The mechanism for the poly-condensation event of conjugated polymers with ending 4-hydroxycoumarin has
been proposed. It happened under H2SO4 acidic conditions only using enolic-coumarins without any substituent
at third position. It was studied using Matrix assisted laser desorption/ionization time-of-flight (MALDI-Tof)
mass spectrometry. Besides, some physicochemical properties were analyzed using Thermo-gravimetric (TGA),
X-ray and UV-Vis analysis
Visible Spectrophotometric Determination of Gemigliptin Using Charge Transfer...Ratnakaram Venkata Nadh
A visible spectrophotometric method was developed and validated for the determination of gemigliptin present in bulk drug and tablet formulation. It involves an indirect method of charge transfer complex formation in presence of NBS, metol and suphanilic acid. Gemigliptin was subjected to oxidation with excess amount of oxidant (NBS) and the unconsumed NBS oxidizes metol to give p-N-methylbenzoquinone monoamine (PNMM) which in turn forms a charge transfer complex with sulphanilic acid. Then validated the above developed method as per the current ICH guidelines. An excellent correlation coefficient (> 0.999) was found for the obtained regression equation
(y = –0.0302x + 0.928) in the range of 2.0–30.0 μg mL-1. The method was found to be simple and rapid because it does not involve any solvent extraction. The recovery levels of the drug were in the range 99.92 – 100.08.
International Journal of Pharmaceutical Science Invention (IJPSI) is an international journal intended for professionals and researchers in all fields of Pahrmaceutical Science. IJPSI publishes research articles and reviews within the whole field Pharmacy and Pharmaceutical Science, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
Synthesis and characterization of some Chromium(III) complexes of dibasic tri...IJERA Editor
Coordination complexes of Cr(III)with four tridentate Schiff base ligands viz. N-(2-hydroxy-1-naphthaldehyde)- -(4-nitrobenzoyl)hydrazone(HNNH = H2L 1 ), N-(2-hydroxy-4-methoxybenzaldehyde)- -(2-furoyl) hydrazone (HMFH = H2L 2 ), N-(2-hydroxyacetophenone)- -(2-theonyl) hydrazone (HATH = H2L 3 ) and N-(2- hydroxy-5-methylacetophenone)- -(3-toloyl) hydrazone (HMAT = H2L 4 ) have been synthesized and characterized by elemental analysis, magnetic susceptibility, molar conductance, thermogravimetric analysis and spectral (IR, electronic, NMR) measurements. IR spectra indicates that the ligand behave as dibasic tridentate ligand in a chelate coordinating to Cr(III) ion through ketonic oxygen, azomethine nitrogen and by both enolic and phenolic protons (except in H2L 1 by naphtholic oxygen atom) via double deprotonation of ligands. The magnetic and spectral data indicate chelate in octahedral environment and analytical data suggest 1:1 stoichiometries for the complexes
Mechanistic Aspects of Oxidation of P-Bromoacetophen one by Hexacyanoferrate ...IJERA Editor
The kinetics of oxidation of p-bromoacetophenone by hexacyanoferrate (III) has been studied in alkaline
medium. The order of reaction with respect of both acetophenone and hexacynoferrate (III) has been found to be
unity. The rate of reaction increases with increase in the concentration of sodium hydroxide.On addition of
neutral KCl, reaction rate increases. The effects of solvent and temperature have been also studied. The product
p-bromophenyl glyoxal have been characterized by IR studies.
Kinetics and Thermodynamics of Mandelic Acid Oxidation By Tripropylammonium H...inventionjournals
Two new Versatile reagent Tripropylammonium Fluorochromate(TriPAFC) and Tripropylammonium Chlorochromate(TriPACC) has been employed for the oxidation of Mandelic acid. Rate of the réaction is catalysed by surfactant Sodium LaurylEther Sulphate(SLES). The Oxidation has been studied spectrophotometrically at room température in perchloric acid medium. Rate of TriPAFC and TriPACC oxidation of Mandelic acid has been followed under pseudo-first order condition. Rate constants were calculated by the integrated rate equation. The graph of logk versus time was linear and the slope is near to unity, rate constant calculated from graph also agreed with experimental value shows the first order rate dépendance on Mandelic acid. Product formed in this oxidation of Mandelic acid was analysed, polymerization test were carried to confirm that the reaction follows ionic mechanism and stoichiometric data has been accounted.Temperature of the substrate is varried and from the rate constant value, Thermodynamic parameters like Activation energy, Enthalpy change, Entropy change and change in Gibb’s free energy is calculated using Arrhenius and Eyrings plot. All the kinetic runs were repeated and the rate constants were reproducible within ±2% range.
Synthesis, characterization and antimicrobial evaluation of novel diethyl (2-...iosrphr_editor
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
Determination of Riociguat by Oxidative Coupling Using Visible SpectrophotometryRatnakaram Venkata Nadh
A simple spectrophotometric method was developed to determine riociguat in bulk and tablet formulation. The present method lies on the oxidation of MBTH by Fe+3 ions in acidic medium to form active coupling species and followed by its coupling with riociguat to form the chromophore having lmax 660 nm. Validated the proposed method as per the existing guidelines of ICH. Good linearity (r~ 0.999) was observed for calibration curve in the studied concentration range (6.25 – 37.50 μg mL-1). Reproducibility, accuracy and precision of the method were confirmed from low values of % RSD.
Visible Spectrophotometric Determination of Gemigliptin Using Charge Transfer...Ratnakaram Venkata Nadh
A visible spectrophotometric method was developed and validated for the determination of gemigliptin present in bulk drug and tablet formulation. It involves an indirect method of charge transfer complex formation in presence of NBS, metol and suphanilic acid. Gemigliptin was subjected to oxidation with excess amount of oxidant (NBS) and the unconsumed NBS oxidizes metol to give p-N-methylbenzoquinone monoamine (PNMM) which in turn forms a charge transfer complex with sulphanilic acid. Then validated the above developed method as per the current ICH guidelines. An excellent correlation coefficient (> 0.999) was found for the obtained regression equation
(y = –0.0302x + 0.928) in the range of 2.0–30.0 μg mL-1. The method was found to be simple and rapid because it does not involve any solvent extraction. The recovery levels of the drug were in the range 99.92 – 100.08.
International Journal of Pharmaceutical Science Invention (IJPSI) is an international journal intended for professionals and researchers in all fields of Pahrmaceutical Science. IJPSI publishes research articles and reviews within the whole field Pharmacy and Pharmaceutical Science, new teaching methods, assessment, validation and the impact of new technologies and it will continue to provide information on the latest trends and developments in this ever-expanding subject. The publications of papers are selected through double peer reviewed to ensure originality, relevance, and readability. The articles published in our journal can be accessed online.
Synthesis and characterization of some Chromium(III) complexes of dibasic tri...IJERA Editor
Coordination complexes of Cr(III)with four tridentate Schiff base ligands viz. N-(2-hydroxy-1-naphthaldehyde)- -(4-nitrobenzoyl)hydrazone(HNNH = H2L 1 ), N-(2-hydroxy-4-methoxybenzaldehyde)- -(2-furoyl) hydrazone (HMFH = H2L 2 ), N-(2-hydroxyacetophenone)- -(2-theonyl) hydrazone (HATH = H2L 3 ) and N-(2- hydroxy-5-methylacetophenone)- -(3-toloyl) hydrazone (HMAT = H2L 4 ) have been synthesized and characterized by elemental analysis, magnetic susceptibility, molar conductance, thermogravimetric analysis and spectral (IR, electronic, NMR) measurements. IR spectra indicates that the ligand behave as dibasic tridentate ligand in a chelate coordinating to Cr(III) ion through ketonic oxygen, azomethine nitrogen and by both enolic and phenolic protons (except in H2L 1 by naphtholic oxygen atom) via double deprotonation of ligands. The magnetic and spectral data indicate chelate in octahedral environment and analytical data suggest 1:1 stoichiometries for the complexes
Mechanistic Aspects of Oxidation of P-Bromoacetophen one by Hexacyanoferrate ...IJERA Editor
The kinetics of oxidation of p-bromoacetophenone by hexacyanoferrate (III) has been studied in alkaline
medium. The order of reaction with respect of both acetophenone and hexacynoferrate (III) has been found to be
unity. The rate of reaction increases with increase in the concentration of sodium hydroxide.On addition of
neutral KCl, reaction rate increases. The effects of solvent and temperature have been also studied. The product
p-bromophenyl glyoxal have been characterized by IR studies.
Kinetics and Thermodynamics of Mandelic Acid Oxidation By Tripropylammonium H...inventionjournals
Two new Versatile reagent Tripropylammonium Fluorochromate(TriPAFC) and Tripropylammonium Chlorochromate(TriPACC) has been employed for the oxidation of Mandelic acid. Rate of the réaction is catalysed by surfactant Sodium LaurylEther Sulphate(SLES). The Oxidation has been studied spectrophotometrically at room température in perchloric acid medium. Rate of TriPAFC and TriPACC oxidation of Mandelic acid has been followed under pseudo-first order condition. Rate constants were calculated by the integrated rate equation. The graph of logk versus time was linear and the slope is near to unity, rate constant calculated from graph also agreed with experimental value shows the first order rate dépendance on Mandelic acid. Product formed in this oxidation of Mandelic acid was analysed, polymerization test were carried to confirm that the reaction follows ionic mechanism and stoichiometric data has been accounted.Temperature of the substrate is varried and from the rate constant value, Thermodynamic parameters like Activation energy, Enthalpy change, Entropy change and change in Gibb’s free energy is calculated using Arrhenius and Eyrings plot. All the kinetic runs were repeated and the rate constants were reproducible within ±2% range.
Synthesis, characterization and antimicrobial evaluation of novel diethyl (2-...iosrphr_editor
The IOSR Journal of Pharmacy (IOSRPHR) is an open access online & offline peer reviewed international journal, which publishes innovative research papers, reviews, mini-reviews, short communications and notes dealing with Pharmaceutical Sciences( Pharmaceutical Technology, Pharmaceutics, Biopharmaceutics, Pharmacokinetics, Pharmaceutical/Medicinal Chemistry, Computational Chemistry and Molecular Drug Design, Pharmacognosy & Phytochemistry, Pharmacology, Pharmaceutical Analysis, Pharmacy Practice, Clinical and Hospital Pharmacy, Cell Biology, Genomics and Proteomics, Pharmacogenomics, Bioinformatics and Biotechnology of Pharmaceutical Interest........more details on Aim & Scope).
Determination of Riociguat by Oxidative Coupling Using Visible SpectrophotometryRatnakaram Venkata Nadh
A simple spectrophotometric method was developed to determine riociguat in bulk and tablet formulation. The present method lies on the oxidation of MBTH by Fe+3 ions in acidic medium to form active coupling species and followed by its coupling with riociguat to form the chromophore having lmax 660 nm. Validated the proposed method as per the existing guidelines of ICH. Good linearity (r~ 0.999) was observed for calibration curve in the studied concentration range (6.25 – 37.50 μg mL-1). Reproducibility, accuracy and precision of the method were confirmed from low values of % RSD.
The synthesis of polyoxychloropropylenepoxymethacrylate oligoesters by esterification of polyoxychloropropylenetriepoxide by methacrylic acid has been carried out. It has been established that by varying the conditions of carrying out of the reaction, one can prepare, mainly, the mono-, di- and trimethacrylic oligoesters. On the basis of epoxy diane ED-20 and synthesized polyoxychloropropylenepoxymethacrylate oligoesters as modifiers there have been prepared the self-extinction compositions, which after curing by N, N1–diaminodiphenylsulfone possess higher physical-mechanical, adhesion and heat-physical properties.
Abstract
A small set of amphetamines has been analyzed by gas chromatography (GC) high-resolution time-of-flight mass spectrometry (TOFMS) using a microplasma photoionization (MPPI) soft-ionization source. This plasma-based, wavelength selectable ionization source enables ionization of the test compounds and their corresponding derivatives at ~8-12 eV that is a softer alternative to electron ionization at 70 eV. Three plasma gases were used in this study: Xe plasma that emits photons at resonance lines of 9.57 eV and 8.44 eV; Kr plasma at 10.63 eV and 10.02 eV, and Ar plasma at 11.82 eV and 11.61 eV. Derivatization of the test compounds with trifluoroacetic anhydride and α-methoxy-α-(trifluoromethyl)-phenylacetyl pyrazole was evaluated because the MPPI mass spectra of the underivatized amphetamines yield primarily iminium ions, which make the identification of the test compounds by GC-TOFMS inconclusive. The MPPI mass spectra of the TFA-derivatized amphetamines yield abundant molecular ions, when using Xe as plasma gas, and enough fragment ions with the Ar plasma that can help in formula generation. The structure elucidation of two "known unknowns" designer drugs using this "tunable" soft-ionization source and a high-resolution TOF mass spectrometer is presented in this study.
Determination of % purity of a compound by by Using DSCMUL
What is % purity?
Different methods to determine % Purity.
Determination of % purity of Organic Compound By Using DSC:
•1) Polycyclic aromatic Hydrocarbons e. g Benzo[c]phenanthrene, BcPh, C18H12
•2) Ibuprofen medicine
•3) Phenacetin samples at different purity ratios
•4) Methamphetamine Paracetamol and Mixture of both.
•5) AZT (C10H13N5O4; 3´-azido-2,3´-dideoxythymidine)
Quantitative Analysis of 30 Drugs in Whole Blood by SPE and UHPLC-TOF-MSAnnex Publishers
Abstract
An Ultra-High Pressure Liquid Chromatography Time-of-Flight Mass Spectrometry (UHPLC-TOF-MS) method for quantitative analysis of 30 drugs in whole blood was developed and validated. The method was used for screening and quantification of common drugs and drugs of abuse in whole blood received from autopsy cases and living persons. The compounds included: alprazolam, amphetamine, benzoylecgonine, bromazepam, cathine, cathinone, chlordiazepoxide, cocaine, codeine, clonazepam, 7-aminoclonazepam, diazepam, nordiazepam, flunitrazepam, 7-aminoflunitrazepam, ketamine, ketobemidone, 3,4-Methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), methamphetamine, methadone, morphine, 6-monoacetylmorphine, nitrazepam, 7-aminonitrazepam, oxazepam, temazepam, tramadol, O-desmethyltramadol, and zolpidem. Blood samples (200 μL) were subjected to Solid Phase Extraction (SPE). Target drugs were quantified using a Waters ACQUITY UPLC system coupled to a Waters SYNAPT G2 TOF-MS apparatus. Extraction recoveries ranged from 41% (7-aminoclonazepam) to 111% (ketamine) and matrix effects ranged from -13% (temazepam) to 50% (7-aminonitrazepam). For all compounds, a quadratic polynomial was applied for fitting the calibration curves. Lower Limits of Quantification (LOQ) ranged from 0.005 to 0.05 mg/kg. Satisfactory precisions below 15% and accuracies within 85-115% were obtained for all compounds at concentrations exceeding the LOQ. In conclusion, we present a validated UHPLC-TOF-MS method for simultaneous quantification of 30 drugs in whole blood with a run time of 15 min using 200 μL of whole blood.
Keywords: Drugs of abuse, UHPLC-TOF-MS, Whole blood, SPE, Quantification
Prediction of methoxyl groups content in lignin based on ultimate analysisMichal Jablonsky
Different lignins (44 samples) were used in this study for predicting the correlation between the content of methoxyl groups in lignin and the hydrogen and oxygen contents. A significant linear correlation was found between the content of methoxyl groups of the lignin and its H and O contents. The contents of O and H were determined by ultimate analysis in previous studies reported in literature. The content of methoxyl groups (wt%) of lignin was calculated using the following equation: OCH3 = -18.5769 + 4.0658(H) + 0.34543(O), where the correlation coefficient was 0.766. The average absolute error of this correlation is 13.9% .
Synthesis of 3-methoxy-6-phenyl-6, 6a-dihydro-[1] benzopyrano-[3, 4-b] [1] be...IOSR Journals
Abstract: The 3-methoxy-6-phenyl-6,6a-dihydro-[1]benzopyrano-[3,4-b][1]benzopyran has been synthesised according to eight-steps synthesis. The target compound was obtained using a synthetic route based on two key cyclisations steps including the platinum chlorides-catalysed of alkynones and intramolecular oxo-Michael addition.
Quantitative Evaluation of Dissociation Mechanisms in Methylorange and MethylredAI Publications
Several computational chemistry programs were evaluated as aids to teaching a part of qualitative analytical chemistry. Computational chemical calculations can predict absorption spectra, thus enabling the modeling of indicator dissociation mechanisms using a personal computer. An updated MNDO program among 51 programs was previously found to be the best predictor to explain the dissociation mechanisms of isobenzofuranones and sulfonephthaleins. Therefore, the further quantitative analysis was performed for methyl-orange and methyl-red. Computational chemical analysis can be used for quantitative explanation of indicator dissociation mechanisms.
Perfluorocyclohexenyl Aryl Ether Polymers via Polycondensation of Decafluoroc...aaaa zzzz
ABSTRACT: A novel class of semifluorinated perfluorocyclohex- enyl (PFCH) aryl ether homo/copolymers was successfully synthesized with high yield through the step-growth polymer- ization of commercially available bisphenols and decafluorocy- clohexene in the presence of a triethylamine base. The synthesized polymers exhibit variable thermal properties depending on the functional spacer group (R). PFCH aryl ether copolymers with random and alternating architectures were also prepared from versatile bis-perfluorocyclohexenyl aryl ether monomers. The PFCH polymers show high thermal
stabilities with a 5% decomposition temperature ranging from 359 to 444 ﰀC in air and nitrogen atmosphere. These semifluori- nated PFCH aromatic ether polymers contain intact enchained PFCH olefin moieties, making further reactions such as cross- linking and application specific functionalization possible. VC 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014, 52, 232–238
Oxidative Coupling: A Tranquil Approach for Determination of Selexipag by Vis...Ratnakaram Venkata Nadh
The present study is a first report on development of a spectrophotometric method for determination of selexipag (used to cure pulmonary arterial hypertension) in bulk and tablet formulation and its validation. The basis of the proposed method is formation of a chromophore (of λ max 600 nm) in presence of acidic ferric chloride by oxidative coupling reaction between selexipag and MBTH (3-methylbenzo-thiazolin-2-one hydrazone) solution. Regression analysis (r > 0.999) shows that the plotted calibration curve exhibits good linearity in the studied range of concentration (5 – 30 μg mL-1). As per the existing guidelines of ICH, various parameters of the method were tested for validation. Low values of R.S.D. (< 2%) were observed indicating that the proposed method is reproducible, accurate and precise
Some physicochemical properties such as density, refractive index, solubility, conductance, dissociation constant etc. have been studied for some newly synthesized chalcones in different solvents at 308.15 K.
A simple, sensitive, precise, accurate, highly reproducible and economical, visible spectrophotometric
method for the determination lurasidone in bulk form was developed and validated. The method is
based on the formation of an oxidative coupling product by the reaction of lurasidone with 3-methylbenzothiazolin-
2-one hydrazone as a chromogenic reagent in presence of ferric chloride. The linear regression
analysis data for the calibration plot showed good linear relationship within the concentration range of 0–100
μg/mL with a correlation coefficient (r) value of 0.9997. The limits of detection and quantitation are 0.6 and
1.7 μg/mL, respectively. The method was tested and validated according to ICH guidelines. The results
demonstrated that the procedure is accurate, precise and reproducible (RSD < 2%).
Wave Frequency Invariance by Mathematically Based - Model TechnologyIJERA Editor
Frequency Invariance is an interesting complexity saving property that is shared by all the digital active
suppression method described in this paper .It follows from their same basic construction with silent
measurement tones and is possible due to the properties of the DFT. Frequency invariance applies both to the
model based. It means that if the RF signal and to the non –model based cancellers. It means that if the RF
signal changes its frequency location, the RFI estimate coefficient represented by the matrix K which are dived
do not read to be re-computed This is possible to achieve provided that a few criteria, which are described
below, are met. Technical details showing that the frequency invariance for the deterministic and stochastic RFI
cancellers can be found in respectively. Author complexity advantage with frequency invariance is that RFI
from several RF signal can be cancelled independently of each other and by using the same estimator
coefficients, k. Thats why this can be used in a scenario whose several amateur radio signal s in different HAM
band, or with two sufficiently separated AM radio station,
A Review of Intel Galileo Development Board’s TechnologyIJERA Editor
Intel Galileo, A Smart Arduino Based Development Board is cost-effective and efficient development board by
Intel Corporation. Three variants- Gen 1, Gen 2 and Edison is already being launched in the market. Intel, being
a market leader in development of Processor Technology is constantly researching and improving the Galileo
Technology. The board can lay strong foundation for embedded system researchers to develop various DIY
projects and build more energy efficient and cost effective products taking Galileo as the central controller. The
aim of this research paper is to highlight Intel Galileo Development Board Technology- Its features, Board
Components, Technology Available till date and Platform for programming various projects.
Role of the Biochemistry Labs in Promoting the Health Care Services for the I...IJERA Editor
The health care in the State of Kuwait depends to a greater extent on the biochemical and clinical labs attached
at each hospital. The data obtained from these laboratories will facilitate the process of diagnosing the disease
accurately. This will have a positive impact on the selection of appropriate treatment for the patients in general
and for diabetics specifically.
The main objective of this research was to build a profile for lab analysis and a database for building a
comprehensive system of integrated activities to raise health care for diabetic patients in Kuwait. The study
revealed the burden of admitted diabetic cases on the blood chemistry laboratory in Sabah Hospital (in relation
to length of stay and total numbers of lab requests). The aim was fulfilled by designing a model of the
biochemical tests for diabetics; filling in forms from the reality of patient data, completing and analyzing the
results electronically.
The study showed the importance of biochemical and clinical labs since they act as the link of patient's
information at the secondary health care level.
In this article, the issues that have captured the attention of researchers in multinational corporations (MNC) are
discussed and the emerging research agenda is laid out. The first part focuses on understanding the history, and
contemporary scale and significance of multinationals as economic actors. Two opposing perspectives are
distinguished, the economic and the political. In the past, there was a rigid divide between these but,
increasingly, researchers are using elements of both perspectives to understand the dynamics of multinationals.
The crucial additional feature here is the importation of insights from institutional literature on the relationship
between firms and national contexts. Multinational corporations (MNCs) are playing a large and growing role in
shaping our world, both economically and politically. Public and academic opinion has long been mired in an
inconclusive debate as to whether these phenomena are beneficial things that should be encouraged or harmful
things that need intensive governmental regulation. The integrating thesis of this book is that the question as to
whether they are good or bad is the wrong question and is based on the fundamentally faulty premise that all
foreign subsidiaries are essentially similar, i.e., MNCs are homogeneous entities The inevitability of
heterogeneity results in the imperatives of disaggregation and the fallacy of generalization if these complex,
differentiated phenomena are to be properly understood.
The Nanotechnological Innovation in Food IndustryIJERA Editor
The perspectives of direct energy action (DEA) technologies are discussed. The new classification of DEA
technologies is proposed. The possibilities of DEA technologies using in food nanotechnologies are analyzing.
The concepts of heat mass transfer during extraction and drying are considered in terms of food industry. The
hydrodynamic flows from food raw capillary structures are classified. The conditions of laminar and turbulent
barodiffusion are determined. The problem of combined DEA technologies processes simulation and the
objectives of experimental research are formulated. The new dimensionless number called as the number of
energy action is discussed. It is shown that the impulse electromagnetic field is an effective instrument for DEA
technology implementation
The synthesis of polyoxychloropropylenepoxymethacrylate oligoesters by esterification of polyoxychloropropylenetriepoxide by methacrylic acid has been carried out. It has been established that by varying the conditions of carrying out of the reaction, one can prepare, mainly, the mono-, di- and trimethacrylic oligoesters. On the basis of epoxy diane ED-20 and synthesized polyoxychloropropylenepoxymethacrylate oligoesters as modifiers there have been prepared the self-extinction compositions, which after curing by N, N1–diaminodiphenylsulfone possess higher physical-mechanical, adhesion and heat-physical properties.
Abstract
A small set of amphetamines has been analyzed by gas chromatography (GC) high-resolution time-of-flight mass spectrometry (TOFMS) using a microplasma photoionization (MPPI) soft-ionization source. This plasma-based, wavelength selectable ionization source enables ionization of the test compounds and their corresponding derivatives at ~8-12 eV that is a softer alternative to electron ionization at 70 eV. Three plasma gases were used in this study: Xe plasma that emits photons at resonance lines of 9.57 eV and 8.44 eV; Kr plasma at 10.63 eV and 10.02 eV, and Ar plasma at 11.82 eV and 11.61 eV. Derivatization of the test compounds with trifluoroacetic anhydride and α-methoxy-α-(trifluoromethyl)-phenylacetyl pyrazole was evaluated because the MPPI mass spectra of the underivatized amphetamines yield primarily iminium ions, which make the identification of the test compounds by GC-TOFMS inconclusive. The MPPI mass spectra of the TFA-derivatized amphetamines yield abundant molecular ions, when using Xe as plasma gas, and enough fragment ions with the Ar plasma that can help in formula generation. The structure elucidation of two "known unknowns" designer drugs using this "tunable" soft-ionization source and a high-resolution TOF mass spectrometer is presented in this study.
Determination of % purity of a compound by by Using DSCMUL
What is % purity?
Different methods to determine % Purity.
Determination of % purity of Organic Compound By Using DSC:
•1) Polycyclic aromatic Hydrocarbons e. g Benzo[c]phenanthrene, BcPh, C18H12
•2) Ibuprofen medicine
•3) Phenacetin samples at different purity ratios
•4) Methamphetamine Paracetamol and Mixture of both.
•5) AZT (C10H13N5O4; 3´-azido-2,3´-dideoxythymidine)
Quantitative Analysis of 30 Drugs in Whole Blood by SPE and UHPLC-TOF-MSAnnex Publishers
Abstract
An Ultra-High Pressure Liquid Chromatography Time-of-Flight Mass Spectrometry (UHPLC-TOF-MS) method for quantitative analysis of 30 drugs in whole blood was developed and validated. The method was used for screening and quantification of common drugs and drugs of abuse in whole blood received from autopsy cases and living persons. The compounds included: alprazolam, amphetamine, benzoylecgonine, bromazepam, cathine, cathinone, chlordiazepoxide, cocaine, codeine, clonazepam, 7-aminoclonazepam, diazepam, nordiazepam, flunitrazepam, 7-aminoflunitrazepam, ketamine, ketobemidone, 3,4-Methylenedioxyamphetamine (MDA), 3,4-methylenedioxymethamphetamine (MDMA), methamphetamine, methadone, morphine, 6-monoacetylmorphine, nitrazepam, 7-aminonitrazepam, oxazepam, temazepam, tramadol, O-desmethyltramadol, and zolpidem. Blood samples (200 μL) were subjected to Solid Phase Extraction (SPE). Target drugs were quantified using a Waters ACQUITY UPLC system coupled to a Waters SYNAPT G2 TOF-MS apparatus. Extraction recoveries ranged from 41% (7-aminoclonazepam) to 111% (ketamine) and matrix effects ranged from -13% (temazepam) to 50% (7-aminonitrazepam). For all compounds, a quadratic polynomial was applied for fitting the calibration curves. Lower Limits of Quantification (LOQ) ranged from 0.005 to 0.05 mg/kg. Satisfactory precisions below 15% and accuracies within 85-115% were obtained for all compounds at concentrations exceeding the LOQ. In conclusion, we present a validated UHPLC-TOF-MS method for simultaneous quantification of 30 drugs in whole blood with a run time of 15 min using 200 μL of whole blood.
Keywords: Drugs of abuse, UHPLC-TOF-MS, Whole blood, SPE, Quantification
Prediction of methoxyl groups content in lignin based on ultimate analysisMichal Jablonsky
Different lignins (44 samples) were used in this study for predicting the correlation between the content of methoxyl groups in lignin and the hydrogen and oxygen contents. A significant linear correlation was found between the content of methoxyl groups of the lignin and its H and O contents. The contents of O and H were determined by ultimate analysis in previous studies reported in literature. The content of methoxyl groups (wt%) of lignin was calculated using the following equation: OCH3 = -18.5769 + 4.0658(H) + 0.34543(O), where the correlation coefficient was 0.766. The average absolute error of this correlation is 13.9% .
Synthesis of 3-methoxy-6-phenyl-6, 6a-dihydro-[1] benzopyrano-[3, 4-b] [1] be...IOSR Journals
Abstract: The 3-methoxy-6-phenyl-6,6a-dihydro-[1]benzopyrano-[3,4-b][1]benzopyran has been synthesised according to eight-steps synthesis. The target compound was obtained using a synthetic route based on two key cyclisations steps including the platinum chlorides-catalysed of alkynones and intramolecular oxo-Michael addition.
Quantitative Evaluation of Dissociation Mechanisms in Methylorange and MethylredAI Publications
Several computational chemistry programs were evaluated as aids to teaching a part of qualitative analytical chemistry. Computational chemical calculations can predict absorption spectra, thus enabling the modeling of indicator dissociation mechanisms using a personal computer. An updated MNDO program among 51 programs was previously found to be the best predictor to explain the dissociation mechanisms of isobenzofuranones and sulfonephthaleins. Therefore, the further quantitative analysis was performed for methyl-orange and methyl-red. Computational chemical analysis can be used for quantitative explanation of indicator dissociation mechanisms.
Perfluorocyclohexenyl Aryl Ether Polymers via Polycondensation of Decafluoroc...aaaa zzzz
ABSTRACT: A novel class of semifluorinated perfluorocyclohex- enyl (PFCH) aryl ether homo/copolymers was successfully synthesized with high yield through the step-growth polymer- ization of commercially available bisphenols and decafluorocy- clohexene in the presence of a triethylamine base. The synthesized polymers exhibit variable thermal properties depending on the functional spacer group (R). PFCH aryl ether copolymers with random and alternating architectures were also prepared from versatile bis-perfluorocyclohexenyl aryl ether monomers. The PFCH polymers show high thermal
stabilities with a 5% decomposition temperature ranging from 359 to 444 ﰀC in air and nitrogen atmosphere. These semifluori- nated PFCH aromatic ether polymers contain intact enchained PFCH olefin moieties, making further reactions such as cross- linking and application specific functionalization possible. VC 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2014, 52, 232–238
Oxidative Coupling: A Tranquil Approach for Determination of Selexipag by Vis...Ratnakaram Venkata Nadh
The present study is a first report on development of a spectrophotometric method for determination of selexipag (used to cure pulmonary arterial hypertension) in bulk and tablet formulation and its validation. The basis of the proposed method is formation of a chromophore (of λ max 600 nm) in presence of acidic ferric chloride by oxidative coupling reaction between selexipag and MBTH (3-methylbenzo-thiazolin-2-one hydrazone) solution. Regression analysis (r > 0.999) shows that the plotted calibration curve exhibits good linearity in the studied range of concentration (5 – 30 μg mL-1). As per the existing guidelines of ICH, various parameters of the method were tested for validation. Low values of R.S.D. (< 2%) were observed indicating that the proposed method is reproducible, accurate and precise
Some physicochemical properties such as density, refractive index, solubility, conductance, dissociation constant etc. have been studied for some newly synthesized chalcones in different solvents at 308.15 K.
A simple, sensitive, precise, accurate, highly reproducible and economical, visible spectrophotometric
method for the determination lurasidone in bulk form was developed and validated. The method is
based on the formation of an oxidative coupling product by the reaction of lurasidone with 3-methylbenzothiazolin-
2-one hydrazone as a chromogenic reagent in presence of ferric chloride. The linear regression
analysis data for the calibration plot showed good linear relationship within the concentration range of 0–100
μg/mL with a correlation coefficient (r) value of 0.9997. The limits of detection and quantitation are 0.6 and
1.7 μg/mL, respectively. The method was tested and validated according to ICH guidelines. The results
demonstrated that the procedure is accurate, precise and reproducible (RSD < 2%).
Wave Frequency Invariance by Mathematically Based - Model TechnologyIJERA Editor
Frequency Invariance is an interesting complexity saving property that is shared by all the digital active
suppression method described in this paper .It follows from their same basic construction with silent
measurement tones and is possible due to the properties of the DFT. Frequency invariance applies both to the
model based. It means that if the RF signal and to the non –model based cancellers. It means that if the RF
signal changes its frequency location, the RFI estimate coefficient represented by the matrix K which are dived
do not read to be re-computed This is possible to achieve provided that a few criteria, which are described
below, are met. Technical details showing that the frequency invariance for the deterministic and stochastic RFI
cancellers can be found in respectively. Author complexity advantage with frequency invariance is that RFI
from several RF signal can be cancelled independently of each other and by using the same estimator
coefficients, k. Thats why this can be used in a scenario whose several amateur radio signal s in different HAM
band, or with two sufficiently separated AM radio station,
A Review of Intel Galileo Development Board’s TechnologyIJERA Editor
Intel Galileo, A Smart Arduino Based Development Board is cost-effective and efficient development board by
Intel Corporation. Three variants- Gen 1, Gen 2 and Edison is already being launched in the market. Intel, being
a market leader in development of Processor Technology is constantly researching and improving the Galileo
Technology. The board can lay strong foundation for embedded system researchers to develop various DIY
projects and build more energy efficient and cost effective products taking Galileo as the central controller. The
aim of this research paper is to highlight Intel Galileo Development Board Technology- Its features, Board
Components, Technology Available till date and Platform for programming various projects.
Role of the Biochemistry Labs in Promoting the Health Care Services for the I...IJERA Editor
The health care in the State of Kuwait depends to a greater extent on the biochemical and clinical labs attached
at each hospital. The data obtained from these laboratories will facilitate the process of diagnosing the disease
accurately. This will have a positive impact on the selection of appropriate treatment for the patients in general
and for diabetics specifically.
The main objective of this research was to build a profile for lab analysis and a database for building a
comprehensive system of integrated activities to raise health care for diabetic patients in Kuwait. The study
revealed the burden of admitted diabetic cases on the blood chemistry laboratory in Sabah Hospital (in relation
to length of stay and total numbers of lab requests). The aim was fulfilled by designing a model of the
biochemical tests for diabetics; filling in forms from the reality of patient data, completing and analyzing the
results electronically.
The study showed the importance of biochemical and clinical labs since they act as the link of patient's
information at the secondary health care level.
In this article, the issues that have captured the attention of researchers in multinational corporations (MNC) are
discussed and the emerging research agenda is laid out. The first part focuses on understanding the history, and
contemporary scale and significance of multinationals as economic actors. Two opposing perspectives are
distinguished, the economic and the political. In the past, there was a rigid divide between these but,
increasingly, researchers are using elements of both perspectives to understand the dynamics of multinationals.
The crucial additional feature here is the importation of insights from institutional literature on the relationship
between firms and national contexts. Multinational corporations (MNCs) are playing a large and growing role in
shaping our world, both economically and politically. Public and academic opinion has long been mired in an
inconclusive debate as to whether these phenomena are beneficial things that should be encouraged or harmful
things that need intensive governmental regulation. The integrating thesis of this book is that the question as to
whether they are good or bad is the wrong question and is based on the fundamentally faulty premise that all
foreign subsidiaries are essentially similar, i.e., MNCs are homogeneous entities The inevitability of
heterogeneity results in the imperatives of disaggregation and the fallacy of generalization if these complex,
differentiated phenomena are to be properly understood.
The Nanotechnological Innovation in Food IndustryIJERA Editor
The perspectives of direct energy action (DEA) technologies are discussed. The new classification of DEA
technologies is proposed. The possibilities of DEA technologies using in food nanotechnologies are analyzing.
The concepts of heat mass transfer during extraction and drying are considered in terms of food industry. The
hydrodynamic flows from food raw capillary structures are classified. The conditions of laminar and turbulent
barodiffusion are determined. The problem of combined DEA technologies processes simulation and the
objectives of experimental research are formulated. The new dimensionless number called as the number of
energy action is discussed. It is shown that the impulse electromagnetic field is an effective instrument for DEA
technology implementation
Secure Syntactic key Ranked Search over Encrypted Cloud in DataIJERA Editor
In Today‟s world cloud computing is one of the most effective data storage centre. The data owners usually
want to share or outsource their data. They find cloud is the alternative storage data centre to outsource their
data from local sites to cloud server. Outsourcing data will have great flexibility and economically effective.
Usually outsourcing data is sensitive data. So we need to provide some security to that data.
As data is sensitive we use access control mechanisms to stop accessing unauthorized users in clouds. The data
must be encrypted before it is going to outsource. Which obsoletes traditional data utilization based on plaintext
keyword search Thus, enabling an encrypted cloud data search service is of paramount importance. Cloud
usually maintains multiple users and also stores huge amount of data in it. In the proposed system we use a
multiple search keyword for searching most relevant data stored in clouds. In early system, the scheme is
entirely focused on single key search or a Boolean keyword search.
In implementing system we overcome the all the problems in the existing system like single key search
technique, unauthorized users access on data stored in clouds. We used Access Control method to to avoid
unauthorized access from data stored in clouds. For multi keyword search we proposed “coordinate matching”
that is “ as many matches as possible” for the given query.
An Evaluation System of Surface Water Quality in Algeria (Application on the ...IJERA Editor
Easily accessible surface waters remain very fragile and very vulnerable to various types of pollution. Chellif,
Macta and Tafna Basins are considered as the main water resources feeding the North West of Algeria; however,
protection and conservation of these water resources become the major concern of the researchers. The
evaluation system of the water quality is based on the measure of physic-chemical parameters of the surface
water according to the uses of water for drink, industry or agriculture. In this work we have to proceed to an
application of this system to the surface waters on the three basins. Physic-chemical analyses are used for a
period of three years (2012-2014) and several points chosen on the three catchments are taken into account.
In this paper we shall apply the quality index calculation method for the Water Quality Evaluation system
(WQES) and the follow-up of the impacts of the anthropologic activities on the natural environment The main
results are the validation of the WQES method for different type of pollution as mineral, organic, heavy metals
in the West of Algeria, this methodology give us possibility for better investigation of the water pollution
The Recent Trend: Vigorous unidentified validation access control system with...IJERA Editor
Service Providers can grow their business by selling our cloud authentication service that can be fully branded
to the Service Provider or if required a Service. The proposed enhanced decentralized access control scheme for
secure data storage in clouds that supports anonymous authentication. In the proposed scheme, the cloud verifies
the authenticity of the series without knowing the user’s identity before storing data. The scheme also has the
added feature of access control in which only valid users are able to decrypt the stored information. The scheme
prevents replay attacks and supports creation, modification, and reading data stored in the cloud. It addresses
user revocation. Moreover, our authentication and access control scheme is decentralized and robust, unlike
other access control schemes designed for clouds which are centralized. The communication, hiding attributes,
increasing high security in access, computation, and storage overheads are comparable to centralized
approaches.
In Existing, it is based on ABE (attribute based encryption) technique which is a centralized approach, where a
single Key Distribution Centre (KDC) distributes secret keys and attributes to all users using asymmetric key
approach. We propose a new decentralized access control method for storing data by providing security in
clouds and also we hide the attributes and access rule of a user. The cloud validates the authentication of the
sequence without knowing the users characteristics previous to the data store. By using this approach only
certified users have right to use the suitable attributes. In future, time based file revocation scheme can be used
to assure the deletion of a file. When time limit of a file expires, we implement the policy based renewal of time
to that file.
New Technique Using Multiple Symmetric keys for Multilevel EncryptionIJERA Editor
In a world of accelerating communications, cryptography has become an essential component of the modern
means of communication systems. The emergence of the webas a reliable medium for commerce and
communication has made cryptography an essential component. Many algorithms or ciphers are in use
nowadays. The quality of the cipher is judged byits ability to prevent an unrelated party fromknowingthe
original content of the encrypted message. The proposed “Multilevel Encryption Model” is a cryptosystem that
adopts the basic principles of cryptography. It uses five symmetric keys (multiple)
in floating point numbers, plaintext, substitution techniques and key combinations with unintelligible
sequence to produce the ciphertext. The decryption process is also designed to reproduce the plaintext
The Research on the Additives of the High Performance ConcreteIJERA Editor
With the development of technologies of admixture and additive in concrete ,the technological base for making
up high performance concrete has been laid. High performance concrete should have not only high strength,but
also excellent durability ,relatively high temperature crack resistance and relatively high volume stability ,etc .
The most effective ingredients for making up high performance concrete are super- plasticizing agent ,fly ash or
slag powder ,silicon powder . Main properties and usages of these materials are briefly expounded to provide
some practical guides for making up high performance concrete.
Effect of Guar Flour Supplementation on Quality and Shelf Life of Muffins IJERA Editor
The drought resistant and lesser explored legume, Guar bean (Cyamopsis tetragonoloba), was used to prepare
muffins with higher protein content. In present study, the muffins were prepared using three varieties of treated
guar flour i.e. G 80, Ageta 112, HG 365 at supplementation levels 10, 15 and 5 per cent respectively, for storage
studies under different conditions. The moisture content, water activity (aw), free fatty acids, peroxide value,
microbial analysis and sensory evaluation were done at a regular interval of seven days. Moisture content of
muffins increased significantly with increase in time of storage under both ambient and refrigerated conditions.
Water activity value increased with increase in time period under both the storage conditions. Addition of guar
flour to muffin had no effect on the water activity that increased gradually upto 0.83. Guar supplemented
muffins showed higher moisture content than control and maximum in G 80 supplemented muffins. Formation
of free fatty acids (% oleic acid) and peroxide value increased with increased storage period. The changes in
values were more readily pronounced at ambient temperatures. The overall acceptability was maximum for
Ageta 112 supplemented muffins however the acceptability reduced with increased storage. The microbial
analysis showed that refrigerated muffins were acceptable even at 28th day of storage analysis while the muffins
at ambient conditions showed lesser shelf life. Muffins supplemented with HG 365 were spoiled at 21st day of
storage analysis under ambient storage conditions.
MIMO Systems for Military Communication/Applications.IJERA Editor
The Military is embracing the communication revolution, turning to a new generation of sophisticated systems
to enable faster, richer, less costly, more flexible, reliable, compact, mobile, jam resistant, low probability of
detection, re configurable and spectrally efficient communication. Many of these features can be added to a
great extent in the existing systems, by utilising MIMO technology appropriately and judiciously. MIMO finds
applications in wireless communication, NLOS communication, satellite communication, HF communication,
Optical Fibre Communication. MIMO makes these technologies more suitable by introducing features
mandatory for military communication such as Ant jamming capability, Low Probability of Intercept, low
visibility of satellite earth Antennas by reducing their aperture area. MIMO can also provide redundancy by
employing no extra resources, thereby increasing reliability. MIMO is highly effective to communicate with
Unmanned Aerial Vehicles (1).
Synthesis Of Cobalt Doped Titania Nano Materials Assisted By Anionic Heteroge...IJERA Editor
: This paper presents about the synthesis of (0.25-1.0) wt.% cobalt doped titania nanomaterials
without surfactants: pure Co2+/TiO2 and in presence of 1,4-Butane sultone and 1,3-Propane sultone Anionic
Gemini surfactants and CTAB (Heterogemini surfactant)-0.5wt.%Co2+/TiO2-HgS(1&2).The synthesized nano
photocatalysts have been characterized by using various advanced techniques like X-Ray Diffraction (XRD),
Ultraviolet-visible Diffuse Reflection Spectroscopy (UV-Vis DRS), X-ray Photoelectron Spectroscopy (XPS),
Scanning Electron Microscopy (SEM), Energy Dispersive Spectrometry (EDS), Fourier Transform Infrared
Spectroscopic Studies (FT-IR), Transmission Electron Microscopy (TEM). From the characterization studies all
the catalysts synthesized were reported in anatase phase. TEM indicates the particles size of prepared catalysts
reported with 7-10 nm and 15 nm for pure Co2+/ TiO2 catalyst. From XPS studies Cobalt was found to be in +2
oxidation state. From BET results the surface area was reported to be-89.51 and 77.93 (m2
/g) for Co2+/TiO2-
HgS(1)& Co2+/TiO2-HgS(2). From UV-DRS studies absorbance band shifted more towards visible region (red
shift). In order to find out the efficiency of the synthesized photocatalyst the photocatalytic activity studies were
carried out by degradation of Acid Red as a model azo dye pollutant in presence of the visible light irradiation.
The antibacterial activity of the synthesized catalysts against Escherichia coli was also studied. Thus from the
results 0.5wt.% Co2+/TiO2-HgS(1) exhibited highest photocatalytic activity for the degradation of azo dye Acid
Red as well as proved to be an excellent antibacterial agent
Analytical and Experimental analysis ofthermal characteristics throughTriangu...IJERA Editor
Microscale heat transfer technique is widely intended for best cooling applications in electronic devices as high
heat transfer coefficients are achieved in microscale convection. In present study, analysis of thermal
characteristics has been carried out by analytical calculations along with experimental investigation for a straight
microchannel heat sink of equilateral triangular cross section of 173.21 μm hydraulic diameter with distilled
water as the working fluid. Designed Heater input watts and Reynolds number based on flow rate are varied for
optimized microchannel geometry. Experimental analysis is carried out under constant heat flux condition. The
microchannels are produced on highly accurate micro wire cut EDM. The Reynolds number is varied from 100
to 700. The major intension for this work is to enhance heat transfer coefficient and minimize pressure drop
across microchannel. The Reynolds number, temperature distribution, pressure distribution, heat transfer
coefficient, hydrodynamic entrance length, thermal entrance length, equivalent thermal resistances parameters
are calculated for microchannel heat sink performance analysis. The results of analytical calculations are verified
with experimental investigation. It is found that heat transfer coefficient and pressure drop increases with
increase in Reynolds numbers and decrease in microchannel heat sink hydraulic diameter. Also channel length is
directly proportional to temperature rise
Big Data for New Industrialization and Urbanization Development: A Case Study...IJERA Editor
Industrialization and urbanization are considered as interdependent processes of recent economic development.
Innovations in technology and higher affordability of electronic devices have facilitated current age of big data.
Use of digital data provided modern urbanization which is an essential element of industrialization and rapid
income growth globally. Most manufacturing and service production is efficient when undertaken in urbanized
areas where organizations can readily follow best practice in technology and management. Over the past three
decades, China has achieved enormous economic growth, accompanied by a growing number of large cities.
The purpose of this paper is to identify prominent issues relating influence of big data on modern
industrialization and urbanization development in China as well as in other regions. The case study of China
was taken to understand the advancement of big data on industrialization and urbanization enhancement. It was
investigated that industrialization and the rise of the service sector appear to have influenced the growth of
urbanization, but their role was relatively small when compared to the direct effects of economic growth. In the
coming years, urbanization will become increasingly an opportunity as well as a challenge to the country‟s
effort to sustain rapid growth and maintain effective development
Digitization of Speedometer Incorporating Arduino and Tracing of Location Usi...IJERA Editor
This paper deals with the method of telemetric field which has grown exponentially in recent years. A correct
characterization is to handle, analyze the signals from the sensor which switches, positions and detects the
speed. Placing the sensor on the wheels of the train, a continuous pulse train of signal will be proportional to
train speed and it is sent toArduino microcontroller to analyze, process and simultaneously data will be stored
in memory and displayed. In addition, GPS is used to trace the current location and it is viewed with the help of
LCD placed in every compartment. Thus the simulation has been carried out using MATLAB/SIMULINK
software. Both the simulation and experimental results under diverse conditions are presented to clearly describe
the process of characterization of our system.
An Overview of the Entrepreneurial Process in Distance Education (DE) of UNESAIJERA Editor
This article presents a panoramic view of entrepreneurship of Distance Education (DE) at UniversityEstácio de
Sá (UNESA) of Brazil. It is based on field research, interviews and bibliographical research on the processes of
teaching and learning in Distance Education (DE), especially those used in academic education. The aim of this
article is to show the existence of the entrepreneur process in the Distance Education of University Estácio de Sá
(DE-UNESA). To this end, the article takes a qualitative approach denoting interpretative grounds and connects
the entrepreneurial process with the DE-UNESA. It presents a graphic illustrating the entrepreneurial process
model by adding the factor-educator or educational. In addition, describes information about DE-UNESA
backdrop developer of a continuous educational entrepreneurship.
Leave one out cross validated Hybrid Model of Genetic Algorithm and Naïve Bay...IJERA Editor
This paper presents a new approach to select reduced number of features in databases. Every database has a
given number of features but it is observed that some of these features can be redundant and can be harmful as
well as confuse the process of classification. The proposed method first applies a binary coded genetic algorithm
to select a small subset of features. The importance of these features is judged by applying Naïve Bayes (NB)
method of classification. The best reduced subset of features which has high classification accuracy on given
databases is adopted. The classification accuracy obtained by proposed method is compared with that reported
recently in publications on eight databases. It is noted that proposed method performs satisfactory on these
databases and achieves higher classification accuracy but with smaller number of feature
Strategies and Modeling of Reverse Logistics Networks of an Industry in IndiaIJERA Editor
Among the various aspects of SCM, emphasis has been placed on reverse logistics: closing the loop of a supply
chain by integrating waste materials into logistic management decisions. Logistics network design is commonly
recognized as a strategic supply chain issue of prime importance. While consumers traditionally dispose of
products at the end of their life cycle, product take-back legislations introduced by governments shift this
responsibility from consumers to manufacturers. As a result, manufacturers have to collect products at the endof-life
(EOL) and control their recovery or disposal. Product recovery, which encompasses reuse,
remanufacturing and materials recycling, requires a structured reverse logistic network in order to collect
products efficiently at the end of their life cycle. Meanwhile, ever growing concern for environmental problems
and pressure from the global competitive marketplace toward further improvement of customer service, have
been presenting industries with a new challenge; development and management of effective reverse logistics
processes. The purpose of this paper is to present an overview to reverse logistics, and to provide insights on
how to manage the creation of economically efficient EOL product returns and recycling practice in an Industry
of India.
A Computational Investigation of Flow Structure Within a Sinuous DuctIJERA Editor
In the present investigation the distribution of mean velocity are experimentally studied on three constant area
rectangular curved ducts with an aspect ratio of 2.4. First one is C-shape, second one is S-shape and third one
is a DS-shape duct. The experiment is carried out at mass averaged mean velocity of 40m/s for all the ducts.
The velocity distribution shows for C-duct, the bulk flow shifting from outer wall to the inner wall along the
flow passage and for S-duct, the bulk flow shifting from outer wall to the inner wall in the first half and from
inner wall to the outer wall in the second half along the flow passage of curved ducts are very instinct. Due to
the imbalance of centrifugal force and radial pressure gradient, secondary motions in the forms of counter
rotating vortices have been generated within both the curved duct. For DS-duct the velocity distributions shows
the Bulk of flow shifting from inner watt to outer wall in the first bend and third bend of the duct and outer wall
to inner wall in the second bend and forth bend of the duct along the flow passage is very instinct. Flow at end
of the DS-duct is purely uniform in nature due to non existence of secondary motion. The experimental results
then were numerically validated with the help of Fluent, which shows a good agreement between the
experimental and predicted results for all the ducts
In this work a new prodrug polymer was
prepared with two attachment groups (amid-ester), using di
functional spacer such as ethanol amine, which could react with
polyacrylic acid producing amide group, with remain ethanol
terminal group which could react with captopril acyl chloride,
producing ester group with extended the arm substituted drug to
improve the hydrolysis and to prevent the steric effect of polymer
chains. Many advantages enhanced the prodrug of polymer. The
prepared polymers were characterized by FTIR, 1H –NMR
spectroscopies. Controlled drug release was studied in different
pH values at 37℃, using UV. Spectra with comparing with
calibration curve. The modification percentage test was studied,and swelling percentage was calculated and all physical properties were observed.
In this work, the synthetic hydroxyapatite (HAP) was studied using different preparation routes to decrease the crystal size and to study the temperature effect on the HAP nano-sized hydroxyapatite crystallization. X-ray diffraction (XRD) analysis indicated that all samples were composed by crystalline and amorphous phases . The sample with greater quantity of amorphous phase (40% of total mass) was studied. The nano-sized hydroxyapatite powder was heated and studied at 300, 500, 700, 900 and 1150 °C. All samples were characterized by XRD and their XRD patterns refined using the Rietveld method. The crystallites presented an anisotropic form, being larger in the [001] direction. It was observed that the crystallite size increased continuously with the heating temperature and the eccentricity of the ellipsoidal shape changed from 2.75 at 300 °C to 1.94, 1.43, 1.04 and 1.00 respectively at 500, 700, 900 and 1150 °C. In order to better characterize the morphology of the HAP the samples were also examined using atomic force microscopy (AFM), infrared spectrometry (IR) and thermogravimetric analysis (TGA).
International Journal of Engineering Research and DevelopmentIJERD Editor
Electrical, Electronics and Computer Engineering,
Information Engineering and Technology,
Mechanical, Industrial and Manufacturing Engineering,
Automation and Mechatronics Engineering,
Material and Chemical Engineering,
Civil and Architecture Engineering,
Biotechnology and Bio Engineering,
Environmental Engineering,
Petroleum and Mining Engineering,
Marine and Agriculture engineering,
Aerospace Engineering.
International Journal of Engineering Research and Applications (IJERA) is an open access online peer reviewed international journal that publishes research and review articles in the fields of Computer Science, Neural Networks, Electrical Engineering, Software Engineering, Information Technology, Mechanical Engineering, Chemical Engineering, Plastic Engineering, Food Technology, Textile Engineering, Nano Technology & science, Power Electronics, Electronics & Communication Engineering, Computational mathematics, Image processing, Civil Engineering, Structural Engineering, Environmental Engineering, VLSI Testing & Low Power VLSI Design etc.
New Schiff base ligand (E)-6-(2-(4-
(dimethylamino)benzylideneamino)-2-phenylacetamido)-3,3-
dimethyl-7-oxo-4-thia-1-azabicyclo[3.2.0]heptane-2-carboxylic
acid = (HL) Figure(1) was prepared via condensation of
Ampicillin and 4(dimethylamino)benzaldehyde in methanol
.Polydentate mixed ligand complexes were obtained from 1:1:2
molar ratio reactions with metal ions and HL, 2NA on reaction
with MCl2 .nH2O salt yields complexes corresponding to the
formulas [M(L)(NA)2Cl] ,where M =
Fe(II),Co(II),Ni(II),Cu(II),and Zn(II) and NA=nicotinamide.
The 1H-NMR, FT-IR, UV-Vis and elemental analysis
were used for the characterization of the ligand. The complexes
were structurally studied through AAS, FT-IR, UV-Vis,
chloride contents, conductance, and magnetic susceptibility
measurements. All complexes are non-electrolytes in DMSO
solution. Octahedral geometries have been suggested for each
of the complexes. The Schiff base ligands function as
tridentates and the deprotonated enolic form is preferred for
coordination. In order to evaluate the effect of the bactericidal
activity, these synthesized complexes, in comparison to the un
complexed Schiff base has been screened against bacterial
species, Staphy
A novel flame retardant application technique was developed for cotton apparel fabric using spirocyclic
pentaerythritol di (phosphoryl chloride) (SPDPC), which was further synthesized into bis diglycol spirocyclic
pentaerythritol bisphosphorate (BSPB). The flame retardant agent was then attached to the fabric using a
sol-gel process. The treated fabric was tested on a vertical flame tester which showed very high flame
retardancy as compared to the untreated cotton. TGA analysis exhibited a slow rate of weight loss and
higher ultimate degradation temperature for the FR treated sample. The FR treated sample showed modest
loss in strength while retaining 86.4% of its original strength. The fabric’s appearance did not alter and the
change in stiffness was insignificant as a result of the FR finish.
Experimental and theoretical studies on the photodegradation of 2-ethylhexyl ...Maciej Przybyłek
2-Ethylhexyl 4-methoxycinnamate (EHMC) is one of the most commonly used sunscreen ingredient. In this study we investigated photodegradation of EHMC in the presence of such common oxidizing and chlorinating systems as H2O2, H2O2/HCl, H2O2/UV, and H2O2/HCl/UV. Reaction products were detected by gas chromatography with a mass spectrometric detector (GC-MS). As a result of experimental studies chloro-substituted 4-methoxycinnamic acid (4-MCA), 4-methoxybenzaldehyde (4-MBA) and 4-methoxyphenol (4-MP) were identified. Experimental studies were enriched with DFT and MP2 calculations. We found that reactions of 4-MCA, 4-MBA and 4-MP with Cl2 and HOCl were in all cases thermodynamically favorable. However, reactivity indices provide a better explanation of the formation of particular chloroorganic compounds. Generally, those isomeric forms of mono- and dichlorinated compounds which exhibits the highest hardness were identified. Nucleophilicity of the chloroorganic compounds precursors were examined by means of the Fukui function.
Synthesis and Characterization of Nano Hydroxyapatite with Agar-Agar Bio-PolymerIJERA Editor
Hydroxyapatite used for bone replacement is one of the most active areas of ceramic biomaterials research currently. It is a desirable implant material due to its biocompatibility and osteoconductive properties. Agar agar is a biological polymer frequently used in tissue engineering and pharmaceutical for potential use in bone replacement. Nano hydroxyapatite was successfully synthesized by wet chemical precipitation method . In this work nHAp/agar composite were synthesized and characterization of the compound were done by using characterization Fourier transform infrared(FTIR), X-ray diffract ration (XRD), Transmission electron microscope(TEM) and Energy dispersive analysis of X-ray spectrum(EDAX).
Visible Spectrophotometric Determination of Gemigliptin Using Charge Transfer...Ratnakaram Venkata Nadh
A visible spectrophotometric method was developed and validated for the determination of gemigliptin present in bulk drug and tablet formulation. It involves an indirect method of charge transfer complex formation in presence of NBS, metol and suphanilic acid. Gemigliptin was subjected to oxidation with excess amount of oxidant (NBS) and the unconsumed NBS oxidizes metol to give p-N-methylbenzoquinone monoamine (PNMM) which in turn forms a charge transfer complex with sulphanilic acid. Then validated the above developed method as per the current ICH guidelines. An excellent correlation coefficient (> 0.999) was found for the obtained regression equation
(y = –0.0302x + 0.928) in the range of 2.0–30.0 μg mL-1. The method was found to be simple and rapid because it does not involve any solvent extraction. The recovery levels of the drug were in the range 99.92 – 100.08.
Synthesis of graphene oxide-TiO2 nanocomposite as an adsorbent for the enrich...Nanomedicine Journal (NMJ)
Abstract
Objective(s):
In our study, graphene oxide-TiO2 nanocomposite (GO/TiO2) was prepared and used for the enrichment of rutin from real samples for the first time.
Materials and Methods:
The synthesized GO/TiO2 was characterized by X-ray diffraction, scanning electron microscopy, and FT-IR spectra. The enrichment process is fast and highly efficient. The factors including contact time, pH, and amount of GO/TiO2 affecting the adsorption process were studied.
Results:
The maximum adsorption capacity for ciprofloxacin was calculated to be 59.5 mg/g according to the Langmuir adsorption isotherm. The method yielded a linear calibration curve in the concentration ranges from 15 to 200 μg/L for the rutin with regression coefficients (r2) of 0.9990. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were found to be 8 μg/Land 28 μg/L, respectively. Both the intra-day and inter-day precisions (RSDs) were < 10% .
Conclusion:
The developed approach offered wide linear range, and good reproducibility. Owing to the diverse structures and unique characteristic, GO/TiO2 possesses great potential in the enrichment and analysis of trace rutin in real aqueous samples.
Evaluation of mechanical and thermal properties of microwave irradiated poly ...Mukarram Zubair
Poly (styrene-co-methyl methacrylate) (P(S-co-MMA)) was blended with pristine graphene (G) by melt mixing technique and treated under microwave irradiation. The nanocomposites were irradiated for 5 and 10 min at frequency 1245 MHz.
Structure changes in the irradiated nanocomposites were observed by Fourier transform infrared spectroscopy and Raman spectroscopy. The irradiated composites showed a significant increase in the storage modulus i.e. 21% for 0.1% and 31% for
1% graphene polymer composites after 5 min irradiation. However at higher irradiation (10 min), degradation of nanocomposites was observed. The concept of improvement of interfacial interaction between graphene and P(S-co-MMA) chains at 5-min microwave exposure and degradation of nanocomposites at higher irradiation duration was assessed and supported by X-ray diffraction and scanning electron
microscopy.
Pyroligneous Liquor Produced at Different Heating Rates in Pyrolysis of Eucal...CrimsonpublishersMCDA
The objective of this research was to analyze the influence of two different heating rates (2.67 °C/min, 0.67 °C/min), reaching 500 °C as final temperature in pyrolysis, on the chemical composition of the pyroligneous liquor produced. Three pyrolysis sessions were performed for each heating rate on Eucalyptus urograndis wood chips in an oven-muffle connected to a gas-collecting system. The gravimetric yield was calculated, and the chemical compounds of pyroligneous liquors were identified through gas chromatograph-mass spectrometer. Heating rates did not affect the gravimetric yield of final products. However, qualitative differences were observed in the chemical composition of pyroligneous liquors produced. The presence of 1-hidroxy 2-propanone, 4-methylphenol (p-cresol), and 5-hidroxymethyl 2-furaldehyde compounds was detected only in the pyroligneous liquor produced at the highest heating rate (2.67 °C/min).
https://crimsonpublishers.com/mcda/fulltext/MCDA.000527.php
For more open access journals in Crimson Publishers please click on link: https://crimsonpublishers.com
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Biomass is considered as a potential source of energy production.Gasification can be employed to convert
dilute biomass energy source in to gaseous products holding concentrated form of energy. A steady state model for fluidized
bed biomass gasifier is developed based on reaction kinetics and hydrodynamic aspects of fluidization. The presence of
sorbent for absorption of carbon dioxide from the product gas is also incorporated in the model.The developed model
predicts the variation of syngas composition, temperature, pressure and velocity along the height of gasifier. Experiments
were carried out in a lab scale fluidized bed biomass gasifier and the results were used to validate the model.An increase of
50.35% in H2 mole fraction and a decrease of 50.88 % in CO2 mole fraction were observed when CaO was used as the
sorbent.
Physicochemical and Spectroscopic Characterization of Biofield Energy Treated...rachelsalk
The p-anisidine is widely used as chemical intermediate in the production of various dyes, pigments, and pharmaceuticals. This study was aimed to evaluate the effect of biofield energy treatment on the physicochemical and spectroscopic properties of p-anisidine. The study was performed after dividing the sample in two groups; one was remained as untreated and another was subjected to Mr. Trivedi’s biofield energy treatment. Afterward, both the control and treated samples of p-anisidine were evaluated using X-ray diffraction (XRD), surface area analyzer, differential scanning calorimetry (DSC), thermogravimetric analysis-derivative thermogravimetry (TGA-DTG), Fourier transform infrared (FT-IR), and ultraviolet-visible (UV-Vis) spectroscopy. The XRD analysis showed the increase in unit cell volume from 683.81 → 690.18 × 10-24 cm3 and crystallite size from 83.84→84.62 nm in the treated sample with respect to the control. The surface area analysis exhibited the significant increase (25.44%) in the surface area of treated sample as compared to control. The DSC thermogram of control p-anisidine showed the latent heat of fusion and melting temperature and 146.78 J/g and 59.41°C, respectively, which were slightly increased to 148.89 J/g and 59.49°C, respectively after biofield treatment. The TGA analysis showed the onset temperature of thermal degradation at 134.68°C in the control sample that was increased to 150.02°C after biofield treatment. The result showed about 11.39% increase in onset temperature of thermal degradation of treated p-anisidine as compared to the control. Moreover, the Tmax (temperature at which maximum thermal degradation occurs) was also increased slightly from 165.99°C (control) to 168.10°C (treated). This indicated the high thermal stability of treated p-anisidine as compared to the control. However, the FT-IR and UV spectroscopic studies did not show any significant changes in the spectral properties of treated p-anisidine with respect to the control.
Physicochemical and Spectroscopic Characterization of Biofield Energy Treated...wilhelm mendel
The p-anisidine is widely used as chemical intermediate in the production of various dyes, pigments, and pharmaceuticals. This study was aimed to evaluate the effect of biofield energy treatment on the physicochemical and spectroscopic properties of p-anisidine. The study was performed after dividing the sample in two groups; one was remained as untreated and another was subjected to Mr. Trivedi’s biofield energy treatment. Afterward, both the control and treated samples of p-anisidine were evaluated using X-ray diffraction (XRD), surface area analyzer, differential scanning calorimetry (DSC), thermogravimetric analysis-derivative thermogravimetry (TGA-DTG), Fourier transform infrared (FT-IR), and ultraviolet-visible (UV-Vis) spectroscopy. The XRD analysis showed the increase in unit cell volume from 683.81 → 690.18 × 10-24 cm3 and crystallite size from 83.84→84.62 nm in the treated sample with respect to the control. The surface area analysis exhibited the significant increase (25.44%) in the surface area of treated sample as compared to control. The DSC thermogram of control p-anisidine showed the latent heat of fusion and melting temperature and 146.78 J/g and 59.41°C, respectively, which were slightly increased to 148.89 J/g and 59.49°C, respectively after biofield treatment. The TGA analysis showed the onset temperature of thermal degradation at 134.68°C in the control sample that was increased to 150.02°C after biofield treatment. The result showed about 11.39% increase in onset temperature of thermal degradation of treated p-anisidine as compared to the control. Moreover, the Tmax (temperature at which maximum thermal degradation occurs) was also increased slightly from 165.99°C (control) to 168.10°C (treated). This indicated the high thermal stability of treated p-anisidine as compared to the control. However, the FT-IR and UV spectroscopic studies did not show any significant changes in the spectral properties of treated p-anisidine with respect to the control.
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Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
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Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
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Indigenized remote control interface card suitable for MAFI system CCR equipment. Compatible for IDM8000 CCR. Backplane mounted serial and TCP/Ethernet communication module for CCR remote access. IDM 8000 CCR remote control on serial and TCP protocol.
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Physicochemical Properties and Proposed Mechanism in the Obtainment of 4-Hidroxycoumarin Conjugated Polymers Using MALDI-T of Analysis
1. Hugo A. Garro.et. al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 6, Issue 3, (Part - 4) March 2016, pp.84-89
www.ijera.com 84|P a g e
Physicochemical Properties and Proposed Mechanism in the
Obtainment of 4-Hidroxycoumarin Conjugated Polymers Using
MALDI-T of Analysis
Hugo A. Garro*1
,Joaquín Morillas1
, Ezequiel F. Bruna-Haupt1
, Gabriela
Petroselli*2
,Carlos R. Pungitore1
, Carlos E. Tonn1
and Rosa Erra-Balsells2
1
INTEQUI-CONICET. Area de Química Orgánica.Facultad de Química, Bioquímica y Farmacia. Universidad
Nacional de San Luis. 5700 San Luis, Argentina.
2
CIHIDECAR-CONICET. Departamento de Química Orgánica, Facultad de Ciencias Exactas y
Naturales.Universidad de Buenos Aires, 1428 Buenos Aires, Argentina.
ABSTRACT
The mechanism for the poly-condensation event of conjugated polymers with ending 4-hydroxycoumarin has
been proposed. It happened under H2SO4 acidic conditions only using enolic-coumarins without any substituent
at third position. It was studied using Matrix assisted laser desorption/ionization time-of-flight (MALDI-Tof)
mass spectrometry. Besides, some physicochemical properties were analyzed using Thermo-gravimetric (TGA),
X-ray and UV-Vis analysis.
Keywords: Self-condensation mechanism, MALDI-Tof, X-ray, TGA, UV-Vis,telechelic polymer, applications
I. INTRODUCTION
Fragmentation of analyte molecules upon
laser irradiation can be substantially reduced by
embedding them in a light absorbing matrix. As a
result, intact analyte molecules are desorbed and
ionized along with the matrix and can be analyzed
in a mass spectrometer. This soft ionization
technique is mostly combined with time-of-flight
mass analyzers. So, Tof-MS not only presents the
advantage of being capable to provide a complete
mass spectrum per event, but also it has virtually
unlimited mass range, needs small amount of
analyte, and the equipment has a relatively low
cost.1-6
In the last years, coumarins polymers have
emerged as structures with important nonlinear
optical (NLO) properties. This field is concerned
with the interactions of electromagnetic fields and
different material such as coumarins polymers to
produce compounds with changes in phase,
frequency or amplitude. The main applications of
these materials with nonlinear optical properties are
in doublers of frequency for lasers, optical
communications, computers and laser resistance
devices.7
X-ray scattering are largely used to
calculate the periodicity and the thickness of
constituent phases in the one-dimensional model
for semi-crystalline compounds. The decrease of
the periodicity was undoubtedly observed with the
increase of the isothermal crystallization time,
while the ambiguity in the attribution of the phases
to the amorphous and crystal thickness was source
of large debate.5, 6
Also stability and thermal
behavior can be used to determine the sample
moisture content, hydration level, and
decomposition temperature.
In thermogravimetry (TGA), the change in
sample mass is measured by a thermo-balance as a
function of temperature or time. In a related
method, differential thermal analysis (DTA), the
temperature difference between a sample and a
reference material is measured.8, 9
Furthermore the
composition of polymer materials can be
determined by measuring their infrared spectra
using a Fourier transform infrared (FT-IR)
spectrometer and then comparing the results with a
commercially available or specifically prepared
spectral data base.10, 11
As coumarins have chemical,
biologics and physicochemical advantages, they
result attractive to be incorporated into a polymeric
chain. Taking in account our previous work 12
where semi-telechelic polymers with a functional
group 4-hydroxycoumarin were prepared, we try to
elucidate the mechanism of synthesis involucrate
and some physicochemical properties of these
compounds. Herein, we describe the polymers
preparation using different synthetic pathways and
the employment of thermo-gravimetric and
spectroscopies analyses.
II. EXPERIMENTAL
Samples
All identified polymers were made in a
single reaction in a 125 ml round-bottom flask
RESEARCH ARTICLE OPEN ACCESS
2. Hugo A. Garro.et. al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 6, Issue 3, (Part - 4) March 2016, pp.84-89
www.ijera.com 85|P a g e
equipped with a stir bar. 4-hidroxicoumarin and the
other coumarins employed in each reaction (200
mg, 1.2 mmol) were added to 20 ml of acetone, or
butanone, or cyclehexanone (3.6 mol). Then,
increased concentrations of sulfuric acid: 0.5%,
1%, 2%, 3%, 5%, 10%, 20% and 30% v/v, were
added successively under argon atmosphere and air
atmosphere. This yellow solution was stirred at 80°
C for 12 h (when we used toluene as co-solvent,
temperature reaches 105 °C and in p-xilene co-
solvent 138 °C). After cooled to room temperature,
sodium carbonate 10% v/v solution was added, and
the mixture was stirred for 20 min whit ethylic
ether. Organic layer was then separated and wash
tree times with distillated water. After dried with
anhydrous sodium sulfate, the solution was
concentrated giving yellow-orange oil which was
chromatographed on silica gel (1:9 ethyl acetate /
hexane) to afford products as intense orange
viscous oil.
MALDI-Tof/Tof MS and LDI-Tof/Tof MS
Analysis
See reference 12
for details.
Diffraction X-Ray
The initial structural identification and
characterization of the sample was carried out by
laboratory XRPD (CuK, : 1.5418 Å). XRPD
diagrams were collected in a Rigaku D-Max-IIIC
diffractometer with Bragg-Brentano geometry by
using monochromatic CuK radiation (Ni filter) in
a continuous mode from angular range 2° < 2 θ<
40°. In order to allow the ordering of the
hydrocarbonates chains, the sample was put in a
holder and kept horizontal for 24 hours.
Thermal Analysis
Thermogravimetric (TGA) and differential
thermal analysis (DTA) curves were obtained with
a Shimadzu TGA-51 Thermal Analyzer and DTA-
50 Thermal Analyzer, using platinum pans, flowing
air at 50 ml/min and a heating rate of 10 °C/min
from room temperature to 900 °C.
Uv-Vis Analysis
UV-Visible diffuse reflectance spectra of
the collected material were recorded on a Cary
Varian 5E spectrophotometer equipped with a
PTFE-coated integration sphere. The optical
absorption spectra were measured in a transmission
mode on the same spectrophotometer using a
quartz tube.
Energy Minimization Simulation
The Gabedit software package 13
was used
to draw the polymeric molecule. The geometry was
initially optimized using the classic quasi-Newton
method, followed by semi-empirical optimization
using the software MOPAC 2009,14, 15
as
implemented in Gabedit. This conformation was
used to obtain the parameters and topology files for
the GROMACS software package.16, 17
It is afford a
graphic interphase for computational chemistry
packages. We used the following parameters:
Minimum RMS gradient: 0.10000
Step interval: 2.00000
Frame interval: 10
Terminate steps: 10000
Heating rate: 0
Target temperature: 300° K
Properties: π-bond orders and steric energy
summary
III. RESULTS AND DISCUSSION
Synthesis and Structural Elucidation
Coumarins with different chemical groups
and pattern of substitution and several
concentration of sulfuric acid were usedin order to
obtain polymers. The reaction products were
characterized by MALDI-MS and LDI-MS (i.e.,
without needing the presence of a secondary
molecule as photo-sensitizer or matrix in the
sample). Using 4-hydroxycoumarin (which shows
keto-enol behavior) as starting material the
expected polymers were obtained (Fig. 1).
Fig.1.Keto-enolic equilibrium of 4-
hydroxycoumarin showing the most negative
carbon at C-3.
We also envisaged the synthesis of several
polymers with higher building block weight using
different ketones, like butanone, but none
polymerization was observed by LDI-MS analysis
of the reaction mixture. The reaction of 4-
hydroxycoumarin in acetone with H2SO4 produce
polymers with difference of 40 Da and the higher
molecular weight detected was 562.6 Da.12
Using
other solvents with substantial higher boiling point
like toluene and p-xylene, in the presence of
acetone, it was observed the same pattern of 40
mass units repetitions of the main chain and new
compounds with higher molecular weight (Fig. 2).
3. Hugo A. Garro.et. al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 6, Issue 3, (Part - 4) March 2016, pp.84-89
www.ijera.com 86|P a g e
Fig. 2. Positive ion MALDI mass spectrum of
reaction product of 4-hydroxycoumarin with H2SO4
5% in acetone and p-xilene; matrix employed:
pirene.
For example, signal at m/z 764.8 can be
assigned to a polymer with the following structure
(with fifteen units of propene building block):
These results clearly indicate that an
increasein the reaction temperature produce chain
elongation with higher molecular weight polymers.
Other coumarins were used in acidic acetone. The
positive ion LDI mass spectrum of 6-
hydroxycoumarin before the reaction is shown in
Fig. 3a. Some intense signals are detected [M + H]+
at m/z 163.13, [M + Na]+
at m/z 185.17, [M + K]+
at
m/z 201.17, [2M + Na]+
at m/z 347.32 and [2M +
K]+
at m/z 363.22). After the reaction (Fig. 3b.) no
polymerization products were detected, but the
reactant is no longer observed indicating that some
reaction is taking place.
Fig. 3. Positive ion LDI mass spectra of 6-
hydroxycoumarin with H2SO4 5% in acetone a)
before the reaction b) reaction product.
A similar behavior was observed when 4-
hydroxy-3-nitrocoumarin was studied. In this case
the signals detected for the reactants were [M + H]+
at m/z 208.25, [M + Na]+
at m/z 230.25, [M + K]+
at
m/z 246.27, [2M + Na]+
at m/z 437.32, [2M + K]+
at
m/z 453.34 and [3M + K]+
at m/z 660.27 (Fig. 4a.).
After the reaction takes place, when these
compounds were used, those signals were not
longer observed, however not evidence of
polymerization was detected either (Fig. 4b.). This
evidence suggests that phenol-coumarins that
cannot form enolates like 6-hydroxicoumarin or
when position three is occupied like 4-hydroxy-3-
nitrocoumarin, were not able to form these
materials, denoting the main role of keto-enol
equilibrium presents in 4-hydroxycoumarin.
Fig. 4.Positive ion LDI mass spectra of 4-hydroxy-
3-nitrocoumarin with H2SO4 5% in acetone a)
before the reaction b) reaction product.
Proposed Mechanism for the Poly-Condensation
Event
Respect to the origin of the fragments
of 40 mass units and oligomeric chain, the
followingbehavior is proposed (Fig. 5). In first
time, we suggest the enolization of the solvent
propanone with the consequent polarization of
the oxygen atom. This phenomenon would occur
spontaneously thanks to the acidity provided by the
surrounding medium (H2SO4 5% has given the best
yields), that generate a positive charge in the
oxygen atom. An event like this would cause an
environment devoid of electrons over the carbon
adjacent, generating a potential electrophile, which
would be able to suffer a nucleophilic attack.
As we know, the aromatic compound 4-
hydroxycoumarin is capable to submit forms keto-
enolic, being located at position three of
this core themost negative electron
density. Therefore, this α-carbon adjacent to a
carbonyl group could react
with a polarized acetone molecule and
condensewith different monomers of solvent. This
reactionwould be able to extend the length of the
strings by a cationic type polymerization. Finally,
by loss of multiples water molecules, these chains
become on polymers formed by repetitive units of
propene. Furthermore, the new extended system
might be the driving force for this dehydration.
4. Hugo A. Garro.et. al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 6, Issue 3, (Part - 4) March 2016, pp.84-89
www.ijera.com 87|P a g e
Fig. 5. Proposed mechanism for the poly-condensation event.
X Ray Diffraction Studies
To achieve an approximation of the
macromolecular structure of these products an X-
ray diffraction study was realized. Fig. 6 shows the
patterns of the glass sample holder (black) and this
new material (red). Here, we can see the presence
of two broad peaks centered in values of interplanar
distances 5.4 Å and 7.4 Å,
with a considerable intensity respect to the glass
sample holder. The appearance of these
peaks indicates the existence of one phase
with some degree of order in the planes, which
could be related to partial ordering of the
hydrocarbon chains (combs of 40 mass units).
The peak width at half height, which reaches
approximately 6 Å, suggests thatthis arrangement is
not complete, but occurs partially in the
different zones within the semi-hard material.
7 1 4
3 0 0
6 0 0
9 0 0
d 2 = 7 .4 A
d 1 = 5 .4 A
Intensity(a.u.)
In te rp la n a r s p a c in g (A )
Fig. 6. X-ray diffraction pattern of collected
material, employing length wave of = 1.5418 Å,
CuKat room temperature.
Thermo-Gravimetric Analysis (TGA and DTA)
Fig. 7 describes the thermal behavior of the
polymers obtained by calcination of the sample at
900 °C. Black line shows the TGA curve,
two main mass losses can be observed. The first of
these is between 60 °C and 400 °C, which
corresponds to 86.3% of the total mass sample,
followed by a second event that occurs
between 400 °C and 600 °C, associated with a
12.6% loss of mass.This second event shows
two exothermic peaks centeredat 467 °C and
568 °C in DTAcurves (red line), typicallyobserved
in decomposition processes. Apparently,
the TGA analysis shows that this material breaks
down fast.
The differential analysis show that the first
process occurs with a downward peak (300 °C)
corresponding to an endothermic event, which is
typical when aromatic compounds are presents
(such as coumarin), because their start taking
heat to break the aromatic system.
Regarding the thermal nature of the DTA peaks
associatedwith the first decomposition, they
present a complex pattern, which shows the
existence of two exothermic peaks (339 °C and
393 ºC).
5. Hugo A. Garro.et. al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 6, Issue 3, (Part - 4) March 2016, pp.84-89
www.ijera.com 88|P a g e
Fig. 7. Thermogram of the obtained material at the
range of room temperature to 900 °C. In black:
curve of TGA analysis. Red: DTA analysis.
UV-Vis Study
Coumarins show strong absorption in the UV-Vis
region, nearly at 355 nm. The UV spectrum shows
two considerable peaks at 230 and 266 nm with an
excellent molar extinction coefficient of 1 x 105
for
230 nm(Fig. 8). This value gives potential
applications as organic nonlinear optical material to
these products.18
Figure 8. UV-Vis spectrum of collected material
with 10-3
mM concentration and= 1 x 105
for 230
nm.
Energy Minimization Simulation Study
Observing the UV-Visible spectrum (Fig.
8)which showed absorption at 266 nm as a larger
wavelength value, it is appears anomalous
considering the number of conjugated double bonds
presents. This phenomenon can be rationalized
considering a possible steric inhibition of resonance
due to the distance of separationfor the methyl
groups in the side chain, which generates some
steric hindrance. Using computer calculation was
possible demonstrate that it is not possible to
achieve a perfect coplanarity of all double bonds
presents in the polyene chain (Fig. 9); as a matter
of fact, some angle values were different to the
180° for trans-configurations and for those 120°
expected in optimal sp2
hybridizations (this could be
the reason for the hypsochromic shift observed).
Figure 9. a) Tridimensional conformation of complete polymer obtained showing the lack of planarity. b) Zoom
in showing anomalous values of dihedral angles.
0 1 0 0 2 0 0 3 0 0 4 0 0 5 0 0 6 0 0 7 0 0 8 0 0 9 0 0
0
2
4
6
8
1 0
1 2
DTAsignal(V)
m
0
= 0 .1 2 m g
m
1
= 1 .5 2 m g
m
0
= 1 1 .1 m g
Mass(mg)
T (ºC )
-1 0
0
1 0
2 0
3 0
4 0
6. Hugo A. Garro.et. al. Int. Journal of Engineering Research and Applications www.ijera.com
ISSN: 2248-9622, Vol. 6, Issue 3, (Part - 4) March 2016, pp.84-89
www.ijera.com 89|P a g e
Materials Solubility
During the process of synthesis there was
not formed precipitate. After isolation and
identification, the solubility of the material in the
most common organic solvents was tested.These
polymers are soluble in hexane, cyclohexane,
DMF, diethyl ether, petroleum ether, carbon
tetrachloride, chloroform, dichloromethane, ethyl
acetate and methanol at room temperature, and
logically in acetone. On the other hand, these
samples are not soluble in water both at room
temperature and boiling water. Finally, the sample
was subjected to carbonization by incineration, and
the resulting residue could not be dissolved in any
of the previously mentioned solvents, including
boiling water.
IV. CONCLUSIONS
MALDI-Tof spectra show that the main
repeating unit in the obtained compound is a
propene group which derives from dehydration of
propanone solvent under H2SO4 acidic condition,
but when other ketones are used no products were
obtained. In the same way, coumarins that cannot
form enolates or when position three is occupied
were incapable to form these polymers. Moreover,
this new material proved to have some degree
of macromolecular order and elastic behavior, with
potential applications on the field of nonlinear
optics due to its extended conjugated system and its
considerable molar extinction coefficient.
V. FUNDING
Financial supports from CONICET (PIP
00360), UNSL (PROICO 2/1214), ANPCyT
(PICT-2011-1416) are gratefully acknowledged.
G.P., C.R.P., C.E.T. and R.E.B are in CONICET
researchers staff. We also wish to thank to Drs. S.
Larregola, E. Brusau and M. Funes for they helpful
advices and support for X-ray studies, thermal
behavior, FT-IR and UV-Vis analysis, respectively.
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