Chemistry Commons^™

Isolation Of Curcumin From Tumeric, Ram Mohan, Andrew Anderson, Matthew Mitchell

Scholarship

No abstract provided.

The Discovery-Oriented Approach To Organic Chemistry. 3. Boron-Trifluoride Catalyzed Rearrangement Of Cis- And Trans-Stilbene Oxides. An Exercise In 1H Nmr Spectroscopy For Sophomore Organic Laboratories, Ram Mohan, Erik Sgariglia, Regina Schopp, Kostas Gavardinas

Scholarship

Epoxides, or oxiranes, are among the most versatile intermediates in organic synthesis. Yet very few examples of laboratory experiments involving reactions of epoxides are to be found in lab texts. We have developed a discovery-oriented laboratory experiment that involves the rearrangement of both cis- and trans-stilbene oxides with boron trifluoride etherate. The identity of the product can be easily determined by ¹H NMR spectroscopy and, in case of the trans isomer, by preparation of the semicarbazone derivative as well. In spite of the simplicity of the experiment, the element of discovery ensures that student interest and enthusiasm are retained.

Octafluoro-Meso Tetraarylporphyrins And Methods For Making These Compounds, Stephen G. Dimagno

Department of Chemistry: Faculty Publications

The novel compounds of the present invention are f-octafluoro-meso-tetraarylporphyrins of formula (I) and their metallic complexes of formula (II):

B-octafluoro-meso-tetraaryl porphyrins are Synthesized by reacting 3,4-difluoropyrrole with an aromatic aldehyde in the presence of boron trifluoride etherate, followed by oxidation. The difluoropyrrole used in this reaction is pro duced by reacting 3,3,4,4-tetrafluoropyrroline or its corre sponding Salt, 3,3,4,4-tetrafluoropyrrolidinium Salt, with a base Such as potassium tert-butoxide. The metalloporphyrins of the present invention are Synthesized by deprontonating B-octafluoro-meso-tetraarylporphyrin ligands and treating Said ligands with metal ions.

Surface Composition Of MnXCo1-XO Solid Solutions By X-Ray Photoelectron And Auger Spectroscopies, Marjorie Langell, F. Gevrey, M. W. Nydegger

Marjorie A. Langell Publications

Auger and X-ray photoelectron spectroscopies have been used to study the surface composition of Mn_xCo_1-xO (0 ≤ x ≤ 1) solid solutions. The polycrystalline materials, which are bulk homogeneous, present clear signs of deviation in surface composition at x_bulk ≈ 0.2–0.4 to become surface-enriched in manganese at the expense of the cobalt. Whether on stoichiometric or cobalt-depleted surfaces, cobalt retains the characteristic XPS 2p satellite structure and binding energies of the rock salt monoxide (CoO or Mn_xCo_1-xO) environment. Manganese 2p XP spectra are appropriately monoxide-like for the stoichiometric surfaces …

Parameters Influencing Sediments Resuspension And The Link To Sorption Of Inorganic Compounds, Eid A. Alkhatib, Keith Castor

Chemistry & Physics Faculty Publications

In the aquatic environment, the accumulation of chemicalcontaminants by sediments poses a potential threat to endemiclife forms and drinking water resources. Trace metals such asCd, Cu, Cr, Ni, Pb, and toxic organic compounds, are among awide variety of contaminants having an affinity for sediments.In this study, experiments were performed simulating sedimentresuspension in the lower Housatonic River, Connecticut, using aParticle Entrainment Simulator. Analyses of grain sizedistributions, porosities and total organic contents of thesediments suggested that these parameters influence theredistribution and entrainment of settleable solids in the watercolumn. These findings were established by evaluating the impactof one parameter on sediment resuspension as …

Pyrolysis-Mass Spectrometry For Rapid Classification Of Oysters According To Rearing Area, J. Krupcík, P. Oswald, I. Spánik, P. Májek, M. Bajdichová, P. Sandra, Daniel W. Armstrong

Chemistry Faculty Research & Creative Works

Current concern for the safety and traceability of food, as well as the desire of oyster farmers, for marketing reason, to emphasize the geographical origin of their production, requires new methods to make possible a real product identification. In this study, 181 oyster samples were analyzed to determine their origin area. These samples were collected in nine French rearing areas at four different times of the year (spring, summer, and the beginning and end of autumn) and from four to eight sites in each area to provide a variability parameter. Analysis of fingerprints after Curie point pyrolysis-mass spectrometry, by an …

Enantiomeric High-Performance Liquid Chromatographic Separation Of Β- Substituted Tryptophan Analogues, G. Török, A. Péter, E. Vékes, J. Sápi, M. Laronze, J. Y. Laronze, Daniel W. Armstrong

Chemistry Faculty Research & Creative Works

The high-performance liquid chromatographic enantioresolution of β- substituted tryptophan analogues by direct and indirect methods is reported. The direct separation was carried out on chiral crown ether-bonded, on the macrocyclic antibiotic teicoplanin-bonded or on different derivatized β- cyclodextrin-bonded phases. The indirect resolution was achieved by applying pre-column derivatization with the chiral reagents 1-fluoro-2,4- dinitrophenyl-5-L-alanine amide (FDAA) and 2,3,4,6-tetra-O-acetyl-β-D- glucopyranosyl isothiocyanate (GITC). In the separation of all four isomers of the analytes, the indirect methods seemed to be more efficient than the direct methods. In most cases, the FDAA derivatives of the stereoisomers could be separated with better selectivity in methanol-containing …

The Effects Of Argon Dilution On Hydrogenated Amorphous Silicon Prepared By D.C. Plasma Glow Discharge : Optical And Infrared Spectroscopic Studies, Aniszawati Azis

Student Works (2000-2009)

Hydrogenated amorphous silicon (a-Si :H) films were prepared from the discharge of pure silane and silane diluted in argon using a home-built hori zontal direct current(d.c.) plasma glow discharge system. The effects of argon dilution of silane on the optical properties, chemical bonding properties, hydrogen content and microstructure parameter of the films produced were studied and analyzed. Film thickness, refractive index, optical energy gap and the Urbach tail bandwidth were obtained from the optical transmission spectra of the films while the H content and the microstructure parameter were derived from the Fourier Transform infra-red(FTIR) spectra of the films. The FTIR …

Reaction Of Alpine-Borane With Aldehydes: Reactivity Rate Assessment By Observation Of The Disappearance Of The Carbonyl N - Pi* Peak By Uv-Visible Spectroscopy, Layla Bland, Michael J. Panigot

Journal of the Arkansas Academy of Science

Due to an unexpectedly difficult reduction of indole-3-carbaldehyde and of isobutyraldehyde using the chiral reducing agent Alpine-Borane, the reactivity of several aliphatic, aromatic, and unsaturated aldehydes was investigated. This was done in order to determine whether there was a relationship between aldehyde structure and reduction rate. It was found that aliphatic aldehydes and aromatic aldehydes with no strongly electron-donating groups on the arene ring reduced faster than unsaturated aldehydes.

Study Of The Amplitude Of Pressure And Thrust Oscillations In A Lab-Scale Hybrid Rocket, Ann Wright, Lawrence Dunn, Brian Alford, Justin Patton, M. Keith Hudson

Journal of the Arkansas Academy of Science

Hybrid rockets are being studied as a potential replacement for the solid rocket boosters on the NASA space shuttle. One physical characteristic of hybrid rockets that must be understood and overcome is potentially severe pressure oscillations during combustion. Pressure oscillations inside the rocket combustion chamber lead to oscillations in the thrust of the rocket. These oscillations are damaging to potential human passengers and cargo and must be minimized. Current theories surmise that the oscillations are caused by combustion chamber geometry, oxygen feed line parameters, and/or fuel combustion characteristics. This study focuses on the role of the fuel characteristics in pressure …

3-Hydroxykynurenine And 3-Hydroxyanthranilic Acid Generate Hydrogen Peroxide And Promote Α-Crystallin Cross Linking By Metal Ion Reduction, Lee E. Goldstein, Michael C. Leopold, Xudong Huang, Craig S. Atwood, Aleister J. Saunders, Mariana Hartshorn, James T. Lim, Et Al.

Chemistry Faculty Publications

The kynurenine pathway catabolite 3-hydroxykynurenine (3HK) and redox-active metals such as copper and iron are implicated in cataractogenesis. Here we investigate the reaction of kynurenine pathway catabolites with copper and iron, as well as interactions with the major lenticular structural proteins, the R-crystallins. The o-aminophenol kynurenine catabolites 3HK and 3-hydroxyanthranilic acid (3HAA) reduced Cu(II)>Fe(III) to Cu(I) and Fe(II), respectively, whereas quinolinic acid and the nonphenolic kynurenine catabolites kynurenine and anthranilic acid did not reduce either metal. Both 3HK and 3HAA generated superoxide and hydrogen peroxide in a copper-dependent manner. In addition, 3HK and 3HAA fostered copper-dependent R-crystallin cross-linking. 3HK- …

The Measurement Of Surface Areas Of Some Silicates By Solution Adsorption, Oğuz İnel, Fatma Tümsek

Turkish Journal of Chemistry

In this study, the adsorption from solution technique was used for the determination of surface areas of some silicate samples (bentonite, sepiolite, zeolitic tuff and kaolin). Methylene blue (MB), orthophenanthroline (OP) and p-nitrophenol (PNP) were selected as solutes. The adsorption data was found to conform with the Langmuir equation within the concentration range studied, and Langmuir constants were determined for each of the samples. The surface area values obtained were compared with those determined by nitrogen adsorption. Also the results were discussed with respect to the cation exchange capacities of the samples. The specific surface area values of the samples …

Synthesis Of 4-Benzyl-1-Piperazineglyoxime And Its Use In The Spectrophotometric Determination Of Nickel, Mustafa Maci̇t, Hümeyra Bati, Beki̇r Bati

Turkish Journal of Chemistry

A new reagent, 4-benzyl-1-piperazineglyoxime(BPGH_2), was synthesized and used for developing a simple and rapid extractive method for the spectrophotometric determination of nickel. This method is based on the selective extraction of nickel complex from aqueous solution into carbontetrachloride and the measurement of the absorption at 267 nm. The method was applied to the determination of nickel ion in some standard and practical samples.

Flavonol Glycosides From Consolida Armeniaca, Mustafa Küçüki̇slamoğlu, Nuretti̇n Yayli, Hasan Basri̇ Şentürk, Hasan Genç, Seçki̇n Özden

Turkish Journal of Chemistry

Three known flavonol glycosides, i.e., kaempferol 3,7-O-\( \alpha \)-L-dirhamnopyranoside ({\bfseries 1}), kaempferol 3-O-\( \beta \)-D-glucopyranosyl-(1\( \ra \)2)-\( \alpha$-L-rhamnopyranoside-7-O-\( \alpha \)-L-rhamnopyranoside ({\bfseries 2}) and kaempferol 3-O-\( \alpha \)-L-rhamnopyranoside-7-O-\( \beta \)-D-glucopyranosyl-(1\( \ra \)2)-\( \alpha \)-L-rhamnopyranoside ({\bfseries 3}), were isolated for the first time from the flowers of {\itshape Consolida armeniaca}, and the structures of flavonol glycosides were deduced by high field 1D and 2D NMR and FAB-MS spectroscopies. The acetyl derivatives of {\bfseries 1-3} were also prepared ({\bfseries 1a, 2a, 3a}) and identified by NMR and positive FAB mass spectra.

High Fluorescence Emissions Of Some Natural Benzofurane Derivatives Isolated From Styrax Officinalis, Siddik İçli̇, Hüseyi̇n Anil, Bi̇rcan Di̇ndar, Özgen Alankuş Çalişkan, Yurdanur Yayla, Andrey O. Doroshenko, Serap Alp

Turkish Journal of Chemistry

The fluorescent properties of several natural benzofuran derivatives, egonols, isolated from {\it Styrax officinalis}, were determined. The studied egonol derivatives were found to be effective UV organic luminophores, with quantum yields of near to unity, \( \varphi_{f} \) = 0.92. The fluorescence quenching experiments with electron donor molecules of aniline, N,N-dimethylaniline and carbazolocarbazole, presented very high efficiency of quenching at above diffusion quenching rates of 4.5$\times$10\( ^{10} \), 2.1$\times$10\( ^\times \) and 5.6$\times$10\( ^{12} \) s\( ^{-1} \)mol\( ^{-1} \), respectively. A strong electron acceptor molecule, tetranitrofluorenone, presented quenching rate of 2.6$\times$10\( ^{11} \) s\( ^{-1} \)mol\( ^{-1} \). It …

Adsorption Of Some Heavy Metal Ions From Aqueous Solution By Activated Carbon And Comparison Of Percent Adsorption Results Of Activated Carbon With Those Of Some Other Adsorbents, İlhan Uzun, Fuat Güzel

Turkish Journal of Chemistry

In this study, removal of some heavy metals ions (Mn^{2+}, Fe^{2+}, Ni^{2+} and Cu^{2+}) from aqueous solution by adsorption was investigated. For this purpose, high-grade MnSO_4.H_2O, FeSO_4.7H_2O, NiSO_4.7H_2O and CuSO_4.5H_2O were used as heavy metal samples. The commercial activated carbon (Merck 2514), chitosan and agar were used as adsorbents. The pH of each solution was not controlled. This is because the net interaction between the adsorbent and the heavy metal could be disturbed by the buffer solution. Therefore, all experiments were carried out in a pH range from 5.3 to 5.5. The equilibrium adsorption contact times were determined for M …

Investigation Of The Synthesis Of Some Dehydroalanine Derivatives, Si̇bel Süzen, John Michael Williams

Turkish Journal of Chemistry

Dehydroamino acids represent an important class of compound as they are key intermediates in unusual amino acid and in the design of peptides and are constituents of a variety of naturally occurring antibiotic and phytotoxic peptides. In view of the importance of proteins and peptides containing hydroxyamino acids and the problems associated with their synthesis and dehydration, an investigation was performed on model compounds in order to examine the difficulties of the dehydration reactions. The preparation and properties of the model dehydroalanine derivatives have been studied.

Zinc Determination In Pleural Fluid, Nazan Demi̇r, Yaşar Demi̇r, Ebubeki̇r Bakan, İrfan Küfrevi̇oğlu

Turkish Journal of Chemistry

In this study, an enzymatic zinc determination method was applied to pleural fluid, the basis of which was the regaining of the activity of apo carbonic anhydrase by the zinc present in the sample. The method was used for pleural fluid zinc determination in order to show the application to body fluids other than serum. For this purpose, pleural fluids were obtained from 20 patients and zinc concentrations were determined. Carbonic anhydrase was purified by affinity chromatography from bovine erythrocytes. The zinc present in its structure was removed by dialysis against dipicolinic acid, resulting in apoenzyme obtained at a ratio …

Kinetics Of The Photolysis Of Benzenetricarbonylchromium(0) In Chloroform, Leslianna Federici, Patrick E. Hoggard

Chemistry and Biochemistry

In contrast to the photolysis of Cr(CO)₃(C₆H₆) in nonhalogenated solvents, in which the products are CrL(CO)₂(C₆H₆) in the presence of a donor L, or Cr(CO)₆ and C₆H₆ if no donor is present, the photo-reaction in chloroform yields CrCl₃. No significant portion of the reaction occurs through absorption of 254nm light by CHCl₃• The quantum yield is 1.4, consistent with a mechanism in which several radicals are formed upon chlorination of the chromium, which then cause further decomposition of the reactant. …

A Study On N-Hydroxyamide Ethoxycarbonylhydrazones, A. Aykut İki̇zler, Ahmet Demi̇rbaş, Rza Abbasoğlu

Turkish Journal of Chemistry

The structures and electronic properties of N-hydroxyamide ethoxycarbonylhydrazones were investigated by a quantum-chemical method AMl. The total energies, heats of formation, dipol moments, ionization potentials, proton affinities and energies of frontier molecular orbitals (E_{HOMO} and E_{LUMO}) were calculated and discussed. The stabilities of the tautomeric forms and of E and Z isomers for these compounds were determined. The complex forming ability of these compounds with metal cations was also studied. The geometry and electronic properties of the complexes formed by N-hydroxyacetamide ethoxycarbonylhydrazone with Ni^{2+} and Cu^{2+} were investigated using ZINDO/1 semiempirical method. Moreover, these complexes were synthesized and identified.

Determination Of Thermodynamic Parameters Of Some Complexes Of 9-Ethyl-3-Carbazolecarboxaldehyde 4-Phenyl-3-Thiosemicarbazone (Eccapt), E. Güler Akgemci̇, Tevfi̇k Atalay

Turkish Journal of Chemistry

The complexes of Cu(II), Co(II), Zn(II), and Cd(II) with 9-ethyl-3-carbazolecarboxaldehyde 4-phenyl-3-thiosemicarbazone were synthesized and their stability constants were determined using a spectrophotometric method at different temperatures (25, 30, 35 and 40 \pm 0.1°C) and ionic strengths (0.05, 0.01 and 0.20 M KNO_3) in 50% (v/v) aqueous DMF. From these constants, the thermodynamic stability constants and thermodynamic parameters (\Delta G°, \Delta H° and \Delta S°) were calculated.

Preparation Of Optically Active Amino Acid Derivatives Of Some Methylated 5-Amino-Azaheterocycles, Mashooda Hasan, Farzana Shaheen, Uzma Yunus, Shazia Munir

Turkish Journal of Chemistry

The present paper describes the reduction of 1-methyl-5-nitro-benzimidazoles ({\bf 1A, 2A}) and 1,3-dimethyl-2H-5-nitro-benzimidazol-2-one ({\bf 3}) to 5-aminobenzimidazoles ({\bf 4A, 5A}) and 1,3-dimethyl-2H-5-amino-benzimidazol-2-one ({\bf 6}) respectively with hydrazine hydrate in absolute ethanol in the presence of graphite. Compounds {\bf 5A} and {\bf 6} were converted to 2-ethyl-5-(phthaloyl-L-phenylalanyl)amino-1-methylbenzimidazole ({\bf 7}) and 1,3-dimethyl-5-(phthaloyl-L-phenylalanyl)aminobenzimidazol-2-one ({\bf 8}). Characterization of the synthesized compounds was done with the help of mass spectrometry and ^1H NMR spectroscopic studies. Optical activity of the amino acid derivatives {\bf 7} and {\bf 8} was also recorded.

Stereoselective Synthesis Of Butenolide And Butyrolactone Derivatives, Abdulkadi̇r Sirit

Turkish Journal of Chemistry

Optically active butenolide and $\gamma$-butyrolactone derivatives were prepared by removing (R)-phenyl glycinol and (1R, 2R)-norpseudoephedrine used as chiral auxiliaries from butenolides and \gamma-butyrolactones in two steps. The structures of these products were determined using ^1H NMR, ^{13}C NMR, Mass spect., IR and microanalysis.

Spectroscopic Studies Of Charge-Transfer Complexes Of 2,3-Dichloro-5,6-Dicyano-P-Benzo-Quinone, M. S. Subhani̇, N. K. Bhatti̇, M. Mohammad, A. Y. Khan

Turkish Journal of Chemistry

Charge-transfer complexes of 2,3-dichloro-5, 6-dicyano-p-benzoquinone (DDQ) p-acetotoluidide, acetanilid, biphenyl and naphthalene were studied and their absorption spectra in solution were recorded. Absorption spectral data were obtained in CH_2Cl_2, CHCl_3, CCl_4 and mixture (CH_2Cl_2 + V) at different temperatures. Two charge-transfer bands were observed in each case. Spectral characterization of these complexes was determined and correlated with the ionization potential of the donor. Variation in thermodynamic parameters were also found to be due to change in donor and solvent.

The Effect Of Acetone On Calomel Formation On A Mercury Film Electrode Surface In Chloride Medium, F. Ni̇l Ertaş, H. İsmet Gökçel, Hüseyi̇n Tural

Turkish Journal of Chemistry

In the presence of chloride ions, calomel formation takes place on the mercury thin film electrodes under open-circuit conditions, which leads to high base currents and erratic performance in ASV meas- urements. This study describes the effect of chloride concentration on the calomel formation on the surface by following the cathodic peak on the anodic scan. The effect of acetone on the surface reaction and baseline stability was studied. Application of the method with a sea water sample is also given.

The Rate Of Grafting And Some Kinetic Parameters Of The Graft Copolymerization Of Methacrylic Acid On Poly (Ethylene Terephthalate) Fibers With Azobisisobutyronitrile, Meltem Çeli̇k, Mehmet Saçak

Turkish Journal of Chemistry

In this study the rate of grafting and some kinetic parameters of the graft copolymerization of methacrylic acid on poly(ethylene terephthalate) fibers with azobisisobutyronitrile was investigated. The rate of grafting was found to be proportional to the 0.94 and 1.22 powers of initiator and monomer concentrations, respectively. By carrying out the graft copolymerization reaction at four different temperatures ranging from 70 ^oC to 90 ^oC, the overall rate activation energy of the reaction was found to be 130.4 kJ/mol. The overall rate constants were also calculated.

Modification Of Polyester And Polyamide Fabrics By Different In Situ Plasma Polymerization Methods, T. Öktem, N. Seventeki̇n, H. Ayhan, Erhan Pi̇şki̇n

Turkish Journal of Chemistry

In order to increase the hydrophilicities, and therefore to impart soil resistance and to improve dyeability, poly(ethylene terephthalate) (PET) and polyamide (PAm) fabrics were treated in low-temperature plasmas. Five different modification types were applied. Fabrics were directly treated in acrylic acid, water, air, O_2 and argon plasma. The plasma conditions (i.e., exposure time and discharge power) were changed to control the extent of plasma surface modification. Wettability, soil resistance and dyebility of PET fabrics were significantly improved by this method. More hydrophilic surfaces were created by all the methods.

Polarographic Determination Of Fluvoxamine Maleate In Tablets, Fi̇kri̇ye Elmali, Güzi̇n Alpdoğan, Sidika Sungur, Şule Aycan

Turkish Journal of Chemistry

The differential pulse polarographic (DPP) method was developed for the determination of fluvoxamine maleate (I). At pH = 3. 7, (I) give a peak at - 0. 73 V in aqueous solution. The developed method was applied to the assay of the drug substance in commercial tablet formulations. The results were statistically compared with those obtained by reference methods (HPLC and direct current polarographic method) using t- and F- tests at 95 % confidence level.

Electroanalysis Using Differential Pulse Methods And Stripping Techniques., Enda Howard

Masters

Application of a differential pulse waveform to a microelectrode or a rotating disk electrode results in a peaked response for amperometric redox reactions. Based on these observations models were proposed and tested for these methods. Simulations of the models were carried out by inputting the relevant equations into Microsoft Excel. The microelectrode study revealed a good correlation between one model and the numerical derivative of the current following a linear sweep potential waveform. Experimentally the derivative can be obtained numerically following a linear sweep. The alternative differential pulse waveform requires more sophisticated equipment and the response can be affected by …

Enantioselective Complexation Of Amino Acids By 6a-Deoxy-6a-Hydroxyethylamino- Β -Cyclodextrin And Its Metallo-Derivatives In Aqueous Solution, Nicole Van Hoof, Noel Russell, Mary Mcnamara, Raphael Darcy

Articles

Enantioselectivity towards several amino acids by metallo-6A-deoxy-6A-hydroxyethylamino-β-cyclodextrins (metallo- β CDea’s) was investigated by potentiometric titration of the various amino acid/metallo- β CDea systems with NaOH solution. It was shown that the cyclodextrin derivative is capable of distinguishing between enantiomers of amino acid species in the presence of certain metal ions (Co, Ni, Cu and Zn). Ni- β CDea complexes show the most enantioselectivity,whereas for Cu and Co2C-_CDea complexes less selectivity is observed. As expected, Zn- β CDea complexes exhibit no enantioselectivity. Stability and selectivity, however, do not go hand in hand, since the most stable complexes are formed …