Su, Wen-ting

    2002-06-01

    Principal component regression (PCR) method is used to analyse five components: acetaminophen, p-aminophenol, caffeine, chlorphenamine maleate and guaifenesin. The basic principle and the analytical step of the approach are described in detail. The computer program of LHG is based on VB language. The experimental result shows that the PCR method has no systematical error as compared to classical method. The experimental result shows that the average recovery of each component is all in the range from 96.43% to 107.14%. Each component obtains satisfactory result without any pre-separation. The approach is simple, rapid and suitable for the computer-aid analysis. PMID:12938324

  8. Competitive removal of hazardous dyes from aqueous solution by MIL-68(Al): Derivative spectrophotometric method and response surface methodology approach

    NASA Astrophysics Data System (ADS)

    Tehrani, Mahnaz Saghanejhad; Zare-Dorabei, Rouholah

    2016-05-01

    MIL-68(Al) as a metal-organic framework (MOF) was synthesized and characterized by different techniques such as SEM, BET, FTIR, and XRD analysis. This material was then applied for simulations removal of malachite green (MG) and methylene blue (MB) dyes from aqueous solutions using second order derivative spectrophotometric method (SODS) which was applied to resolve the overlap between the spectra of these dyes. The dependency of dyes removal efficiency in binary solutions was examined and optimized toward various parameters including initial dye concentration, pH of the solution, adsorbent dosage and ultrasonic contact time using central composite design (CCD) under response surface methodology (RSM) approach. The optimized experimental conditions were set as pH 7.78, contact time 5 min, initial MB concentration 22 mg L- 1, initial MG concentration 12 mg L- 1 and adsorbent dosage 0.0055 g. The equilibrium data was fitted to isotherm models such as Langmuir, Freundlich and Tempkin and the results revealed the suitability of the Langmuir model. The maximum adsorption capacity of 666.67 and 153.85 mg g- 1 was obtained for MB and MG removal respectively. Kinetics data fitting to pseudo-first order, pseudo-second order and Elovich models confirmed the applicability of pseudo-second order kinetic model for description of the mechanism and adsorption rate. Dye-loaded MIL-68(Al) can be easily regenerated using methanol and applied for three frequent sorption/desorption cycles with high performance. The impact of ionic strength on removal percentage of both dyes in binary mixture was studied by using NaCl and KCl soluble salts at different concentrations. According to our findings, only small dosage of the proposed MOF is considerably capable to remove large amounts of dyes at room temperature and in very short time that is a big advantage of MIL-68(Al) as a promising adsorbent for adsorptive removal processes.

  9. Competitive removal of hazardous dyes from aqueous solution by MIL-68(Al): Derivative spectrophotometric method and response surface methodology approach.

    PubMed

    Tehrani, Mahnaz Saghanejhad; Zare-Dorabei, Rouholah

    2016-05-01

    MIL-68(Al) as a metal-organic framework (MOF) was synthesized and characterized by different techniques such as SEM, BET, FTIR, and XRD analysis. This material was then applied for simulations removal of malachite green (MG) and methylene blue (MB) dyes from aqueous solutions using second order derivative spectrophotometric method (SODS) which was applied to resolve the overlap between the spectra of these dyes. The dependency of dyes removal efficiency in binary solutions was examined and optimized toward various parameters including initial dye concentration, pH of the solution, adsorbent dosage and ultrasonic contact time using central composite design (CCD) under response surface methodology (RSM) approach. The optimized experimental conditions were set as pH7.78, contact time 5min, initial MB concentration 22mgL(-1), initial MG concentration 12mgL(-1) and adsorbent dosage 0.0055g. The equilibrium data was fitted to isotherm models such as Langmuir, Freundlich and Tempkin and the results revealed the suitability of the Langmuir model. The maximum adsorption capacity of 666.67 and 153.85mgg(-1) was obtained for MB and MG removal respectively. Kinetics data fitting to pseudo-first order, pseudo-second order and Elovich models confirmed the applicability of pseudo-second order kinetic model for description of the mechanism and adsorption rate. Dye-loaded MIL-68(Al) can be easily regenerated using methanol and applied for three frequent sorption/desorption cycles with high performance. The impact of ionic strength on removal percentage of both dyes in binary mixture was studied by using NaCl and KCl soluble salts at different concentrations. According to our findings, only small dosage of the proposed MOF is considerably capable to remove large amounts of dyes at room temperature and in very short time that is a big advantage of MIL-68(Al) as a promising adsorbent for adsorptive removal processes. PMID:26890205

  10. A method for normalization of X-ray absorption spectra

    SciTech Connect

    Weng, T.-C.; Waldo, G.S.; Penner-Hahn, J.E.

    2010-07-20

    Accurate normalization of X-ray absorption data is essential for quantitative analysis of near-edge features. A method, implemented as the program MBACK, to normalize X-ray absorption data to tabulated mass absorption coefficients is described. Comparison of conventional normalization methods with MBACK demonstrates that the new normalization method is not sensitive to the shape of the background function, thus allowing accurate comparison of data collected in transmission mode with data collected using fluorescence ion chambers or solid-state fluorescence detectors. The new method is shown to have better reliability and consistency and smaller errors than conventional normalization methods. The sensitivity of the new normalization method is illustrated by analysis of data collected during an equilibrium titration.

  11. A simple, reproducible and sensitive spectrophotometric method to estimate microalgal lipids.

    PubMed

    Chen, Yimin; Vaidyanathan, Seetharaman

    2012-04-29

    Quantification of total lipids is a necessity for any study of lipid production by microalgae, especially given the current interest in microalgal carbon capture and biofuels. In this study, we employed a simple yet sensitive method to indirectly measure the lipids in microalgae by measuring the fatty acids (FA) after saponification. The fatty acids were reacted with triethanolamine-copper salts (TEA-Cu) and the ternary TEA-Cu-FA complex was detected at 260 nm using a UV-visible spectrometer without any colour developer. The results showed that this method could be used to analyse low levels of lipids in the range of nano-moles from as little as 1 mL of microalgal culture. Furthermore, the structure of the TEA-Cu-FA complex and related reaction process are proposed to better understand this assay. There is no special instrument required and the method is very reproducible. To the best of our knowledge, this is the first report of the use of UV absorbance of copper salts with FA as a method to estimate lipids in algal cultures. It will pave the way for a more convenient assay of lipids in microalgae and can readily be expanded for estimating lipids in other biological systems.

  12. Simultaneous spectrophotometric determination of four metals by two kinds of partial least squares methods

    NASA Astrophysics Data System (ADS)

    Gao, Ling; Ren, Shouxin

    2005-10-01

    Simultaneous determination of Ni(II), Cd(II), Cu(II) and Zn(II) was studied by two methods, kernel partial least squares (KPLS) and wavelet packet transform partial least squares (WPTPLS), with xylenol orange and cetyltrimethyl ammonium bromide as reagents in the medium pH = 9.22 borax-hydrochloric acid buffer solution. Two programs, PKPLS and PWPTPLS, were designed to perform the calculations. Data reduction was performed using kernel matrices and wavelet packet transform, respectively. In the KPLS method, the size of the kernel matrix is only dependent on the number of samples, thus the method was suitable for the data matrix with many wavelengths and fewer samples. Wavelet packet representations of signals provide a local time-frequency description, thus in the wavelet packet domain, the quality of the noise removal can be improved. In the WPTPLS by optimization, wavelet function and decomposition level were selected as Daubeches 12 and 5, respectively. Experimental results showed both methods to be successful even where there was severe overlap of spectra.

  13. Simultaneous determination of calcium and magnesium in water using artificial neural network spectro-photometric method

    NASA Astrophysics Data System (ADS)

    Ji, Hongwei; Li, Shuang; Xin, Huizhen; Cao, Hengxia

    2010-09-01

    A new analytical method using Back-Propagation (BP) artificial neural networks and spectrophotometry for simultaneous determination of calcium and magnesium in tap water, the Yellow River water and seawater is established. By condition experiment, the optimum analytical conditions for calcium, magnesium and Arsenazo (III) color reactions are obtained. Levenberg-Marquart (L-M) algorithm is used for calculation in BP neural network. The topological structure of three-layer BP ANN network architecture is chosen as 11-10-2 (nodes). The initial value of gradient coefficient μ is fixed at 0.001 and the increase factor and reduction factor of μ take the default values of the system. The data are processed by computers with our own programs written in MATLAB 7.0. The relative standard deviations of the calculated results for calcium and magnesium are 2.31% and 2.14%, respectively. The results of standard addition method show that the recoveries of calcium and magnesium are 103.6% and 100.8% in the tap water, 103.2% and 96.6% in the Yellow River water (Lijin district of Shandong Province), and 98.8%-103.3% and 98.43%-103.4% in seawater from Jiaozhou Bay of Qingdao. It is found that 14 common cations and anions do not interfere with the determination of calcium and magnesium under the optimum experimental conditions. The comparative experiments do not show any obvious difference between the results obtained by this new method and those obtained by the classical complexometric titration method in seawater medium. This method exhibits good reproducibility and high accuracy in the determination of calcium and magnesium and can be used for the simultaneous determination of Ca2+ and Mg2+ in tap water and natural water.

  14. ABSORPTION METHOD FOR SEPARATING METAL CATIONS

    DOEpatents

    Tompkins, E.R.; Parker, G.W.

    1959-03-10

    An improved method is presented for the chromatographic separation of fission products wherein a substantial reduction in liquid volume is obtained. The process consists in contacting a solution containing fission products with a body of ion-exchange adsorbent to effect adsorption of fission product cations. The loaded exchange resin is then contacted with a small volume of a carboxylic acid eluant, thereby recovering the fission products. The fission product carrying eluate is acidified without increasing its volume to the volume of the original solution, and the acidified eluate is then used as a feed solution for a smaller body of ion-exchange resin effecting readsorption of the fission product cations.

  15. Derivative Spectrophotometric Method for Estimation of Antiretroviral Drugs in Fixed Dose Combinations

    PubMed Central

    P.B., Mohite; R.B., Pandhare; S.G., Khanage

    2012-01-01

    Purpose: Lamivudine is cytosine and zidovudine is cytidine and is used as an antiretroviral agents. Both drugs are available in tablet dosage forms with a dose of 150 mg for LAM and 300 mg ZID respectively. Method: The method employed is based on first order derivative spectroscopy. Wavelengths 279 nm and 300 nm were selected for the estimation of the Lamovudine and Zidovudine respectively by taking the first order derivative spectra. The conc. of both drugs was determined by proposed method. The results of analysis have been validated statistically and by recovery studies as per ICH guidelines. Result: Both the drugs obey Beer’s law in the concentration range 10-50 μg mL-1,for LAM and ZID; with regression 0.9998 and 0.9999, intercept – 0.0677 and – 0.0043 and slope 0.0457 and 0.0391 for LAM and ZID, respectively.The accuracy and reproducibility results are close to 100% with 2% RSD. Conclusion: A simple, accurate, precise, sensitive and economical procedures for simultaneous estimation of Lamovudine and Zidovudine in tablet dosage form have been developed. PMID:24312779

  16. The Spectrophotometric Method of Determining the Transmission of Solar Energy in Salt Gradient Solar Ponds

    NASA Technical Reports Server (NTRS)

    Giulianelli, J.

    1984-01-01

    In order to predict the thermal efficiency of a solar pond it is necessary to know total average solar energy reaching the storage layer. One method for determining this energy for water containing dissolved colored species is based upon spectral transmission measurements using a laboratory spectrophotometer. This method is examined and some of the theoretical ground work needed to discuss the measurement of transmission of light water. Results of in situ irradiance measurements from oceanography research are presented and the difficulties inherent in extrapolating laboratory data obtained with ten centimeter cells to real three dimensional pond situations is discussed. Particular emphasis is put on the need to account for molecular and particulate scattering in measurements done on low absorbing solutions. Despite these considerations it is expected that attenuation calculations based upon careful measurements using a dual beam spectrophotometer technique combined with known attenuation coefficients will be useful in solar pond modeling and monitoring for color buildup. Preliminary results using the CSM method are presented.

  17. The spectrophotometric method of determining the transmission of solar energy in salt gradient solar ponds

    NASA Astrophysics Data System (ADS)

    Giulianelli, J.

    1984-09-01

    In order to predict the thermal efficiency of a solar pond it is necessary to know total average solar energy reaching the storage layer. One method for determining this energy for water containing dissolved colored species is based upon spectral transmission measurements using a laboratory spectrophotometer. This method is examined and some of the theoretical ground work needed to discuss the measurement of transmission of light water. Results of in situ irradiance measurements from oceanography research are presented and the difficulties inherent in extrapolating laboratory data obtained with ten centimeter cells to real three dimensional pond situations is discussed. Particular emphasis is put on the need to account for molecular and particulate scattering in measurements done on low absorbing solutions. Despite these considerations it is expected that attenuation calculations based upon careful measurements using a dual beam spectrophotometer technique combined with known attenuation coefficients will be useful in solar pond modeling and monitoring for color buildup. Preliminary results using the CSM method are presented.

  18. Spectrophotometric and TLC-densitometric methods for the simultaneous determination of Ezetimibe and Atorvastatin calcium.

    PubMed

    Baghdady, Yehia Z; Al-Ghobashy, Medhat A; Abdel-Aleem, Abdel-Aziz E; Weshahy, Soheir A

    2013-01-01

    Three sensitive methods were developed for simultaneous determination of Ezetimibe (EZB) and Atorvastatin calcium (ATVC) in binary mixtures. First derivative (D(1)) spectrophotometry was employed for simultaneous determination of EZB (223.8 nm) and ATVC (233.0 nm) with a mean percentage recovery of 100.23 ± 1.62 and 99.58 ± 0.84, respectively. Linearity ranges were 10.00-30.00 μg mL(-1) and 10.00-35.00 μg mL(-1), respectively. Isosbestic point (IS) spectrophotometry, in conjunction with second derivative (D(2)) spectrophotometry was employed for analysis of the same mixture. Total concentration was determined at IS, 224.6 nm and 238.6 nm over a concentration range of 10.00-35.00 μg mL(-1) and 5.00-30.00 μg mL(-1), respectively. ATVC concentration was determined using D(2) at 313.0 nm (10.00-35.00 μg mL(-1)) with a mean recovery percentage of 99.72 ± 1.36, while EZB was determined mathematically at 224.6 nm (99.75 ± 1.43) and 238.6 nm (99.80 ± 0.95). TLC-densitometry was employed for the determination of the same mixture; 0.10-0.60 μg band(-1) for both drugs. Separation was carried out on silica gel plates using diethyl ether-ethyl acetate (7:3 v/v). EZB and ATVC were resolved with Rf values of 0.78 and 0.13. Determination was carried out at 254.0 nm with a mean percentage recovery of 99.77 ± 1.30 and 99.86 ± 0.97, respectively. Methods were validated according to ICH guidelines and successfully applied for analysis of bulk powder and pharmaceutical formulations. Results were statistically compared to a reported method and no significant difference was noticed regarding accuracy and precision.

  19. Spectrophotometric determination of copper(II) with o-bromophenylfluorone.

    PubMed

    Yamaguchi, Takako; Samma, Megumi; Kamino, Shinichiro; Matsushita, Momoka; Hashimoto, Tomoyuki; Fujita, Yoshikazu

    2009-12-01

    A simple, reliable and sensitive spectrophotometric method for the determination of copper(II) was established with o-bromophenylfluorone (OBPF), a novel chemical probe, in the presence of poly(N-vinylpyrrolidone). Beer's law was obeyed in the range of 8-160 ng ml(-1), with an apparent molar absorptivity at 570 nm, the relative standard deviation being 3.64 x 10(5) dm3 mol(-1) cm(-1) and 0.72% (n = 5). This method was applied to the recovery tests of copper(II) in human urine, bovine serum and tap water; the results were satisfactory.

  20. Novel spectrophotometric determination of chloramphenicol and dexamethasone in the presence of non labeled interfering substances using univariate methods and multivariate regression model updating

    NASA Astrophysics Data System (ADS)

    Hegazy, Maha A.; Lotfy, Hayam M.; Rezk, Mamdouh R.; Omran, Yasmin Rostom

    2015-04-01

    Smart and novel spectrophotometric and chemometric methods have been developed and validated for the simultaneous determination of a binary mixture of chloramphenicol (CPL) and dexamethasone sodium phosphate (DSP) in presence of interfering substances without prior separation. The first method depends upon derivative subtraction coupled with constant multiplication. The second one is ratio difference method at optimum wavelengths which were selected after applying derivative transformation method via multiplying by a decoding spectrum in order to cancel the contribution of non labeled interfering substances. The third method relies on partial least squares with regression model updating. They are so simple that they do not require any preliminary separation steps. Accuracy, precision and linearity ranges of these methods were determined. Moreover, specificity was assessed by analyzing synthetic mixtures of both drugs. The proposed methods were successfully applied for analysis of both drugs in their pharmaceutical formulation. The obtained results have been statistically compared to that of an official spectrophotometric method to give a conclusion that there is no significant difference between the proposed methods and the official ones with respect to accuracy and precision.

  1. Novel spectrophotometric determination of chloramphenicol and dexamethasone in the presence of non labeled interfering substances using univariate methods and multivariate regression model updating.

    PubMed

    Hegazy, Maha A; Lotfy, Hayam M; Rezk, Mamdouh R; Omran, Yasmin Rostom

    2015-04-01

    Smart and novel spectrophotometric and chemometric methods have been developed and validated for the simultaneous determination of a binary mixture of chloramphenicol (CPL) and dexamethasone sodium phosphate (DSP) in presence of interfering substances without prior separation. The first method depends upon derivative subtraction coupled with constant multiplication. The second one is ratio difference method at optimum wavelengths which were selected after applying derivative transformation method via multiplying by a decoding spectrum in order to cancel the contribution of non labeled interfering substances. The third method relies on partial least squares with regression model updating. They are so simple that they do not require any preliminary separation steps. Accuracy, precision and linearity ranges of these methods were determined. Moreover, specificity was assessed by analyzing synthetic mixtures of both drugs. The proposed methods were successfully applied for analysis of both drugs in their pharmaceutical formulation. The obtained results have been statistically compared to that of an official spectrophotometric method to give a conclusion that there is no significant difference between the proposed methods and the official ones with respect to accuracy and precision.

  2. A reliable method for spectrophotometric determination of glycine betaine in cell suspension and other systems.

    PubMed

    Valadez-Bustos, Ma Guadalupe; Aguado-Santacruz, Gerardo Armando; Tiessen-Favier, Axel; Robledo-Paz, Alejandrina; Muñoz-Orozco, Abel; Rascón-Cruz, Quintin; Santacruz-Varela, Amalio

    2016-04-01

    Glycine betaine is a quaternary ammonium compound that accumulates in a large variety of species in response to different types of stress. Glycine betaine counteracts adverse effects caused by abiotic factors, preventing the denaturation and inactivation of proteins. Thus, its determination is important, particularly for scientists focused on relating structural, biochemical, physiological, and/or molecular responses to plant water status. In the current work, we optimized the periodide technique for the determination of glycine betaine levels. This modification permitted large numbers of samples taken from a chlorophyllic cell line of the grass Bouteloua gracilis to be analyzed. Growth kinetics were assessed using the chlorophyllic suspension to determine glycine betaine levels in control (no stress) cells and cells osmotically stressed with 14 or 21% polyethylene glycol 8000. After glycine extraction, different wavelengths and reading times were evaluated in a spectrophotometer to determine the optimal quantification conditions for this osmolyte. Optimal results were obtained when readings were taken at a wavelength of 290 nm at 48 h after dissolving glycine betaine crystals in dichloroethane. We expect this modification to provide a simple, rapid, reliable, and cheap method for glycine betaine determination in plant samples and cell suspension cultures.

  3. Spectrophotometric Method for Differentiation of Human Skin Melanoma. II. Diagnostic Characteristics

    NASA Astrophysics Data System (ADS)

    Petruk, V. G.; Ivanov, A. P.; Kvaternyuk, S. M.; Barunb, V. V.

    2016-05-01

    Experimental data on the spectral dependences of the optical diffuse reflection coefficient for skin from different people with melanoma or nevus are presented in the form of the probability density of the diffuse reflection coefficient for the corresponding pigmented lesions. We propose a noninvasive technique for differentiating between malignant and benign tumors, based on measuring the diffuse reflection coefficient for a specific patient and comparing the value obtained with a pre-set threshold. If the experimental result is below the threshold, then it is concluded that the person has melanoma; otherwise, no melanoma is present. As an example, we consider the wavelength 870 nm. We determine the risk of malignant transformation of a nevus (its transition to melanoma) for different measured diffuse reflection coefficients. We have studied the errors in the method, its operating characteristics and probability characteristics as the threshold diffuse reflection coefficient is varied. We find that the diagnostic confidence, sensitivity, specificity, and effectiveness (accuracy) parameters are maximum (>0.82) for a threshold of 0.45-0.47. The operating characteristics for the proposed technique exceed the corresponding parameters for other familiar optical approaches to melanoma diagnosis. Its distinguishing feature is operation at only one wavelength, and consequently implementation of the experimental technique is simplified and made less expensive.

  4. A simple and sensitive spectrophotometric method for the determination of trace amounts of nitrite in environmental and biological samples using 4-amino-5-hydroxynaphthalene-2,7-disulphonic acid monosodium salt

    NASA Astrophysics Data System (ADS)

    Nagaraja, Padmarajaiah; Al-Tayar, Naef Ghllab S.; Shivakumar, Anantharaman; Shrestha, Ashwine K.; Gowda, Avinash K.

    2010-05-01

    A very simple, sensitive, fairly selective and rapid spectrophotometric method for the determination of trace amounts of nitrite has been described. This method is based on the diazotized intramolecular coupling of electrophilic diazonium cation with the phenolic group of 4-amino-5-hydroxynaphthalene-2,7-disulphonic acid monosodium salt (AHNDMS) in a phosphate buffer solution of pH 7.5. The cyclic product has a purple color with maximum absorbance at 560 nm and is stable for 6 h. Optimum reaction conditions and other important analytical parameters for the maximum color development were established. Beer's law was found to obey for nitrite in the concentration range of 0.1-1.6 μg ml -1 with molar absorptivity of 2.6 × 10 4 l mol -1 cm -1 and Sandell's sensitivity of 0.0075 μg ml -1. The effect of interfering ions on the determination is described. The recommended method was applied for the determination of nitrite in different water, soil and human saliva samples. The performance of the recommended method was evaluated in terms of Student's t-test and variance ratio F-test, which indicated the significance of proposed method over the reference method.

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

    NASA Astrophysics Data System (ADS)

    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.

  6. 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

    NASA Astrophysics Data System (ADS)

    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.

  7. A rapid spectrophotometric determination of persulfate anion in ISCO.

    PubMed

    Liang, Chenju; Huang, Chiu-Fen; Mohanty, Nihar; Kurakalva, Rama Mohan

    2008-11-01

    Due to a gradual increase in the use of persulfate as an in situ chemical oxidation (ISCO) oxidant, a simple measurement of persulfate concentration is desirable to analyze persulfate distribution at designated time intervals on/off a site. Such a distribution helps evaluate efficacy of ISCO treatment at a site. This work proposes a spectrophotometric determination of persulfate based on modification of the iodometric titration method. The analysis of absorption spectra of a yellow color solution resulting from the reaction of persulfate and iodide in the presence of sodium bicarbonate reveals an absorbance at 352 nm, without significant interferences from the reagent matrix. The calibration graph was linear in the range of persulfate solution concentration of 0-70 mM at 352 nm. The proposed method is validated by the iodometric titration method. The solution pH was at near neutral and the presence of iron activator does not interfere with the absorption measurement. Also, analysis of persulfate in a groundwater sample using the proposed method indicates a good agreement with measurements by the titration method. This proposed spectrophotometric quantification of persulfate provides a simple and rapid method for evaluation of ISCO effectiveness at a remediation site.

  8. Spectrophotometric Methods for the Determination of Linagliptin in Binary Mixture with Metformin Hydrochloride and Simultaneous Determination of Linagliptin and Metformin Hydrochloride using High Performance Liquid Chromatography

    PubMed Central

    El-Bagary, Ramzia I.; Elkady, Ehab F.; Ayoub, Bassam M.

    2013-01-01

    Simple, accurate and precise Zero order, first derivative spectrophotometric and chromatographic methods have been developed and validated for the determination of linagliptin (LNG) and metformin HCl (MET). The zero order and first derivative spectrophotometric methods were used for the determination of LNG in the range of 5-30 μg mL−1 by measuring the absorbance at 299 nm and 311 respectively. Besides, a reversed-phase liquid chromatographic (RP-LC) method is described for the simultaneous determination of LNG and MET. Chromatographic separation was achieved on a Symmetry® Waters C18 column (150 mm × 4.6 mm, 5 μm). Isocratic elution based on potassium dihydrogen phosphate buffer pH (4.6) - methanol (30:70, v/v) at a flow rate of 1 mLmin−1 with UV detection at 260 nm was performed. Linearity, accuracy and precision were found to be acceptable over the concentration ranges of 0.125-4 μg mL−1 and 20-800 μg mL−1 for LNG and MET, respectively. The results were statistically compared using one-way analysis of variance (ANOVA). The optimized methods were validated and proved to be specific, robust, precise and accurate for the quality control of the drugs in their pharmaceutical preparation. PMID:23675288

  9. RECTIFIED ABSORPTION METHOD FOR THE SEPARATION OF HYDROGEN ISOTOPES

    DOEpatents

    Hunt, C.D.; Hanson, D.N.

    1961-10-17

    A method is described for separating and recovering heavy hydrogen isotopes from gaseous mixtures by multiple stage cyclic absorption and rectification from an approximate solvent. In particular, it is useful for recovering such isoteoes from ammonia feedstock streams containing nitrogen solvent. Modifications of the process ranging from isobaric to isothermal are provided. Certain impurities are tolerated, giving advantages over conventional fractional distillation processes. (AEC)

  10. Absorption-coefficient-determination method for particulate materials.

    PubMed

    Lindberg, J D; Douglass, R E; Garvey, D M

    1994-07-01

    A method is presented for determining the optical absorption coefficient, or the imaginary refractive index, of particulate material that has been collected from aerosols or hydrosols by means of filtration. The method, based on the Kubelka-Munk theory of diffuse reflectance, is nondestructive and requires no other knowledge of the sample than the amount present, the specific gravity, and an estimate of the real index of refraction. The theoretical development of the method is discussed along with an analysis of photometric and gravimetric errors. We test the method by comparing results obtained for powdered didymium glass with measurements made before the glass was crushed. An example of the method's application to the determination of the absorption coefficient of atmospheric dust at UV, visible, and near-IR wavelengths is also presented.

  11. Absorption-coefficient-determination method for particulate materials.

    PubMed

    Lindberg, J D; Douglass, R E; Garvey, D M

    1994-07-01

    A method is presented for determining the optical absorption coefficient, or the imaginary refractive index, of particulate material that has been collected from aerosols or hydrosols by means of filtration. The method, based on the Kubelka-Munk theory of diffuse reflectance, is nondestructive and requires no other knowledge of the sample than the amount present, the specific gravity, and an estimate of the real index of refraction. The theoretical development of the method is discussed along with an analysis of photometric and gravimetric errors. We test the method by comparing results obtained for powdered didymium glass with measurements made before the glass was crushed. An example of the method's application to the determination of the absorption coefficient of atmospheric dust at UV, visible, and near-IR wavelengths is also presented. PMID:20935789

  12. Extractive Spectrophotometric Methods for the Determination of Zolmitriptan in Bulk Drug and Pharmaceutical Formulation Using Bromocresol Green

    NASA Astrophysics Data System (ADS)

    Prashanth, K. N.; Swamy, N.; Basavaiah, K.

    2013-11-01

    Considering the basic property of zolmitriptan (ZMT) to generate ion-pairs with sulfonephthalein dyes two methods have been developed for its assay in bulk drug and dosage form. The first method (method A) is based on the formation of a colored ion-pair complex (1:1 drug:dye) of ZMT with bromocresol green (BCG) at pH 4.20 ± 0.01 and extraction of the complex into chloroform followed by measurement of the yellow ion-pair complex at 435 nm. In the second method (method B), the drug-dye ion-pair complex was treated with ethanolic potassium hydroxide in ethanolic medium and the resulting base form of the dye was measured at 630 nm. Beer's law was obeyed in the concentration range of 0.8-18.0 and 0.08-1.4 μg/ml for method A and B, respectively, and the corresponding molar absorptivity values were 1.50ṡ104 and 1.52ṡ105 l/(molṡcm). The Sandell sensitivity values were 0.0191 and 0.0019 μg/cm2 for method A and method B, respectively. The stoichiometry of the ion-pair complex formed between the drug and dye (1:1) was determined by Job's continuous variation method and the stability constant of the complex was also calculated. The proposed method was successfully extended to dosage form (tablets).

  13. Method and apparatus for aerosol particle absorption spectroscopy

    DOEpatents

    Campillo, Anthony J.; Lin, Horn-Bond

    1983-11-15

    A method and apparatus for determining the absorption spectra, and other properties, of aerosol particles. A heating beam source provides a beam of electromagnetic energy which is scanned through the region of the spectrum which is of interest. Particles exposed to the heating beam which have absorption bands within the band width of the heating beam absorb energy from the beam. The particles are also illuminated by light of a wave length such that the light is scattered by the particles. The absorption spectra of the particles can thus be determined from an analysis of the scattered light since the absorption of energy by the particles will affect the way the light is scattered. Preferably the heating beam is modulated to simplify the analysis of the scattered light. In one embodiment the heating beam is intensity modulated so that the scattered light will also be intensity modulated when the particles absorb energy. In another embodiment the heating beam passes through an interferometer and the scattered light reflects the Fourier Transform of the absorption spectra.

  14. Method for processing seismic data to identify anomalous absorption zones

    DOEpatents

    Taner, M. Turhan

    2006-01-03

    A method is disclosed for identifying zones anomalously absorptive of seismic energy. The method includes jointly time-frequency decomposing seismic traces, low frequency bandpass filtering the decomposed traces to determine a general trend of mean frequency and bandwidth of the seismic traces, and high frequency bandpass filtering the decomposed traces to determine local variations in the mean frequency and bandwidth of the seismic traces. Anomalous zones are determined where there is difference between the general trend and the local variations.

  15. Comparison of a silver nanoparticle-based method and the modified spectrophotometric methods for assessing antioxidant capacity of rapeseed varieties.

    PubMed

    Szydłowska-Czerniak, Aleksandra; Tułodziecka, Agnieszka

    2013-12-01

    The antioxidant capacity of 15 rapeseed varieties was determined by the proposed silver nanoparticle-based (AgNP) method and three modified assays: ferric reducing antioxidant power (FRAP), 2,2'-diphenyl-1-picrylhydrazyl (DPPH) and Folin-Ciocalteu reducing capacity (FC). The average antioxidant capacities of the studied rapeseed cultivars ranged between 5261-9462, 3708-7112, 18864-31245 and 5816-9937 μmol sinapic acid (SA)/100g for AgNP, FRAP, DPPH and FC methods, respectively. There are significant, positive correlations between antioxidant capacities of the studied rapeseed cultivars determined by four analytical methods (r=0.5971-0.9149, p<0.05). The comparable precision for the proposed AgNP method (RSD=1.4-4.4%) and the modified FRAP, DPPH and FC methods (RSD=1.0-4.4%, 0.7-2.1% and 0.8-3.6%, respectively), demonstrate the benefit of the AgNP method in the routine analysis of antioxidant capacity of rapeseed cultivars. The principal component analysis (PCA) and hierarchical cluster analysis (HCA) were used for discrimination the quality of the studied rapeseed varieties based on their antioxidant potential determined by different analytical methods. Three main groups were identified by HCA, while the classification and characterisation of rapeseed varieties within each of these groups were obtained from PCA. The chemometric analyses demonstrated that, rapeseed variety S13 had the highest antioxidant capacity, thus this cultivar should be considered as the richest source of natural antioxidants.

  16. Development and validation of a rapid stability indicating HPLC-method using monolithic stationary phase and two spectrophotometric methods for determination of antihistaminic acrivastine in capsules.

    PubMed

    Gouda, Ayman A; Hashem, Hisham; Jira, Thomas

    2014-09-15

    Simple, rapid and accurate high performance liquid chromatographic (HPLC) and spectrophotometric methods are described for determination of antihistaminic acrivastine in capsules. The first method (method A) is based on accurate, sensitive and stability indicating chromatographic separation method. Chromolith® Performance RP-18e column, a relatively new packing material consisting of monolithic rods of highly porous silica, was used as stationary phase applying isocratic binary mobile phase of ACN and 25 mM NaH2PO4 pH 4.0 in the ratio of 22.5:77.5 at flow rate of 5.0 mL/min and 40°C. A diode array detector was used at 254 nm for detection. The elution time of acrivastine was found to be 2.080±0.032. The second and third methods (methods B and C) are based on the oxidation of acrivastine with excess N-bromosuccinimide (NBS) and determination of the unconsumed NBS with, metol-sulphanilic acid (λmax: 520 nm) or amaranth dye (λmax: 530 nm). The reacted oxidant corresponds to the drug content. Beer's law is obeyed over the concentration range 1.563-50, 2.0-20 and 1.0-10 μg mL(-1) for methods A, B and C, respectively. The limits of detection and quantitation were 0.40, 0.292 and 0.113 μg mL(-1) and 0.782, 0.973 and 0.376 μg mL(-1) for methods A, B and C, respectively. The HPLC method was validated for system suitability, linearity, precision, limits of detection and quantitation, specificity, stability and robustness. Stability tests were done through exposure of the analyte solution for four different stress conditions and the results indicate no interference of degradants with HPLC-method. The proposed methods was favorably applied for determination of acrivastine in capsules formulation. Statistical comparison of the obtained results from the analysis of the studied drug to those of the reported method using t- and F-tests showed no significant difference between them.

  17. Validated spectrophotometric methods for the determination of amlodipine besylate in drug formulations using 2,3-dichloro 5,6-dicyano 1,4-benzoquinone and ascorbic acid.

    PubMed

    Rahman, Nafisur; Nasrul Hoda, Md

    2003-02-26

    Two simple and sensitive spectrophotometric methods have been proposed for the determination of amlodipine besylate either in pure form or in pharmaceutical formulations. The first method is based on the charge transfer complexation reaction of the drug with 2,3-dichloro 5,6-dicyano 1,4-benzoquinone (DDQ) to give coloured product having maximum absorbance at 580 nm. The second procedure depends on the measurement of purple red colour produced by the interaction of drug with ascorbic acid in N,N-dimethylformamide medium (DMF) which absorbed maximally at 530 nm. Under the optimized experimental conditions, Beer's law was obeyed in the concentration ranges of 1-125 and 10-140 microg ml(-1) with DDQ and ascorbic acid, respectively. Both the methods were applied successfully for the analysis of amlodipine besylate in dosage forms. Results of analyses were validated statistically and through recovery studies.

  18. Method for making a photodetector with enhanced light absorption

    DOEpatents

    Kane, James

    1987-05-05

    A photodetector including a light transmissive electrically conducting layer having a textured surface with a semiconductor body thereon. This layer traps incident light thereby enhancing the absorption of light by the semiconductor body. A photodetector comprising a textured light transmissive electrically conducting layer of SnO.sub.2 and a body of hydrogenated amorphous silicon has a conversion efficiency about fifty percent greater than that of comparative cells. The invention also includes a method of fabricating the photodetector of the invention.

  19. Disk scattering and absorption by an improved computational method.

    PubMed

    Willis, T M; Weil, H

    1987-09-15

    A computer method for determining the scattering, absorption, and internal field structure of thin flat disks of arbitrary refractive index is described. The code is shown to be accurate for all angles of incidence for radii up to at least two free space wavelengths and for media ranging from pure dielectric to highly conductive ones. The accuracy of the method is assessed by comparison with published experimental data and with results computed by other methods. The applicability of this technique for analyzing clouds of disk-shaped aerosols is also discussed.

  20. Determination of the relative contribution of quercetin and its glucosides to the antioxidant capacity of onion by cyclic voltammetry and spectrophotometric methods.

    PubMed

    Zielinska, Danuta; Wiczkowski, Wieslaw; Piskula, Mariusz Konrad

    2008-05-28

    This paper describes the use of cyclic voltammetry (CV), spectrophotometric methods [Trolox equivalent antioxidant capacity (TEAC), peroxyl radical trapping capacity (PRTC), DPPH radical scavenging activity (RSA), and Folin-Ciocalteu reagent (FCR) reducing capacity], and photochemiluminescence (PCL) for the measurement of the antioxidant capacity of onion var. Sochaczewska and var. Szalotka. The antioxidant and reducing activity of the dominant onion flavonoids quercetin (Q), quercetin-3- O-beta-glucoside (Q3G), quercetin-4'- O-beta-glucoside (Q4'G), and quercetin-3,4'-di- O-beta-glucoside (Q3,4'G) were determined by spectrophotometric (TEAC and PRTC) and CV methods, respectively. The contribution of quercetin and its glucosides to the antioxidant capacity of onion was calculated in consequence of the qualitative and quantitative analysis of onion flavonoids by high-performance liquid chromatography-ultraviolet-mass spectrometry. The dominant forms of quercetin in the onion var. Sochaczewska and Szalotka included Q4'G (61 and 54%), Q3,4'G (37 and 44%), Q3G (1.4 and 1.1%), and free quercetin (1.1 and 0.7%), respectively. The CV experiment showed the highest reducing activity of Q while Q3G, Q4'G, and Q3,4'G exhibited about 68, 51, and 30% of the reducing power noted for Q. The order of the reducing activity of onion flavonoids was confirmed by their free radical scavenging activity and evaluated by TEAC and PRTC assays as follows: Q > Q3G > Q4'G > Q3,4'G. The Q4'G and Q3,4'G showed poor antioxidant activity under both applied spectrophotometric assays but still exhibited reducing activity based on CV experiments. The reducing capacity of onions determined by CV method was twice higher than the antioxidant capacity formed by water-soluble compounds (ACW) evaluated by PCL, and it was about 50% higher than PRTC and DPPH RSA results and the converted FCR reducing capacity. In contrast, the reducing capacity of onions determined by the CV method was 3-fold and about four

  1. A new spectrophotometric method for determination of EDTA in water using its complex with Mn(III).

    PubMed

    Andrade, Carlos Eduardo O; Oliveira, André F; Neves, Antônio A; Queiroz, Maria Eliana L R

    2016-11-01

    EDTA is an important ligand used in many industrial products as well as in agriculture, where it is employed to assist in phytoextraction procedures and the absorption of nutrients by plants. Due to its intensive use and recalcitrance, it is now considered an emerging pollutant in water, so there is great interest in techniques suitable for its monitoring. This work proposes a method based on formation of the Mn(III)-EDTA complex after oxidation of the Mn(II)-EDTA complex by PbO2 immobilized on cyanoacrylate spheres. A design of experiments (DOE) based on the Doehlert matrix was used to determine the optimum conditions of the method, and the influence of the variables was evaluated using a multiple linear regression (MLR) model. The optimized method presented a linear response in the range from 0.77 to 100.0μmolL(-1), with analytical sensitivity of 7.7×10(3)Lmol(-1), a coefficient of determination of 0.999, and a limit of detection of 0.23μmolL(-1). The method was applied using samples fortified at different concentration levels, and the recoveries achieved were between 97.0 and 104.9%. PMID:27305647

  2. A new spectrophotometric method for determination of EDTA in water using its complex with Mn(III)

    NASA Astrophysics Data System (ADS)

    Andrade, Carlos Eduardo O.; Oliveira, André F.; Neves, Antônio A.; Queiroz, Maria Eliana L. R.

    2016-11-01

    EDTA is an important ligand used in many industrial products as well as in agriculture, where it is employed to assist in phytoextraction procedures and the absorption of nutrients by plants. Due to its intensive use and recalcitrance, it is now considered an emerging pollutant in water, so there is great interest in techniques suitable for its monitoring. This work proposes a method based on formation of the Mn(III)-EDTA complex after oxidation of the Mn(II)-EDTA complex by PbO2 immobilized on cyanoacrylate spheres. A design of experiments (DOE) based on the Doehlert matrix was used to determine the optimum conditions of the method, and the influence of the variables was evaluated using a multiple linear regression (MLR) model. The optimized method presented a linear response in the range from 0.77 to 100.0 μmol L- 1, with analytical sensitivity of 7.7 × 103 L mol- 1, a coefficient of determination of 0.999, and a limit of detection of 0.23 μmol L- 1. The method was applied using samples fortified at different concentration levels, and the recoveries achieved were between 97.0 and 104.9%.

  3. Selective and sensitive spectrophotometric method for the determination of trace amounts of zirconium in environmental and biological samples using 4-chloro-N-(2,6-dimethylphenyl)-2-hydroxy-5-sulfamoylbenzamide

    NASA Astrophysics Data System (ADS)

    Al-Kady, Ahmed S.

    2012-11-01

    A simple, selective and sensitive spectrophotometric method for the determination of trace amounts of Zr(IV) in aqueous samples was performed, based on complexation reaction between Zr(IV) and 4-chloro-N-(2,6-dimethylphenyl)-2-hydroxy-5-sulfamoylbenzamide (xipamide). The important analytical parameters and their effects on the reported system were investigated. Zr(IV) react with xipamide in the ratio 1:1 in the pH range 8 to form a complex with an absorption maximum 333 nm. The apparent stability constant (log βn) and the free energy change (ΔG∗) of formation of the complex was calculated using the results of mole ratio and continuous variation methods. Beer's law was obeyed in the concentration range 0.2-3.6 μg/mL. For more accurate analysis, Ringbom optimum concentration range was found from 0.3 to 3.5 μg/mL. The molar absorptivity, Sandell sensitivity, detection and quantification limits were also calculated. Taking a constant concentration of Zr(IV) and determining its concentration in the presence of large number of foreign ions tested the effect of foreign ions. The practical applicability of the elaborated method was examined using for determination of mentioned ion in water samples, biological, plant leaves and soil samples where excellent agreements between reported and obtained results were achieved. The relative standard deviation (n = 6) were 0.195%. The precision and accuracy of the results were comparable via F and t test at the 95% confidence level.

  4. The development of spectrophotometric and electroanalytical methods for ascorbic acid and acetaminophen and their applications in the analysis of effervescent dosage forms.

    PubMed

    Săndulescu, R; Mirel, S; Oprean, R

    2000-08-01

    The electroanalytical study of ascorbic acid, acetaminophen and of several mixtures of these compounds in different ratios has been made by using a carbon paste electrode (CPE-graphite:solid paraffin 2:1) as working electrode and an Ag/AgCl reference electrode. The potential curves were recorded using different concentrations of ascorbic acid and acetaminophen by measuring samples between 10 and 50 microl. The oxidation reactions were studied in a potential range from -0.1 to +1.3 V with different sweep rates, at different current sensitivities, in stationary working conditions and stirring before each replicate. The oxidation of ascorbic acid occurs at +0.31 +/- 0.02 V and the oxidation of acetaminophen at +0.60 +/- 0.05 V; meanwhile, the current has a linear variation for the following concentration ranges: 10(-3)-10(-2) M for the ascorbic acid and 3 x 10(-6)-7.5 x 10(-3) M for acetaminophen (r2 = 0.999 for both ascorbic acid and acetaminophen). The mixtures of ascorbic acid and acetaminophen were made as follows: 1:1, 1:2, 1:3, 2:1, and 3:1. The studies revealed the alteration of the voltammograms processed according to the validation methodology. The best potential variation range for different current sensitivities, the influence of the sweep rate, of the solvent volume and of the pH were studied. The mutual interferences of the compounds in the mixtures and the electroactive compounds in the pharmaceutical dosage forms, especially effervescent ones, also made the object of the research. The same mixtures were studied using the direct spectrophotometric method that revealed a lot of spectral interferences. In order to solve this problem, an appropriate separation or an indirect spectrophotometric method (the apparent content curves method) were used. The spectrophotometric and voltammetric methods developed were used to determine ascorbic acid and acetaminophen in different dosage forms (vials, tablets, suppositories and effervescent dosage forms). The results

  5. Spectrophotometric catalogs and databases

    NASA Astrophysics Data System (ADS)

    Burnashev, V. I.; Burnasheva, B. A.

    2014-06-01

    An overview is given of different spectrophotometric catalogs, including a brief description of the applications of absolute spectrophotometry in evolutionary population synthesis. Observational data for different stars are given. A list of catalogs is presented, including those containing intrinsic energy distributions for stars of different temperatures and luminosities, spectrophotometric standards, extragalactic sources, and theoretically calculated spectra. A number of useful links and Internet resources are provided.

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

    NASA Astrophysics Data System (ADS)

    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.

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

    PubMed

    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. PMID:25062051

  8. Development of Simultaneous Derivative Spectrophotometric and HPLC Methods for Determination of 17-Beta-Estradiol and Drospirenone in Combined Dosage Form

    PubMed Central

    Aydoğmuş, Zeynep; Yılmaz, Ece Merve; Yörüsün, Sevgi; Akpınar, Samet

    2015-01-01

    Simple, rapid spectrophotometric, and reverse-phase high performance liquid chromatographic methods were developed for the concurrent analysis of 17-beta-estradiol (ESR) and drospirenone (DRS). The spectrophotometric method was based on the determination of first derivative spectra and determined ESR and DRS using the zero-crossing technique at 208 and 282 nm, respectively, in methanol. The linear range was 0.5–32.0 µg·mL−1 for DRS and 0.5–8.0 µg·mL−1 for EST. The limit of detection (LOD) values were 0.14 µg·mL−1 and 0.10 µg·mL−1 and limit of quantification (LOQ) values were 0.42 µg·mL−1 and 0.29 µg·mL−1 for ESR and DRS, respectively. The chromatographic method was based on the separation of both analytes on a C18 column with a mobile phase containing acetonitrile and water (70 : 30, v/v). Detection was performed with a UV-photodiode array detector at 279 nm. The linear range was 0.08–2.5 µg·mL−1 for DRS and 0.23–7.5 µg·mL−1 for EST. LOD values were 0.05 µg·mL−1 and 0.02 µg·mL−1 and LOQ values were 0.15 µg·mL−1 and 0.05 µg·mL−1 for ESR and DRS, respectively. These recommended methods have been applied for the simultaneous determination of ESR and DRS in their tablets. PMID:27347530

  9. Development of Simultaneous Derivative Spectrophotometric and HPLC Methods for Determination of 17-Beta-Estradiol and Drospirenone in Combined Dosage Form.

    PubMed

    Aydoğmuş, Zeynep; Yılmaz, Ece Merve; Yörüsün, Sevgi; Akpınar, Samet

    2015-01-01

    Simple, rapid spectrophotometric, and reverse-phase high performance liquid chromatographic methods were developed for the concurrent analysis of 17-beta-estradiol (ESR) and drospirenone (DRS). The spectrophotometric method was based on the determination of first derivative spectra and determined ESR and DRS using the zero-crossing technique at 208 and 282 nm, respectively, in methanol. The linear range was 0.5-32.0 µg·mL(-1) for DRS and 0.5-8.0 µg·mL(-1) for EST. The limit of detection (LOD) values were 0.14 µg·mL(-1) and 0.10 µg·mL(-1) and limit of quantification (LOQ) values were 0.42 µg·mL(-1) and 0.29 µg·mL(-1) for ESR and DRS, respectively. The chromatographic method was based on the separation of both analytes on a C18 column with a mobile phase containing acetonitrile and water (70 : 30, v/v). Detection was performed with a UV-photodiode array detector at 279 nm. The linear range was 0.08-2.5 µg·mL(-1) for DRS and 0.23-7.5 µg·mL(-1) for EST. LOD values were 0.05 µg·mL(-1) and 0.02 µg·mL(-1) and LOQ values were 0.15 µg·mL(-1) and 0.05 µg·mL(-1) for ESR and DRS, respectively. These recommended methods have been applied for the simultaneous determination of ESR and DRS in their tablets. PMID:27347530

  10. Spectrophotometric determination of diphenhydramine. HC1 in pharmaceutical preparations.

    PubMed

    Maghssoudi, R H; Fawzi, A B; Moosavi Meerkalaiee, M A

    1977-07-01

    A new spectrophotometric method has been developed for determining diphenhydramine. HC1, based on solvent extraction into chloroform of the complex formed with bromocresol green. The complex solution in chloroform showed maximum absorption at 415 nm and obeyed Beer's law over the concentration range of 3.0-12.0 microgram/ml. The molar absorptivity of the complex was 2.02 x 10(4). Complex formation and extraction was complete and quantitative over the pH range from 2 to 5. The ratio of diphenhydramine to bromocresol green was 1:1. Excipients, coloring matter, flavoring agents, and other substances likely to be present in diphenhydramine preparations do not interfere in the determination. Direct determinations in tablet, capsule, sirup, and lotion preparations were carried out satisfactorily, and the average recovery was 100 +/- 1.0%.

  11. Analytical method for promoting process capability of shock absorption steel.

    PubMed

    Sung, Wen-Pei; Shih, Ming-Hsiang; Chen, Kuen-Suan

    2003-01-01

    Mechanical properties and low cycle fatigue are two factors that must be considered in developing new type steel for shock absorption. Process capability and process control are significant factors in achieving the purpose of research and development programs. Often-used evaluation methods failed to measure process yield and process centering; so this paper uses Taguchi loss function as basis to establish an evaluation method and the steps for assessing the quality of mechanical properties and process control of an iron and steel manufacturer. The establishment of this method can serve the research and development and manufacturing industry and lay a foundation in enhancing its process control ability to select better manufacturing processes that are more reliable than decision making by using the other commonly used methods.

  12. Development and validation of a novel, simple, and accurate spectrophotometric method for the determination of lead in human serum.

    PubMed

    Shayesteh, Tavakol Heidari; Khajavi, Farzad; Khosroshahi, Abolfazl Ghafuri; Mahjub, Reza

    2016-01-01

    The determination of blood lead levels is the most useful indicator of the determination of the amount of lead that is absorbed by the human body. Various methods, like atomic absorption spectroscopy (AAS), have already been used for the detection of lead in biological fluid, but most of these methods are based on complicated, expensive, and highly instructed instruments. In this study, a simple and accurate spectroscopic method for the determination of lead has been developed and applied for the investigation of lead concentration in biological samples. In this study, a silica gel column was used to extract lead and eliminate interfering agents in human serum samples. The column was washed with deionized water. The pH was adjusted to the value of 8.2 using phosphate buffer, and then tartrate and cyanide solutions were added as masking agents. The lead content was extracted into the organic phase containing dithizone as a complexion reagent and the dithizone-Pb(II) complex was formed and approved by visible spectrophotometry at 538 nm. The recovery was found to be 84.6 %. In order to validate the method, a calibration curve involving the use of various concentration levels was calculated and proven to be linear in the range of 0.01-1.5 μg/ml, with an R (2) regression coefficient of 0.9968 by statistical analysis of linear model validation. The largest error % values were found to be -5.80 and +11.6 % for intra-day and inter-day measurements, respectively. The largest RSD % values were calculated to be 6.54 and 12.32 % for intra-day and inter-day measurements, respectively. Further, the limit of detection (LOD) was calculated to be 0.002 μg/ml. The developed method was applied to determine the lead content in the human serum of voluntary miners, and it has been proven that there is no statistically significant difference between the data provided from this novel method and the data obtained from previously studied AAS. PMID:26631397

  13. Development and validation of a novel, simple, and accurate spectrophotometric method for the determination of lead in human serum.

    PubMed

    Shayesteh, Tavakol Heidari; Khajavi, Farzad; Khosroshahi, Abolfazl Ghafuri; Mahjub, Reza

    2016-01-01

    The determination of blood lead levels is the most useful indicator of the determination of the amount of lead that is absorbed by the human body. Various methods, like atomic absorption spectroscopy (AAS), have already been used for the detection of lead in biological fluid, but most of these methods are based on complicated, expensive, and highly instructed instruments. In this study, a simple and accurate spectroscopic method for the determination of lead has been developed and applied for the investigation of lead concentration in biological samples. In this study, a silica gel column was used to extract lead and eliminate interfering agents in human serum samples. The column was washed with deionized water. The pH was adjusted to the value of 8.2 using phosphate buffer, and then tartrate and cyanide solutions were added as masking agents. The lead content was extracted into the organic phase containing dithizone as a complexion reagent and the dithizone-Pb(II) complex was formed and approved by visible spectrophotometry at 538 nm. The recovery was found to be 84.6 %. In order to validate the method, a calibration curve involving the use of various concentration levels was calculated and proven to be linear in the range of 0.01-1.5 μg/ml, with an R (2) regression coefficient of 0.9968 by statistical analysis of linear model validation. The largest error % values were found to be -5.80 and +11.6 % for intra-day and inter-day measurements, respectively. The largest RSD % values were calculated to be 6.54 and 12.32 % for intra-day and inter-day measurements, respectively. Further, the limit of detection (LOD) was calculated to be 0.002 μg/ml. The developed method was applied to determine the lead content in the human serum of voluntary miners, and it has been proven that there is no statistically significant difference between the data provided from this novel method and the data obtained from previously studied AAS.

  14. Absorption-emission optrode and methods of use thereof

    DOEpatents

    Hirschfeld, Tomas B.

    1990-01-01

    A method and apparatus for monitoring the physical and chemical properties of a sample fluid by measuring an optical signal generated by a fluorescent substance and modulated by an absorber substance. The emission band of the fluorescent substance overlaps the absorption band of the absorber substance, and the degree of overlap is dependent on the physical and chemical properties of the sample fluid. The fluorescent substance and absorber substance are immobilized on a substrate so that an effective number of molecules thereof are sufficiently close for resonant energy transfer to occur, thereby providing highly efficient modulation of the fluorescent emissions of the fluorescent substance by the absorber substance.

  15. Absorption-emission optrode and methods of use thereof

    DOEpatents

    Hirschfeld, T.B.

    1990-05-29

    A method and apparatus are described for monitoring the physical and chemical properties of a sample fluid by measuring an optical signal generated by a fluorescent substance and modulated by an absorber substance. The emission band of the fluorescent substance overlaps the absorption band of the absorber substance, and the degree of overlap is dependent on the physical and chemical properties of the sample fluid. The fluorescent substance and absorber substance are immobilized on a substrate so that an effective number of molecules thereof are sufficiently close for resonant energy transfer to occur, thereby providing highly efficient modulation of the fluorescent emissions of the fluorescent substance by the absorber substance. 4 figs.

  16. Spectrophotometric determination of oxiconazole in topical lotion using methyl orange.

    PubMed

    Milano, Julie; Cardoso, Simone Gonçalves

    2005-04-01

    A spectrophotometric method is described for the determination of oxiconazole in raw material and in topical lotion. This method is based on the reaction of the oxiconazole with methyl orange in buffered aqueous solution of citric acid at pH 2.3. The chromogen, being extractable with dichloromethane, could be measured quantitatively with maximum absorption at 427 nm. The Lambert-Beer law was obeyed in the concentration range of 4.0-14.0 microg ml(-1). A prospective validation of the method showed that the method was linear (r=0.9995), precise (intra-day: CV=1.57% and inter-day: CV=1.50%) and accurate (mean recoveries: 99.69%). The results compared favourably with those of the HPLC method.

  17. Spectrophotometric Attachment for the Vacuum Ultraviolet

    NASA Technical Reports Server (NTRS)

    Axelrod, Norman N.

    1961-01-01

    An absorption spectrophotometric attachment to a vacuum ultraviolet monochromator has been built and tested. With an empty sample chamber, the ratio of the radiant flux through the sample chamber to the radiant flux through the reference chamber was measured. By optimizing conditions at the entrance slit, the ratio was constant within experimental error over the region 1000-1600 A. The transmittance of thin celluloid films was measured with the attachment.

  18. Comparative study for determination of some polycyclic aromatic hydrocarbons 'PAHs' by a new spectrophotometric method and multivariate calibration coupled with dispersive liquid-liquid extraction.

    PubMed

    Abdel-Aziz, Omar; El Kosasy, A M; El-Sayed Okeil, S M

    2014-12-10

    A modified dispersive liquid-liquid extraction (DLLE) procedure coupled with spectrophotometric techniques was adopted for simultaneous determination of naphthalene, anthracene, benzo(a)pyrene, alpha-naphthol and beta-naphthol in water samples. Two different methods were used, partial least-squares (PLS) method and a new derivative ratio method, namely extended derivative ratio (EDR). A PLS-2 model was established for simultaneous determination of the studied pollutants in methanol, by using twenty mixtures as calibration set and five mixtures as validation set. Also, in methanol a novel (EDR) method was developed for determination of the studied pollutants, where each component in the mixture of the five PAHs was determined by using a mixture of the other four components as divisor. Chemometric and EDR methods could be also adopted for determination of the studied PAH in water samples after transferring them from aqueous medium to the organic one by utilizing dispersive liquid-liquid extraction technique, where different parameters were investigated using a full factorial design. Both methods were compared and the proposed method was validated according to ICH guidelines and successfully applied to determine these PAHs simultaneously in spiked water samples, where satisfactory results were obtained. All the results obtained agreed with those of published methods, where no significant difference was observed. PMID:24934969

  19. Kinetic spectrophotometric H-point standard addition method for the simultaneous determination of diloxanide furoate and metronidazole in binary mixtures and biological fluids.

    PubMed

    Issa, Mahmoud Mohamed; Nejem, R'afat Mahmoud; Abu Shanab, Alaa Mohamed; Shaat, Nahed Talab

    2013-10-01

    Simple, reliable, and sensitive kinetic spectrophotometric method has been developed for the simultaneous determination of diloxanide furoate and metronidazole using H-point standard addition method (HPSAM). The method is based on the oxidation rate difference of diloxanide and metronidazole by potassium permanganate in basic medium. A green color has been developed and measured at 610 nm. Different experimental parameters were carefully optimized. The limiting logarithmic and the initial-rate methods were adopted for the construction of the calibration curve of each individual reaction with potassium permanganate. Under the optimum conditions, Beer's law was obeyed in the range of 1.0-20.0 and 5.0-25.0 μg ml(-1) for diloxanide furoate and metronidazole, respectively. The detection limits were 0.22 μg ml(-1) for diloxanide furoate and 0.83 μg ml(-1) for metronidazole. Correlation coefficients of the regression equations were greater than 0.9970 in all cases. The precision of the method was satisfactory; the maximum value of relative standard deviation did not exceed 1.06% (n=5). The accuracy, expressed as recovery was between 99.4% and 101.4% with relative error of 0.12 and 0.14 for diloxanide furoate and metronidazole, respectively. The proposed method was successfully applied for the simultaneous determination of both drugs in pharmaceutical dosage forms and human urine samples and compared with alternative HPLC method.

  20. Femtosecond Chirp-Free Transient Absorption Method And Apparatus

    DOEpatents

    McBranch, Duncan W.; Klimov, Victor I.

    2001-02-20

    A method and apparatus for femtosecond transient absorption comprising phase-sensitive detection, spectral scanning and simultaneous controlling of a translation stage to obtain TA spectra information having at least a sensitivity two orders of magnitude higher than that for single-shot methods, with direct, simultaneous compensation for chirp as the data is acquired. The present invention includes a amplified delay translation stage which generates a splittable frequency-doubled laser signal at a predetermined frequency f, a controllable means for synchronously modulating one of the laser signals at a repetition rate of f/2, applying the laser signals to a material to be sample, and acquiring data from the excited sample while simultaneously controlling the controllable means for synchronously modulating.

  1. Comparative Study of Novel Ratio Spectra and Isoabsorptive Point Based Spectrophotometric Methods: Application on a Binary Mixture of Ascorbic Acid and Rutin

    PubMed Central

    Darwish, Hany W.; Bakheit, Ahmed H.; Naguib, Ibrahim A.

    2016-01-01

    This paper presents novel methods for spectrophotometric determination of ascorbic acid (AA) in presence of rutin (RU) (coformulated drug) in their combined pharmaceutical formulation. The seven methods are ratio difference (RD), isoabsorptive_RD (Iso_RD), amplitude summation (A_Sum), isoabsorptive point, first derivative of the ratio spectra (1DD), mean centering (MCN), and ratio subtraction (RS). On the other hand, RU was determined directly by measuring the absorbance at 358 nm in addition to the two novel Iso_RD and A_Sum methods. The work introduced in this paper aims to compare these different methods, showing the advantages for each and making a comparison of analysis results. The calibration curve is linear over the concentration range of 4–50 μg/mL for AA and RU. The results show the high performance of proposed methods for the analysis of the binary mixture. The optimum assay conditions were established and the proposed methods were successfully applied for the assay of the two drugs in laboratory prepared mixtures and combined pharmaceutical tablets with excellent recoveries. No interference was observed from common pharmaceutical additives. PMID:26885440

  2. Spectrophotometric and reversed-phase high-performance liquid chromatographic methods for simultaneous determination of escitalopram oxalate and clonazepam in combined tablet dosage form.

    PubMed

    Gandhi, Santosh Vilashchand; Dhavale, Nilesh Dnyandev; Jadhav, Vijay Yeshawantrao; Sabnis, Shweta Sadanand

    2008-01-01

    Simple, accurate, precise, and sensitive ultraviolet spectrophotometric and reversed-phase high-performance liquid chromatographic (RP-HPLC) methods for simultaneous estimation of escitalopram oxalate (ESC) and clonazepam (CLO) in combined tablet dosage form have been developed and validated. The spectroscopic method employs an absorbance correction method using 238.6 and 308 nm as 2 wavelengths for estimation with methanol and water as solvents. Beer's law is obeyed in the concentration range of 10.0-50.0 and 0.5-3.0 micro/mL for ESC and CLO, respectively. The RP-HPLC method uses a Jasco HPLC system with HiQ SiL C18 column (250 x 4.6 mm id) acetonitrile-0.005 M tetrabutylammonium hydrogen sulfate (55 + 45, v/v) as the mobile phase, and satranidazole as an internal standard. The detection was carried out using an ultraviolet detector set at 287 nm. For the HPLC method, Beer's law is obeyed in the concentration range of 10.0-60.0 and 0.5-3.0 microg/mL for ESC and CLO, respectively. Both methods have been successfully applied for the analysis of the drugs in a pharmaceutical formulation. Results of analysis were validated statistically and by recovery studies. PMID:18376583

  3. A New Spectrophotometric Method for Determination of Phenylpropanolamine HCl in its Pharmaceutical Formulations via Reaction with 2,3,5,6-tetrachloro-1,4-benzoquinone

    PubMed Central

    Walash, M. I.; El-Enany, N.; Saad, S.

    2010-01-01

    A selective and simple spectrophotometric method has been developed for the determination of phenylpropanolamine HCl (PPA) in its dosage forms. The method was based on the formation of a colored N-vinyl chlorobenzoquinone derivative of PPA through its reaction with 2,3,5,6-tetrachloro-1,4-benzoquinone in presence of acetaldehyde. The colored product exhibits maximum absorbance at 650 nm. Different experimental parameters affecting formation and stability of the product were carefully studied and optimized. The stoichiometry of the reaction was determined, and the reaction pathway was postulated. The absorbance concentration plot was rectilinear over the range of 5-100 μg/mL with Limit of Detection (LOD) and Limit of Quantitation (LOQ) of 0.244 μg/mL and 0.74 μg/mL respectively. The analytical performance of the method was fully validated, and the results were satisfactory. The proposed method was successfully applied to the determination of PPA in its commercial dosage forms including tablets, capsules and syrups with good recoveries. Statistical comparison of the results with those of the comparison method showed good agreement and proved that there was no significant difference in the accuracy and precision between the reference and the proposed methods. The mechanism of the reaction pathway was postulated. PMID:23675189

  4. A Parallel Iterative Method for Computing Molecular Absorption Spectra.

    PubMed

    Koval, Peter; Foerster, Dietrich; Coulaud, Olivier

    2010-09-14

    We describe a fast parallel iterative method for computing molecular absorption spectra within TDDFT linear response and using the LCAO method. We use a local basis of "dominant products" to parametrize the space of orbital products that occur in the LCAO approach. In this basis, the dynamic polarizability is computed iteratively within an appropriate Krylov subspace. The iterative procedure uses a matrix-free GMRES method to determine the (interacting) density response. The resulting code is about 1 order of magnitude faster than our previous full-matrix method. This acceleration makes the speed of our TDDFT code comparable with codes based on Casida's equation. The implementation of our method uses hybrid MPI and OpenMP parallelization in which load balancing and memory access are optimized. To validate our approach and to establish benchmarks, we compute spectra of large molecules on various types of parallel machines. The methods developed here are fairly general, and we believe they will find useful applications in molecular physics/chemistry, even for problems that are beyond TDDFT, such as organic semiconductors, particularly in photovoltaics.

  5. Automatic flow analysis method to determine traces of Mn²⁺ in sea and drinking waters by a kinetic catalytic process using LWCC-spectrophotometric detection.

    PubMed

    Chaparro, Laura; Ferrer, Laura; Leal, Luz O; Cerdà, Víctor

    2016-02-01

    A new automatic kinetic catalytic method has been developed for the measurement of Mn(2+) in drinking and seawater samples. The method is based on the catalytic effect of Mn(2+) on the oxidation of tiron by hydrogen peroxide in presence of Pb(2+) as an activator. The optimum conditions were obtained at pH 10 with 0.019 mol L(-1) 2'2 bipyridyl, 0.005 mol L(-1) tiron and 0.38 mol L(-1) hydrogen peroxide. Flow system is based on multisyringe flow injection analysis (MSFIA) coupled with a lab-on-valve (LOV) device exploiting on line spectrophotometric detection by a Liquid Waveguide Capillary Cell (LWCC), 1m optical length and performed at 445 nm. Under the optimized conditions by a multivariate approach, the method allowed the measurement of Mn(2+) in a range of 0.03-35 µg L(-1) with a detection limit of 0.010 µg L(-1), attaining a repeatability of 1.4% RSD. The method was satisfactorily applied to the determination of Mn(2+) in environmental water samples. The reliability of method was also verified by determining the manganese content of the certified standard reference seawater sample, CASS-4.

  6. Two new spectrophotometric reagents for copper.

    PubMed

    Stookey, L

    1970-07-01

    Two ferroin-type compounds are proposed as spectrophotometric reagents for copper(I): 6-methyl-2-pyridylhydrazidine, which forms a yellow complex with lambda(max) 426 nm and molar absorptivity 700 l.mole(-1).mm(-1), and 3-(6-methyl-2-pyridyl)-5,6-diphenyl-1,2,4-triazine, which forms a red-orange complex with (lambda)max 492 nm and molar absorptivity of 955 l.mole(-1).mm(-1). These reagents are specific for copper and the complexes can be extracted into isopentanol for increased sensitivity.

  7. Spectrophotometric determination of nitrite using salbutamol sulfate as a reagent

    SciTech Connect

    Agrawal, Y.K.; Bhatt, P.N.

    1988-01-01

    A simple spectrophotometric method for the trace determination of nitrite (NO/sub 2//sup /minus//) is described. Nitrite is reacted with Salbutamol sulfate in acidic medium which gives a yellow color in alkaline medium (less than or equal to pH 7) and can be determined in the presence of several cations and anions. Beer's law is obeyed in the range of 1.8 to 27.6 ppm of nitrite with the molar absorptivity 1.8 /times/ 10/sup 3/ 1 /times/ mole /sup /minus/1/ /times/ cm/sup /minus/1/ at 410 nm. The proposed method can also be utilized for the determination of nitrate (NO/sub 3//sup /minus//) after its reduction to nitrite. The method has been applied for the determination of various samples containing traces of nitrite.

  8. [Spectrophotometric determination of cinnarizine based on charge-transfer reaction].

    PubMed

    Xu, B; Zhao, F; Tong, S

    1999-12-01

    The charge-transfer (CT) complex formed between cinnarizine as the donor and 7, 7, 8, 8-Tetracyanoquinodimethane (TCNQ) as the acceptor in acetone-methanol has been studied by spectrophotometric method. Beer's law is obeyed in the range of 0-18 microg x mL(-1) of cinnarizine. The apparent molar absorptivity of CT complex at 743 nm is 1.58 x 10(4) L x mol(-1) x cm(-1). The composition of CT complex is found to be 1 : 1 by Bent-French and Job's methods. The relative standard deviation is less than 3% (n = 10). The method has been applied to the determination of cinnarizine in tablets with satisfactory results. PMID:15822327

  9. Spectrophotometric determination of hydroxylamine and its derivatives in pharmaceuticals.

    PubMed

    Deepa, Boppana; Balasubramanian, Natesan; Nagaraja, Karachalacherevu Seetharamiah

    2004-12-01

    A sensitive spectrophotometric method for the determination of hydroxylamine is described. The method is based on the oxidation of hydroxylamine to nitrite using sodium arsenate under alkaline condition. The formed nitrite is determined based on the diazo coupling reaction between p-nitroaniline and N-(1-naphthyl)ethylenediamine dihydrochloride [NEDA]. The system obeys Beer's law over the concentration range 0-7 microg of hydroxylamine at 545 nm and the colour is stable for 3 h. The molar absorptivity of the colour system is found to be 6.7 x 10(4) l mol(-1) cm(-1). The relative standard deviation is 1.2% for ten determinations at 4 microg of hydroxylamine. Interferences due to various foreign ions have been studied and the method has been applied to the determination of hydroxylamine and its derivatives used in pharmaceutical formulations after hydrolysis.

  10. Sustained prediction ability of net analyte preprocessing methods using reduced calibration sets. Theoretical and experimental study involving the spectrophotometric analysis of multicomponent mixtures.

    PubMed

    Goicoechea, H C; Olivieri, A C

    2001-07-01

    A newly developed multivariate method involving net analyte preprocessing (NAP) was tested using central composite calibration designs of progressively decreasing size regarding the multivariate simultaneous spectrophotometric determination of three active components (phenylephrine, diphenhydramine and naphazoline) and one excipient (methylparaben) in nasal solutions. Its performance was evaluated and compared with that of partial least-squares (PLS-1). Minimisation of the calibration predicted error sum of squares (PRESS) as a function of a moving spectral window helped to select appropriate working spectral ranges for both methods. The comparison of NAP and PLS results was carried out using two tests: (1) the elliptical joint confidence region for the slope and intercept of a predicted versus actual concentrations plot for a large validation set of samples and (2) the D-optimality criterion concerning the information content of the calibration data matrix. Extensive simulations and experimental validation showed that, unlike PLS, the NAP method is able to furnish highly satisfactory results when the calibration set is reduced from a full four-component central composite to a fractional central composite, as expected from the modelling requirements of net analyte based methods.

  11. Direct and selective flow-injection method for the simultaneous spectrophotometric determination of calcium and magnesium in red and white wines using online dilution based on "Zone Sampling".

    PubMed

    Themelis, D G; Tzanavaras, P D; Trellopoulos, A V; Sofoniou, M C

    2001-11-01

    The present work reports a selective and simple flow injection method for the direct and simultaneous determination of calcium and magnesium ions in red, rose, and white wines. Both ions react with methylthymol blue (MTB) at a strongly basic medium to form colored complexes that are monitored spectrophotometrically (lambda(max) = 610 nm). The simultaneous determination is achieved by online masking of magnesium by 8-hydroxyquinoline (8-HQ). Incorporating an online dilution mode based on the "zone sampling" technique in the FI system, the determination of both analytes was achieved without any pretreatment of the samples, in the range 0-350 mg L(-1) and 0-200 mg L(-1) for Ca(II) and Mg(II), respectively. The 3 sigma detection limits were quite satisfactory (2.1 and 1.8 mg L(-1) for Ca(II) and Mg(II) respectively), and the precision was 1.2% (at a mixture of 100.0 mg L(-1) Ca(II) + 100.0 mg L(-1) Mg(II), n = 12). A detailed study of interferences proved that the proposed method is highly selective. The application of the method to the direct analysis of red, rose, and white wines yielded excellent results compared with those obtained by using FAAS as a reference method (e(r) < 2.8%).

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

    PubMed

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

    2015-05-01

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

  13. Spectrophotometric determination of triclosan in personal care products

    NASA Astrophysics Data System (ADS)

    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.

  14. Correction method for the self-absorption effects in fluorescence extended X-ray absorption fine structure on multilayer samples.

    PubMed

    Li, Wen Bin; Yang, Xiao Yue; Zhu, Jing Tao; Tu, Yu Chun; Mu, Bao Zhong; Yu, Hai Sheng; Wei, Xiang Jun; Huang, Yu Ying; Wang, Zhan Shan

    2014-05-01

    A novel correction method for self-absorption effects is proposed for extended X-ray absorption fine structure (EXAFS) detected in the fluorescence mode on multilayer samples. The effects of refraction and multiple reflection at the interfaces are fully considered in this correction method. The correction is performed in k-space before any further data analysis, and it can be applied to single-layer or multilayer samples with flat surfaces and without thickness limit when the model parameters for the samples are known. The validity of this method is verified by the fluorescence EXAFS data collected for a Cr/C multilayer sample measured at different experimental geometries. PMID:24763646

  15. Comparison among the methods for hydrogen peroxide measurements to evaluate advanced oxidation processes: Application of a spectrophotometric method using copper(II) ion and 2,9-dimethyl-1,10-phenanthroline

    SciTech Connect

    Kosaka, Koji; Yamada, Harumi; Matsui, Saburo; Echigo, Shinya; Shishida, Kenichi

    1998-12-01

    Hydrogen peroxide (H{sub 2}O{sub 2}) in the range of several tens to several hundreds of micromoles per liter is usually added to the process water in advanced oxidation processes (AOPs). In this study, a spectrophotometric method using copper(II) ion and 2,9-dimethyl-1, 10-phenanthroline (DMP) for measuring H{sub 2}O{sub 2} concentration was compared with other methods [i.e., spectrophotometric methods using titanium oxalate and N,N-diethyl-p-phenylenediamine (DPD) and a fluorometric method using p-hydroxyphenyl acetic acid (POHPAA)]. Particular attention was paid to sensitivities and effects of coexisting substances. The most sensitive method was the fluorometric method, followed in order by DPD, DMP, and the titanium oxalate colorimetric method; their detection limits in 1-cm cells were 0.16, 0.77, 0.80, and 29 {micro}M, respectively. Therefore, the DMP method was found to be reasonably sensitive when applied to AOPs. In the DMP method, copper(II)-DMP complexes react with humic acid, and colored chemicals are produced. However, the slopes of the calibration curves of H{sub 2}O{sub 2} containing up to 10 mg of C L{sup {minus}1} from humic acid did not change significantly as compared to that in ultrapure water. The effect of chlorine on the DMP method was not observed up to at least 23 {micro}M (0.8 mg of Cl L{sup {minus}1}) of free chlorine, although the DPD and fluorometric methods are known to be interfered by chlorine. From this study, it was concluded that the DMP method is suitable to be used in AOPs.

  16. [The Establishment of the Method of the Fiber Optic Chemical Sensor Synchronous Absorption-Fluorescence].

    PubMed

    Zhang Li-hua; Iburaim, Arkin

    2016-03-01

    A new method of simultaneously measuring fiber-optic chemical sensor absorption spectrum and fluorescence spectrum is established. Make synchronous absorption-fluorescence cuvette, establish synchronous absorption-fluorescence spectrometry instrumentation combined by fiber optic chemical sensor technology, measure the synchronous absorption-fluorescence spectrums of solutions of rhodamine B, vitamin B2 and vitamin B6, compared by absorption spectroscopy measured by traditional UV-Visible photometric method and fluorescence spectroscopy measured by traditional fluorescence method. Synchronous absorption-fluorescence method measure absorption spectrums and fluorescence spectrums the same to traditional photometric and fluorescence spectroscopy of rhodamine B, vitamin B2 and vitamin B6. The maximum wavelength of fluorescence intensity method has high accuracy relatively compared with fluorescence, but the maximum wavelength of absorption has a slight deviation. Synchronous absorption-fluorescence method means simultaneously measure the absorption spectrums and fluorescence spectrums of the fluorescent substance, making two spectrums to one. The method measured the maximum emission wavelength with high accuracy, though in measuring maximum absorption wavelength there is a slight deviation, but it is worth further studying. PMID:27400519

  17. Spectrophotometric analysis of lithium carbonate used for bipolar disorder.

    PubMed

    May, James; Hickey, Michelle; Triantis, Iasonas; Palazidou, Eleni; Kyriacou, Panayiotis A

    2015-03-01

    Lithium therapy is the gold standard of treatment for patients with Bipolar Disorder. However, despite its effectiveness, it is a potentially hazardous drug requiring regular monitoring of blood levels to ensure toxic levels are not reached. This paper describes the spectrophotometric analysis of Lithium carbonate in solution as a first step in developing a portable home monitoring device for blood lithium analysis.. Using a high-end spectrophotometer, solutions of lithium carbonate (Li2CO3) have been optically fingerprinted. Preliminary measurements indicate that the ultraviolet region shows a strong distinction between different lithium concentrations. Utilizing second derivative absorption curves, the region of 220 nm to 230 nm demonstrated the ability to differentiate between concentrations representing those found in patients. Furthermore, the method could determine to within a 1-6% accuracy whether an unknown solution of Li2CO3 is either inside or outside the high-end of the therapeutic limit. PMID:25798326

  18. Spectrophotometric methods for the determination of benazepril hydrochloride in its single and multi-component dosage forms.

    PubMed

    El-Yazbi, F A; Abdine, H H; Shaalan, R A

    1999-06-01

    Three sensitive and accurate methods are presented for the determination of benazepril in its dosage forms. The first method uses derivative spectrophotometry to resolve the interference due to formulation matrix. The second method depends on the color formed by the reaction of the drug with bromocresol green (BCG). The third one utilizes the reaction of benazepril, after alkaline hydrolysis, with 3-methylbenzothialozone (MBTH) hydrazone where the produced color is measured at 593 nm. The latter method was extended to develop a stability-indicating method for this drug. Moreover, the derivative method was applied for the determination of benazepril in its combination with hydrochlorothiazide. The proposed methods were applied for the analysis of benazepril in the pure form and in tablets. The coefficient of variation was less than 2%.

  19. Simultaneous determination of antazoline and naphazoline by the net analyte signal standard addition method and spectrophotometric technique.

    PubMed

    Asadpour-Zeynali, Karim; Ghavami, Raoof; Esfandiari, Roghayeh; Soheili-Azad, Payam

    2010-01-01

    A novel net analyte signal standard addition method (NASSAM) was used for simultaneous determination of the drugs anthazoline and naphazoline. The NASSAM can be applied for determination of analytes in the presence of known interferents. The proposed method is used to eliminate the calibration and prediction steps of multivariate calibration methods; the determination is carried out in a single step for each analyte. The accuracy of the predictions against the H-point standard addition method is independent of the shape of the analyte and interferent spectra. The net analyte signal concept was also used to calculate multivariate analytical figures of merit, such as LOD, selectivity, and sensitivity. The method was successfully applied to the simultaneous determination of anthazoline and naphazoline in a commercial eye drop sample.

  20. Spectrophotometric determination of metronidazole and secnidazole in pharmaceutical preparations.

    PubMed

    Saffaj, T; Charrouf, M; Abourriche, A; Abboud, Y; Bennamara, A; Berrada, M

    2004-10-01

    A rapid and sensitive spectrophotometric method is proposed for determination of metronidazole and secnidazole. The method depends on the reduction of metronidazole and secnidazole molecule with zinc dust and hydrochloric acid flowed by diazotization and coupling with 8-quinolinol to give red colored chromogens easily measured spectrophotometrically which has lambda(max) = 500 nm. The experimental conditions were optimized and Berr's law was obeyed over the applicable concentration ranges both techniques were applied successfully to a wide variety of pharmaceutical preparations. PMID:15474063

  1. Methods for deacidizing gaseous mixtures by phase enhanced absorption

    DOEpatents

    Hu, Liang

    2012-11-27

    An improved process for deacidizing a gaseous mixture using phase enhanced gas-liquid absorption is described. The process utilizes a multiphasic absorbent that absorbs an acid gas at increased rate and leads to reduced overall energy costs for the deacidizing operation.

  2. Chemometric-assisted spectrophotometric methods and high performance liquid chromatography for simultaneous determination of seven β-blockers in their pharmaceutical products: A comparative study

    NASA Astrophysics Data System (ADS)

    Abdel Hameed, Eman A.; Abdel Salam, Randa A.; Hadad, Ghada M.

    2015-04-01

    Chemometric-assisted spectrophotometric methods and high performance liquid chromatography (HPLC) were developed for the simultaneous determination of the seven most commonly prescribed β-blockers (atenolol, sotalol, metoprolol, bisoprolol, propranolol, carvedilol and nebivolol). Principal component regression PCR, partial least square PLS and PLS with previous wavelength selection by genetic algorithm (GA-PLS) were used for chemometric analysis of spectral data of these drugs. The compositions of the mixtures used in the calibration set were varied to cover the linearity ranges 0.7-10 μg ml-1 for AT, 1-15 μg ml-1 for ST, 1-15 μg ml-1 for MT, 0.3-5 μg ml-1 for BS, 0.1-3 μg ml-1 for PR, 0.1-3 μg ml-1 for CV and 0.7-5 μg ml-1 for NB. The analytical performances of these chemometric methods were characterized by relative prediction errors and were compared with each other. GA-PLS showed superiority over the other applied multivariate methods due to the wavelength selection. A new gradient HPLC method had been developed using statistical experimental design. Optimum conditions of separation were determined with the aid of central composite design. The developed HPLC method was found to be linear in the range of 0.2-20 μg ml-1 for AT, 0.2-20 μg ml-1 for ST, 0.1-15 μg ml-1 for MT, 0.1-15 μg ml-1 for BS, 0.1-13 μg ml-1 for PR, 0.1-13 μg ml-1 for CV and 0.4-20 μg ml-1 for NB. No significant difference between the results of the proposed GA-PLS and HPLC methods with respect to accuracy and precision. The proposed analytical methods did not show any interference of the excipients when applied to pharmaceutical products.

  3. Chemometric-assisted spectrophotometric methods and high performance liquid chromatography for simultaneous determination of seven β-blockers in their pharmaceutical products: a comparative study.

    PubMed

    Abdel Hameed, Eman A; Abdel Salam, Randa A; Hadad, Ghada M

    2015-04-15

    Chemometric-assisted spectrophotometric methods and high performance liquid chromatography (HPLC) were developed for the simultaneous determination of the seven most commonly prescribed β-blockers (atenolol, sotalol, metoprolol, bisoprolol, propranolol, carvedilol and nebivolol). Principal component regression PCR, partial least square PLS and PLS with previous wavelength selection by genetic algorithm (GA-PLS) were used for chemometric analysis of spectral data of these drugs. The compositions of the mixtures used in the calibration set were varied to cover the linearity ranges 0.7-10 μg ml(-1) for AT, 1-15 μg ml(-1) for ST, 1-15 μg ml(-1) for MT, 0.3-5 μg ml(-1) for BS, 0.1-3 μg ml(-1) for PR, 0.1-3 μg ml(-1) for CV and 0.7-5 μg ml(-1) for NB. The analytical performances of these chemometric methods were characterized by relative prediction errors and were compared with each other. GA-PLS showed superiority over the other applied multivariate methods due to the wavelength selection. A new gradient HPLC method had been developed using statistical experimental design. Optimum conditions of separation were determined with the aid of central composite design. The developed HPLC method was found to be linear in the range of 0.2-20 μg ml(-1) for AT, 0.2-20 μg ml(-1) for ST, 0.1-15 μg ml(-1) for MT, 0.1-15 μg ml(-1) for BS, 0.1-13 μg ml(-1) for PR, 0.1-13 μg ml(-1) for CV and 0.4-20 μg ml(-1) for NB. No significant difference between the results of the proposed GA-PLS and HPLC methods with respect to accuracy and precision. The proposed analytical methods did not show any interference of the excipients when applied to pharmaceutical products.

  4. Liquid chromatography and chemometric-assisted spectrophotometric methods for the analysis of two multicomponent mixtures containing cough suppressant drugs.

    PubMed

    El-Gindy, Alaa; Emara, Samy; Mesbah, Mostafa K; Hadad, Ghada M

    2005-01-01

    Three methods were applied for the analysis of 2 multicomponent mixtures containing dextromethorphan hydrobromide, phenylephrine hydrochloride, chlorpheniramine maleate, methylparaben, and propylparaben, together with either sodium benzoate (Mix 1) or ephedrine hydrochloride and benzoic acid (Mix 2). In the first method, liquid chromatography was used for their simultaneous determination using an ODS column with a mobile phase consisting of acetonitrile-phosphate buffer, pH 2.7 (40 + 60, v/v), containing 5mM heptanesulfonic acid sodium salt and ultraviolet (UV) detection at 214 nm. Also, 2 chemometric methods, principal component regression, and partial least squares were used. For both chemometric calibrations, a concentration set of the mixture consisting of each compound in each mixture was prepared in distilled water. The absorbance data in the UV spectra were measured for the 76 or 71 wavelength points in the spectral region 210-240 or 210-224 nm considering the intervals of deltagamma = 0.4 or 0.2 nm for Mix 1 and Mix 2, respectively. The 2 chemometric methods did not require any separation step. These methods were successfully applied for the analysis of the 2 multicomponent combinations in synthetic mixtures and in commercial syrups, and the results were compared with each other. PMID:16152922

  5. Number of Nanoparticles per Cell through a Spectrophotometric Method - A key parameter to Assess Nanoparticle-based Cellular Assays

    PubMed Central

    Unciti-Broceta, Juan D.; Cano-Cortés, Victoria; Altea-Manzano, Patricia; Pernagallo, Salvatore; Díaz-Mochón, Juan J.; Sánchez-Martín, Rosario M.

    2015-01-01

    Engineered nanoparticles (eNPs) for biological and biomedical applications are produced from functionalised nanoparticles (NPs) after undergoing multiple handling steps, giving rise to an inevitable loss of NPs. Herein we present a practical method to quantify nanoparticles (NPs) number per volume in an aqueous suspension using standard spectrophotometers and minute amounts of the suspensions (up to 1 μL). This method allows, for the first time, to analyse cellular uptake by reporting NPs number added per cell, as opposed to current methods which are related to solid content (w/V) of NPs. In analogy to the parameter used in viral infective assays (multiplicity of infection), we propose to name this novel parameter as multiplicity of nanofection. PMID:25976173

  6. Number of Nanoparticles per Cell through a Spectrophotometric Method - A key parameter to Assess Nanoparticle-based Cellular Assays.

    PubMed

    Unciti-Broceta, Juan D; Cano-Cortés, Victoria; Altea-Manzano, Patricia; Pernagallo, Salvatore; Díaz-Mochón, Juan J; Sánchez-Martín, Rosario M

    2015-05-15

    Engineered nanoparticles (eNPs) for biological and biomedical applications are produced from functionalised nanoparticles (NPs) after undergoing multiple handling steps, giving rise to an inevitable loss of NPs. Herein we present a practical method to quantify nanoparticles (NPs) number per volume in an aqueous suspension using standard spectrophotometers and minute amounts of the suspensions (up to 1 μL). This method allows, for the first time, to analyse cellular uptake by reporting NPs number added per cell, as opposed to current methods which are related to solid content (w/V) of NPs. In analogy to the parameter used in viral infective assays (multiplicity of infection), we propose to name this novel parameter as multiplicity of nanofection.

  7. General Subject 1. Report to ICUMSA on the determination of commercial alpha-amylase activity by a spectrophotometric method

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A report is given on a new industrial method for the determination of the activity or strength of commercial alpha-amylase at a sugarcane factory or refinery, as well as a recommendation. At the present time, the activities or strengths of commercial alpha-amylases cannot be directly compared becau...

  8. Variable path length spectrophotometric probe

    DOEpatents

    O'Rourke, Patrick E.; McCarty, Jerry E.; Haggard, Ricky A.

    1992-01-01

    A compact, variable pathlength, fiber optic probe for spectrophotometric measurements of fluids in situ. The probe comprises a probe body with a shaft having a polished end penetrating one side of the probe, a pair of optic fibers, parallel and coterminous, entering the probe opposite the reflecting shaft, and a collimating lens to direct light from one of the fibers to the reflecting surface of the shaft and to direct the reflected light to the second optic fiber. The probe body has an inlet and an outlet port to allow the liquid to enter the probe body and pass between the lens and the reflecting surface of the shaft. A linear stepper motor is connected to the shaft to cause the shaft to advance toward or away from the lens in increments so that absorption measurements can be made at each of the incremental steps. The shaft is sealed to the probe body by a bellows seal to allow freedom of movement of the shaft and yet avoid leakage from the interior of the probe.

  9. [Simultaneous determination of calcium and magnesium by calculative spectrophotometric complexometric titration].

    PubMed

    Liao, Li-fu; Xiao, Xi-lin; Yang, Ming-hui; Yang, Jing

    2007-12-01

    A new spectrophotometric complexometric titration method coupled with chemometrics for the determination of mixtures of metal ions has been developed. In the method described here, the titrant is a mixture of EDTA and two indicators. In the process of titration, both the volumetric addition of titrant and the progress of titration reaction can be characterized simultaneously by chemometric calculation with the absorption spectra, and then the titration curves can be obtained. With the titration curves, a matrix equation can be established, and thus the concentration of each component in the mixture of metal ions can be calculated with principal component regression. The method only needs the information of absorption spectra to obtain the analytical results, and is free of volumetric measurements. So the method is simple, convenient and precise, and has been applied to the simultaneous determination of mixtures of calcium and magnesium using malachite green and Cu-PAN as indicators with satisfactory results.

  10. Simplified reversed-phase HPLC method with spectrophotometric detection for the assay of verapamil in rat plasma.

    PubMed

    Lau-Cam, C A; Piemontese, D

    1998-02-01

    A high-performance liquid chromatographic (HPLC) method was developed for the assay of verapamil in rat plasma. After deproteinization of the plasma sample with an acetonitrile-perchloric acid (8:2) mixture containing dextromethorphan, the internal standard, an aliquot of the supernatant was directly analyzed on a cyanopropylsilane column with methanol-acetonitrile-triethylamine acetate buffer (10:30:60) as the mobile phase and detection at 235 mm. At a flow rate of 1.5 ml min-1, a complete analysis was completed in less than 6 min. The method was linear for verapamil concentrations in the range 0.5-10 micrograms ml-1 (r = 0.9999). Recoveries for the same drug concentrations from spiked rat plasma ranged from 85.6-93.0% (n = 8). The mean RSD values for intraday and interday assay reproducibility (n = 3) were, in both cases, less than 0.9%. The limit of detectability was about 0.1 microgram ml-1. The method was found useful to monitor the plasma levels of verapamil in rats that had received this drug by the nasal, oral and intravenous routes of administration.

  11. A simple spectrophotometric determination of meptyldinocap by its hydrolysis.

    PubMed

    Kurup, Sunita; Pillai, Ajai Kumar

    2013-01-01

    A simple spectrophotometric method is proposed for the determination of meptyldinocap (2,4-dinitro-6-octylphenyl crotonate). The method is based on the hydrolysis of meptyldinocap by hydroxylamine solution in alkaline medium to give 2,4-dinitro-6-octylphenol (2,4-DNOP), having maximum absorption at 380 nm. The reaction is found to be instantaneous in presence of ethanol. Beer's law is valid over the concentration range of 1.2-13 microg mL(-1) with molar absorptivity and Sandell's sensitivity of 3.22 x 10(6) L mol(-1) cm(-1) and 0.0001 microg cm(-2) respectively. The limit of detection and quantification were 0.0892 and 0.2703 microg mL(-1), respectively. The tolerance limits of interfering ions are discussed. All variables were studied in order to optimize the reaction conditions. The validity of the method was checked by its simultaneous determination in fruits and water samples and the results were statistically compared with those of a reference method by applying the Student's t-test and F-test.

  12. Direct spectrophotometric determination of alkylphenol polyethoxylate nonionic surfactants in wastewater.

    PubMed

    Zhu, Zhenzhong; Li, Zaijun; Hao, Zhuoli; Chen, Jian

    2003-11-01

    A new spectrophotometric method is proposed for direct determination of alkylphenol polyethoxylate, RO(CH(2)CH(2)O)(n)H (where R is alkylphenyl and n is the degree of polymerization), in wastewater. The method is based on the formation of ternary complex, Pb(II)-meso-tetra-(3,5-dibromo-4-hydrooxyphenyl)-Porphyrin (T(DBHP)P)-alkylphenol polyethoxylate (APE). Under optimum reaction conditions, T(DBHP)P reacts with lead(II) and APE to form a yellow ternary complex with the maximum absorption peak at 479 nm. The color reaction is rapidly completed and the absorbance remains stable for at least 24h under room temperature. The apparent molar absorption coefficients were 0.4-4.3 x 10(4) L mol(-1) cm(-1) for n=5-50. As little as 0.02 microg mL(-1) of APE can be detected. The effects of various substances on the determination of APE were also investigated in detail. It was found that all the studied co-existing substances, especially cationic and anionic surfactants, which always seriously interfere in some reported methods, could be tolerated in considerable amounts. The method offered the advantages of simplicity, rapidity, sensitivity and selectivity without any prior separation or extraction. PMID:14511721

  13. Spectrophotometric determination of the protolytic dissociation constants of the new chromogenic reagent "palladiazo"-I Investigations with sodium hydroxide, perchloric acid and different aqueous buffer solutions.

    PubMed

    Pérez-Butsamante, J A; Burriel-Martí, F

    1971-02-01

    The "palladiazo" reagent has been subjected to a detailed spectrophotometric investigation in concentrated perchloric acid, different aqueous buffers and concentrated sodium hydroxide solutions. K(1)-K(10) and (1)-(10) values corresponding to the instability constants of the protolytic equilibria involved and to the molar absorptivities at 540 and 630 run of the different proton complex species of the system have been calculated by a number of analytical and graphical spectrophotometric methods. Special attention has been paid to the study of the complicated phenomena implied by the interaction of the reagent with perchloric acid, which has been shown to give rise to alteration of the initial isomeric composition of the reagent and to the formation of addition and/or oxidation products derived from side-reactions undergone by the reagent with the medium. All the instability constants and molar absorptivities, which have been determined by several methods, are tabulated for comparison.

  14. Photothermal method for absorption measurements in anisotropic crystals

    NASA Astrophysics Data System (ADS)

    Stubenvoll, M.; Schäfer, B.; Mann, K.; Novak, O.

    2016-02-01

    A measurement system for quantitative determination of both surface and bulk contributions to the photo-thermal absorption has been extended to anisotropic optical media. It bases upon a highly sensitive Hartmann-Shack wavefront sensor, accomplishing precise on-line monitoring of wavefront deformations of a collimated test beam transmitted perpendicularly through the laser-irradiated side of a cuboid sample. Caused by the temperature dependence of the refractive index as well as thermal expansion, the initially plane wavefront of the test beam is distorted. Sign and magnitude depend on index change and expansion. By comparison with thermal theory, a calibration of the measurement is possible, yielding a quantitative absolute measure of bulk and surface absorption losses from the transient wavefront distortion. Results for KTP and BBO single crystals are presented.

  15. [Absorption of aqueous extracts from Salviae Miltiorrhizae Radix et Rhizoma by everted intestinal sac method].

    PubMed

    Zhao, Jie; Xu, Xue-lin; Yi, Hong; Zhang, Hong-min; Liu, Xiao-qian; Zhu, Jing-jing; Wang, Zhi-min

    2015-08-01

    To study the absorptive characteristics of aqueous extracts from Salviae Miltiorrhizae Radix et Rhizoma by in vitro rat everted intestinal sac model. Three representative ingredients in aqueous extracts from Salviae Miltiorrhizae Radix et Rhizome--protocatechuic aldehyde (PAL), posmarinic acid (RA) and salvianolic acid B (SAB), were selected as the study objects. An UPLC method was established to determine and measure their cumulative absorption amount, in order to explain the absorption characteristics of ingredients in different intestinal sections. According to the experimental result, RA and SAB showed the passive absorption in ileum, which conformed to the first-order absorption rate; with low and medium doses, they showed a zero-order absorption rate in jejunum, which was reflected in the coexistence of both positive and passive absorptions; PAL showed a passive absorption manner both in ileum and jejunum. According to the experiment for absorption in different intestinal sections, RA and SAB were mainly absorbed in jejunum, while PAL was absorbed mainly in ileum. All of the three ingredients in aqueous extracts from Salviae Miltiorrhizae Radix et rhizome--PAL, RA and SAB could be absorbed in intestines, but with differences in the absorption rate and mechanism, which indicated that the intestinal absorption of aqueous extracts from Salviae Miltiorrhizae Radix et rhizome was selectivity, instead of a simple semi-permeable membrane penetration process.

  16. Spectrophotometric determination of magnesium in pharmaceutical preparations by cost-effective sequential injection analysis.

    PubMed

    Tesfaldet, Zeriet O; van Staden, Jacobus F; Stefan, Raluca I

    2004-11-15

    A simple and rapid, inexpensive spectrophotometric method was proposed for magnesium assay in pharmaceutical preparations by sequential injection analysis (SIA). The method is based on the reaction between o-cresolphthalein complexone (CPC) and Mg(II) in alkaline media, yielding a pink colored complex with absorption maximum at 570nm. Since the formation constant between Ca-CPC and Mg-CPC is similar, initially a sample/standard solution was aspirated into the holding coil followed by a mixture of masking-buffer solutions. This was done because masking of calcium should be accomplished before Mg-CPC complexation. Then the reagent was introduced into the reaction coil to produce a colored complex, which is measured spectrophotometrically at 570nm. In this way the interference of calcium was reduced. Furthermore, all the parameters that affect the reaction were evaluated. The calibration curve is linear over a range of 0-20mgl(-1) of Mg(II) with a detection limit of 0.24mgl(-1). A sample throughput of 80 samples per hour and relative standard deviation <2.0% were achieved. The proposed method was successfully applied for the assay of magnesium in three different compositions of pharmaceutical preparations (tablets). The results were found to be in good agreement with the manual flame atomic absorption spectrophotometry (FAAS) and UV-Vis spectrophotometry methods and with the claimed values by the manufactures. The t-test shows no significant difference at 95% confidence level.

  17. A method for monitoring nuclear absorption coefficients of aviation fuels

    NASA Technical Reports Server (NTRS)

    Sprinkle, Danny R.; Shen, Chih-Ping

    1989-01-01

    A technique for monitoring variability in the nuclear absorption characteristics of aviation fuels has been developed. It is based on a highly collimated low energy gamma radiation source and a sodium iodide counter. The source and the counter assembly are separated by a geometrically well-defined test fuel cell. A computer program for determining the mass attenuation coefficient of the test fuel sample, based on the data acquired for a preset counting period, has been developed and tested on several types of aviation fuel.

  18. Spectrophotometric determination of ofloxacin in pharmaceuticals by redox reaction

    NASA Astrophysics Data System (ADS)

    Ramesh, P. J.; Basavaiah, K.; Rajendraprasad, N.; Devi, O. Zenita; Vinay, K. B.

    2011-07-01

    Two simple spectrophotometric methods have been developed to analyze ofloxacin (OFX) in pharmaceuticals. The methods are based on the oxidation of OFX by a measured excess of cerium(IV) sulfate in H2SO4 medium. This was followed by the determination of the unreacted oxidant by reacting it with either p-toluidine ( p-TD) and measuring the absorbance at 525 nm (method A) or o-dianisidine ( o-DA) and measuring the absorbance at 470 nm (method B). In both methods, the amount of cerium(IV) sulfate reacted corresponds to the amount of OFX. Calibration graphs were linear over the ranges of 0-120 and 0-4 g/ml OFX for methods A and B, respectively. The calculated molar absorptivity (2.34ṡ103 and 5.99ṡ104), Sandell sensitivity, and limit of quantification for the methods are reported. The intra-day precision (%RSD) and accuracy (%RE) were < 8.0 and ≤ 4.0%, respectively, and the inter-day RSD and RE values were within 5 and 4.0%, respectively. The applicability of the methods was demonstrated by determining OFX in tablets with an accuracy (%RE) of < 3% and precision (%RSD) of ≤2.65%. The accuracy of the methods was further ascertained by recovery experiments via a standard-addition procedure.

  19. Selectivity of the optical-absorption method based on an instrumental pick out of Fourier components in the absorption spectrum

    NASA Astrophysics Data System (ADS)

    Pisarevsky, Yu. V.; Kolesnikov, S. A.; Kolesnikova, E. S.; Turutin, Yu. A.; Konopelko, L. A.; Shor, N. B.

    2016-06-01

    The introduction of interference-polarization filters (IPFs) in the structure of an optical-absorption analyzer makes it possible to pick out a harmonic (a Fourier component of the absorption spectrum) providing measurement with the highest sensitivity. The selectivity of such a method of analysis is determined by overlapping the oscillations of the measured and interfering components. By the example of measurement in benzene in the presence of an interfering component (toluene), the possibility is considered for the optimization of selectivity due to the variation of the path-difference dispersion for ordinary and extraordinary interfering rays. The metrological characteristics of the interference-polarization analyzer of C6H6 confirming the results of calculations are given.

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

    PubMed

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

    2014-01-01

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

  1. [Study of the Detecting System of CH4 and SO2 Based on Spectral Absorption Method and UV Fluorescence Method].

    PubMed

    Wang, Shu-tao; Wang, Zhi-fang; Liu, Ming-hua; Wei, Meng; Chen, Dong-ying; Wang, Xing-long

    2016-01-01

    According to the spectral absorption characteristics of polluting gases and fluorescence characteristics, a time-division multiplexing detection system is designed. Through this system we can detect Methane (CH4) and sulfur dioxide (SO2) by using spectral absorption method and the SO2 can be detected by using UV fluorescence method. The system consists of four parts: a combination of a light source which could be switched, the common optical path, the air chamber and the signal processing section. The spectral absorption characteristics and fluorescence characteristics are measured first. Then the experiment of detecting CH4 and SO2 through spectral absorption method and the experiment of detecting SO2 through UV fluorescence method are conducted, respectively. Through measuring characteristics of spectral absorption and fluorescence, we get excitation wavelengths of SO2 and CH4 measured by spectral absorption method at the absorption peak are 280 nm and 1.64 μm, respectively, and the optimal excitation wavelength of SO2 measured by UV fluorescence method is 220 nm. we acquire the linear relation between the concentration of CH4 and relative intensity and the linear relation between the concentration of SO2 and output voltage after conducting the experiment of spectral absorption method, and the linearity are 98.7%, 99.2% respectively. Through the experiment of UV fluorescence method we acquire that the relation between the concentration of SO2 and the voltage is linear, and the linearity is 99.5%. Research shows that the system is able to be applied to detect the polluted gas by absorption spectrum method and UV fluorescence method. Combing these two measurement methods decreases the costing and the volume, and this system can also be used to measure the other gases. Such system has a certain value of application. PMID:27228784

  2. [Study of the Detecting System of CH4 and SO2 Based on Spectral Absorption Method and UV Fluorescence Method].

    PubMed

    Wang, Shu-tao; Wang, Zhi-fang; Liu, Ming-hua; Wei, Meng; Chen, Dong-ying; Wang, Xing-long

    2016-01-01

    According to the spectral absorption characteristics of polluting gases and fluorescence characteristics, a time-division multiplexing detection system is designed. Through this system we can detect Methane (CH4) and sulfur dioxide (SO2) by using spectral absorption method and the SO2 can be detected by using UV fluorescence method. The system consists of four parts: a combination of a light source which could be switched, the common optical path, the air chamber and the signal processing section. The spectral absorption characteristics and fluorescence characteristics are measured first. Then the experiment of detecting CH4 and SO2 through spectral absorption method and the experiment of detecting SO2 through UV fluorescence method are conducted, respectively. Through measuring characteristics of spectral absorption and fluorescence, we get excitation wavelengths of SO2 and CH4 measured by spectral absorption method at the absorption peak are 280 nm and 1.64 μm, respectively, and the optimal excitation wavelength of SO2 measured by UV fluorescence method is 220 nm. we acquire the linear relation between the concentration of CH4 and relative intensity and the linear relation between the concentration of SO2 and output voltage after conducting the experiment of spectral absorption method, and the linearity are 98.7%, 99.2% respectively. Through the experiment of UV fluorescence method we acquire that the relation between the concentration of SO2 and the voltage is linear, and the linearity is 99.5%. Research shows that the system is able to be applied to detect the polluted gas by absorption spectrum method and UV fluorescence method. Combing these two measurement methods decreases the costing and the volume, and this system can also be used to measure the other gases. Such system has a certain value of application.

  3. Spectrophotometric determination of carminic acid in human plasma and fruit juices by second order calibration of the absorbance spectra-pH data matrices coupled with standard addition method.

    PubMed

    Samari, Fayezeh; Hemmateenejad, Bahram; Shamsipur, Mojtaba

    2010-05-14

    A simple analytical method based on the second-order calibration of the pH gradient spectrophotometric data was developed for assay of carminic acid (CA) in human plasma and orange juice over the concentration range of 1.5-14.0microM. The multi-way data analysis method was coupled with standard addition to encounter the significant effects of plasma and juices matrices on the acid-base behavior and UV-vis. absorbance spectra of CA. Thus, the standard addition three-way calibration data of plasma or fruit juices samples were analyzed by parallel factor analysis (PARAFAC) and the concentration related scores were used to derive a standard addition plot such as one obtained in univariate standard addition method. The number of PARAFAC components was obtained utilizing different criteria such as core consistency and residual errors through pf-test implementation. The applicability of the proposed method was evaluated by analysis of human plasma and fruit juices spiked with different levels of standard CA solutions. The results confirmed the success of the proposed method in the analysis of pH gradient spectrophotometric data for determination of CA. The recoveries were between 86.7 and 106.7. PMID:20441865

  4. Chemometrics-assisted spectrophotometric method for simultaneous determination of Pb2+ and Cu2+ ions in different foodstuffs, soil and water samples using 2-benzylspiro [isoindoline-1,5‧-oxazolidine]-2‧,3,4‧-trione using continuous wavelet transformation and partial least squares - Calculation of pKf of complexes with rank annihilation factor analysis

    NASA Astrophysics Data System (ADS)

    Abbasi Tarighat, Maryam; Nabavi, Masoume; Mohammadizadeh, Mohammad Reza

    2015-06-01

    A new multi-component analysis method based on zero-crossing point-continuous wavelet transformation (CWT) was developed for simultaneous spectrophotometric determination of Cu2+ and Pb2+ ions based on the complex formation with 2-benzyl espiro[isoindoline-1,5oxasolidine]-2,3,4 trione (BSIIOT). The absorption spectra were evaluated with respect to synthetic ligand concentration, time of complexation and pH. Therefore according the absorbance values, 0.015 mmol L-1 BSIIOT, 10 min after mixing and pH 8.0 were used as optimum values. The complex formation between BSIIOT ligand and the cations Cu2+ and Pb2+ by application of rank annihilation factor analysis (RAFA) were investigated. Daubechies-4 (db4), discrete Meyer (dmey), Morlet (morl) and Symlet-8 (sym8) continuous wavelet transforms for signal treatments were found to be suitable among the wavelet families. The applicability of new synthetic ligand and selected mother wavelets were used for the simultaneous determination of strongly overlapped spectra of species without using any pre-chemical treatment. Therefore, CWT signals together with zero crossing technique were directly applied to the overlapping absorption spectra of Cu2+ and Pb2+. The calibration graphs for estimation of Pb2+ and Cu 2+were obtained by measuring the CWT amplitudes at zero crossing points for Cu2+ and Pb2+ at the wavelet domain, respectively. The proposed method was validated by simultaneous determination of Cu2+ and Pb2+ ions in red beans, walnut, rice, tea and soil samples. The obtained results of samples with proposed method have been compared with those predicted by partial least squares (PLS) and flame atomic absorption spectrophotometry (FAAS).

  5. Chemometrics-assisted spectrophotometric method for simultaneous determination of Pb²⁺ and Cu²⁺ ions in different foodstuffs, soil and water samples using 2-benzylspiro [isoindoline-1,5'-oxazolidine]-2',3,4'-trione using continuous wavelet transformation and partial least squares - calculation of pKf of complexes with rank annihilation factor analysis.

    PubMed

    Abbasi Tarighat, Maryam; Nabavi, Masoume; Mohammadizadeh, Mohammad Reza

    2015-06-15

    A new multi-component analysis method based on zero-crossing point-continuous wavelet transformation (CWT) was developed for simultaneous spectrophotometric determination of Cu(2+) and Pb(2+) ions based on the complex formation with 2-benzyl espiro[isoindoline-1,5 oxasolidine]-2,3,4 trione (BSIIOT). The absorption spectra were evaluated with respect to synthetic ligand concentration, time of complexation and pH. Therefore according the absorbance values, 0.015 mmol L(-1) BSIIOT, 10 min after mixing and pH 8.0 were used as optimum values. The complex formation between BSIIOT ligand and the cations Cu(2+) and Pb(2+) by application of rank annihilation factor analysis (RAFA) were investigated. Daubechies-4 (db4), discrete Meyer (dmey), Morlet (morl) and Symlet-8 (sym8) continuous wavelet transforms for signal treatments were found to be suitable among the wavelet families. The applicability of new synthetic ligand and selected mother wavelets were used for the simultaneous determination of strongly overlapped spectra of species without using any pre-chemical treatment. Therefore, CWT signals together with zero crossing technique were directly applied to the overlapping absorption spectra of Cu(2+) and Pb(2+). The calibration graphs for estimation of Pb(2+) and Cu (2+)were obtained by measuring the CWT amplitudes at zero crossing points for Cu(2+) and Pb(2+) at the wavelet domain, respectively. The proposed method was validated by simultaneous determination of Cu(2+) and Pb(2+) ions in red beans, walnut, rice, tea and soil samples. The obtained results of samples with proposed method have been compared with those predicted by partial least squares (PLS) and flame atomic absorption spectrophotometry (FAAS).

  6. Chemometrics-assisted spectrophotometric method for simultaneous determination of Pb²⁺ and Cu²⁺ ions in different foodstuffs, soil and water samples using 2-benzylspiro [isoindoline-1,5'-oxazolidine]-2',3,4'-trione using continuous wavelet transformation and partial least squares - calculation of pKf of complexes with rank annihilation factor analysis.

    PubMed

    Abbasi Tarighat, Maryam; Nabavi, Masoume; Mohammadizadeh, Mohammad Reza

    2015-06-15

    A new multi-component analysis method based on zero-crossing point-continuous wavelet transformation (CWT) was developed for simultaneous spectrophotometric determination of Cu(2+) and Pb(2+) ions based on the complex formation with 2-benzyl espiro[isoindoline-1,5 oxasolidine]-2,3,4 trione (BSIIOT). The absorption spectra were evaluated with respect to synthetic ligand concentration, time of complexation and pH. Therefore according the absorbance values, 0.015 mmol L(-1) BSIIOT, 10 min after mixing and pH 8.0 were used as optimum values. The complex formation between BSIIOT ligand and the cations Cu(2+) and Pb(2+) by application of rank annihilation factor analysis (RAFA) were investigated. Daubechies-4 (db4), discrete Meyer (dmey), Morlet (morl) and Symlet-8 (sym8) continuous wavelet transforms for signal treatments were found to be suitable among the wavelet families. The applicability of new synthetic ligand and selected mother wavelets were used for the simultaneous determination of strongly overlapped spectra of species without using any pre-chemical treatment. Therefore, CWT signals together with zero crossing technique were directly applied to the overlapping absorption spectra of Cu(2+) and Pb(2+). The calibration graphs for estimation of Pb(2+) and Cu (2+)were obtained by measuring the CWT amplitudes at zero crossing points for Cu(2+) and Pb(2+) at the wavelet domain, respectively. The proposed method was validated by simultaneous determination of Cu(2+) and Pb(2+) ions in red beans, walnut, rice, tea and soil samples. The obtained results of samples with proposed method have been compared with those predicted by partial least squares (PLS) and flame atomic absorption spectrophotometry (FAAS). PMID:25766479

  7. Spectrophotometric Investigations of Macrolide Antibiotics: A Brief Review

    PubMed Central

    Keskar, Mrudul R; Jugade, Ravin M

    2015-01-01

    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. PMID:26609215

  8. Spectrophotometric Analysis of Pigments: A Critical Assessment of a High-Throughput Method for Analysis of Algal Pigment Mixtures by Spectral Deconvolution

    PubMed Central

    Thrane, Jan-Erik; Kyle, Marcia; Striebel, Maren; Haande, Sigrid; Grung, Merete; Rohrlack, Thomas; Andersen, Tom

    2015-01-01

    The Gauss-peak spectra (GPS) method represents individual pigment spectra as weighted sums of Gaussian functions, and uses these to model absorbance spectra of phytoplankton pigment mixtures. We here present several improvements for this type of methodology, including adaptation to plate reader technology and efficient model fitting by open source software. We use a one-step modeling of both pigment absorption and background attenuation with non-negative least squares, following a one-time instrument-specific calibration. The fitted background is shown to be higher than a solvent blank, with features reflecting contributions from both scatter and non-pigment absorption. We assessed pigment aliasing due to absorption spectra similarity by Monte Carlo simulation, and used this information to select a robust set of identifiable pigments that are also expected to be common in natural samples. To test the method’s performance, we analyzed absorbance spectra of pigment extracts from sediment cores, 75 natural lake samples, and four phytoplankton cultures, and compared the estimated pigment concentrations with concentrations obtained using high performance liquid chromatography (HPLC). The deviance between observed and fitted spectra was generally very low, indicating that measured spectra could successfully be reconstructed as weighted sums of pigment and background components. Concentrations of total chlorophylls and total carotenoids could accurately be estimated for both sediment and lake samples, but individual pigment concentrations (especially carotenoids) proved difficult to resolve due to similarity between their absorbance spectra. In general, our modified-GPS method provides an improvement of the GPS method that is a fast, inexpensive, and high-throughput alternative for screening of pigment composition in samples of phytoplankton material. PMID:26359659

  9. Standard test method for ultraviolet absorbance and absorptivity of petroleum products

    SciTech Connect

    Not Available

    1980-01-01

    This method covers the measurement of the ultraviolet absorption of a variety of petroleum products. It covers the absorbance of liquids of the absorptivity of liquids or the absorptivity of liquids and solids, or both, at wavelengths in the region 220 to 400 nm of the spectrum. The use of this method implies that the conditions of measurement - wavelength, solvent, if any, sample path length, and sample concentration - are specified by reference to one of the examples of the application of this method in the appendixes or by a statement of other conditions of measurement. Examples of the application of this method are the determination of the absorbance of white mineral oil, the absorptivity of refined petroleum wax, and the absorptivity of USP petrolatum. The ultraviolet absorbance of a liquid is determined by measuring the absorption spectrum of the undiluted liquid in a cell of known path length under specified conditions. The ultraviolet absorptivity of a solid or a liquid is determined by measuring the absorbance, at specified wavelengths, of a solution of the liquid or solid at known concentration in a cell of known path length.

  10. Software system for numerical simulation of minor gas constituents lidar sensing by the differential absorption method

    NASA Astrophysics Data System (ADS)

    Bochkovskii, D. A.; Matvienko, G. G.; Romanovskii, O. A.; Kharchenko, O. V.; Yakovlev, S. V.

    2014-11-01

    This paper reports the development of LIDAS (LIdar Differential Absorption Sensing) program-algorithmic system for laser remote sensing of minor gas constituents (MGCs) of the atmosphere by the differential absorption method (DIAL). The system includes modules for the search of wavelengths informative for laser gas analysis by the differential absorption method, for numerical simulation of lidar sensing of atmospheric MGCs, and for calculation of errors of methodical, atmospheric, spectral, and instrumental origin. Lidar sensing of gas constituents by the differential absorption method as applied to problems of sensing of atmospheric MGCs is simulated numerically. Results of experiments on remote sensing of gas constituents of the atmosphere with the use of RO laser are presented.

  11. A method of predicting the energy-absorption capability of composite subfloor beams

    NASA Technical Reports Server (NTRS)

    Farley, Gary L.

    1987-01-01

    A simple method of predicting the energy-absorption capability of composite subfloor beam structure was developed. The method is based upon the weighted sum of the energy-absorption capability of constituent elements of a subfloor beam. An empirical data base of energy absorption results from circular and square cross section tube specimens were used in the prediction capability. The procedure is applicable to a wide range of subfloor beam structure. The procedure was demonstrated on three subfloor beam concepts. Agreement between test and prediction was within seven percent for all three cases.

  12. Successive spectrophotometric resolution as a novel technique for the analysis of ternary mixtures of pharmaceuticals

    NASA Astrophysics Data System (ADS)

    Lotfy, Hayam M.; Tawakkol, Shereen M.; Fahmy, Nesma M.; Shehata, Mostafa A.

    2014-03-01

    A novel spectrophotometric technique was developed for the simultaneous determination of ternary mixtures, without prior separation steps. This technique was called successive spectrophotometric resolution technique. The technique was based on either the successive ratio subtraction or successive derivative subtraction. The mathematical explanation of the procedure was illustrated. In order to evaluate the applicability of the methods a model data as well as an experimental data were tested. The results from experimental data related to the simultaneous spectrophotometric determination of lidocaine hydrochloride (LH), calcium dobesilate (CD) and dexamethasone acetate (DA); in the presence of hydroquinone (HQ), the degradation product of calcium dobesilate were discussed. The proposed drugs were determined at their maxima 202 nm, 305 nm, 239 nm and 225 nm for LH, CD, DA and HQ respectively; by successive ratio subtraction coupled with constant multiplication method to obtain the zero order absorption spectra, while by applying successive derivative subtraction they were determined at their first derivative spectra at 210 nm for LH, 320 nm or P292-320 for CD, 256 nm or P225-252 for DA and P220-233 for HQ respectively. The calibration curves were linear over the concentration range of 2-20 μg/mL for both LH and DA, 6-50 μg/mL for CD, and 3-40 μg/mL for HQ. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulation containing the cited drugs with no interference from other dosage form additives. The proposed methods were validated according to the ICH guidelines. The obtained results were statistically compared with those of the official BP methods for LH, DA, and CD, and with the official USP method for HQ; using student t-test, F-test, and one way ANOVA, showing no significant difference with respect to accuracy and precision.

  13. Successive spectrophotometric resolution as a novel technique for the analysis of ternary mixtures of pharmaceuticals.

    PubMed

    Lotfy, Hayam M; Tawakkol, Shereen M; Fahmy, Nesma M; Shehata, Mostafa A

    2014-01-01

    A novel spectrophotometric technique was developed for the simultaneous determination of ternary mixtures, without prior separation steps. This technique was called successive spectrophotometric resolution technique. The technique was based on either the successive ratio subtraction or successive derivative subtraction. The mathematical explanation of the procedure was illustrated. In order to evaluate the applicability of the methods a model data as well as an experimental data were tested. The results from experimental data related to the simultaneous spectrophotometric determination of lidocaine hydrochloride (LH), calcium dobesilate (CD) and dexamethasone acetate (DA); in the presence of hydroquinone (HQ), the degradation product of calcium dobesilate were discussed. The proposed drugs were determined at their maxima 202 nm, 305 nm, 239 nm and 225 nm for LH, CD, DA and HQ respectively; by successive ratio subtraction coupled with constant multiplication method to obtain the zero order absorption spectra, while by applying successive derivative subtraction they were determined at their first derivative spectra at 210 nm for LH, 320 nm or P(292-320) for CD, 256 nm or P(225-252) for DA and P(220-233) for HQ respectively. The calibration curves were linear over the concentration range of 2-20 μg/mL for both LH and DA, 6-50 μg/mL for CD, and 3-40 μg/mL for HQ. The proposed methods were checked using laboratory-prepared mixtures and were successfully applied for the analysis of pharmaceutical formulation containing the cited drugs with no interference from other dosage form additives. The proposed methods were validated according to the ICH guidelines. The obtained results were statistically compared with those of the official BP methods for LH, DA, and CD, and with the official USP method for HQ; using student t-test, F-test, and one way ANOVA, showing no significant difference with respect to accuracy and precision.

  14. Method of determining pH by the alkaline absorption of carbon dioxide

    DOEpatents

    Hobbs, David T.

    1992-01-01

    A method for measuring the concentration of hydroxides in alkaline solutions in a remote location using the tendency of hydroxides to absorb carbon dioxide. The method includes the passing of carbon dioxide over the surface of an alkaline solution in a remote tank before and after measurements of the carbon dioxide solution. A comparison of the measurements yields the absorption fraction from which the hydroxide concentration can be calculated using a correlation of hydroxide or pH to absorption fraction.

  15. Extractive spectrophotometric determination of niobium(V) with thiocyanate and amides

    SciTech Connect

    Patel, K.S. ); Das, M. )

    1991-07-01

    A new procedure for extractive spectrophotometric determination of niobium(V) with thiocyanate and 10 amides (derived from condensation of aceticanhydride with amines) is described. The value of molar absorptivity of the complexes in benzene lie in the range of (3.10 - 4.20){times}10{sup 4} 1 mole{sup {minus}1} cm{sup {minus}1} at absorption maximum 395 - 400 nm. Among these, the most sensitive compound, N-octylacetamide has been chosen for the detailed studies. The limit for detection is 0.01 {mu}g Nb/ml of the aqueous solution. The effect of various analytical variables on the determination of the metal has been examined. The method is simple, rapid and being free from interferences of almost all metal ions except Mo. Its application for the analysis of the metal to ore, slag, steel and water has been tested.

  16. Spectrophotometric Assay of Mebendazole in Dosage Forms Using Sodium Hypochlorite

    NASA Astrophysics Data System (ADS)

    Swamy, N.; Prashanth, K. N.; Basavaiah, K.

    2014-07-01

    A simple, selective and sensitive spectrophotometric method is described for the determination of mebendazole (MBD) in bulk drug and dosage forms. The method is based on the reaction of MBD with hypochlorite in the presence of sodium bicarbonate to form the chloro derivative of MBD, followed by the destruction of the excess hypochlorite by nitrite ion. The color was formed by the oxidation of iodide with the chloro derivative of MBD to iodine in the presence of starch and forming the blue colored product, which was measured at 570 nm. The optimum conditions that affect the reaction were ascertained and, under these conditions, a linear relationship was obtained in the concentration range of 1.25-25.0·g/ml MBD. The calculated molar absorptivity and Sandell sensitivity values are 9.56·103 l·mol-1·cm-1 and 0.031 μg/cm2, respectively. The limits of detection and quantification are 0.11 and 0.33 μg/ml, respectively. The proposed method was applied successfully to the determination of MBD in bulk drug and dosage forms, and no interference was observed from excipients present in the dosage forms. The reliability of the proposed method was further checked by parallel determination by the reference method and also by recovery studies.

  17. New Spectrophotometric Assay of Pyrantel Pamoate in Pharmaceuticals and Spiked Human Urine Using Three Complexing Agents

    NASA Astrophysics Data System (ADS)

    Swamy, N.; Prashanth, K. N.; Basavaiah, K.

    2015-07-01

    Three simple, rapid, inexpensive, and highly sensitive spectrophotometric methods are described for the quantifi cation of pyrantel pamoate (PYP) in pure drug and formulations. The methods are based on the molecular charge-transfer (CT) complexation reaction involving pyrantel base (PYL) as n-donor and iodine as σ-acceptor (I 2 , method A), and 2,4-dinitrophenol (DNP, method B) or picric acid (PA, method C) as π-acceptors. Spectrophotometrically, the CT complexes showed absorption maxima at 380, 420, and 430 nm, for methods A, B, and C, respectively. Under optimum conditions, Beer's law was obeyed over the concentration ranges 0.12-2.9, 0.12-3.75, and 0.12-2.9 μg/ml for methods A, B, and C, respectively. The apparent molar absorptivity of the CT complexes at the respective λmax are calculated to be 2.63 × 10 5 , 6.91 × 10 4 , and 1.73 × 10 5 l/mol· cm respectively and the corresponding Sandell sensitivity values are 0.0009, 0.003, and 0.0012. The limits of detection (LOD) and quantification (LOQ) are calculated to be (0.02 and 0.07), (0.05 and 0.15), and (0.02 and 0.07) μg/ml with methods A, B, and C, respectively. The intra-day and inter-day accuracy expressed as %RE and precision expressed as %RSD are less than 3%. The methods have been applied to the determination of PYP in tablets, suspensions, and spiked human urine. Parallel assay by a reference method and statistical analysis of the results obtained show no significant difference between the proposed methods and the reference method with respect to accuracy and precision, as evident from the Student's t and variation ratio tests. The accuracy of the methods has been further ascertained by recovery tests via the standard addition technique.

  18. Comparison of a spectrophotometric microdilution method with RPMI-2% glucose with the National Committee for Clinical Laboratory Standards reference macrodilution method M27-P for in vitro susceptibility testing of amphotericin B, flucytosine, and fluconazole against Candida albicans.

    PubMed Central

    Rodríguez-Tudela, J L; Berenguer, J; Martínez-Suárez, J V; Sanchez, R

    1996-01-01

    The National Committee for Clinical Laboratory Standards has proposed a reference broth macrodilution method for in vitro antifungal susceptibility testing of yeasts (the M27-P method). This method is cumbersome and time-consuming and includes MIC endpoint determination by visual and subjective inspection of growth inhibition after 48 h of incubation. An alternative microdilution procedure was compared with the M27-P method for determination of the amphotericin B, flucytosine, and fluconazole susceptibilities of 8 American Type Culture Collection strains (6 of them were quality control or reference strains) and 50 clinical isolates of candida albicans. This microdilution method uses as culture medium RPMI 1640 supplemented with 18 g of glucose per liter (RPMI-2% glucose). Preparation of drugs, basal medium, and inocula was done by following the recommendations of the National Committee for Clinical Laboratory Standards. The MIC endpoint was calculated objectively from the turbidimetric data read at 24 h. Increased growth of C. albicans in RPMI-2% glucose and its spectrophotometric reading allowed for the rapid (24 h) and objective calculation of MIC endpoints compared with previous microdilution methods with standard RPMI 1640. Nevertheless, good agreement was shown between the M27-P method and this microdilution test. The MICs obtained for the quality control or reference strains by the microdilution method were in the ranges published for those strains. For clinical isolates, the percentages of agreement were 100% for amphotericin B and fluconazole and 98.1% for flucytosine. These data suggest that this microdilution method may serve as a less subjective and more rapid alternative to the M27-P method for antifungal susceptibility testing of yeasts. PMID:8878570

  19. On the absorption of drugs using chronic dog ileal loop method.

    PubMed

    Kukan, M; Bezek, S; Trnovec, T; Gabauer, I; Styk, J

    1994-01-01

    The absorption rate of three model drugs, i.e., pentacaine (highly lipophilic), stobadine (moderately lipophilic) and acetylsalicylic acid (hydrophilic), was studied using the chronic dog ileal loop method. The drugs were dissolved either in 0.9% unbuffered solution of NaCl or in antacid mixture. When using 0.9% NaCl, the half-lives of absorption (t1/2 (dis)) of pentacaine and stobadine were (mean +/- SD) 23.2 +/- 7.8 min and 20.8 +/- 7.2 min, respectively. For stobadine a good agreement was found between its t1/2 (dis) from the ileum and its absorption half-life determined from blood concentrations after oral administration to dogs. The absorption of acetylsalicylic acid accounted for only 10-20% of the dose introduced into the loop over 45 min; thus, a reliable value of t1/2 (dis) could not be determined. The administration of unbuffered solution of NaCl into the loop was accompanied by rapid increase of pH from acidic to basic value. The antacid mixture failed to affect the absorption rate of the drugs studied. Sampling from the ileum was limited to 35-55 min due to rapid absorption of water. These results suggest that: 1) measurement of the absorption rate of some drugs, e.g., stobadine, by using the chronic dog ileal loop method may adequately predict their absorption rate after peroral administration to the dog, 2) interactions of antacids with drug absorption in the ileum may not play a significant role because of the strong buffering capacity of the ileum, and 3) rapid absorption of water from the ileum does not allow to reliably determine the value of t1/2 (dis) for slowly absorbed drugs. PMID:7837833

  20. A method for determination mass absorption coefficient of gamma rays by Compton scattering.

    PubMed

    El Abd, A

    2014-12-01

    A method was proposed for determination mass absorption coefficient of gamma rays for compounds, alloys and mixtures. It is based on simulating interaction processes of gamma rays with target elements having atomic numbers from Z=1 to Z=92 using the MCSHAPE software. Intensities of Compton scattered gamma rays at saturation thicknesses and at a scattering angle of 90° were calculated for incident gamma rays of different energies. The obtained results showed that the intensity of Compton scattered gamma rays at saturations and mass absorption coefficients can be described by mathematical formulas. These were used to determine mass absorption coefficients for compound, alloys and mixtures with the knowledge of their Compton scattered intensities. The method was tested by calculating mass absorption coefficients for some compounds, alloys and mixtures. There is a good agreement between obtained results and calculated ones using WinXom software. The advantages and limitations of the method were discussed.

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

    ERIC Educational Resources Information Center

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

    2011-01-01

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

  2. Developments in Methods for Measuring the Intestinal Absorption of Nanoparticle-Bound Drugs

    PubMed Central

    Liu, Wei; Pan, Hao; Zhang, Caiyun; Zhao, Liling; Zhao, Ruixia; Zhu, Yongtao; Pan, Weisan

    2016-01-01

    With the rapid development of nanotechnology, novel drug delivery systems comprising orally administered nanoparticles (NPs) have been paid increasing attention in recent years. The bioavailability of orally administered drugs has significant influence on drug efficacy and therapeutic dosage, and it is therefore imperative that the intestinal absorption of oral NPs be investigated. This review examines the various literature on the oral absorption of polymeric NPs, and provides an overview of the intestinal absorption models that have been developed for the study of oral nanoparticles. Three major categories of models including a total of eight measurement methods are described in detail (in vitro: dialysis bag, rat gut sac, Ussing chamber, cell culture model; in situ: intestinal perfusion, intestinal loops, intestinal vascular cannulation; in vivo: the blood/urine drug concentration method), and the advantages and disadvantages of each method are contrasted and elucidated. In general, in vitro and in situ methods are relatively convenient but lack accuracy, while the in vivo method is troublesome but can provide a true reflection of drug absorption in vivo. This review summarizes the development of intestinal absorption experiments in recent years and provides a reference for the systematic study of the intestinal absorption of nanoparticle-bound drugs. PMID:27455239

  3. Alkaline solution absorption of carbon dioxide method and apparatus

    DOEpatents

    Hobbs, D.T.

    1991-01-01

    Disclosed is a method for measuring the concentration of hydroxides (or pH) in alkaline solutions, using the tendency of hydroxides to adsorb CO{sub 2}. The method comprises passing CO{sub 2} over the surface of an alkaline solution in a remote tank before and after measurements of the CO{sub 2} concentration. Comparison of the measurements yields the adsorption fraction from which the hydroxide concentration can be calculated using a correlation of hydroxide or pH to adsorption fraction. A schematic is given of a process system according to a preferred embodiment of the invention. 2 figs.

  4. Development of a reliable analytical method for the precise extractive spectrophotometric determination of osmium(VIII) with 2-nitrobenzaldehydethiocarbohydrazone: Analysis of alloys and real sample.

    PubMed

    Zanje, Sunil B; Kokare, Arjun N; Suryavanshi, Vishal J; Waghmode, Duryodhan P; Joshi, Sunil S; Anuse, Mansing A

    2016-12-01

    The proposed method demonstrates that the osmium(VIII) forms complex with 2-NBATCH from 0.8molL(-1) HCl at room temperature. The complex formed was extracted in 10mL of chloroform with a 5min equilibration time. The absorbance of the red colored complex was measured at 440nm against the reagent blank. The Beer's law was obeyed in the range of 5-25μgmL(-1), the optimum concentration range was 10-20μgmL(-1) of osmium(VIII) as evaluated by Ringbom's plot. Molar absorptivity and Sandell's sensitivity of osmium(VIII)-2NBATCH complex in chloroform is 8.94×10(3)Lmol(-1)cm(-1) and 0.021μgcm(-2), respectively. The composition of osmium(VIII)-2NBATCH complex was 1:2 investigated from Job's method of continuous variation, Mole ratio method and slope ratio method. The interference of diverse ions was studied and masking agents were used wherever necessary. The present method was successfully applied for determination of osmium(VIII) from binary, ternary and synthetic mixtures corresponding to alloys and real samples. The validity of the method was confirmed by finding the relative standard deviation for five determinations which was 0.29%.

  5. Development of a reliable analytical method for the precise extractive spectrophotometric determination of osmium(VIII) with 2-nitrobenzaldehydethiocarbohydrazone: Analysis of alloys and real sample.

    PubMed

    Zanje, Sunil B; Kokare, Arjun N; Suryavanshi, Vishal J; Waghmode, Duryodhan P; Joshi, Sunil S; Anuse, Mansing A

    2016-12-01

    The proposed method demonstrates that the osmium(VIII) forms complex with 2-NBATCH from 0.8molL(-1) HCl at room temperature. The complex formed was extracted in 10mL of chloroform with a 5min equilibration time. The absorbance of the red colored complex was measured at 440nm against the reagent blank. The Beer's law was obeyed in the range of 5-25μgmL(-1), the optimum concentration range was 10-20μgmL(-1) of osmium(VIII) as evaluated by Ringbom's plot. Molar absorptivity and Sandell's sensitivity of osmium(VIII)-2NBATCH complex in chloroform is 8.94×10(3)Lmol(-1)cm(-1) and 0.021μgcm(-2), respectively. The composition of osmium(VIII)-2NBATCH complex was 1:2 investigated from Job's method of continuous variation, Mole ratio method and slope ratio method. The interference of diverse ions was studied and masking agents were used wherever necessary. The present method was successfully applied for determination of osmium(VIII) from binary, ternary and synthetic mixtures corresponding to alloys and real samples. The validity of the method was confirmed by finding the relative standard deviation for five determinations which was 0.29%. PMID:27380306

  6. Optimization on microlattice materials for sound absorption by an integrated transfer matrix method.

    PubMed

    Cai, Xiaobing; Yang, Jun; Hu, Gengkai

    2015-04-01

    Materials with well-defined microlattice structures are superlight, stable, and thus bear great potential in sound absorption. An integrated transfer matrix method (TMM) is proposed to evaluate the sound absorbing efficiency of these lattice materials, in which a massive number of micropores are densely placed. A comparison between integrated TMM and conventional TMM reveals that the proposed approach offers better predictions on sound absorption of microlattice. This approach is then employed to optimize the microlattice material to determine the best pore and porosity that lead to maximum absorbing efficiency capability and minimum required thickness to attain a target sound absorption. PMID:25920886

  7. Deriving brown carbon from multiwavelength absorption measurements: Method and application to AERONET and Aethalometer observations

    DOE PAGES

    Wang, X.; Heald, C. L.; Sedlacek, A.; de Sa, S. S.; Martin, S. T.; Alexander, M. L.; Watson, T. B.; Aiken, A. C.; Springston, S. R.; Artaxo, P.

    2016-10-13

    The radiative impact of organic aerosols (OA) is a large source of uncertainty in estimating the global direct radiative effect (DRE) of aerosols. This radiative impact includes not only light scattering but also light absorption from a subclass of OA referred to as brown carbon (BrC). However the absorption properties of BrC are poorly understood leading to large uncertainties in modelling studies. To obtain observational constraints from measurements, a simple Absorption Ångström Exponent (AAE) method is often used to separate the contribution of BrC absorption from that of black carbon (BC). However, this attribution method is based on assumptions regardingmore » the spectral dependence of BC that are often violated in the ambient atmosphere. Here we develop a new method that decreases the uncertainties associated with estimating BrC absorption. By applying this method to multi-wavelength absorption aerosol optical depth (AAOD) measurements at AERONET sites worldwide and surface aerosol absorption measurements at multiple ambient sites, we estimate that BrC globally contributes 6-40% of the absorption at 440nm. We find that the mass absorption coefficient of OA (OA-MAC) is positively correlated with BC/OA mass ratio. Based on the variability of BC properties and BC/OA emission ratio, we estimate a range of 0.05-1.2 m2/g for OA-MAC at 440nm. Using the combination of AERONET and OMI UV absorption observations we estimate that the AAE388/440nm for BrC is generally ~4 world-wide, with a smaller value in Europe (< 2). Our analyses of two surface sites (Cape Cod, to the southeast of Boston, and the GoAmazon2014/5 T3 site, to the west of Manaus, Brazil) reveal no significant relationship between BrC absorptivity and photochemical aging in typical urban influenced conditions. However, the absorption of BrC measured during the biomass burning season near Manaus is found to decrease with photochemical aging with a lifetime of ~1 day. This lifetime is comparable to

  8. Optimization on microlattice materials for sound absorption by an integrated transfer matrix method.

    PubMed

    Cai, Xiaobing; Yang, Jun; Hu, Gengkai

    2015-04-01

    Materials with well-defined microlattice structures are superlight, stable, and thus bear great potential in sound absorption. An integrated transfer matrix method (TMM) is proposed to evaluate the sound absorbing efficiency of these lattice materials, in which a massive number of micropores are densely placed. A comparison between integrated TMM and conventional TMM reveals that the proposed approach offers better predictions on sound absorption of microlattice. This approach is then employed to optimize the microlattice material to determine the best pore and porosity that lead to maximum absorbing efficiency capability and minimum required thickness to attain a target sound absorption.

  9. Measurement of the absorption coefficient of scattering liquid media by the calorimetric method

    NASA Astrophysics Data System (ADS)

    Butenin, A. V.; Kogan, B. Ya.

    2012-02-01

    Using the example of a number of hydrosols (gold nanorods and nanoshells, silver nanoshells, zinc phthalocyanine nanoparticles), we show that the absorption coefficient of a scattering liquid medium can be measured from its heating by a short-time laser irradiation. The degree of heating was determined from expansion of the liquid in an ampoule with a capillary (the principle of liquid thermometer). Irradiation was performed at a wavelength of 671 or 1069 nm. From the transmission of samples of hydrosols at these wave-lengths, the sum of the absorption and scattering coefficients has been determined. To measure the absorption spectra of scattering liquids by this method, a laser with a tunable radiation wavelength is required. In the case of monodisperse colloidal solutions, the method ensures the measurement of the absorption and scattering cross-section ratio of particles.

  10. A comparison of methods to estimate photosynthetic light absorption in leaves with contrasting morphology.

    PubMed

    Olascoaga, Beñat; Mac Arthur, Alasdair; Atherton, Jon; Porcar-Castell, Albert

    2016-03-01

    Accurate temporal and spatial measurements of leaf optical traits (i.e., absorption, reflectance and transmittance) are paramount to photosynthetic studies. These optical traits are also needed to couple radiative transfer and physiological models to facilitate the interpretation of optical data. However, estimating leaf optical traits in leaves with complex morphologies remains a challenge. Leaf optical traits can be measured using integrating spheres, either by placing the leaf sample in one of the measuring ports (External Method) or by placing the sample inside the sphere (Internal Method). However, in leaves with complex morphology (e.g., needles), the External Method presents limitations associated with gaps between the leaves, and the Internal Method presents uncertainties related to the estimation of total leaf area. We introduce a modified version of the Internal Method, which bypasses the effect of gaps and the need to estimate total leaf area, by painting the leaves black and measuring them before and after painting. We assess and compare the new method with the External Method using a broadleaf and two conifer species. Both methods yielded similar leaf absorption estimates for the broadleaf, but absorption estimates were higher with the External Method for the conifer species. Factors explaining the differences between methods, their trade-offs and their advantages and limitations are also discussed. We suggest that the new method can be used to estimate leaf absorption in any type of leaf independently of its morphology, and be used to study further the impact of gap fraction in the External Method.

  11. An Accurate Method for Computing the Absorption of Solar Radiation by Water Vapor

    NASA Technical Reports Server (NTRS)

    Chou, M. D.

    1980-01-01

    The method is based upon molecular line parameters and makes use of a far wing scaling approximation and k distribution approach previously applied to the computation of the infrared cooling rate due to water vapor. Taking into account the wave number dependence of the incident solar flux, the solar heating rate is computed for the entire water vapor spectrum and for individual absorption bands. The accuracy of the method is tested against line by line calculations. The method introduces a maximum error of 0.06 C/day. The method has the additional advantage over previous methods in that it can be applied to any portion of the spectral region containing the water vapor bands. The integrated absorptances and line intensities computed from the molecular line parameters were compared with laboratory measurements. The comparison reveals that, among the three different sources, absorptance is the largest for the laboratory measurements.

  12. Determination of protolytic equilibria for methyl 3-azido-6-iodo-2,3,6-trideoxy-α- D- arabino-hexopyranoside by ab initio and spectrophotometric methods

    NASA Astrophysics Data System (ADS)

    Dąbrowska, Aleksandra; Makowski, Mariusz; Jacewicz, Dagmara; Chylewska, Agnieszka; Chmurzyński, Lech

    2008-12-01

    UV absorption spectra of methyl 3-azido-6-iodo-2,3,6-trideoxy-α- D- arabino-hexopyranoside were recorded over a wide pH range. On this basis, a relationship between absorbance and pH was plotted, from which deprotonation equilibrium constants of this compound were determined. Further, quantum-mechanical calculations were performed at the ab initio level both in the gas phase by using the Restricted Hartree Fock (RHF), Møller-Plesset (MP2) methods and under consideration of solvation effects within the Polarizable Continuum Model (PCM), which enabled location of preferred protonation and deprotonation centers of this compound. The results provided the basis for discussion of the influence of substituents in the sugar ring on protolytic equilibria occurring in aqueous solutions of 3-azido-2,3-dideoxy sugars.

  13. Simultaneous spectrophotometric determination of trace amounts of uranium, thorium, and zirconium using the partial least squares method after their preconcentration by alpha-benzoin oxime modified Amberlite XAD-2000 resin.

    PubMed

    Ghasemi, Jahan B; Zolfonoun, E

    2010-01-15

    A new solid phase extraction method for separation and preconcentration of trace amounts of uranium, thorium, and zirconium in water samples is proposed. The procedure is based on the adsorption of U(VI), Th(IV) and Zr(IV) ions on a column of Amberlite XAD-2000 resin loaded with alpha-benzoin oxime prior to their simultaneous spectrophotometric determination with Arsenazo III using orthogonal signal correction partial least squares method. The enrichment factor for preconcentration of uranium, thorium, and zirconium was found to be 100. The detection limits for U(VI), Th(IV) and Zr(IV) were 0.50, 0.54, and 0.48microgL(-1), respectively. The precision of the method, evaluated as the relative standard deviation obtained by analyzing a series of 10 replicates, was below 4% for all elements. The practical applicability of the developed sorbent was examined using synthetic seawater, natural waters and ceramic samples. PMID:20006073

  14. Catalytic spectrophotometric determination of iodine in coal by pyrohydrolysis decomposition.

    PubMed

    Wu, Daishe; Deng, Haiwen; Wang, Wuyi; Xiao, Huayun

    2007-10-10

    A method for the determination of iodine in coal using pyrohydrolysis for sample decomposition was proposed. A pyrohydrolysis apparatus system was constructed, and the procedure was designed to burn and hydrolyse coal steadily and completely. The parameters of pyrohydrolysis were optimized through the orthogonal experimental design. Iodine in the absorption solution was evaluated by the catalytic spectrophotometric method, and the absorbance at 420 nm was measured by a double-beam UV-visible spectrophotometer. The limit of detection and quantification of the proposed method were 0.09 microg g(-1) and 0.29 microg g(-1), respectively. After analysing some Chinese soil reference materials (SRMs), a reasonable agreement was found between the measured values and the certified values. The accuracy of this approach was confirmed by the analysis of eight coals spiked with SRMs with an indexed recovery from 94.97 to 109.56%, whose mean value was 102.58%. Six repeated tests were conducted for eight coal samples, including high sulfur coal and high fluorine coal. A good repeatability was obtained with a relative standard deviation value from 2.88 to 9.52%, averaging 5.87%. With such benefits as simplicity, precision, accuracy and economy, this approach can meet the requirements of the limits of detection and quantification for analysing iodine in coal, and hence it is highly suitable for routine analysis. PMID:17920390

  15. 3-Aminophenol as a novel coupling agent for the spectrophotometric determination of sulfonamide derivatives.

    PubMed

    Nagaraja, P; Yathirajan, H S; Raju, C R; Vasantha, R A; Nagendra, P; Hemantha Kumar, M S

    2003-12-01

    A rapid, simple and sensitive spectrophotometric method for the determination of some sulfa drugs is described. The method is based on the formation of orange yellow colored azo product by the diazotization of sulfonamides, viz., dapsone (DAP), sulfathiazole (SFT), sulfadiazine (SFD), sulfacetamide (SFA), sulfamethoxazole (SFMx), sulfamerazine (SFMr), sulfaguanidine (SFG) and sulfadimidine (SFDd) followed by a coupling reaction with 3-aminophenol in aqueous medium. Absorbance of the resulting orange yellow product is measured at 460 nm and is stable for 6 days at 27 degrees C. Beer's law is obeyed in the concentration range of 0.05-8.0 microg/ml at the wavelength of maximum absorption. The method is successfully employed for the determination of sulfonamides in various pharmaceutical preparations and common excipients used as additives in pharmaceuticals do not interfere in the proposed method. Plausible reaction mechanism is proposed for the formation of the azo product.

  16. Spectrophotometric estimation of cobalt with ninhydrin.

    PubMed

    Mahmood, Karamat; Wattoo, Feroza Hamid; Wattoo, Muhammad Hamid Sarwar; Imran, Muhammad; Asad, Muhammad Javaid; Tirmizi, Syed Ahmed; Wadood, Abdul

    2012-04-01

    A violet coloured complex was developed when cobalt metal reacts with ninhydrin at pH 8.2, using sodium acetate buffer solution. Absorbance of the complex was measured at 395 nm. Various factors, such as volume of the ligand used, solution pH, stability of the complex with time and interference of other metals, which effect the complex formation have been studied in detail. Present developed method can be used for the spectrophotometric estimation of cobalt with ninhydrin complex. The method is simple, selective and cheap for the determination of cobalt in very less time.

  17. Sensitized spectrophotometric determination of Cr(III) ion for speciation of chromium ion in surfactant media using α-benzoin oxime

    NASA Astrophysics Data System (ADS)

    Ghaedi, Mehrorang; Asadpour, Enayat; Vafaie, Azam

    2006-01-01

    A simple and accurate micellanized spectrophotometric method for determination of trace amounts of Cr(III) ion in tab and top water and a synthetic mixture has been described. The micellar method is based on effect of organized molecular assemblies such as micelles in spectrophotometric measurement due to their effect on the systems of interest. The ability of micellar system in solubilizing of sparingly soluble ligand or complexes has been used for increasing figures of merit of an analytical method. Due to solubility increasing in aqueous media requirement for a primary extraction can be eliminated. Using the α-benzoin oxime (α-BO) spectrophotometric determination of Cr(III) ion has been performed and results are compared. The spectrophotometric determination of Cr(III) ion using α-BO in the presence of non-ionic surfactant Triton X-100 has been performed. The influence of type and amount of surfactant, pH, complexation time and amount of ligand were examined. Finally, the repeatability, accuracy and the effect of interfering ions on the determination of Cr(III) ion was evaluated. The proposed methods successfully with recovery yield of almost 100% have been applied to the rapid and simple determination of Cr(III) ion in the real samples. There is a good agreement between methods and atomic absorption spectrometry. The Beers law is obeyed over the concentration range of 0.1-13.7 μg mL-1 for micellar media. The detection limit is 0.8 ng mL-1. The molar absorptivity of complex is 5350 L mol-1 cm-1.

  18. The Rigorous Evaluation of Spectrophotometric Data to Obtain an Equilibrium Constant.

    ERIC Educational Resources Information Center

    Long, John R.; Drago, Russell S.

    1982-01-01

    Most students do not know how to determine the equilibrium constant and estimate the error in it from spectrophotometric data that contain experimental errors. This "dry-lab" experiment describes a method that may be used to determine the "best-fit" value of the 1:1 equilibrium constant to spectrophotometric data. (Author/JN)

  19. Prediction of sound absorption in rigid porous media with the lattice Boltzmann method

    NASA Astrophysics Data System (ADS)

    da Silva, Andrey Ricardo; Mareze, Paulo; Brandão, Eric

    2016-02-01

    In this work, sound absorption phenomena associated with the viscous shear stress within rigid porous media is investigated with a simple isothermal lattice Boltzmann BGK model. Simulations are conducted for different macroscopic material properties such as sample thickness and porosity and the results are compared with the exact analytical solution for materials with slit-like structure in terms of acoustic impedance and sound absorption coefficient. The numerical results agree very well with the exact solution, particularly for the sound absorption coefficient. The small deviations found in the low frequency limit for the real part of the acoustic impedance are attributed to the ratio between the thicknesses of the slit and the viscous boundary layer. The results suggest that the lattice Boltzmann method can be a very compelling numerical tool for simulating viscous sound absorption phenomena in the time domain, particularly due to its computational simplicity when compared to traditional continuum based techniques.

  20. Absorption and impedance boundary conditions for phased geometrical-acoustics methods.

    PubMed

    Jeong, Cheol-Ho

    2012-10-01

    Defining accurate acoustical boundary conditions is of crucial importance for room acoustic simulations. In predicting sound fields using phased geometrical acoustics methods, both absorption coefficients and surface impedances of the boundary surfaces can be used, but no guideline has been developed on which boundary condition produces accurate results. In this study, various boundary conditions in terms of normal, random, and field incidence absorption coefficients and normal incidence surface impedance are used in a phased beam tracing model, and the simulated results are validated with boundary element solutions. Two rectangular rooms with uniform and non-uniform absorption distributions are tested. Effects of the neglect of reflection phase shift are also investigated. It is concluded that the impedance, random incidence, and field incidence absorption boundary conditions produce reasonable results with some exceptions at low frequencies for acoustically soft materials.

  1. Enhanced plasmonic light absorption engineering of graphene: simulation by boundary-integral spectral element method.

    PubMed

    Niu, Jun; Luo, Ma; Zhu, Jinfeng; Liu, Qing Huo

    2015-02-23

    Graphene's relatively poor absorption is an essential obstacle for designing graphene-based photonic devices with satisfying photo-responsivity. To enhance the tunable light absorption of graphene, appropriate excitation of localized surface plasmon resonance is considered as a promising approach. In this work, the strategy of incorporating periodic cuboid gold nanoparticle (NP) cluster arrays and cylindrical gold NP arrays with Bragg reflectors into graphene-based photodetectors are theoretically studied by the boundary-integral spectral element method (BI-SEM). With the BI-SEM, the models can be numerically analyzed with excellent accuracy and efficiency. Numerical simulation shows that the proposed structures can effectively engineer the light absorption in graphene by tuning plasmon resonance. In the spectra of 300 nm to 1000 nm, a maximum light absorption of 67.54% is observed for the graphene layer with optimal parameters of the photodetector model.

  2. Enhancing prediction power of chemometric models through manipulation of the fed spectrophotometric data: A comparative study.

    PubMed

    Saad, Ahmed S; Hamdy, Abdallah M; Salama, Fathy M; Abdelkawy, Mohamed

    2016-10-01

    Effect of data manipulation in preprocessing step proceeding construction of chemometric models was assessed. The same set of UV spectral data was used for construction of PLS and PCR models directly and after mathematically manipulation as per well known first and second derivatives of the absorption spectra, ratio spectra and first and second derivatives of the ratio spectra spectrophotometric methods, meanwhile the optimal working wavelength ranges were carefully selected for each model and the models were constructed. Unexpectedly, number of latent variables used for models' construction varied among the different methods. The prediction power of the different models was compared using a validation set of 8 mixtures prepared as per the multilevel multifactor design and results were statistically compared using two-way ANOVA test. Root mean squares error of prediction (RMSEP) was used for further comparison of the predictability among different constructed models. Although no significant difference was found between results obtained using Partial Least Squares (PLS) and Principal Component Regression (PCR) models, however, discrepancies among results was found to be attributed to the variation in the discrimination power of adopted spectrophotometric methods on spectral data. PMID:27235828

  3. Enhancing prediction power of chemometric models through manipulation of the fed spectrophotometric data: A comparative study

    NASA Astrophysics Data System (ADS)

    Saad, Ahmed S.; Hamdy, Abdallah M.; Salama, Fathy M.; Abdelkawy, Mohamed

    2016-10-01

    Effect of data manipulation in preprocessing step proceeding construction of chemometric models was assessed. The same set of UV spectral data was used for construction of PLS and PCR models directly and after mathematically manipulation as per well known first and second derivatives of the absorption spectra, ratio spectra and first and second derivatives of the ratio spectra spectrophotometric methods, meanwhile the optimal working wavelength ranges were carefully selected for each model and the models were constructed. Unexpectedly, number of latent variables used for models' construction varied among the different methods. The prediction power of the different models was compared using a validation set of 8 mixtures prepared as per the multilevel multifactor design and results were statistically compared using two-way ANOVA test. Root mean squares error of prediction (RMSEP) was used for further comparison of the predictability among different constructed models. Although no significant difference was found between results obtained using Partial Least Squares (PLS) and Principal Component Regression (PCR) models, however, discrepancies among results was found to be attributed to the variation in the discrimination power of adopted spectrophotometric methods on spectral data.

  4. Self-referencing spectrophotometric measurements

    DOEpatents

    O'Rourke, Patrick E.; Van Hare, David R.

    1994-01-01

    A method for measuring the concentration of a chemical substance by spectrophotometry comprising the steps of placing a sample of a photoreactive substance between the light source and a spectrophotometer, obtaining an absorption spectrum of the substance using a fixed amount of light from the light source, obtaining a second absorption spectrum after a short interval, comparing the two to determine the concentration of the chemical substance from the difference in the spectra. If the chemical substance is not photoreactive, a photoreactive mixture can be made with a photoreactive dye that has photoreactive properties unique to the mixture. Alternatively, an optically transparent substrate can absorb the substance or the dye/substance mixture.

  5. Highly sensitive catalytic spectrophotometric determination of ruthenium

    NASA Astrophysics Data System (ADS)

    Naik, Radhey M.; Srivastava, Abhishek; Prasad, Surendra

    2008-01-01

    A new and highly sensitive catalytic kinetic method (CKM) for the determination of ruthenium(III) has been established based on its catalytic effect on the oxidation of L-phenylalanine ( L-Pheala) by KMnO 4 in highly alkaline medium. The reaction has been followed spectrophotometrically by measuring the decrease in the absorbance at 526 nm. The proposed CKM is based on the fixed time procedure under optimum reaction conditions. It relies on the linear relationship where the change in the absorbance (Δ At) versus added Ru(III) amounts in the range of 0.101-2.526 ng ml -1 is plotted. Under the optimum conditions, the sensitivity of the proposed method, i.e. the limit of detection corresponding to 5 min is 0.08 ng ml -1, and decreases with increased time of analysis. The method is featured with good accuracy and reproducibility for ruthenium(III) determination. The ruthenium(III) has also been determined in presence of several interfering and non-interfering cations, anions and polyaminocarboxylates. No foreign ions interfered in the determination ruthenium(III) up to 20-fold higher concentration of foreign ions. In addition to standard solutions analysis, this method was successfully applied for the quantitative determination of ruthenium(III) in drinking water samples. The method is highly sensitive, selective and very stable. A review of recently published catalytic spectrophotometric methods for the determination of ruthenium(III) has also been presented for comparison.

  6. On-site spectrophotometric determination of antimony in water, soil and dust samples of Central India.

    PubMed

    Shrivas, Kamlesh; Agrawal, Kavita; Harmukh, Neetu

    2008-06-30

    A new, selective and sensitive on-site spectrophotometric method for the determination of antimony at trace level in water, soil and dust samples of Central India has been demonstrated. It is based on the color reaction of Sb(III) with I(-) ions in the presence of a cationic surfactant cetylpyridinium chloride (CPC) in acidic media, and subsequent extraction of the complex with N-phenylbenzimidoylthiourea (PBITU) into chloroform to give a yellow colored complex. The value of apparent molar absorptivity of the complex in the terms of Sb is (7.84) x 10(4)l mol(-1)cm(-1) at 440 nm. The detection limit of the method is 5 ng ml(-1). In addition, the present method is free from interferences of all metal ions that are associated during the determination of antimony in environmental samples.

  7. On-site spectrophotometric determination of antimony in water, soil and dust samples of Central India.

    PubMed

    Shrivas, Kamlesh; Agrawal, Kavita; Harmukh, Neetu

    2008-06-30

    A new, selective and sensitive on-site spectrophotometric method for the determination of antimony at trace level in water, soil and dust samples of Central India has been demonstrated. It is based on the color reaction of Sb(III) with I(-) ions in the presence of a cationic surfactant cetylpyridinium chloride (CPC) in acidic media, and subsequent extraction of the complex with N-phenylbenzimidoylthiourea (PBITU) into chloroform to give a yellow colored complex. The value of apparent molar absorptivity of the complex in the terms of Sb is (7.84) x 10(4)l mol(-1)cm(-1) at 440 nm. The detection limit of the method is 5 ng ml(-1). In addition, the present method is free from interferences of all metal ions that are associated during the determination of antimony in environmental samples. PMID:18155833

  8. Product yield in oxygenation of linoleate by soybean lipoxygenase: the value of the molar extinction coefficient in the spectrophotometric assay.

    PubMed

    Gibian, M J; Vandenberg, P

    1987-06-01

    Two iodimetric methods and a gravimetric method were used to determine the spectrophotometric molar absorptivity of the purified product of lipoxygenase-catalyzed dioxygenation of linoleate (13-LS-hydroperoxy-cis,trans-9,11-octadecadienoate). Earlier determinations had led to the use of values varying from 24,000 to 28,000 M-1 cm-1 for epsilon at 235 nm. In the current work, the two iodimetric values (spectrophotometric and titrimetric) average 22,500, while gravimetric analysis of scrupulously purified material gives 22,900. Final 235-nm absorbancies for lipoxygenase runs over a wide range of linoleic acid concentrations up to 200 microM give a constant final percentage completion. If one assumes a 100% reaction, epsilon is 23,600. Each method has less than 1.5% standard error; the average of the three independent methods is 23,000 +/- 580 (2.5%), all being lower than the previous values. In the enzyme-catalyzed reaction of linoleate at less than 200 microM substrate, only 235-nm-absorbing material is formed. Above 200 microM linoleate, yields at 235 nm decrease and yields of materials absorbing at 280 nm increase (the latter is known to arise from lipoxygenase-catalyzed reaction of linoleyl hydroperoxide). Below 200 microM substrate, linoleate purified by HPLC produces only one HPLC-observable product, 13-linoleyl hydroperoxide. At higher substrate concentrations other HPLC peaks arise, again with higher wave-length absorptions. Spectrophotometric data using the epsilon determined here agree with those from the O2 electrode. It is concluded that at S less than 200 microM, saturating air, and sufficient enzyme, soybean lipoxygenase-1 produces a sole product and the reaction proceeds to completion.

  9. A simple method to incorporate water vapor absorption in the 15 microns remote temperature sounding

    NASA Technical Reports Server (NTRS)

    Dallu, G.; Prabhakara, C.; Conhath, B. J.

    1975-01-01

    The water vapor absorption in the 15 micron CO2 band, which can affect the remotely sensed temperatures near the surface, are estimated with the help of an empirical method. This method is based on the differential absorption properties of the water vapor in the 11-13 micron window region and does not require a detailed knowledge of the water vapor profile. With this approach Nimbus 4 IRIS radiance measurements are inverted to obtain temperature profiles. These calculated profiles agree with radiosonde data within about 2 C.

  10. Method of determining pH by the alkaline absorption of carbon dioxide

    DOEpatents

    Hobbs, D.T.

    1992-10-06

    A method is described for measuring the concentration of hydroxides in alkaline solutions in a remote location using the tendency of hydroxides to absorb carbon dioxide. The method includes the passing of carbon dioxide over the surface of an alkaline solution in a remote tank before and after measurements of the carbon dioxide solution. A comparison of the measurements yields the absorption fraction from which the hydroxide concentration can be calculated using a correlation of hydroxide or pH to absorption fraction. 2 figs.

  11. [A novel hyperspectra absorption enhancing method based on morphological top-hat transformation].

    PubMed

    Li, Hui; Lin, Qi-zhong; Wang, Qin-jun; Liu, Qing-jie; Chen, Yu

    2010-09-01

    Hyperspectral characteristics analysis of ground features is the basis for applications of high-resolution imaging technology to ground target identification and ground features classification. Based on morphological multi-scale Top-Hat transformation, a novel spectral absorption enhancing algorithms was put forward, which enhanced spectral absorption features while maintaining shape features of the absorption peak bands. Eleven reflectance spectra of different mineral groups were chosen from the mineral spectral library of the United States Geological Survey (USGS), and we used a K-means clustering analysis on both the absorption-enhanced spectra and the original reflectance spectra. Results showed that, firstly, clustering groups of the absorption-enhanced spectra (AES) had better similarity within the same clustering group, and greater difference between different groups, furthermore, they were more consistent with the geological background of these minerals compared with clustering result of the original spectra (OS). Secondly, while all the original spectra were re-sampled to their ASTER spectra and the AES clustering result was displayed in the form of ASTER spectra of the minerals, we could easily describe both the representative spectral feature of each clustering group, and the typical spectral differences between every two groups. These fully demonstrate that the absorption-enhanced spectra have enhanced absorption features of the mineral spectra, and improved the separability of hyper-spectra. Accordingly, feature analysis based on absorption enhanced spectra can be used as reference for information extracting based on multi-spectral remote sensing image data, and it is a very useful method of hyperspectral analysis. PMID:21105412

  12. Deriving brown carbon from multiwavelength absorption measurements: method and application to AERONET and Aethalometer observations

    NASA Astrophysics Data System (ADS)

    Wang, Xuan; Heald, Colette L.; Sedlacek, Arthur J.; de Sá, Suzane S.; Martin, Scot T.; Lizabeth Alexander, M.; Watson, Thomas B.; Aiken, Allison C.; Springston, Stephen R.; Artaxo, Paulo

    2016-10-01

    The radiative impact of organic aerosols (OA) is a large source of uncertainty in estimating the global direct radiative effect (DRE) of aerosols. This radiative impact includes not only light scattering but also light absorption from a subclass of OA referred to as brown carbon (BrC). However, the absorption properties of BrC are poorly understood, leading to large uncertainties in modeling studies. To obtain observational constraints from measurements, a simple absorption Ångström exponent (AAE) method is often used to separate the contribution of BrC absorption from that of black carbon (BC). However, this attribution method is based on assumptions regarding the spectral dependence of BC that are often violated in the ambient atmosphere. Here we develop a new AAE method which improves upon previous approaches by using the information from the wavelength-dependent measurements themselves and by allowing for an atmospherically relevant range of BC properties, rather than fixing these at a single assumed value. We note that constraints on BC optical properties and mixing state would help further improve this method. We apply this method to multiwavelength absorption aerosol optical depth (AAOD) measurements at AERONET sites worldwide and surface aerosol absorption measurements at multiple ambient sites. We estimate that BrC globally contributes up to 40 % of the seasonally averaged absorption at 440 nm. We find that the mass absorption coefficient of OA (OA-MAC) is positively correlated with the BC / OA mass ratio. Based on the variability in BC properties and BC / OA emission ratio, we estimate a range of 0.05-1.5 m2 g-1 for OA-MAC at 440 nm. Using the combination of AERONET and OMI UV absorption observations we estimate that the AAE388/440 nm for BrC is generally ˜ 4 worldwide, with a smaller value in Europe (< 2). Our analyses of observations at two surface sites (Cape Cod, to the southeast of Boston, and the GoAmazon2014/5 T3 site, to the west of

  13. Introduction of the carbon dioxide absorption method with closed circle breathing into anesthesia practice.

    PubMed

    Foregger, R

    2000-07-01

    The circle breathing CO2 absorption system for use during acetylene anesthesia was described by Carl Gauss in 1924/1925. The apparatus was manufactured by Drägerwerk of Lübeck. A considerable number of publications on the apparatus employing the closed circle method of CO2 absorption appeared in the medical press soon thereafter. Later apparatus models, also built by Drägerwerk, were adapted for nitrous oxide-oxygen-ether anesthesia and introduced into practice by Paul Sudeck and Helmut Schmidt. Information about all this was transmitted to America through the German medical press, including the Draeger-Hefte. American anesthesia machine manufacturers began to develop closed circle CO2 absorbers several years later. Claims that the circle breathing CO2 absorption method was introduced into anesthesia practice by Brian Sword are not valid. PMID:10969391

  14. Influence of protein composition and hydrolysis method on intestinal absorption of protein in man.

    PubMed

    Keohane, P P; Grimble, G K; Brown, B; Spiller, R C; Silk, D B

    1985-09-01

    An intestinal perfusion technique has been used in normal human subjects to investigate the influence that starter protein composition and hydrolysis procedure have on absorption of amino acid residues from partial enzymic hydrolysates of whole protein. Five starter proteins were studied. Three (egg albumin, casein/soy/lactalbumin, and lactalbumin) were hydrolysed by papain, a second lactalbumin starter protein, and a meat/soy/lactalbumin blend were hydrolysed by a porcine pancreatic enzyme system. Irrespective of starter protein composition or hydrolysis method used, four amino acid residues (threonine, glutamic acid, phenylalanine, and histidine) were absorbed significantly faster from all hydrolysates compared with absorption from their equivalent free amino acid mixtures. In contrast, both starter protein composition and hydrolysis method influenced absorption characteristics of up to nine other amino acid residues. PMID:4029718

  15. Method for improving terahertz band absorption spectrum measurement accuracy using noncontact sample thickness measurement.

    PubMed

    Li, Zhi; Zhang, Zhaohui; Zhao, Xiaoyan; Su, Haixia; Yan, Fang; Zhang, Han

    2012-07-10

    The terahertz absorption spectrum has a complex nonlinear relationship with sample thickness, which is normally measured mechanically with limited accuracy. As a result, the terahertz absorption spectrum is usually determined incorrectly. In this paper, an iterative algorithm is proposed to accurately determine sample thickness. This algorithm is independent of the initial value used and results in convergent calculations. Precision in sample thickness can be improved up to 0.1 μm. A more precise absorption spectrum can then be extracted. By comparing the proposed method with the traditional method based on mechanical thickness measurements, quantitative analysis experiments on a three-component amino acid mixture shows that the global error decreased from 0.0338 to 0.0301.

  16. Size separation method for absorption characterization in brown carbon: Application to an aged biomass burning sample

    NASA Astrophysics Data System (ADS)

    Di Lorenzo, Robert A.; Young, Cora J.

    2016-01-01

    The majority of brown carbon (BrC) in atmospheric aerosols is derived from biomass burning (BB) and is primarily composed of extremely low volatility organic carbons. We use two chromatographic methods to compare the contribution of large and small light-absorbing BrC components in aged BB aerosols with UV-vis absorbance detection: (1) size exclusion chromatography (SEC) and (2) reverse phase high-performance liquid chromatography. We observe no evidence of small molecule absorbers. Most BrC absorption arises from large molecular weight components (>1000 amu). This suggests that although small molecules may contribute to BrC absorption near the BB source, analyses of aerosol extracts should use methods selective to large molecular weight compounds because these species may be responsible for long-term BrC absorption. Further characterization with electrospray ionization mass spectrometry (MS) coupled to SEC demonstrates an underestimation of the molecular size determined through MS as compared to SEC.

  17. Method of analyzing multiple sample simultaneously by detecting absorption and systems for use in such a method

    DOEpatents

    Yeung, Edward S.; Gong, Xiaoyi

    2004-09-07

    The present invention provides a method of analyzing multiple samples simultaneously by absorption detection. The method comprises: (i) providing a planar array of multiple containers, each of which contains a sample comprising at least one absorbing species, (ii) irradiating the planar array of multiple containers with a light source and (iii) detecting absorption of light with a detetion means that is in line with the light source at a distance of at leaat about 10 times a cross-sectional distance of a container in the planar array of multiple containers. The absorption of light by a sample indicates the presence of an absorbing species in it. The method can further comprise: (iv) measuring the amount of absorption of light detected in (iii) indicating the amount of the absorbing species in the sample. Also provided by the present invention is a system for use in the abov metho.The system comprises; (i) a light source comrnpising or consisting essentially of at leaat one wavelength of light, the absorption of which is to be detected, (ii) a planar array of multiple containers, and (iii) a detection means that is in line with the light source and is positioned in line with and parallel to the planar array of multiple contiainers at a distance of at least about 10 times a cross-sectional distance of a container.

  18. A new photoacoustic method based on the modulation of the light induced absorption coefficient

    NASA Astrophysics Data System (ADS)

    Engel, S.; Wenisch, C.; Müller, F. A.; Gräf, S.

    2016-04-01

    The present study reports on a new photoacoustic (PA) measurement method that is suitable for the investigation of light induced absorption effects including e.g. excited state absorption. Contrary to the modulation of the radiation intensity used in conventional PA-methods, the key principle of this novel setup is based on the modulation of the induced absorption coefficient by light. For this purpose, a pump-probe setup with a pulsed pump laser beam and a continuous probe laser beam is utilized. In this regime, the potential influence of heat on the PA-signal is much smaller when compared to arrangements with pulsed probe beam and continuous pump beam. Beyond that, the negative effect of thermal lenses can be neglected. Thus, the measurement technique is well-suited for materials exhibiting a strong absorption at the pump wavelength. The quantitative analysis of the induced absorption coefficient was achieved by the calibration of the additional PA-signal caused by the continuous probe laser to the PA-signal resulting from the pulsed pump laser using thallium bromoiodide (KRS-5) as sample material.

  19. A benchmarking method to measure dietary absorption efficiency of chemicals by fish.

    PubMed

    Xiao, Ruiyang; Adolfsson-Erici, Margaretha; Åkerman, Gun; McLachlan, Michael S; MacLeod, Matthew

    2013-12-01

    Understanding the dietary absorption efficiency of chemicals in the gastrointestinal tract of fish is important from both a scientific and a regulatory point of view. However, reported fish absorption efficiencies for well-studied chemicals are highly variable. In the present study, the authors developed and exploited an internal chemical benchmarking method that has the potential to reduce uncertainty and variability and, thus, to improve the precision of measurements of fish absorption efficiency. The authors applied the benchmarking method to measure the gross absorption efficiency for 15 chemicals with a wide range of physicochemical properties and structures. They selected 2,2',5,6'-tetrachlorobiphenyl (PCB53) and decabromodiphenyl ethane as absorbable and nonabsorbable benchmarks, respectively. Quantities of chemicals determined in fish were benchmarked to the fraction of PCB53 recovered in fish, and quantities of chemicals determined in feces were benchmarked to the fraction of decabromodiphenyl ethane recovered in feces. The performance of the benchmarking procedure was evaluated based on the recovery of the test chemicals and precision of absorption efficiency from repeated tests. Benchmarking did not improve the precision of the measurements; after benchmarking, however, the median recovery for 15 chemicals was 106%, and variability of recoveries was reduced compared with before benchmarking, suggesting that benchmarking could account for incomplete extraction of chemical in fish and incomplete collection of feces from different tests.

  20. [Concentration retrieving method of SO2 using differential optical absorption spectroscopy based on statistics].

    PubMed

    Liu, Bin; Sun, Chang-Ku; Zhang, Chi; Zhao, Yu-Mei; Liu, Jun-Ping

    2011-01-01

    A concentration retrieving method using statistics is presented, which is applied in differential optical absorption spectroscopy (DOAS) for measuring the concentration of SO2. The method uses the standard deviation of the differential absorption to represents the gas concentration. Principle component analysis (PCA) method is used to process the differential absorption spectrum. In the method, the basis data for the concentration retrieval of SO2 is the combination of the PCA processing result, the correlation coefficient, and the standard deviation of the differential absorption. The method is applied to a continuous emission monitoring system (CEMS) with optical path length of 0.3 m. Its measuring range for SO2 concentration is 0-5 800 mg x m(-3). The nonlinear calibration and the temperature compensation for the system were executed. The full scale error of the retrieving concentration is less than 0.7% FS. And the measuring result is -4.54 mg x m(-3) when the concentration of SO2 is zero. PMID:21428087

  1. Simultaneous spectrophotometric determination of Fe(III) and Al(III) using orthogonal signal correction-partial least squares calibration method after solidified floating organic drop microextraction.

    PubMed

    Rohani Moghadam, Masoud; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh

    2015-01-25

    A solidified floating organic drop microextraction (SFODME) procedure was developed for the simultaneous extraction and preconcentration of Fe(III) and Al(III) from water samples. The method was based on the formation of cationic complexes between Fe(III) and Al(III) and 3,5,7,2',4'-pentahydroxyflavone (morin) which were extracted into 1-undecanol as ion pairs with perchlorate ions. The absorbance of the extracted complexes was then measured in the wavelength range of 300-450 nm. Finally, the concentration of each metal ion was determined by the use of the orthogonal signal correction-partial least squares (OSC-PLS) calibration method. Several experimental parameters that may be affected on the extraction process such as the type and volume of extraction solvent, pH of the aqueous solution, morin and perchlorate concentration and extraction time were optimized. Under the optimum conditions, Fe(III) and Al(III) were determined in the ranges of 0.83-27.00 μg L(-1) (R(2)=0.9985) and 1.00-32.00 μg L(-1) (R(2)=0.9979) of Fe(III) and Al(III), respectively. The relative standard deviations (n=6) at 12.80 μg L(-1) of Fe(III) and 17.00 μg L(-)(1) of Al(III) were 3.2% and 3.5%, respectively. An enhancement factors of 102 and 96 were obtained for Fe(III) and Al(III) ions, respectively. The procedure was successfully applied to determination of iron and aluminum in steam and water samples of thermal power plant; and the accuracy was assessed through the recovery experiments and independent analysis by electrothermal atomic absorption spectroscopy (ETAAS). PMID:25168229

  2. Simultaneous spectrophotometric determination of Fe(III) and Al(III) using orthogonal signal correction-partial least squares calibration method after solidified floating organic drop microextraction

    NASA Astrophysics Data System (ADS)

    Rohani Moghadam, Masoud; Haji Shabani, Ali Mohammad; Dadfarnia, Shayessteh

    2015-01-01

    A solidified floating organic drop microextraction (SFODME) procedure was developed for the simultaneous extraction and preconcentration of Fe(III) and Al(III) from water samples. The method was based on the formation of cationic complexes between Fe(III) and Al(III) and 3,5,7,2‧,4‧-pentahydroxyflavone (morin) which were extracted into 1-undecanol as ion pairs with perchlorate ions. The absorbance of the extracted complexes was then measured in the wavelength range of 300-450 nm. Finally, the concentration of each metal ion was determined by the use of the orthogonal signal correction-partial least squares (OSC-PLS) calibration method. Several experimental parameters that may be affected on the extraction process such as the type and volume of extraction solvent, pH of the aqueous solution, morin and perchlorate concentration and extraction time were optimized. Under the optimum conditions, Fe(III) and Al(III) were determined in the ranges of 0.83-27.00 μg L-1 (R2 = 0.9985) and 1.00-32.00 μg L-1 (R2 = 0.9979) of Fe(III) and Al(III), respectively. The relative standard deviations (n = 6) at 12.80 μg L-1 of Fe(III) and 17.00 μg L-1 of Al(III) were 3.2% and 3.5%, respectively. An enhancement factors of 102 and 96 were obtained for Fe(III) and Al(III) ions, respectively. The procedure was successfully applied to determination of iron and aluminum in steam and water samples of thermal power plant; and the accuracy was assessed through the recovery experiments and independent analysis by electrothermal atomic absorption spectroscopy (ETAAS).

  3. A novel 3D absorption correction method for quantitative EDX-STEM tomography.

    PubMed

    Burdet, Pierre; Saghi, Z; Filippin, A N; Borrás, A; Midgley, P A

    2016-01-01

    This paper presents a novel 3D method to correct for absorption in energy dispersive X-ray (EDX) microanalysis of heterogeneous samples of unknown structure and composition. By using STEM-based tomography coupled with EDX, an initial 3D reconstruction is used to extract the location of generated X-rays as well as the X-ray path through the sample to the surface. The absorption correction needed to retrieve the generated X-ray intensity is then calculated voxel-by-voxel estimating the different compositions encountered by the X-ray. The method is applied to a core/shell nanowire containing carbon and oxygen, two elements generating highly absorbed low energy X-rays. Absorption is shown to cause major reconstruction artefacts, in the form of an incomplete recovery of the oxide and an erroneous presence of carbon in the shell. By applying the correction method, these artefacts are greatly reduced. The accuracy of the method is assessed using reference X-ray lines with low absorption.

  4. A novel 3D absorption correction method for quantitative EDX-STEM tomography.

    PubMed

    Burdet, Pierre; Saghi, Z; Filippin, A N; Borrás, A; Midgley, P A

    2016-01-01

    This paper presents a novel 3D method to correct for absorption in energy dispersive X-ray (EDX) microanalysis of heterogeneous samples of unknown structure and composition. By using STEM-based tomography coupled with EDX, an initial 3D reconstruction is used to extract the location of generated X-rays as well as the X-ray path through the sample to the surface. The absorption correction needed to retrieve the generated X-ray intensity is then calculated voxel-by-voxel estimating the different compositions encountered by the X-ray. The method is applied to a core/shell nanowire containing carbon and oxygen, two elements generating highly absorbed low energy X-rays. Absorption is shown to cause major reconstruction artefacts, in the form of an incomplete recovery of the oxide and an erroneous presence of carbon in the shell. By applying the correction method, these artefacts are greatly reduced. The accuracy of the method is assessed using reference X-ray lines with low absorption. PMID:26484792

  5. Error Reduction Methods for Integrated-path Differential-absorption Lidar Measurements

    NASA Technical Reports Server (NTRS)

    Chen, Jeffrey R.; Numata, Kenji; Wu, Stewart T.

    2012-01-01

    We report new modeling and error reduction methods for differential-absorption optical-depth (DAOD) measurements of atmospheric constituents using direct-detection integrated-path differential-absorption lidars. Errors from laser frequency noise are quantified in terms of the line center fluctuation and spectral line shape of the laser pulses, revealing relationships verified experimentally. A significant DAOD bias is removed by introducing a correction factor. Errors from surface height and reflectance variations can be reduced to tolerable levels by incorporating altimetry knowledge and "log after averaging", or by pointing the laser and receiver to a fixed surface spot during each wavelength cycle to shorten the time of "averaging before log".

  6. Method for measuring changes in light absorption of highly scattering media

    DOEpatents

    Bigio, Irving J.; Johnson, Tamara M.; Mourant, Judith R.

    2002-01-01

    The noninvasive measurement of variations in absorption that are due to changes in concentrations of biochemically relevant compounds in tissue is important in many clinical settings. One problem with such measurements is that the pathlength traveled by the collected light through the tissue depends on the scattering properties of the tissue. It is demonstrated, using both Monte Carlo simulations and experimental measurements, that for an appropriate separation between light-delivery and light-collection fibers, the pathlength of the collected photons is insensitive to scattering parameters for the range of parameters typically found in tissue. This is important for developing rapid, noninvasive, inexpensive, and accurate methods for measuring absorption changes in tissue.

  7. Error reduction methods for integrated-path differential-absorption lidar measurements.

    PubMed

    Chen, Jeffrey R; Numata, Kenji; Wu, Stewart T

    2012-07-01

    We report new modeling and error reduction methods for differential-absorption optical-depth (DAOD) measurements of atmospheric constituents using direct-detection integrated-path differential-absorption lidars. Errors from laser frequency noise are quantified in terms of the line center fluctuation and spectral line shape of the laser pulses, revealing relationships verified experimentally. A significant DAOD bias is removed by introducing a correction factor. Errors from surface height and reflectance variations can be reduced to tolerable levels by incorporating altimetry knowledge and "log after averaging", or by pointing the laser and receiver to a fixed surface spot during each wavelength cycle to shorten the time of "averaging before log".

  8. Food Iron Absorption in Man APPLICATIONS OF THE TWO-POOL EXTRINSIC TAG METHOD TO MEASURE HEME AND NONHEME IRON ABSORPTION FROM THE WHOLE DIET

    PubMed Central

    Björn-Rasmussen, Erik; Hallberg, Leif; Isaksson, Björn; Arvidsson, Bertil

    1974-01-01

    A new radioisotope method to measure iron absorption from the whole diet was used in this study. The method is based on the concept that food iron is absorbed from two pools, the heme iron pool and the nonheme iron pool, which can be especially labeled with two radioiron isotopes given as hemoglobin and as an iron salt. The purpose of this study was to test the accuracy of this two-pool extrinsic tag method. The meals served were composed as an average of 6 wk consumption in the present material of 32 young enlisted men. The mean and total heme and nonheme iron absorption in all the 32 young men was 1.01±0.11. This figure agrees well with the mean daily losses expected for this group of subjects (1.0 mg). The conclusion can therefore be made that there are no major systematic errors of the present method to measure the total iron absorption from a mixed diet. In one series a comparison was made of the absorption of heme and nonheme iron from the meals. A significant correlation between the absorption of the two kinds of iron was found. However, a much greater fraction of the heme iron was absorbed (37%) than of the nonheme iron (5%). The absorption both from breakfast and lunch was in two series found to give a good prediction of the total daily nonheme iron absorption. One series was designed to compare the effect of two levels of iron fortification. There was a significant increase in iron absorption when the level of iron fortification of the meals was increased. PMID:4808639

  9. Optical absorption of dilute nitride alloys using self-consistent Green’s function method

    PubMed Central

    2014-01-01

    We have calculated the optical absorption for InGaNAs and GaNSb using the band anticrossing (BAC) model and a self-consistent Green’s function (SCGF) method. In the BAC model, we include the interaction of isolated and pair N levels with the host matrix conduction and valence bands. In the SCGF approach, we include a full distribution of N states, with non-parabolic conduction and light-hole bands, and parabolic heavy-hole and spin-split-off bands. The comparison with experiments shows that the first model accounts for many features of the absorption spectrum in InGaNAs; including the full distribution of N states improves this agreement. Our calculated absorption spectra for GaNSb alloys predict the band edges correctly but show more features than are seen experimentally. This suggests the presence of more disorder in GaNSb alloys in comparison with InGaNAs. PMID:24475947

  10. Method and apparatus for aerosol-particle absorption spectroscopy. [DOE patent application

    SciTech Connect

    Campillo, A.J.; Lin, H.B.

    1981-06-25

    A method and apparatus are described for determining the absorption spectra, and other properties, of aerosol particles. A heating beam source provides a beam of electromagnetic energy which is scanned through the region of the spectrum which is of interest. Particles exposed to the heating beam which have absorption bands within the band width of the heating beam absorb energy from the beam. The particles are also illuminated by light of a wave length such that the light is scattered by the particles. The absorption spectra of the particles can thus be determined from an analysis of the scattered light since the absorption of energy by the particles will affect the way the light is scattered. Preferably the heating beam is modulated to simplify the analysis of the scattered light. In one embodiment the heating beam is intensity modulated so that the scattered light will also be intensity modulated when the particles absorb energy. In another embodiment the heating beam passes through an interferometer and the scattered light reflects the Fourier Transform of the absorption spectra.

  11. Acoustic anechoic layers with singly periodic array of scatterers: Computational methods, absorption mechanisms, and optimal design

    NASA Astrophysics Data System (ADS)

    Yang, Hai-Bin; Li, Yue; Zhao, Hong-Gang; Wen, Ji-Hong; Wen, Xi-Sen

    2014-10-01

    The acoustic properties of anechoic layers with a singly periodic array of cylindrical scatterers are investigated. A method combined plane wave expansion and finite element analysis is extended for out-of-plane incidence. The reflection characteristics of the anechoic layers with cavities and locally resonant scatterers are discussed. The backing is a steel plate followed by an air half space. Under this approximate zero transmission backing condition, the reflection reduction is induced by the absorption enhancement. The absorption mechanism is explained by the scattering/absorption cross section of the isolated scatterer. Three types of resonant modes which can induce efficient absorption are revealed. Due to the fact that the frequencies of the resonant modes are related to the size of the scatterers, anechoic layers with scatterers of mixed size can broaden the absorption band. A genetic optimization algorithm is adopted to design the anechoic layer with scatterers of mixed size at a desired frequency band from 2 kHz to 10 kHz for normal incidence, and the influence of the incident angle is also discussed.

  12. Results of measurement of radio wave absorption in the ionosphere by the AI method

    NASA Technical Reports Server (NTRS)

    Korinevskaya, N. A.

    1972-01-01

    Median noon absorption values for each month from 1964 through 1967, the diurnal variations of absorption on the regular world days, and the seasonal variations of absorption are given. The dependence of the absorption coefficient on sunspot number is analyzed.

  13. Simple Monte Carlo methods to estimate the spectra evaluation error in differential-optical-absorption spectroscopy.

    PubMed

    Hausmann, M; Brandenburger, U; Brauers, T; Dorn, H P

    1999-01-20

    Differential-optical-absorption spectroscopy (DOAS) permits the sensitive measurement of concentrations of trace gases in the atmosphere. DOAS is a technique of well-defined accuracy; however, the calculation of a statistically sound measurement precision is still an unsolved problem. Usually one evaluates DOAS spectra by performing least-squares fits of reference absorption spectra to the measured atmospheric absorption spectra. Inasmuch as the absorbance from atmospheric trace gases is usually very weak, with optical densities in the range from 10(-5) to 10(-3), interference caused by the occurrence of nonreproducible spectral artifacts often determines the detection limit and the measurement precision. These spectral artifacts bias the least-squares fitting result in two respects. First, spectral artifacts to some extent are falsely interpreted as real absorption, and second, spectral artifacts add nonstatistical noise to spectral residuals, which results in a significant misestimation of the least-squares fitting error. We introduce two new approaches to investigate the evaluation errors of DOAS spectra accurately. The first method, residual inspection by cyclic displacement, estimates the effect of false interpretation of the artifact structures. The second method applies a statistical bootstrap algorithm to estimate properly the error of fitting, even in cases when the condition of random and independent scatter of the residual signal is not fulfilled. Evaluation of simulated atmospheric measurement spectra shows that a combination of the results of both methods yields a good estimate of the spectra evaluation error to within an uncertainty of ~10%.

  14. Improved method of exponential sum fitting of transmissions to describe the absorption of atmospheric gases.

    PubMed

    Armbruster, W; Fischer, J

    1996-04-20

    For climate modeling and atmospheric research, such as investigations of global climate change, remote sensing of cloud properties, or the missing absorption problem in clouds, it is most important to describe adequately the absorption of radiation by atmospheric gases. An improved method for the exponential sum fitting of transmissions (ESPT) is developed to approximate this absorption accurately. Exponentials are estimated separately for any number of atmospheric-model layers, considering the pressure and temperature dependence of the absorption lines directly. As long as the error of the fit exceeds a limit of tolerance, the number of considered exponential terms is successively increased. The accuracy of the method presented yields a root-mean-square error of less than 0.03% for any atmospheric-model layer, whereas the commonly used one-layer techniques gain errors of up to 3% in the transmission functions for the upper layers. The commonly used ESPT methods consider only one atmospheric layer and introduce the pressure and temperature effects for the other model layers afterward.

  15. A test of the possibility of calculating absorption spectra by mixed quantum-classical methods

    NASA Astrophysics Data System (ADS)

    Haug, Kenneth; Metiu, Horia

    1992-10-01

    Some of the most efficient methods for studying systems having a large number of degrees of freedom treat a few degrees of freedom quantum mechanically and the remainder classically. Here we examine how these methods fare when used to calculate the cross section for photon absorption by a quantum system imbedded in a medium. To test the method, we study a model which has two degrees of freedom and mimicks the properties of a one-dimensional alkali atom-He dimer. We treat the electron motion quantum mechanically and the distance between the He atom and the alkali ion classically. Light absorption occurs because the electron is coupled to radiation. The calculation of the absorption cross section by quantum-classical methods fails rather dramatically-at certain frequencies, the absorption coefficient is negative. By comparing with exact quantum calculations, we show that this failure takes place because the time evolution of the classical variables influences the dynamics of the quantum degree of freedom through the Hamiltonian only; important information, which a fully quantum treatment would put in the wave function, is missing. To repair this flaw, we experiment with a method which uses a swarm of classical trajectories to generate a ``classical wave function.'' The results are encouraging, but require substantial computer time when the number of classical variables is large. We argue that in the limit of many classical degrees of freedom, accurate calculations can be performed by using the time-dependent Hartree method and treating some degrees of freedom by exact numerical methods (e.g., a fast Fourier transform procedure) and the others by Gaussian wave packets or any other propagation method that is accurate for a very short time. This procedure leads to a simple time domain picture of dephasing and line broadening in the case of a localized quantum system imbedded in a medium with heavy atoms.

  16. Spectrophotometric analysis of irradiated spices.

    PubMed

    Josimović, 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.

  17. Spectrophotometric determination of rosuvastatin calcium in tablets.

    PubMed

    Uyar, B; Celebier, M; Altinoz, S

    2007-06-01

    Rosuvastatin calcium is a synthetic lipid lowering agent which is used in hypercholesterolemia. It is a selective and competitive inhibitor of HMG-CoA reductase. In this study a simple, rapid and reliable spectrophotometric method was developed for the determination of rosuvastatin calcium in pharmaceutical preparations. The solutions of standard and pharmaceutical samples were prepared in methanol. 243 nm was chosen for measuring absorbances of rosuvastatin calcium. The developed method was validated with respect to linearity range, limit of detection and quantitation, accuracy, precision, specificity and ruggudness. The linearity range of the method was 1.0-60.0 microg mL(-1). The limit of detection was 0.33 microg mL(-1). The developed and validated method was applied to the determination of rosuvastatin calcium in pharmaceutical preparations.

  18. Self-referencing spectrophotometric measurements

    DOEpatents

    O'Rourke, P.E.; Van Hare, D.R.

    1994-03-29

    A method is described for measuring the concentration of a chemical substance by spectrophotometry comprising the steps of placing a sample of a photoreactive substance between the light source and a spectrophotometer, obtaining an absorption spectrum of the substance using a fixed amount of light from the light source, obtaining a second absorption spectrum after a short interval, comparing the two to determine the concentration of the chemical substance from the difference in the spectra. If the chemical substance is not photoreactive, a photoreactive mixture can be made with a photoreactive dye that has photoreactive properties unique to the mixture. Alternatively, an optically transparent substrate can absorb the substance or the dye/substance mixture. 3 figures.

  19. Development of an extractive spectrophotometric method for estimation of uranium in ore leach solutions using 2-ethylhexyl phosphonic acid-mono-2-ethylhexyl ester (PC88A) and tri-n-octyl phosphine oxide (TOPO) mixture as extractant and 2-(5-bromo-2-pyridylozo)-5-diethyl aminophenol (Br-PADAP) as chromophore.

    PubMed

    Biswas, Sujoy; Pathak, P N; Roy, S B

    2012-06-01

    An extractive spectrophotometric analytical method has been developed for the determination of uranium in ore leach solution. This technique is based on the selective extraction of uranium from multielement system using a synergistic mixture of 2-ethylhexyl phosphonic acid-mono-2-ethylhexyl ester (PC88A) and tri-n-octyl phosphine oxide (TOPO) in cyclohexane and color development from the organic phase aliquot using 2-(5-Bromo-2-pyridylazo)-5-diethyl aminophenol (Br-PADAP) as chromogenic reagent. The absorption maximum (λ(max)) for UO(2)(2+)-Br-PADAP complex in organic phase samples, in 64% (v/v) ethanol containing buffer solution (pH 7.8) and 1,2-cyclohexylenedinitrilotetraacetic acid (CyDTA) complexing agent, has been found to be at 576 nm (molar extinction coefficient, ɛ: 36,750 ± 240 L mol(-1)cm(-1)). Effects of various parameters like stability of complex, ethanol volume, ore matrix, interfering ions etc. on the determination of uranium have also been evaluated. Absorbance measurements as a function of time showed that colored complex is stable up to > 24h. Presence of increased amount of ethanol in colored solution suppresses the absorption of a standard UO(2)(2+)-Br-PADAP solution. Analyses of synthetic standard as well as ore leach a solution show that for 10 determination relative standard deviation (RSD) is < 2%. The accuracy of the developed method has been checked by determining uranium using standard addition method and was found to be accurate with a 98-105% recovery rate. The developed method has been applied for the analysis of a number of uranium samples generated from uranium ore leach solutions and results were compared with standard methods like inductively coupled plasma emission spectrometry (ICPAES). The determined values of uranium concentrations by these methods are within ± 2%. This method can be used to determine 2.5-250 μg mL(-1) uranium in ore leach solutions with high accuracy and precision. PMID:22381794

  20. Novel spectrophotometric determination of flumethasone pivalate and clioquinol in their binary mixture and pharmaceutical formulation.

    PubMed

    Abdel-Aleem, Eglal A; Hegazy, Maha A; Sayed, Nour W; Abdelkawy, M; Abdelfatah, Rehab M

    2015-02-01

    This work is concerned with development and validation of three simple, specific, accurate and precise spectrophotometric methods for determination of flumethasone pivalate (FP) and clioquinol (CL) in their binary mixture and ear drops. Method A is a ratio subtraction spectrophotometric one (RSM). Method B is a ratio difference spectrophotometric one (RDSM), while method C is a mean center spectrophotometric one (MCR). The calibration curves are linear over the concentration range of 3-45 μg/mL for FP, and 2-25 μg/mL for CL. The specificity of the developed methods was assessed by analyzing different laboratory prepared mixtures of the FP and CL. The three methods were validated as per ICH guidelines; accuracy, precision and repeatability are found to be within the acceptable limits.

  1. A gamma-ray absorption method for the determination of uranium in ores

    USGS Publications Warehouse

    Hoyte, Alfred F.

    1957-01-01

    Current radioactivity methods used for the determination of uranium in ores are based on the assumption that secular equilibrium exists between the daughter products. Eichholz has developed a method which is claimed to be independent of the degree of equilibrium, but it has been found to be inadequate when used with some types of disequilibriated ores. An absorption method has been developed for the determination of uranium which is independent of the secular equilibrium of the series. With some refinement this method may used to determine the state of equilibrium of an ore.

  2. Spectrophotometric determination of isopropamide iodide and trifluoperazine hydrochloride in presence of trifluoperazine oxidative degradate.

    PubMed

    Abbas, Samah S; Zaazaa, Hala E; Abdelkawy, M; Abdelrahman, Maha M

    2010-04-01

    Four sensitive, selective and precise stability indicating methods for the determination of isopropamide iodide (ISO) and trifluoperazine hydrochloride (TPZ) in their binary mixture and in presence of trifluoperazine oxidative degradate (OXD). Method A is a derivative spectrophotometric one, where ISO was determined by first derivative (D(1)) at 226.4 nm while TPZ was determined by second derivative (D(2)) at 270.2 nm. Method B is the first derivative of the ratio spectra (DD(1)) spectrophotometric method, ISO can be determined by measuring the peak amplitude at 227.4 nm using 5 microg mL(-1) of OXD as a divisor, while TPZ can be determined by measuring the peak amplitude at 249.2 and 261.4 nm using 15 microg mL(-1) of ISO as a divisor. Method C is the isoabsorptive spectrophotometric method. This method allows determination of ISO and TPZ in their binary mixture by measuring total concentration of ISO and TPZ at their isoabsorptive point at lambda(229.8) nm (Aiso1) while TPZ concentration alone can be determined at lambda(max) 311.2 nm, then ISO concentration can be determined by subtraction. On the same basis TPZ can be determined in presence of ISO and OXD, where OXD concentration alone was determined by measuring the peak amplitude at lambda(281.6) and lambda(309.4) nm while total concentration of TPZ and OXD was determined at their isoabsorptive points at (Aiso2 = 270.2 nm), (Aiso3 = 310.6 nm) and (Aiso4 = 331.8 nm) then TPZ concentration was determined by subtraction. Method D is the multivariate calibration techniques [the classical least squares (CLS), principal component regression (PCR) and partial least squares (PLS)], using the information contained in the absorption spectra of ISO, TPZ and OXD mixtures. The selectivity of the proposed methods was checked using laboratory prepared mixtures. The proposed methods have been successfully applied to the analysis of ISO and TPZ in pharmaceutical dosage form without interference from other dosage form

  3. Spectrophotometric determination of the fungicide captan.

    PubMed

    Galeano, Teresa; Guiberteau, Agustina; Mora, Nielene M; Alvarez, Pedro R; Salinas, Francisco

    2002-11-01

    A spectrophotometric method for the determination of the fungicide captan has been developed based on its reaction with thiosemicarbazide. The absorbance was measured at 315 nm. The effects of the proportion of water, thiosemicarbazide concentration, pH and temperature on this reaction was studied to select the best chemical conditions. The calibration graph was obtained between 1.2 and 30 ppm and the detection limit is 0.5 ppm. The RSD (n = 10) was 1.34%. Possible interference of various pesticides was examined. The method was applied to the determination of captan in agrochemical formulations. Results agree well with the labelled values and also with results that were obtained by a polarographic method.

  4. [A new retrieval method for ozone concentration at the troposphere based on differential absorption lidar].

    PubMed

    Fan, Guang-Qiang; Liu, Jian-Guo; Liu, Wen-Qing; Lu, Yi-Huai; Zhang, Tian-Shu; Dong, Yun-Sheng; Zhao, Xue-Song

    2012-12-01

    Aerosols interfere with differential absorption lidar ozone concentration measurement and can introduce significant errors. A new retrieval method was introduced, and ozone concentration and aerosol extinction coefficient were gained simultaneously based on the retrieval method. The variables were analyzed by experiment including aerosol lidar ratio, aerosol wavelength exponent, and aerosol-molecular ratio at the reference point. The results show that these parameters introduce error less than 8% below 1 km. The measurement error derives chiefly from signal noise and the parameters introduce error less than 3% above 1 km. Finally the vertical profile of tropospheric ozone concentration and aerosol extinction coefficient were derived by using this algorithm. The retrieval results of the algorithm and traditional dual-wavelength difference algorithm are compared and analyzed. Experimental results indicate that the algorithm is feasible, and the algorithm can reduce differential absorption lidar measurement error introduced by aerosol.

  5. Spectrophotometric properties of Mercury

    NASA Astrophysics Data System (ADS)

    Domingue, D.; Vilas, F.; Holsclaw, G. M.; Warell, J.; Izenberg, N. R.; Murchie, S. L.; Denevi, B. W.; Blewett, D. T.; McClintock, W. E.

    2009-12-01

    The MEcury Surface, Space ENvironment, GEochemistry, and Ranging (MESSENGER) spacecraft obtained photometric observations of Mercury during three flybys (14 January 2008, 6 October 2008, 29 September 2009) using both the Mercury Dual Imaging System (MDIS) and the Mercury Atmospheric and Surface Composition Spectrometer (MASCS). The MDIS measurements include disk-integrated phase-curve observations taken in 11 narrow-band filters ranging from 430 to 1010 nm. The MDIS measurements also include disk-resolved photometric observations taken during the first flyby of a 200-km by 400-km region (centered on 1.7°S, 123.5°E, and spanning 5.5° of latitude and 10° of longitude) over a phase-angle range between 51° and 120°. The MASCS measurements include disk-integrated phase-curve observations taken from 300 to 1450 nm at a spectral resolution of 2.5 nm. During the third flyby, targeted type regions were observed at multiple viewing geometries, providing disk-resolved photometric measurements at high spectral resolution. Comparisons with ground-based observations show that the phase behavior determined by analysis of the MDIS and MASCS observations is consistent with previous studies. Reflectance measurements from the first two flybys show no definitive absorption features and a distinctive steep, or “red,” slope with increasing wavelength common to space-weathered rocky surfaces. The MDIS spectra show evidence of phase reddening (increased spectral slope with increasing phase angle), similar to that observed on the Moon. The derived photometric properties indicate a more compact, less porous regolith that is smoother on meter scales than regolith on the Moon or S-type asteroids. Although Mercury is darker than the average lunar nearside, the calculated geometric albedo (reflectance at zero phase) is higher for Mercury than the Moon, implying a greater opposition-surge magnitude. The geometric albedo, coupled with the lower reflectance of immature (younger) units on

  6. Determination of Calcium in Cereal with Flame Atomic Absorption Spectroscopy: An Experiment for a Quantitative Methods of Analysis Course

    ERIC Educational Resources Information Center

    Bazzi, Ali; Kreuz, Bette; Fischer, Jeffrey

    2004-01-01

    An experiment for determination of calcium in cereal using two-increment standard addition method in conjunction with flame atomic absorption spectroscopy (FAAS) is demonstrated. The experiment is intended to introduce students to the principles of atomic absorption spectroscopy giving them hands on experience using quantitative methods of…

  7. AN INTERCOMPARISON CF THE INTEGRATING PLATE AND THE LASER TRANSMISSION METHODS FOR DETERMINATION OF AEROSOL ABSORPTION COEFFICIENTS

    SciTech Connect

    Sadler, M.; Charlson, R.J.; Rosen, H.; Novakov, T.

    1980-07-01

    The absorption coefficients determined by the integrating plate method and the laser transmission method are found to be comparable and highly correlated. Furthermore, a high correlation is found between these absorption coefficients and the carbon content of the aerosol in urbanized regions.

  8. Method for the discrimination of superficial and deep absorption variations by time domain fNIRS.

    PubMed

    Zucchelli, Lucia; Contini, Davide; Re, Rebecca; Torricelli, Alessandro; Spinelli, Lorenzo

    2013-01-01

    A method for the discrimination of superficial and deep absorption variations by time domain functional near infrared spectroscopy is presented. The method exploits the estimate of the photon time-dependent pathlength in different domains of the sampled medium and makes use of an approach based on time-gating of the photon distribution of time-of-flights. Validation of the method is performed in the two-layer geometry to focus on muscle and head applications. Numerical simulations varied the thickness of the upper layer, the interfiber distance, the shape of the instrument response function and the photon counts. Preliminary results from in vivo data are also shown.

  9. Method for the discrimination of superficial and deep absorption variations by time domain fNIRS

    PubMed Central

    Zucchelli, Lucia; Contini, Davide; Re, Rebecca; Torricelli, Alessandro; Spinelli, Lorenzo

    2013-01-01

    A method for the discrimination of superficial and deep absorption variations by time domain functional near infrared spectroscopy is presented. The method exploits the estimate of the photon time-dependent pathlength in different domains of the sampled medium and makes use of an approach based on time-gating of the photon distribution of time-of-flights. Validation of the method is performed in the two-layer geometry to focus on muscle and head applications. Numerical simulations varied the thickness of the upper layer, the interfiber distance, the shape of the instrument response function and the photon counts. Preliminary results from in vivo data are also shown. PMID:24409389

  10. FDTD method for laser absorption in metals for large scale problems.

    PubMed

    Deng, Chun; Ki, Hyungson

    2013-10-21

    The FDTD method has been successfully used for many electromagnetic problems, but its application to laser material processing has been limited because even a several-millimeter domain requires a prohibitively large number of grids. In this article, we present a novel FDTD method for simulating large-scale laser beam absorption problems, especially for metals, by enlarging laser wavelength while maintaining the material's reflection characteristics. For validation purposes, the proposed method has been tested with in-house FDTD codes to simulate p-, s-, and circularly polarized 1.06 μm irradiation on Fe and Sn targets, and the simulation results are in good agreement with theoretical predictions.

  11. Microwave absorption properties of amorphous iron nanostructures fabricated by a high-yield method

    NASA Astrophysics Data System (ADS)

    Wang, Zhen; Zuo, Yalu; Yao, Yuelin; Xi, Li; Du, Jihong; Wang, Jianbo; Xue, Desheng

    2013-04-01

    Amorphous Fe nanoparticles and a nanonecklace were synthesized at room temperature by an aqueous reduction procedure, which provided a simple and potential method for volume production of ferromagnetic materials. The morphology was examined by scanning electron microscopy and transmission electron microscopy. The amorphism of Fe nanoparticles and the nanonecklace was confirmed by x-ray diffraction and electron diffraction patterns in transmission electron microscopy. The complex permittivity and permeability behaviour of amorphous iron nanoparticles/paraffin wax (NPPW) and nanonecklace/paraffin wax (NCPW) composites was investigated in 0.1-18 GHz by a coaxial method. The strongest reflection loss values of NPPW and NCPW calculated from permittivity and permeability reached -53.2 dB and -47.8 dB at 6.4 GHz and 4.6 GHz with matching thicknesses of 2.4 mm and 2.3 mm, respectively. Moreover, the frequency ranges of microwave absorption exceeding 90% were around 4.9-8.8 GHz and 3.7-6.1 GHz for NPPW and NCPW, respectively. Comparing the microwave absorption property with crystallized Fe nanostructures, we may conclude that the relatively high resistivity and low permittivity of amorphous Fe nanostructures are favourable for impedance matching, and consequently result in the attracting microwave absorption property of amorphous Fe nanostructures. Thus, amorphous iron nanoparticles and the nanonecklace prepared by a high-yield method have great potential to be a highly efficient microwave absorber.

  12. Method and apparatus for enhancing surface absorption and emissivity in optical pulsed infrared nondestructive evaluation

    NASA Astrophysics Data System (ADS)

    Duan, Yuxia; Zhang, Cunlin; Jin, Wanping; Wu, Naiming

    2009-07-01

    In the application of optical pulsed infrared NDE, the visible light absorption and IR emissivity of the detected object must be considered. One of the simple methods is spraying paint on the highly reflective and low IR emissivity surface before testing. However, for some materials such as with pore space in the surface or easily to be corrupted have to be pretreated by other method and apparatus. Two kinds of apparatus for surface pretreating are designed according to the dimension of the detected object and the testing conditions. One apparatus is independent of the former detecting system, and the other is an improvement of the former system. The basic principle of the two apparatus is covering a flexible membrane of high light absorption and IR emissivity on the specimen surface by vacuum pumping. The paper also present the applications of the method, including the detection of the metal mesh material and the honeycomb structures with aluminum coating. The experimental results show that the technique of covering thin film by vacuum pump is effective for enhancing surface absorption and emissivity; moreover, it does not pollute or damage the sample. The application of the technique has practical significance, because it extends the scope of the application of the optical pulsed thermography nondestructive evaluation.

  13. A Spectrophotometric Study of the Permanganate-Oxalate Reaction: An Analytical Laboratory Experiment

    ERIC Educational Resources Information Center

    Kalbus, Gene E.; Lieu, Van T.; Kalbus, Lee H.

    2004-01-01

    The spectrophotometric method assists in the study of potassium permanganate-oxalate reaction. Basic analytical techniques and rules are implemented in the experiment, which can also include the examination of other compounds oxidized by permanganate.

  14. Systems having optical absorption layer for mid and long wave infrared and methods for making the same

    DOEpatents

    Kuzmenko, Paul J

    2013-10-01

    An optical system according to one embodiment includes a substrate; and an optical absorption layer coupled to the substrate, wherein the optical absorption layer comprises a layer of diamond-like carbon, wherein the optical absorption layer absorbs at least 50% of mid wave infrared light (3-5 .mu.m wavelength) and at least 50% of long wave infrared light (8-13 .mu.m wavelength). A method for applying an optical absorption layer to an optical system according to another embodiment includes depositing a layer of diamond-like carbon of an optical absorption layer above a substrate using plasma enhanced chemical vapor deposition, wherein the optical absorption layer absorbs at least 50% of mid wave infrared light (3-5 .mu.m wavelength) and at least 50% of long wave infrared light (8-13 .mu.m wavelength). Additional systems and methods are also presented.

  15. Application of oxidants to the spectrophotometric determination of amlodipine besylate in pharmaceutical formulations.

    PubMed

    Rahman, Nafisur; Singh, Manisha; Hoda, Md Nasrul

    2004-11-01

    Three new spectrophotometric methods for the determination of amlodipine besylate have been proposed. The first two methods, i.e. A and B, are based on the oxidation of the drug with Fe(III) and the estimation of Fe(II) produced after chelation with either 1,10-phenanthroline or 2,2'-bipyridyl at 500 and 515 nm, respectively. The Beer's law was obeyed in the concentration ranges of 2-10 and 4-14 microg ml(-1) with molar absorptivity of 2.9 x 10(4) and 2.7 x 10(4) l mol(-1) cm(-1) for methods A and B, respectively. The third procedure depends on the interaction of amlodipine besylate with ammonium heptamolybdate tetrahydrate, which resulted in the formation of molybdenum blue (lambda(max) 825 nm). The linear dynamic range and the molar absorptivity values were found to be 15-59 microg ml(-1) and 1.8 x 10(4) l mol(-1) cm(-1), respectively. The results of the proposed procedures were validated statistically and compared with those obtained by the reference method. The proposed methods were applied successfully to the determination of amlodipine besylate in commercial tablets.

  16. Determination of platinum originated from antitumoral drugs in human urine by atomic absorption spectrometric methods.

    PubMed

    da Costa, Anilton Coelho; Vieira, Mariana Antunes; Luna, Aderval Severino; de Campos, Reinaldo Calixto

    2010-10-15

    Cisplatin and carboplatin are the most common platinum-based drugs used in cancer treatment. Pharmacokinetic investigations, the evaluation of the body burden during the treatment, as well as baseline levels of platinum in humans have attracted great interest. Thus, accurate analytical methods for fast and easy Pt monitoring in clinical samples become necessary. In the present study atomic absorption spectrometric methods for the determination of platinum in the forms of cisplatin and carboplatin in human urine were investigated. Platinum, in these different forms, could be determined in urine, after simple sample dilution. Regarding electrothermal atomic absorption spectrometry, the optimum parameters were defined by a central composite design optimization. Multiplicative matrix effects were overcome by using a mixture of HCl and NaCl as modifier. The limit of detection (LOD) was 0.004 mgL(-1) of platinum in the original sample. For the analysis of more concentrated samples, high resolution continuous source flame atomic absorption spectrometry was also investigated. Flame conditions were optimized by a multivariate D-optimal design, using as response the sum of the analyte addition calibration slopes and their standard deviations. Matrix matched external calibration with PtCl(2) calibration solutions, was possible, and the LOD was 0.06 mgL(-1) in the original sample. The results obtained by the proposed procedures were also in good agreement with those obtained by an independent comparative procedure.

  17. Effect of Sn on the optical band gap determined using absorption spectrum fitting method

    SciTech Connect

    Heera, Pawan; Kumar, Anup; Sharma, Raman

    2015-05-15

    We report the preparation and the optical studies on tellurium rich glasses thin films. The thin films of Se{sub 30}Te{sub 70-x} Sn{sub x} system for x= 0, 1.5, 2.5 and 4.5 glassy alloys prepared by melt quenching technique are deposited on the glass substrate using vacuum thermal evaporation technique. The analysis of absorption spectra in the spectral range 400nm–4000 nm at room temperature obtained from UV-VIS-NIR spectrophotometer [Perkin Elmer Lamda-750] helps us in the optical characterization of the thin films under study. The absorption spectrum fitting method is applied by using the Tauc’s model for estimating the optical band gap and the width of the band tail of the thin films. The optical band gap is calculated and is found to decrease with the Sn content.

  18. A projective reconstruction method of underground or hidden structures using atmospheric muon absorption data

    NASA Astrophysics Data System (ADS)

    Bonechi, L.; D'Alessandro, R.; Mori, N.; Viliani, L.

    2015-02-01

    Muon absorption radiography is an imaging technique based on the analysis of the attenuation of the cosmic-ray muon flux after traversing an object under examination. While this technique is now reaching maturity in the field of volcanology for the imaging of the innermost parts of the volcanic cones, its applicability to other fields of research has not yet been proved. In this paper we present a study concerning the application of the muon absorption radiography technique to the field of archaeology, and we propose a method for the search of underground cavities and structures hidden a few metres deep in the soil (patent [1]). An original geometric treatment of the reconstructed muon tracks, based on the comparison of the measured flux with a reference simulated flux, and the preliminary results of specific simulations are discussed in details.

  19. Methods to Parameterize Brown Carbon, Distinguish Brown Carbon Absorption From Enhanced Black Carbon Absorption, and Assess the Stability of Brown Carbon to Photochemical Aging

    NASA Astrophysics Data System (ADS)

    Murphy, S. M.; Pokhrel, R. P.; Beamesderfer, E.; Wagner, N. L.; Langridge, J.; Lack, D.

    2015-12-01

    We present results obtained during the Fire Lab at Missoula Experiment-4 (FLAME-4) with a combination of multi-wavelength photoacoustic and cavity ringdown spectrometers. It will be shown that the single scattering albedo and Angstrom exponent of biomass burning emissions can be better parameterized by the organic carbon to black carbon ratio than by the modified combustion efficiency. Two different methods to distinguish the contribution to aerosol absorption from brown carbon versus black carbon and enhanced black carbon absorption will be presented. One method is based on extending the absorption seen at 660 nm with an assumed Angstrom exponent while the other assumes a similar absorption enhancement (determined via thermal denuder) of black carbon at 660 and 405 nm. Potential errors and advantages of both methods will be discussed. Finally, chamber experiments that show degradation of brown carbon by photochemical oxidation will be presented along with a number of methods by which to assess the amount of brown carbon that is degraded.

  20. A comparison of pharmacokinetic methods for in vivo studies of nonmediated glucose absorption.

    PubMed

    Napier, Kathryn R; McWhorter, Todd J; Fleming, Patricia A

    2012-01-01

    Two pharmacokinetic methods are used primarily to assess systematic bioavailability of orally dosed water-soluble compounds in vivo, but there have been no direct comparisons of the estimates obtained. The "area under the curve" (AUC) method employs a single oral dose of probe compound(s) followed by multiple blood sampling to obtain plasma concentration time curves. Separate injection of probe(s) followed by multiple blood sampling is used to calculate fractional elimination rate (K(el)) and distribution pool space (S). The "steady state feeding" method relies on ad lib. feeding of a marked diet, with a single blood sample taken to measure steady state feeding concentration of probe(s); K(el) is estimated from the decline in probe concentration in excreta after injection, with a single blood sample taken to estimate S. We compared these methods directly in the Australian red wattlebird (Anthochaera carnunculata), measuring absorption of (3)H-L-glucose. The K(el) values estimated using the steady state feeding protocol were significantly higher, and estimates of S and bioavailability consequently lower, compared with the AUC protocol. The AUC method relies on fewer assumptions and allows simultaneous comparisons of absorption by mediated and nonmediated (i.e., paracellular) mechanisms but cannot be easily applied to freely feeding animals. The steady state feeding method allows work with smaller species and exploration of the effects of feeding on nutrient uptake but requires careful attention to the validity of assumptions that increase error in the calculations.

  1. In Situ Density Measurement of Basaltic Melts at High Pressure by X-ray Absorption Method

    NASA Astrophysics Data System (ADS)

    Ando, R.; Ohtani, E.; Suzuki, A.; Urakawa, S.; Katayama, Y.

    2004-12-01

    Density of silicate melt at high pressure is one of the most important properties to understand magma migration in the planetary interior. However, because of experimental difficulties, the density of magma at high pressure is poorly known. Katayama et al. (1996) recently developed a new in situ density measurement method for metallic melts, based on the density dependency of X-ray absorption in the sample. In this study, we tried to measure the density of basaltic melt by this absorption method. When X-ray is transmitted to the sample, the intensity of the transmitted X-ray beam (I) is expressed as follows; I=I0exp(-μ ρ t), where I0 is the intensity of incident X-ray beam, μ is the mass absorption coefficient, ρ is the density of the sample, and t is the thickness of the sample. If t and μ are known, we can determine the density of the sample by measuring I and I0. This is the principle of the absorption method for density measurement. In this study, in order to determine t, we used a single crystalline diamond cylinder as a sample capsule, diamond is less compressive and less deformable so that even at high pressure t (thickness of the sample at the point x) is expressed as follows; t = 2*(R02-x2)1/2, R0 is the inner radius of cylinder at the ambient condition, and x is distance from a center of the capsule. And diamond also shows less absorption so that this make it possible to measure the density of silicate melt with smaller absorption coefficient than metallic melts. In order to know the μ of the sample, we measured both densities (ρ ) and absorptions (I/I0) for some glasses and crystals with same composition of the sample at the ambient condition, and calculated as fallows; μ =ln(I/I0)/ρ . Experiments were made at the beamline (BL22XU) of SPring-8. For generation of high pressure and high temperature, we used DIA-type cubic anvil apparatus (SMAP180) there. We used tungsten carbide anvils with the edge-length of 6 mm. The energy of monochromatic X

  2. Screening of conditions controlling spectrophotometric sequential injection analysis

    PubMed Central

    2011-01-01

    Background Despite its potential benefits over univariate, chemometrics is rarely utilized for optimizing sequential injection analysis (SIA) methods. Specifically, in previous vis-spectrophotometric SIA methods, chemometrically optimized conditions were confined within flow rate and reagent concentrations while other conditions were ignored. Results The current manuscript reports, for the first time, a comprehensive screening of conditions controlling vis-spectrophotometric SIA. A new diclofenac assay method was adopted. The method was based on oxidizing diclofenac by permanganate (a major reagent) with sulfuric acid (a minor reagent). The reaction produced a spectrophotometrically detectable diclofenac form. The 26 full-factorial design was utilized to study the effect of volumes of reagents and sample, in addition to flow rate and concentrations of reagents. The main effects and all interaction order effects on method performance, i.e. namely sensitivity, rapidity and reagent consumption, were determined. The method was validated and applied to pharmaceutical formulations (tablets, injection and gel). Conclusions Despite 64 experiments those conducted in the current study were cumbersome, the results obtained would reduce effort and time when developing similar SIA methods in the future. It is recommended to critically optimize effective and interacting conditions using other such optimization tools as fractional-factorial design, response surface and simplex, rather than full-factorial design that used at an initial optimization stage. In vis-spectrophotometric SIA methods those involve developing reactions with two reagents (major and minor), conditions affecting method performance are in the following order: sample volume > flow rate ≈ major reagent concentration >> major reagent volume ≈ minor reagent concentration >> minor reagent volume. PMID:21333024

  3. Spectrophotometric determination of nitrite in soil and water using cefixime and central composite design.

    PubMed

    Shariati-Rad, Masoud; Irandoust, Mohsen; Mohammadi, Shabnam

    2015-01-01

    The present paper seeks to develop a simple method for the spectrophotometric determination of nitrite in soil and water samples and also measure optimum reaction conditions along with other analytical parameters. The method is based on the diazotization-coupling reaction of nitrite with cefixime and 1-naphthylamine in an acidic solution (Griess reaction). The final product that is an azo dye has an orange color with maximum absorption at 360 nm which Beer's Law is obeyed over the concentration range 0.02-15.00 mg L(-1) of nitrite. Optimal conditions of the variables affecting the reaction were obtained by central composite design (CCD). A detection limit of 4.3×10(-3) mg L(-1) was obtained for determination of nitrite by the proposed method. The proposed method was successfully applied to determine nitrite in soil and water samples. The molar absorptivity of the product of the reaction and RSD in determination of nitrite in real samples are 4.1×10(3) (L mol(-1) cm(-1)) and lower than 10%, respectively.

  4. Spectrophotometric determination of nitrite in soil and water using cefixime and central composite design

    NASA Astrophysics Data System (ADS)

    Shariati-Rad, Masoud; Irandoust, Mohsen; Mohammadi, Shabnam

    2015-10-01

    The present paper seeks to develop a simple method for the spectrophotometric determination of nitrite in soil and water samples and also measure optimum reaction conditions along with other analytical parameters. The method is based on the diazotization-coupling reaction of nitrite with cefixime and 1-naphthylamine in an acidic solution (Griess reaction). The final product that is an azo dye has an orange color with maximum absorption at 360 nm which Beer's Law is obeyed over the concentration range 0.02-15.00 mg L-1 of nitrite. Optimal conditions of the variables affecting the reaction were obtained by central composite design (CCD). A detection limit of 4.3 × 10-3 mg L-1 was obtained for determination of nitrite by the proposed method. The proposed method was successfully applied to determine nitrite in soil and water samples. The molar absorptivity of the product of the reaction and RSD in determination of nitrite in real samples are 4.1 × 103 (L mol-1 cm-1) and lower than 10%, respectively.

  5. Method and apparatus for measuring butterfat and protein content using microwave absorption techniques

    DOEpatents

    Fryer, Michael O.; Hills, Andrea J.; Morrison, John L.

    2000-01-01

    A self calibrating method and apparatus for measuring butterfat and protein content based on measuring the microwave absorption of a sample of milk at several microwave frequencies. A microwave energy source injects microwave energy into the resonant cavity for absorption and reflection by the sample undergoing evaluation. A sample tube is centrally located in the resonant cavity passing therethrough and exposing the sample to the microwave energy. A portion of the energy is absorbed by the sample while another portion of the microwave energy is reflected back to an evaluation device such as a network analyzer. The frequency at which the reflected radiation is at a minimum within the cavity is combined with the scatter coefficient S.sub.11 as well as a phase change to calculate the butterfat content in the sample. The protein located within the sample may also be calculated in a likewise manner using the frequency, S.sub.11 and phase variables. A differential technique using a second resonant cavity containing a reference standard as a sample will normalize the measurements from the unknown sample and thus be self-calibrating. A shuttered mechanism will switch the microwave excitation between the unknown and the reference cavities. An integrated apparatus for measuring the butterfat content in milk using microwave absorption techniques is also presented.

  6. Simultaneous spectrophotometric determination of cyanide and thiocyanate after separation on a melamine-formaldehyde resin.

    PubMed

    Gümüş, G; Demirata, B; Apak, R

    2000-11-01

    A simple indirect spectrophotometric method for the determination of cyanide, based on the oxidation of the cyanide with chlorine (Cl(2)) is described. The residual chlorine is determined by the color reaction with o-tolidine (3,3'-dimethylbenzidine). The maximum absorbance for Cl(2) is at 437 nm. A linear calibration graph (0-4.0x10(-5) M CN(-)) is obtained under optimal reaction conditions at room temperature and pH 11-12. The stoichiometric mole ratio of chlorine to cyanide is 1:1. The effective molar absorptivity for cyanide is 5.87x10(4) l mol(-1) cm(-1) at pH 1.6. The limit of quantification (LOQ) is 3.6x10(-7) M or 9.4 ppb. Effects of pH, excess reagent, sensitivity, reaction time and tolerance limits of interferent ions are reported. The method was applied to the determination of cyanide in a real sample. The basic interferent usually accompanying CN(-), i.e. thiocyanate, is separated from cyanide by sorption on a melamine-formaldehyde resin at pH 9 while cyanide is not retained. Thiocyanate is eluted with 0.4 M NaOH from the column and determined spectrophotometrically using the acidic FeCl(3) reagent. The initial column effluent containing cyanide was analyzed by both the developed chlorine-o-tolidine method and the conventional barbituric acid-pyridine (Spectroquant 14800) procedure, and the results were statistically compared. The developed method is relatively inexpensive and less laborious than the standard (Spectroquant) procedure, and insensitive to the common interferent, cyanate (CNO(-)).

  7. Voltammetric and spectrophotometric techniques for the determination of the antihypertensive drug Prazosin in urine and formulations.

    PubMed

    Arranz, A; de Betoño, S F; Echevarria, C; Moreda, J M; Cid, A; Valentín, J F

    1999-12-01

    A sensitive method was developed to determine Prazosin using a nafion modified carbon paste electrode (NMCPE). Prazosin was accumulated at a potential of 750 mV in Britton-Robinson buffer (pH 6.0) and then a negative sweep was made obtaining a cathodic peak close to 0 V. Cyclic voltammetric studies indicated that the process was quasi-reversible, and fundamentally controlled by adsorption. To obtain a good sensitivity, the instrumental and accumulation variables were studied using differential pulse voltammetry (DPV). Adsorptive voltammetric peak currents showed a linear response for Prazosin concentrations in the range between 4.0 x 10(-11) and 4.0 x 10(-8) M with two different slopes, and a detection limit (LOD) of 3.1 x 10(-11)M was obtained. The variation coefficient (CV) for a 8.0 x 10(-10) M solution (n = 10) was 4.08%. A spectrophotometric study of Prazosin was also carried out and two absorption bands were obtained at 246 and 329 nm (pH 1.8). The band at 329 nm was pH-dependent and its height and position changed with the pH values, so this allowed the pK'a determination (7.14 +/- 0.20) using different methods. The detection limit reached by means of UV-spectrophotometry was 0.9 x 10(-7) M, and the variation coefficient for 1.5 x 10(-5) M Prazosin solutions was 1.14% (n = 10). Although the sensitivity of the UV-spectrophotometric method was lower than that obtained using adsorptive stripping-differential pulse voltammetry (AdS-DPV), it could be applied to the determination of Prazosin in Minipres tablets. The voltammetric method was used for the determination of the drug in human urine samples at trace levels with good recoveries.

  8. Comparisons of selected methods for the determination of kinetic parameters from electrothermal atomic absorption data

    NASA Astrophysics Data System (ADS)

    Fonseca, Rodney W.; Pfefferkorn, Lisa L.; Holcombe, James A.

    1994-12-01

    Three of the methods available for the determination of kinetic parameters for atom formation in ETAAS were compared. In the approach of mcnally and holcombe [ Anal. Chem. 59, 1015 (1987)], Arrhenius-type plots are used to extract activation energy values while an approximation of the order of release is obtained by studying the alignment of the absorption maxima at increasing analyte concentrations. In the method of rojas and olivares [ Spectrochim. Acta47B, 387 (1992)], plots are prepared for different orders of release, with the correct order yielding a longer linear region from whose slope the activation energy is calculated. The method of yan et al. [ Spectrochim. Acta48B, 605 (1993)] uses a single absorption profile for the calculations. Activation energy and the order of release are obtained from the slope and intercept, respectively, on their graph. All three methods assume linear heating rate, constant activation energies, and furnace isothermality. The methods were tested with the same experimental data sets for Cu, Au and Ni using a spatially isothermal cuvette. Since intensive mathematical treatments commonly have deleterious effects on the uncertainty of the final result, the methods were compared using both the original data and a smoothed version of it. In general, the three methods yielded comparable results for the metals studied. However, choosing the most linear plot to determine the correct order of release when using Rojas and Olivares' method was sometimes subjective, and McNally and Holcombe's method provided only estimates for the orders of release that were neither zero nor unity.

  9. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    PubMed

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC. PMID:15910814

  10. Cinchocaine hydrochloride determination by atomic absorption spectrometry and spectrophotometry.

    PubMed

    Abdel-Ghani, Nour T; Youssef, Ahmed F A; Awady, Mohamed A

    2005-05-01

    Two sensitive spectrophotometric and atomic absorption spectrometric procedures have been developed for determination of cinchocaine hydrochloride (Cin.Cl) in pure form and in pharmaceutical formulation. The spectrophotometric method was based on formation of an insoluble colored ion-associate between the cited drug and tetrathiocyanatocobaltate (CoTC) or hexathiocyanatochromate (CrTC) which dissolved and extracted in an organic solvent. The optimal experimental conditions for quantitative extraction such as pH, concentration of the reagents and solvent were studied. Toluene and iso-butyl alcohol proved to be the most suitable solvents for quantitative extraction of Cin-CoTC and Cin-CrTC ion-associates with maximum absorbance at 620 and 555 nm, respectively. The optimum concentration ranges, molar absorptivities, Ringbom ranges and Sandell sensitivities were also evaluated. The atomic absorption spectrometric method is based on measuring of the excess cobalt or chromium in the aqueous solution, after precipitation of the drug, at 240.7 and 357.9 nm, respectively. Linear application ranges, characteristic masses and detection limits were 57.99-361.9, 50.40 and 4.22 microg ml(-1) of Cin.Cl, in case of CoTC, while 37.99-379.9, 18.94 and 0.81 microg ml(-1) in case of CrTC.

  11. An atomic-absorption method for the determination of gold in large samples of geologic materials

    USGS Publications Warehouse

    VanSickle, Gordon H.; Lakin, Hubert William

    1968-01-01

    A laboratory method for the determination of gold in large (100-gram) samples has been developed for use in the study of the gold content of placer deposits and of trace amounts of gold in other geologic materials. In this method the sample is digested with bromine and ethyl ether, the gold is extracted into methyl isobutyl ketone, and the determination is made by atomicabsorption spectrophotometry. The lower limit of detection is 0.005 part per million in the sample. The few data obtained so far by this method agree favorably with those obtained by assay and by other atomic-absorption methods. About 25 determinations can be made per man-day.

  12. Reconstruction of optical absorption coefficient maps of heterogeneous media by photoacoustic tomography coupled with diffusion equation based regularized Newton method.

    PubMed

    Yuan, Zhen; Wang, Qiang; Jiang, Huabei

    2007-12-24

    We describe a novel reconstruction method that allows for quantitative recovery of optical absorption coefficient maps of heterogeneous media using tomographic photoacoustic measurements. Images of optical absorption coefficient are obtained from a diffusion equation based regularized Newton method where the absorbed energy density distribution from conventional photoacoustic tomography serves as the measured field data. We experimentally demonstrate this new method using tissue-mimicking phantom measurements and simulations. The reconstruction results show that the optical absorption coefficient images obtained are quantitative in terms of the shape, size, location and optical property values of the heterogeneities examined.

  13. Spectrophotometric determination of trace amounts of phosphate in water and soil.

    PubMed

    Ganesh, S; Khan, Fahmida; Ahmed, M K; Velavendan, P; Pandey, N K; Kamachi Mudali, U

    2012-01-01

    A simple spectrophotometric method has been developed for the determination of phosphate dissolved in soil and water. The method is based on the formation of phosphomolybdate with added ammonium molybdate followed by reduction with hydrazine in acidic medium. Orthophosphate and molybdate ions condense in acidic solution to give molybdophosphoric (phosphomolybdic) acid, which upon selective reduction (perhaps with hydrazinium sulphate) produces a blue colour, due to molybdenum blue of uncertain composition. 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 830 nm. The system obeys Lambert-Beer's law at 830 nm in the concentration range of 0.5-5 μg/mL of phosphate with a relative standard deviation (RSD) of 0.1% and correlation coefficient of 0.99. Molar absorptivity was determined to be 2.9 × 10⁴ L mol⁻¹ cm⁻¹ at 830 nm. The method is also applicable for the determination of phosphate in nuclear reprocessing plants, medical science, clinical science, agriculture, metallurgy and environmental science.

  14. Spectrophotometric determination of meclozine HCl and papaverine HCl in their pharmaceutical formulations.

    PubMed

    Abdel-Ghani, N T; Shoukry, A F; Issa, Y M; Wahdan, O A

    2002-04-15

    A simple, accurate and highly sensitive spectrophotometric method is proposed for the rapid determination of meclozine and papaverine hydrochlorides using chromotrope 2B (C2B) and chromotrope 2R (C2R). The method consists of extracting the formed ion-associates into chloroform in the case of meclozine HCl and into methylene chloride in case of papaverine HCl. The ion-associates exhibit absorption maxima at 536 and 524 nm for C2B and C2R with meclozine HCl and at 540 and 528 nm with papaverine HCl, respectively. Meclozine can be determined up to 4.0 and 2.6 mg ml(-1), using C2B and C2R, respectively, while papaverine can be determined up to 1.68 and 1.37 mg ml(-1), respectively. The effect of acidity, reagent concentration, time, solvent and stoichiometric ratio of the ion-associates were studied. The molar absorptivity and Sandell sensitivity of the reaction products were calculated. The method was applied to the determination of the drugs in their pure state or pharmaceutical preparations with mean recovery values of 99.63-100.80 and 99.75-100.08% and coefficient of variation 0.945-2.210 and 1.020-1.268 for meclozine HCl and papaverine HCl, respectively. PMID:11929681

  15. Comparison of three methods for measuring light absorption by collected aerosols.

    PubMed

    Ramsey-Bell, D C; Couture, G

    1985-08-01

    Three instruments for measuring absorption of visible light by atmospheric aerosols are compared: the visual comparator; plate diffuser; and photoacoustic spectrometer. Two versions of the photoacoustic spectrometer are tested, one built of acrylic plastic and the other of aluminum. One version of the visual comparator uses Millipore filters for a crucial reflective surface, another a mirror. Several materials collected on Nuclepore filters are used in the comparison. Laboratory generated samples consist of carbon and carbon overlaid with ammonium sulfate. Atmospheric aerosols were collected in Tucson and on an Arizona mountain peak. All methods give reasonably consistent results, even when applied to the lightly absorbing nonurban atmospheric samples. PMID:18223896

  16. Moisture absorption characteristics of the Orbiter thermal protection system and methods used to prevent water ingestion

    NASA Technical Reports Server (NTRS)

    Schomburg, C.; Dotts, R. L.; Tillian, D. J.

    1983-01-01

    The Space Shuttle Orbiter's silica tile Thermal Protection System (TPS) is beset by the moisture absorption problems inherently associated with low density, highly porous insulation systems. Attention is presently given to the comparative success of methods for the minimization and/or prevention of water ingestion by the TPS tiles, covering the development of water-repellent agents and their tile application techniques, flight test program results, and materials improvements. The use of external films for rewaterproofing of the TPS tiles after each mission have demonstrated marginal to unacceptable performance. By contrast, a tile interior waterproofing agent has shown promise.

  17. Spectrophotometric discrimination of river dissolved organic matter

    NASA Astrophysics Data System (ADS)

    Baker, Andy

    2002-11-01

    There is a need to be able to differentiate the dissolved organic matter (DOM) fraction in river waters. Research in the 1970s and 1980s has attempted to utilize both absorbance and fluorescence to distinguish between DOM fractions in river waters, but both were limited by the available technology. Total organic carbon content has, therefore, been widely used as a standard method of measuring DOM concentration, although it has little power to differentiate DOM fractions. Recent advances in fluorescence spectrophotometry enable rapid and optically precise analysis of DOM. Here, we show how a combination of both fluorescence and absorbance can be used to discriminate statistically between spatial variations of DOM in tributaries in a small catchment of the Ouseburn, NE England. The results of the discriminant analysis suggest that about 70% of the samples can be correctly classified to its tributary. Discriminant function 1 explains 60·8% of the variance in the data and the fulvic-like fluorescence intensity has the largest absolute correlation within this function; discriminant function 2 explains a further 21·5% of the variance and the fulvic-like fluorescence emission wavelength has the largest absolute correlation within this function. The discriminant analysis does not correctly classify all tributaries every time, and successfully discriminates between the different tributaries 70% of the time. Occasions when the tributary waters are less well discriminated are due to either episodic pollution events (at two sites) or due to tributaries that have strong seasonal trends in spectrophotometric parameters, which allows the sites to be misclassified. Results suggest that spectrophotometric techniques have considerable potential in the discrimination of DOM in rivers.

  18. Density Measurement for MORB Melts by X-ray Absorption Method

    NASA Astrophysics Data System (ADS)

    Sakamaki, T.; Urakawa, S.; Suzuki, A.; Ohtani, E.; Katayama, Y.

    2006-12-01

    Density of silicate melts at high pressure is one of the most important properties to understand magma migration in the planetary interior and the differentiation of the terrestrial planets. The density measurements of silicate melts have been carried out by several methods (shock compression experiments and sink-float method in static experiments, etc.). However, since these methods have difficulties in acquisition of data at a desired pressure and temperature, the density of the silicate melt have been measured under only a few conditions. Recently a new density measurement was developed by the X-ray absorption method. Advantage of this method is to measure density of liquids at a desired pressure and temperature. In the present study we measured the density of MORB melt by X-ray absorption method. Experiments were carried out at the BL22XU beamline at SPring-8. A DIA-type cubic anvil apparatus was used for generation of high pressure and temperature. We used tungsten carbide anvils with the top anvil sizes of 6 mm and 4 mm. The energy of monochromateized X-ray beam was 23 keV. The intensities of incident and transmitted X-ray were measured by ion chambers. The density of the melt was calculated on the basis of Beer-Lambert law. The starting material was a glass with the MORB composition. Experiments were made from 1 atm to 5 GPa, from 300 to 2000 K. We compared the density of MORB melt with the compression curve of the melt in previous works. The density measured by this study is lower than that expected from the compression curve determined at higher pressures by the sink-float method. Structural change of the MORB melt with increasing pressure might be attributed to this discrepancy.

  19. Density Measurement for MORB Melts by X-ray Absorption Method

    NASA Astrophysics Data System (ADS)

    Sakamaki, T.; Urakawa, S.; Ohtani, E.; Suzuki, A.; Katayama, Y.

    2005-12-01

    Density of silicate melts at high pressure is one of the most important properties to understand magma migration in the planetary interior and the differentiation of the terrestrial planets. The density measurements of silicate melts have been carried out by several methods (shock compression experiments and sink-float method in static experiments, etc.). However, since these methods have difficulties in acquisition of data at a desired pressure and temperature, the density of the silicate melt have been measured under only a few conditions. Recently a new density measurement was developed by the X-ray absorption method. Advantage of this method is to measure density of liquids at a desired pressure and temperature. In the present study we measured the density of MORB melt by X-ray absorption method. Experiments were carried out at the BL22XU beamline at SPring-8. A DIA-type cubic anvil apparatus was used for generation of high pressure and temperature. We used tungsten carbide anvils with the edge-length of 6 mm. The energy of monochromateized X-ray beam was 23 keV. The intensities of incident and transmitted X-ray were measured by ion chambers. The density of the melt was calculated on the basis of Beer-Lambert law. The starting material was a glass with the MORB composition. Experiments were made from 1 atm to 4 GPa, from 300 to 2200 K. We compared the density of MORB melt with the compression curve of the melt in previous works. The density measured by this study is lower than that expected from the compression curve determined at higher pressures by the sink-float method. Structural change of the MORB melt with increasing pressure might be attributed to this discrepancy.

  20. Spectrophotometric determination of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid in pure form and in pharmaceuticals

    NASA Astrophysics Data System (ADS)

    Bazel, Yaroslav; Hunka, Iryna; Kormosh, Zholt; Andruch, Vasil

    2009-12-01

    A new sensitive and selective spectrophotometric method has been developed for the determination of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid in pharmaceuticals in the presence of nicotinic acid. The method is based on the reaction of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid with 1,3,3-trimethyl-5-phenyl-2-[3-(1,3,3-trimethyl-1,3-dihydro-indol-2-ylidene)-propenyl]-3 H-indolium chloride (PIC) followed by the extraction of the formed ion associate into toluene and spectrophotometric detection at 581 nm. Appropriate experimental conditions were found to be pH 7.8-9.8 and 3.6 × 10 -4 mol L -1 of PIC. The molar absorptivity is 5.0 × 10 -4 L mol -1 cm -1. The absorbance obeys Beer's law in the range 0.61-12.60 μg mL -1 of [2-(2,6-dichloro-phenylamino)-phenyl]-acetic acid, and the detection limit calculated from a blank test was 0.20 μg mL -1.

  1. Density, ultrasound velocity, acoustic impedance, reflection and absorption coefficient determination of liquids via multiple reflection method.

    PubMed

    Hoche, S; Hussein, M A; Becker, T

    2015-03-01

    The accuracy of density, reflection coefficient, and acoustic impedance determination via multiple reflection method was validated experimentally. The ternary system water-maltose-ethanol was used to execute a systematic, temperature dependent study over a wide range of densities and viscosities aiming an application as inline sensor in beverage industries. The validation results of the presented method and setup show root mean square errors of: 1.201E-3 g cm(-3) (±0.12%) density, 0.515E-3 (0.15%) reflection coefficient and 1.851E+3 kg s(-1) m(-2) (0.12%) specific acoustic impedance. The results of the diffraction corrected absorption showed an average standard deviation of only 0.12%. It was found that the absorption change shows a good correlation to concentration variations and may be useful for laboratory analysis of sufficiently pure liquids. The main part of the observed errors can be explained by the observed noise, temperature variation and the low signal resolution of 50 MHz. In particular, the poor signal-to-noise ratio of the second reflector echo was found to be a main accuracy limitation. Concerning the investigation of liquids the unstable properties of the reference material PMMA, due to hygroscopicity, were identified to be an additional, unpredictable source of uncertainty. While dimensional changes can be considered by adequate methodology, the impact of the time and temperature dependent water absorption on relevant reference properties like the buffer's sound velocity and density could not be considered and may explain part of the observed deviations.

  2. Absorption spectrophotometric, NMR and theoretical investigations on ground state non-covalent interaction of C₆₀ and C₇₀ with a designed trihomocalix[6]arene in solution.

    PubMed

    Halder, Amal; Kundu, Kshama; Nayak, Sandip K; Chattopadhyay, Subrata; Bhattacharya, Sumanta

    2012-07-01

    The present paper reports the spectroscopic investigations on non-covalent interaction of fullerenes C(60) and C(70) with a designed trihomocalix[6]arene (2) in toluene. UV-vis studies reveal appreciable ground state interaction between fullerenes and 2. Jobs method of continuous variation establishes 1:1 stoichiometry for fullerene-2 complexes. Binding constant (K) data reveals that 2 binds C(70) more strongly compared to C(60), i.e. K(C60-2)-47,540 dm(3)mol(-1) and K(C70-2)-86,360 dm(3)mol(-1). Proton NMR studies provide very good support in favor of strong binding between C(70) and 2. Estimation of solvent reorganization energy (R(S)) evokes that C(70)-2 complex is stabilized more compared to C(60)-2 complex as R(S(C60-2))- -1.162 eV and R(S(C70-2))- -1.244eV. Semiempirical calculations at third parametric level of theory in vacuo evoke the single projection structures of the fullerene-2 complexes and interpret the stability difference between C(60) and C(70) complexes of 2 in terms of enthalpies of formation values.

  3. Method 200.12 - Determination of Trace Elements in Marine Waters by StabilizedTemperature Graphite Furnace Atomic Absorption

    EPA Science Inventory

    This method provides procedures for the determination of total recoverable elements by graphite furnace atomic absorption (GFAA) in marine waters, including estuarine, ocean and brines with salinities of up to 35 ppt.

  4. A real-time in-vivo method for studying the percutaneous absorption of volatile chemicals.

    PubMed

    Thrall, K D; Poet, T S; Corley, R A; Tanojo, H; Edwards, J A; Weitz, K K; Hui, X; Maibach, H I; Wester, R C

    2000-01-01

    Realistic estimates of percutaneous absorption following exposures to solvents in the workplace, or through contaminated soil and water, are critical to understanding human health risks. A method was developed to determine dermal uptake of solvents under non-steady-state conditions using real-time breath analysis in rats, monkeys, and humans. The exhaled breath was analyzed using an ion-trap mass spectrometer, which can quantitate chemicals in the exhaled breath stream in the 1-5 ppb range. The resulting data were evaluated using physiologically-based pharmacokinetic (PBPK) models to estimate dermal permeability constants (Kp) under various exposure conditions. The effects of exposure matrix (soil versus water), occlusion versus non-occlusion, and species differences on the absorption of methyl chloroform, trichloroethylene, and benzene were compared. Exposure concentrations were analyzed before and at 0.5-hour intervals throughout the exposures. The percentage of each chemical absorbed and the corresponding Kp were estimated by optimization of the PBPK model to the medium concentration and the exhaled-breath data. The method was found to be sufficiently sensitive for animal and human dermal studies at low exposure concentrations over small body surface areas, for short periods, using non-steady-state exposure conditions.

  5. Spectrophotometric determination of pipazethate HCl, dextromethorphan HBr and drotaverine HCl in their pharmaceutical preparations.

    PubMed

    Amin, Alaa S; El-Sheikh, Ragaa; Zahran, Faten; Gouda, Ayman Abou El-fetouh

    2007-07-01

    A simple, accurate and highly sensitive spectrophotometric method is proposed for the rapid determination of pipazethate hydrochloride, dextromethorphan hydrobromide and drotaverine hydrochloride using chromotrope 2B (C2B) and chromotrope 2R (C2R). The method consists of extracting the formed ion-associates into chloroform in the case of pipazethate HCl and dextromethorphan HBr or into methylene chloride in the case of drotaverine HCl. The ion-associates exhibit absorption maxima at 528, 540 and 532 nm with C2B and at 526, 517 and 522 nm with C2R for pipazethate HCl, dextromethorphan HBr and drotaverine HCl, respectively. The calibration curves resulting from the measurements of absorbance-concentration relations (at the optimum reaction conditions) of the extracted ion-pairs are linear over the concentration range 4.36-52.32 microg mL(-1) for pipazethate, 3.7-48.15 microg mL(-1) for dextromethorphan and 4.34-60.76 microg mL(-1) for drotaverine, respectively. The effect of acidity, reagent concentration, time, solvent and stoichiometric ratio of the ion-associates were estimated. The molar absorptivity and Sandell sensitivity of the reaction products were calculated. Statistical treatment of the results reflects that the procedure is precise, accurate and easily applied for the determination of the drugs under investigation in pure form and in their pharmaceutical preparations.

  6. Spectrophotometric Determination of Pipazethate HCl and Dextromethorphan HBr using Potassium Permanganate

    PubMed Central

    Gouda, Ayman Abou El-Fetouh; El-Sheikh, Ragaa; El Shafey, Zeineb.; Hossny, Nagda.; El-Azzazy, Rham

    2008-01-01

    Rapid, simple and sensitive validated spectrophotometric methods have been described for the assay of pipazethate HCl (PiCl) and dextromethorphan HBr (DEX) 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 λmax=521, 485, 610 and 664 nm, respectively. Beer’s law is obeyed in the concentration range of 2.0-16 and 2.0-15 μg mL-1 for PiCl and DEX, respectively with correlation coefficient (n=6) ≥ 0.9993. The apparent molar absorptivity and sandell sensitivity values are in the range 1.062-1.484 × 104, 3.35-4.51 × 104 L mol-1 cm-1 and 29.36-41.03, 8.21-11.06 ng cm-2 for PiCl and DEX, 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. PMID:23675101

  7. Application of potassium permanganate to spectrophotometric assay of metoclopramide hydrochloride in pharmaceuticals

    NASA Astrophysics Data System (ADS)

    Devi, O. Zenita; Basavaiah, K.; Vinay, K. B.

    2012-01-01

    Two simple, sensitive, and cost-effective spectrophotometric methods are described for the determination of metoclopramide hydrochloride (MCP) in pharmaceutical dosage forms. The methods are based on a redox reaction between MCP and KMnO4 in alkaline and acid media. Direct spectrophotometry (method A) involves treating MCP with permanganate in an NaOH medium and measuring a bluish green product at 610 nm. In indirect spectrophotometry (method B), MCP is treated with a fixed concentration of KMnO4 in an H2SO4 medium, and after a specified time, the unreacted KMnO4 is measured at 545 nm. Under optimum assay conditions, Beer's law is obeyed over the ranges of 0.75-12.0 and 2.5-30.0 g/ml for methods A and B, respectively. Molar absorptivity values are calculated to be 2.33•104 and 2.66•104 l/mol cm for methods A and B, respectively, and corresponding Sandell's sensitivity values are 0.015 and 0.013 g/cm2. Limits of detection (LOD) and quantification (LOQ) are also reported. The applicability of the developed methods was demonstrated by the determination of MCP in tablet and injection forms. The accuracy and reliability of the proposed methods were further ascertained by recovery studies via standard addition technique.

  8. Dual-isotope method for determination of human zinc absorption: the use of a test meal of turkey meat

    SciTech Connect

    Flanagan, P.R.; Cluett, J.; Chamberlain, M.J.; Valberg, L.S.

    1985-01-01

    The percentage of /sup 65/Zn taken up (absorbed) from extrinsically labeled turkey meat was calculated from the amounts of /sup 65/Zn and a nonabsorbed /sup 51/Cr marker present in the body or in a single stool specimen after 1-2 d. /sup 51/CrCl/sub 3/ proved to be a suitable marker for unabsorbed /sup 65/Zn and so the early determination of /sup 65/Zn absorption was possible. With stool counting, /sup 65/Zn absorption data from first stool samples after 1-2 d were accurate as judged by correlation with the amount of /sup 65/Zn in the body 7-10 d later (retention); results from subsequent stools gave lower absorption values due to the early excretion of some absorbed /sup 65/Zn. The dual-isotope method gave reproducible results when four successive tests of zinc absorption were carried out in a group of six subjects. The average (mean +/- SD) /sup 65/Zn absorption from turkey meals containing 31 mumol (2 mg) and 46 mumol (3 mg) of zinc was 39 +/- 8% and 29 +/- 6%, respectively, measured by stool counting; /sup 65/Zn absorption and retention correlated well in both studies. A series of different beverages was given in place of water with the turkey meal. Orange juice significantly reduced /sup 65/Zn absorption and milk also showed this tendency, but tea, whiskey, wine or beer had no significant effect on the absorption of /sup 65/Zn from the turkey meal. In groups of subjects the mean ratio of /sup 65/Zn absorption from extrinsically labeled turkey meat on two occasions (1.06) was not significantly different from that of the absorption of extrinsic to intrinsic /sup 65/Zn labels (1.16). The dual-isotope technique with either stool or body counting is suitable for the rapid determination of /sup 65/Zn absorption from extrinsically labeled turkey within 2 d.

  9. The global extrapolation of numerical methods for computing concentration profiles in percutaneous drug absorption.

    PubMed

    Twizell, E H

    1989-01-01

    A family of numerical methods is developed and analyzed for the numerical solution of the parabolic partial differential equation together with the associated initial and boundary conditions, which arise in a mathematical model of the transient stage of percutaneous drug absorption. Two global extrapolation procedures are described, the first in time only, the second in both space and time, for improving the accuracy of the computed concentration profiles. The behaviours of two members of the family of methods, before and after extrapolation, are examined by repeating a number of experiments reported in the literature. Modifications to the algorithms, which are necessary in computing concentration profiles after the ointment is removed at the steady state, are outlined.

  10. UV-vis absorption spectroscopy and multivariate analysis as a method to discriminate tequila

    NASA Astrophysics Data System (ADS)

    Barbosa-García, O.; Ramos-Ortíz, G.; Maldonado, J. L.; Pichardo-Molina, J. L.; Meneses-Nava, M. A.; Landgrave, J. E. A.; Cervantes-Martínez, J.

    2007-01-01

    Based on the UV-vis absorption spectra of commercially bottled tequilas, and with the aid of multivariate analysis, it is proved that different brands of white tequila can be identified from such spectra, and that 100% agave and mixed tequilas can be discriminated as well. Our study was done with 60 tequilas, 58 of them purchased at liquor stores in various Mexican cities, and two directly acquired from a distillery. All the tequilas were of the "white" type, that is, no aged spirits were considered. For the purposes of discrimination and quality control of tequilas, the spectroscopic method that we present here offers an attractive alternative to the traditional methods, like gas chromatography, which is expensive and time-consuming.

  11. Spectrophotometric study of complex formation equilibria in the presence of interference using hard-soft net analyte signal method: application to drug-metal complexation.

    PubMed

    Hemmateenejad, Bahram; Nekoeinia, Mohsen; Absalan, Ghodratollah

    2011-01-10

    In this article, the ability of a new and efficient hard-soft method, previously proposed by our research group, is reported for modeling of the complex formation equilibria in the presence of interferences. This method is based on the net analyte signal (NAS) concept, which is a part of total signal that is directly related to the concentration of the component of interest. It monitors the concentration changes of any chemical species involved in the evolutionary process without requiring any pure spectra or having previous knowledge about the presence of the interferences. The proposed hard-soft method based on net analyte signal (HS-NAS) only needs a chemical model for one of the species involved in the reaction under study. The reliability of the method was examined by applying it to the measured data and spectrum of the known real systems of Fe(2+)-azithromycin and Ca(2+)-tetracycline.

  12. Method and apparatus for determination of temperature, neutron absorption cross section and neutron moderating power

    DOEpatents

    Vagelatos, Nicholas; Steinman, Donald K.; John, Joseph; Young, Jack C.

    1981-01-01

    A nuclear method and apparatus determines the temperature of a medium by injecting fast neutrons into the medium and detecting returning slow neutrons in three first energy ranges by producing three respective detection signals. The detection signals are combined to produce three derived indicia each systematically related to the population of slow neutrons returning from the medium in a respective one of three second energy ranges, specifically exclusively epithermal neutrons, exclusively substantially all thermal neutrons and exclusively a portion of the thermal neutron spectrum. The derived indicia are compared with calibration indicia similarly systematically related to the population of slow neutrons in the same three second energy ranges returning from similarly irradiated calibration media for which the relationships temperature, neutron absorption cross section and neutron moderating power to such calibration indicia are known. The comparison indicates the temperature at which the calibration indicia correspond to the derived indicia and consequently the temperature of the medium. The neutron absorption cross section and moderating power of the medium can be identified at the same time.

  13. The method of imbedded Lagrangian element to estimate wave power absorption by some submerged devices

    NASA Astrophysics Data System (ADS)

    Nihous, Gérard C.

    2014-06-01

    A simple approach is described to estimate the wave power absorption potential of submerged devices known to cause wave focusing and flow enhancement. In particular, the presence of a flow-through power take-off (PTO) system, such as low-head turbines, can be accounted for. The wave radiation characteristics of an appropriately selected Lagrangian element (LE) in the fluid domain are first determined. In the limit of a vanishing mass, the LE reduces to a patch of distributed normal dipoles. The hydrodynamic coefficients of this virtual object are then input in a standard equation of motion where the effect of the PTO can be represented, for example, as a dashpot damping term. The process is illustrated for a class of devices recently proposed by Carter and Ertekin (2011), although in a simplified form. Favorable wave power absorption is shown for large ratios of the LE wave radiation coefficient over the LE added mass coefficient. Under optimal conditions, the relative flow reduction from the PTO theoretically lies between 0.50 and , with lower values corresponding to better configurations. Wave power capture widths, the sensitivity of results to PTO damping and sample spectral calculations at a typical site in Hawaiian waters are proposed to further illustrate the versatility of the method.

  14. UV differential optical absorption method for measuring sulfur content in coal

    NASA Astrophysics Data System (ADS)

    Song, Feihu; Xu, Chuanlong; Wang, Shimin

    2012-02-01

    Determining the sulfur content in coal rapidly and accurately can provide a technical basis for the enterprises and the environmental administration departments. A novel method for measuring the sulfur content in coal based on UV differential optical absorption is presented in this paper. However, compared with the applications in atmosphere monitoring, the UV differential optical absorption spectroscopy (DOAS) for the sulfur content measurement in coal has the problems that the concentration range of SO2 in the flue gas is wider and the optical path-length of the gas cell is shorter. To solve these problems, an improved DOAS algorithm based on a finite impulse response (FIR) filter and a nonlinear compensation technique is proposed. An experimental measurement system based on the modified DOAS is designed and established. The standard SO2 gas and five kinds of standard coals are experimentally tested. Theoretical and experimental results show that the lower detection limit of the system is better than 0.014%, and the repeatability of the measurement system fairly meets the national standard of China. The system has advantages of low maintenance and shorter measurement duration (4 min).

  15. Interaction of nickel with 4-(2'-benzothiazolylazo) salicylic acid (BTAS) and simultaneous first-derivative spectrophotometric determination of nickel(II) and iron(III)

    NASA Astrophysics Data System (ADS)

    Hashem, E. Y.; Abu-Bakr, M. S.; Hussain, S. M.

    2003-03-01

    The solution properties of nickel complex with 4-(2'-benzo-thiazolylazo) salicylic acid (BTAS) have been studied by zero-order absorption spectrophotometry in 40% (v/v) ethanol at 20 °C and an ionic strength of 0.1 mol dm -3 (KNO 3). The equilibria that exist in solution were established and the basic characteristics of complexes formed were determined. A new direct spectrophotometric method for the determination of trace amounts of the nickel is proposed based on the formation of the Ni (BTAS) complex at pH 7.0. The absorption maximum, molar absorbtivity, and Sandell's sensitivity of 1:1 (M:L) complex are 525 nm, 0.6×10 4 l mol -1 cm -1 and 2.824×10 -9 μg cm -2, respectively. The use of first-derivative spectrophotometry eliminates the interference of iron and enables the simultaneous determination of nickel and iron using BTAS. Quantitative determination of Ni(II) and Fe(III) is possible in the range (0.59-7.08) and (2.1-8.4) μg ml -1, respectively with a relative standard deviation of 0.5%. The proposed method has been successfully applied to the simultaneous spectrophotometric determination of nickel and iron in steel alloys and aluminum alloys.

  16. Development and validation of an high-performance liquid chromatographic, and a ultraviolet spectrophotometric method for determination of Ambroxol hydrochloride in pharmaceutical preparations

    PubMed Central

    Muralidharan, Selvadurai; Kumar, Jaya Raja; Dhanara, Sokkalingam Arumugam

    2013-01-01

    A high-performance liquid chromatographic (HPLC) and ultraviolet (UV) methods were developed and validated for the quantitative determination of Ambroxol hydrochloride (AMH) in pharmaceutical dosage form. HPLC was carried out by reversed phase (RP) technique on an RP-18 column with a mobile phase composed of acetonitrile and water (pH 3.5 adjusted with orthophosphoric acid [60:40, v/v]). UV method was performed with the λmax at 250 nm. Both the methods showed good linearity, reproducibility, and precision. No spectral or chromatographic interferences from the tablet excipients were found in UV and HPLC. The method was successfully applied to commercial tablets. Validation parameters such as linearity, precision, accuracy, and specificity were determined. The HPLC Limit of detection (LOD) and Limit of quantification (LOQ) for Ambroxol were found to be 1 and 5 ng/ml, respectively. The UV LOD and LOQ for Ambroxol were found to be 1 and 4 μg/ml, respectively. The results were statistically compared using one-way analysis of variance. The proposed economical method could be applicable for routine analysis of AMH and monitoring of the quality of marketed drugs. PMID:23662284

  17. Derivative spectrophotometric and fluorimetric methods for determination of rofecoxib in tablets and in human plasma in presence of its photo-degradation product.

    PubMed

    Shehata, Mostafa A; Hassan, Nagiba Y; Fayed, Ahmad S; El-Zeany, Badr A

    2004-02-01

    Rofecoxib (I) has been determined in the presence of its photo-degradation product (II) using first derivative spectrophotometry ((1)D) and first derivative of the ratio spectra ((1)DD) by measuring the amplitude at 316.3 and 284 nm for (1)D and (1)DD, respectively. (I) can be determined in the presence of up to 70% and 80% of (II) by the (1)D and (1)DD, respectively. The linearity range of both the methods was the same (5.8-26.2 microg ml(-1)) with mean percentage recovery of 100.08 +/- 0.84 and 100.06 +/- 1.06 for (1)D and (1)DD, respectively. (1)D method was used to study kinetics of (I) photo-degradation that was found to follow a first-order reaction. The t(1/2) was 20.2 min while K (reaction rate constant) was 0.0336 mol min(-1). Both methods were applied to the analysis of (I) in bulk powder and in pharmaceutical formulations. Also a spectrofluorimetric method is described to determine (I) at very low concentrations (25-540 ng ml(-1)) where (I) is converted to its photo-degradate (II), which possesses a native fluorescence that could be measured. The proposed method was applied for the analysis of tablets containing rofecoxib as well as to rofecoxib-spiked human plasma.

  18. Spectrophotometric determination of zirconium with xylenol orange

    SciTech Connect

    Antepenko, R J

    1982-05-14

    High purity hydride forming metal films are used as hydrogen isotope occluders and function as electrodes in neutron generator tubes. This use of zirconium occluder films requires reliable analytical methods for routine determination of the zirconium film weight in a production environment. In this study, a spectrophotometric method was evaluated for the determination of zirconium films. The method is based upon the formation of a highly colored zirconium complex with xylenol orange in a dilute perchloric acid medium. Dilute hydrofluoric acid is used in this procedure to selectively dissolve the zirconium film off the substrate. A perchloric acid fuming step is used to remove hydrofluoric acid from the solution. The zirconium solutions are depolymerized before complex formation by heating in 2 N perchloric acid. The zirconium complex exhibits a maximum absorbance in 0.2 to 0.3 M perchloric acid at a wavelength of 531 nanometers. Beer's law is obeyed for zirconium concentrations through 2.1 parts per million. Molybdenum, at concentrations equal to zirconium, does not interfere with the xylenol orange method.

  19. Ultraviolet spectrophotometric determination of tantalum with pyrogallol

    USGS Publications Warehouse

    Dinnin, J.I.

    1953-01-01

    In a search for a more rapid method for the determination of tantalum in rocks and minerals, an intensive study was made of the tantalum-pyrogallol reaction recommended by Platanov and Krivoshlikov, and a better modified spectrophotometric procedure is given. The improved method consists in measuring the absorbancy of the tantalum-pyrogallol complex at 325 m?? in 4N hydrochloric acid and a fixed concentration (0.0175M) of ammonium oxalate. Beer's law is followed for the concentration range up to 40 ?? per ml. Sensitivity in terms of molar absorbancy index is 4775. Most interferences are additive in character and readily correctable. Separations or major corrections are required in the presence of significant amounts of molybdenum, tungsten, antimony, and uranium. The method has been successfully applied to three ores previously analyzed by gravimetric techniques. The method affords greater speed, sensitivity, and reproducibility in the determination of tantalum in rocks and minerals. A more reliable technique for preparing standard solutions of tantalum has been developed.

  20. Amperometric Enzyme Sensor to Check the Total Antioxidant Capacity of Several Mixed Berries. Comparison with Two Other Spectrophotometric and Fluorimetric Methods

    PubMed Central

    Tomassetti, Mauro; Serone, Maruschka; Angeloni, Riccardo; Campanella, Luigi; Mazzone, Elisa

    2015-01-01

    The aim of this research was to test the correctness of response of a superoxide dismutase amperometric biosensor used for the purpose of measuring and ranking the total antioxidant capacity of several systematically analysed mixed berries. Several methods are described in the literature for determining antioxidant capacity, each culminating in the construction of an antioxidant capacity scale and each using its own unit of measurement. It was therefore endeavoured to correlate and compare the results obtained using the present amperometric biosensor method with those resulting from two other different methods for determining the total antioxidant capacity selected from among those more frequently cited in the literature. The purpose was to establish a methodological approach consisting in the simultaneous application of different methods that it would be possible to use to obtain an accurate estimation of the total antioxidant capacity of different mixed berries and the food products containing them. Testing was therefore extended to also cover jams, yoghurts and juices containing mixed berries. PMID:25654720

  1. General Subject 2. Report to ICUMSA on the determination of carry-over alpha-amylase activity in white and refined sugars by a spectrophotometric method

    Technology Transfer Automated Retrieval System (TEKTRAN)

    A report is given on a new industrial method for the determination of carry-over alpha-amylase activity in raw and refined sugars, as well as a recommendation. In recent years, there has been increased concern over carry-over activity of mostly high temperature (HT) and very high temperature (VHT) s...

  2. FIA-Spectrophotometric Method for Determination of Nitrite in Meat Products: An Experiment Exploring Color Reduction of an Azo-Compound

    ERIC Educational Resources Information Center

    Penteado, Jose C.; Angnes, Lucio; Masini, Jorge C.; Oliveira, Paulo C. C.

    2005-01-01

    This article describes the reaction between nitrite and safranine O. This sensitive reaction is based on the disappearance of color of the reddish-orange azo dye, allowing the determination of nitrite at the mg mL-1 level. A factorial optimization of parameters was carried out and the method was applied for the quantification of nitrite in…

  3. New spectrophotometric methods for the determinations of hydrogen sulfide present in the samples of lake water, industrial effluents, tender coconut, sugarcane juice and egg

    NASA Astrophysics Data System (ADS)

    Shyla, B.; Nagendrappa, G.

    2012-10-01

    The new methods are working on the principle that iron(III) is reduced to iron(II) by hydrogen sulfide, catechol and p-toluidine the system 1/hydrogen sulfide the system 2, in acidic medium followed by the reduced iron forming complex with 1,10-phenanthroline with λmax 510 nm. The other two methods are based on redox reactions between electrolytically generated manganese(III) sulfate taken in excess and hydrogen sulfide followed by the unreacted oxidant oxidizing diphenylamine λmax 570 the system 3/barium diphenylamine sulphonate λmax 540 nm, the system 4. The increase/decrease in the color intensity of the dye products of the systems 1 and 2 or 3 and 4 are proportional to the concentration of hydrogen sulfide with its quantification range 0.035-1.40 μg ml-1/0.14-1.40 μg ml-1.

  4. New spectrophotometric methods for the determinations of hydrogen sulfide present in the samples of lake water, industrial effluents, tender coconut, sugarcane juice and egg.

    PubMed

    Shyla, B; Nagendrappa, G

    2012-10-01

    The new methods are working on the principle that iron(III) is reduced to iron(II) by hydrogen sulfide, catechol and p-toluidine the system 1/hydrogen sulfide the system 2, in acidic medium followed by the reduced iron forming complex with 1,10-phenanthroline with λ(max) 510 nm. The other two methods are based on redox reactions between electrolytically generated manganese(III) sulfate taken in excess and hydrogen sulfide followed by the unreacted oxidant oxidizing diphenylamine λ(max) 570 the system 3/barium diphenylamine sulphonate λ(max) 540 nm, the system 4. The increase/decrease in the color intensity of the dye products of the systems 1 and 2 or 3 and 4 are proportional to the concentration of hydrogen sulfide with its quantification range 0.035-1.40 μg ml(-1)/0.14-1.40 μg ml(-1).

  5. Simultaneous multicomponent spectrophotometric monitoring of methyl and propyl parabens using multivariate statistical methods after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction

    NASA Astrophysics Data System (ADS)

    Khani, Rouhollah; Ghasemi, Jahan B.; Shemirani, Farzaneh

    2014-03-01

    A powerful and efficient signal-preprocessing technique that combines local and multiscale properties of the wavelet prism with the global filtering capability of orthogonal signal correction (OSC) is applied for pretreatment of spectroscopic data of parabens as model compounds after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction method (IL-DLLME). In the proposed technique, a mixture of a water-immiscible ionic liquid (as extraction solvent) [Hmim][PF6] and disperser solvent is injected into an aqueous sample solution containing one of the IL's ions, NaPF6, as extraction solvent and common ion source. After preconcentration, the absorbance of the extracted compounds was measured in the wavelength range of 200-700 nm. The wavelet orthogonal signal correction with partial least squares (WOSC-PLS) method was then applied for simultaneous determination of each individual compound. Effective parameters, such as amount of IL, volume of the disperser solvent and amount of NaPF6, were inspected by central composite design to identify the most important parameters and their interactions. The effect of pH on the sensitivity and selectivity was studied according to the net analyte signal (NAS) for each component. Under optimum conditions, enrichment factors of the studied compounds were 75 for methyl paraben (MP) and 71 for propyl paraben (PP). Limits of detection for MP and PP were 4.2 and 4.8 ng mL-1, respectively. The root mean square errors of prediction for MP and PP were 0.1046 and 0.1275 μg mL-1, respectively. The practical applicability of the developed method was examined using hygienic, cosmetic, pharmaceutical and natural water samples.

  6. Simultaneous multicomponent spectrophotometric monitoring of methyl and propyl parabens using multivariate statistical methods after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction.

    PubMed

    Khani, Rouhollah; Ghasemi, Jahan B; Shemirani, Farzaneh

    2014-03-25

    A powerful and efficient signal-preprocessing technique that combines local and multiscale properties of the wavelet prism with the global filtering capability of orthogonal signal correction (OSC) is applied for pretreatment of spectroscopic data of parabens as model compounds after their preconcentration by robust ionic liquid-based dispersive liquid-liquid microextraction method (IL-DLLME). In the proposed technique, a mixture of a water-immiscible ionic liquid (as extraction solvent) [Hmim][PF6] and disperser solvent is injected into an aqueous sample solution containing one of the IL's ions, NaPF6, as extraction solvent and common ion source. After preconcentration, the absorbance of the extracted compounds was measured in the wavelength range of 200-700 nm. The wavelet orthogonal signal correction with partial least squares (WOSC-PLS) method was then applied for simultaneous determination of each individual compound. Effective parameters, such as amount of IL, volume of the disperser solvent and amount of NaPF6, were inspected by central composite design to identify the most important parameters and their interactions. The effect of pH on the sensitivity and selectivity was studied according to the net analyte signal (NAS) for each component. Under optimum conditions, enrichment factors of the studied compounds were 75 for methyl paraben (MP) and 71 for propyl paraben (PP). Limits of detection for MP and PP were 4.2 and 4.8 ng mL(-)(1), respectively. The root mean square errors of prediction for MP and PP were 0.1046 and 0.1275 μg mL(-)(1), respectively. The practical applicability of the developed method was examined using hygienic, cosmetic, pharmaceutical and natural water samples.

  7. A new method to retrieve spectral absorption coefficient of highly-scattering and weakly-absorbing materials

    NASA Astrophysics Data System (ADS)

    Dombrovsky, Leonid A.

    2016-03-01

    A significant uncertainty in the absorption coefficient of highly scattering dispersed materials is typical in the spectral ranges of very weak absorption. The traditional way to identify the main absorption and scattering characteristics of semi-transparent materials is based on spectral measurements of normal-hemispherical reflectance and transmittance for the material sample. Unfortunately this way cannot be used in the case of in vivo measurements of optical properties of biological tissues. A method suggested in the present paper is based on thermal response to the periodic radiative heating of the open surface of a semi-transparent material. It is shown that the period of a variation of the surface temperature is sensitive to the value of an average absorption coefficient in the surface layer. As a result, the monochromatic external irradiation combined with the surface temperature measurements can be used to retrieve the spectral values of absorption coefficient. Possible application of this method to porous semi-transparent ceramics is considered. An example problem is also solved to illustrate the applicability of this method to human skin. The approach suggested enables one to estimate an average absorption coefficient of human skin of a patient just before the thermal processing.

  8. Quality assessment of the saffron samples using second-order spectrophotometric data assisted by three-way chemometric methods via quantitative analysis of synthetic colorants in adulterated saffron

    NASA Astrophysics Data System (ADS)

    Masoum, Saeed; Gholami, Ali; Hemmesi, Marjan; Abbasi, Saleheh

    2015-09-01

    Saffron is a valuable culinary spice that can be used not only for dyes and cooking, but also for many medical purposes. Due to its high price and restriction of its production, various fraud manners in its production have been growing. Addition of synthetic colorants to saffron is the most common way for adulteration. In this work, chemometric methods are proposed to resolve the three-dimensional absorbance spectra-pH data for simultaneous determination of the two colorants Tartrazin and Sunset yellow, in adulterated saffron. The rank deficiency in the concentration mode impaired the system. Therefore, to extirpate the ambiguity, which results from rank deficiency, three-way variation array V was generated by subtracting the first pH spectrum from each spectrum at each pH. This allows the extraction of extent reaction profile and mixture reaction spectral profiles, as well as the relative concentrations of the analytes.

  9. Quality assessment of the saffron samples using second-order spectrophotometric data assisted by three-way chemometric methods via quantitative analysis of synthetic colorants in adulterated saffron.

    PubMed

    Masoum, Saeed; Gholami, Ali; Hemmesi, Marjan; Abbasi, Saleheh

    2015-09-01

    Saffron is a valuable culinary spice that can be used not only for dyes and cooking, but also for many medical purposes. Due to its high price and restriction of its production, various fraud manners in its production have been growing. Addition of synthetic colorants to saffron is the most common way for adulteration. In this work, chemometric methods are proposed to resolve the three-dimensional absorbance spectra-pH data for simultaneous determination of the two colorants Tartrazin and Sunset yellow, in adulterated saffron. The rank deficiency in the concentration mode impaired the system. Therefore, to extirpate the ambiguity, which results from rank deficiency, three-way variation array V was generated by subtracting the first pH spectrum from each spectrum at each pH. This allows the extraction of extent reaction profile and mixture reaction spectral profiles, as well as the relative concentrations of the analytes.

  10. Iminodibenzyl as a novel coupling agent for the spectrophotometric determination of sulfonamide derivatives.

    PubMed

    Nagaraja, Padmarjaiah; Sunitha, Kallanchira R; Vasantha, Ramanathapura A; Yathirajan, Hemmige S

    2002-03-01

    A rapid, selective and simple spectrophotometric method for the determination of sulfa-drugs is described. The method is based on the formation of violet colored azo product by the diazotization of sulfonamides, viz. sulfathiazole (SFT), sulfadiazine (SFD), sulfacetamide (SFA), sulfamethoxazole (SFMx), sulfamerazine (SFMr), sulfaguanidine (SFG) and sulfadimidine (SFDd) followed by a coupling reaction with iminodibenzyl in alcohol medium. Absorbance of the resulting violet azo product is measured at 570-580 nm and is stable for 24 h at 27 degrees C. Beer's law is obeyed in the concentration range of 0.05-6.0 microg ml(-1) at the wavelength of maximum absorption. The method is successfully employed for the determination of sulfonamides in various pharmaceutical preparations and common excipients used as additives in pharmaceuticals do not interfere in the proposed method. The method offers the advantages of simplicity, rapidity and sensitivity without the need for extraction or heating. A reaction mechanism is proposed for the formation of the violet azo product.

  11. Novel oxidative electrophilic coupling reactions of phenoxazine derivatives with MBTH and their applications to spectrophotometric determination of residual chlorine in drinking water and environmental water samples.

    PubMed

    Al-Okab, Riyad Ahmed; Syed, Akheel Ahmed

    2009-10-15

    Novel, sensitive and rapid spectrophotometric methods, using phenoxazine (PNZ), 2-chlorophe-noxazine (CPN) and 2-trifluoromethylphenoxazine (TPN) as chromogenic reagents for the determination of residual chlorine are proposed. The methods are based on the reduction of chlorine by an electrophilic coupling reagent, 3-methyl-2-benzothiazoline hydrazono hydrochloride hydrate (MBTH) in mild hydrochloric acid medium and subsequent coupling with PNZ, CPN or TPN. The blue color formed in the reaction showed maximum absorbance at 680-690 nm and obeyed Beer's law over the range 0.1-2.2 microg ml(-1). The molar absorptivity values with PNZ, CPN and TPN were 2.80 x 10(4), 2.67 x 10(4) and 1.91 x 10(4) l mol(-1)cm(-1) and Sandell's sensitivity values were 0.028, 0.027 and 0.028 microg cm(-2) respectively. The proposed methods were successfully applied in the determination of residual chlorine in drinking water and environmental water samples. The performance of proposed methods was evaluated in terms of Student's t-test and variance ratio F-test which indicated the significance of proposed methods over the standard spectrophotometric method.

  12. On the errors in measuring the particle density by the light absorption method

    SciTech Connect

    Ochkin, V. N.

    2015-04-15

    The accuracy of absorption measurements of the density of particles in a given quantum state as a function of the light absorption coefficient is analyzed. Errors caused by the finite accuracy in measuring the intensity of the light passing through a medium in the presence of different types of noise in the recorded signal are considered. Optimal values of the absorption coefficient and the factors capable of multiplying errors when deviating from these values are determined.

  13. Spectrophotometric investigation and determination of scandium using semi-xylenol orange

    SciTech Connect

    Hafez, M.A.H.; Kenawy, I.M.M.; Kabil, M.A.

    1985-10-01

    The composition, stability constant and molar absorption coefficient of the chelate of scandium ion with Semi-Xylenol Orange (SXO) are determined spectrophotometrically in a medium of chloroacetate buffer. In the scandium-Semi-Xylenol Orange system, Sc(SXO) chelate is formed with a logarithmic stability constant of 19.66 and molar absorptivity of 2.4 x 10/sup 4/ (530 nm) 1 mole/sup -1/ cm/sup -1/. The precision and accuracy attainable in a direct photometric microtitration of Sc/sup + + +/ ion with a 0.001M solution of EDTA using SXO as a metallochromic indicator has been studied. Interferences of different anions and cations on scandium determination are also investigated. Spectrophotometric determination of scandium(III) using SXO at the optimum conditions has been carried out. Beer's law is obeyed for 0-13.49 ..mu..g scandium/25 ml.

  14. Simulation of energy absorption spectrum in NaI crystal detector for multiple gamma energy using Monte Carlo method

    SciTech Connect

    Wirawan, Rahadi; Waris, Abdul; Djamal, Mitra; Handayani, Gunawan

    2015-04-16

    The spectrum of gamma energy absorption in the NaI crystal (scintillation detector) is the interaction result of gamma photon with NaI crystal, and it’s associated with the photon gamma energy incoming to the detector. Through a simulation approach, we can perform an early observation of gamma energy absorption spectrum in a scintillator crystal detector (NaI) before the experiment conducted. In this paper, we present a simulation model result of gamma energy absorption spectrum for energy 100-700 keV (i.e. 297 keV, 400 keV and 662 keV). This simulation developed based on the concept of photon beam point source distribution and photon cross section interaction with the Monte Carlo method. Our computational code has been successfully predicting the multiple energy peaks absorption spectrum, which derived from multiple photon energy sources.

  15. Correction of self-absorption effect in calibration-free laser-induced breakdown spectroscopy by an internal reference method.

    PubMed

    Sun, Lanxiang; Yu, Haibin

    2009-07-15

    A simplified procedure for correcting self-absorption effect was proposed in calibration-free laser-induced breakdown spectroscopy (CF-LIBS). In typical LIBS measurement conditions, the plasma produced is often optically thick, especially for the strong lines of major elements. The selection of self-absorption lines destroys the performance of CF-LIBS, and the familiar correction method based on the curve of growth is complex in implementation. The procedure we proposed, named internal reference for self-absorption correction (IRSAC), first chose an internal reference line for each species, then compared other spectral line intensity of the same species with the reference line to estimate the self-absorption degrees of other spectral lines, and finally achieved an optimal correction by a regressive algorithm. The self-absorption effect of the selected reference line can be ignored, since the reference line with high excitation energy of the upper level is slightly affected by the self-absorption. Through the IRSAC method, the points on the Boltzmann plot become more regular, and the evaluations of the plasma temperature and material composition are more accurate than the basic CF-LIBS.

  16. Simultaneous UV Spectrophotometric Estimation of Ambroxol Hydrochloride and Levocetirizine Dihydrochloride

    PubMed Central

    Prabhu, S. Lakshmana; Shirwaikar, A. A.; Shirwaikar, Annie; Kumar, C. Dinesh; Kumar, G. Aravind

    2008-01-01

    A novel, simple, sensitive and rapid spectrophotometric method has been developed for simultaneous estimation of ambroxol hydrochloride and levocetirizine dihydrochloride. The method involved solving simultaneous equations based on measurement of absorbance at two wavelengths 242 nm and 231 nm, the γ max of ambroxol hydrochloride and levocetirizine dihydrochloride, respectively. Beer's law was obeyed in the concentration range 10–50 μg/ml and 8–24 μg/ml for ambroxol hydrochloride and levocetirizine dihydrochloride respectively. Results of the method were validated statistically and by recovery studies. PMID:20046721

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

    PubMed

    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.

  18. Spectrophotometric determination of norepinephrine with sodium iodate and determination of its acidity constants

    NASA Astrophysics Data System (ADS)

    Hashem, E. Y.; Youssef, A. K.

    2013-05-01

    A spectrophotometric method is proposed for the determination of norepinephrine (NE) and its bitartrate salts. The method was based on the development of a red color (λmax = 495 nm) with sodium iodate in aqueous alcoholic medium at pH 5. The color was stable for at least 4 hrs. The molar reacting ratio of NE to sodium iodate was 1:4. A linear relationship was obtained between the absorption intensity and NE concentration in the range of 3.384-37.224 μg/ml with detection limit of 0.067 μg/ml and correlation coefficient of 0.9972. The present work facilitated the determination of the three acidity constants, 7.564 ± 0.02, 9.036 ± 0.034, and 10.761 ± 0.023. The reaction mechanism was also described. The proposed method was successfully applied for the determination of NE in pharmaceutical formulations. Results for analysis of bulk drugs and injections agree with those of official methods.

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

    PubMed

    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.

  20. Extractive spectrophotometric determination of Cobalt(II) in synthetic and pharmaceutical samples using Cyanex 923.

    PubMed

    Reddy, B Ramachandra; Radhika, P; Kumar, J Rajesh; Priya, D Neela; Rajgopal, K

    2004-02-01

    Cyanex 923 has been proposed as a sensitive analytical reagent for the direct extractive spectrophotometric determination of cobalt(II). Cobalt(II) forms a blue-colored complex with Cyanex 923 in the organic phase. The maximum absorbance of the complex is measured at 635 nm. Beer's law was obeyed in the range 58.9 - 589.0 microg of cobalt. The molar absorptivitiy and Sandell's sensitivity of the complex was calculated to be 6.79 x 10920 l mol(-1) cm(-1) and 0.088 microg cm(-2), respectively. The nature of the extracted species was found to be Co(SCN)2 x 2S. An excellent linearity with a correlation coefficient value of 0.999 was obtained for the Co(II)-Cyanex 923 complex. Stability and regeneration of the reagent (Cyanex 923) for reuse is the main advantage of the present method. The method was successfully applied to the determination of cobalt in synthetic mixtures and pharmaceutical samples was found to give values close to the actual ones. Standard alloy samples, such as high-speed tool BCS 484 and 485, have been tested for the determination of cobalt for the purpose of validating the present method. The results of the proposed method are comparable with atomic absorption spectrometry and were found to be in good agreement.