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Determination Of Morphine And Total Phenolic Content In Poppy Seed Of Turkish OriginGevenkiris, Ali 01 November 2011 (has links) (PDF)
Turkey is important major licid opium poppy (Papaver Somniferum) producer for medicinal and scientific purposes in the world and one of the two traditional producer country. The poppy seeds which are unique part of the opium poppy are used for food purpose. About 25.000 ton/year poppy seeds
were produced for food purpose. Recent years morphine content of commercially available poppy seeds were speculated. Some studies have been reported that poppy seeds from different origins contain a wide variation
of morphine (2 &ndash / 294) &mu / g/g content. They have been used also different sample preparation method (extraction and derivatization) and different instruments (GC-MS) during analyses. In this study morphine content was determined in Turkish origin which were white, yellow and blue poppy seeds
colors by using high pressure liquid chromatography (HPLC). Different sample preparation method (without derivatization) was used. Morphine was eluted from poppy seeds by acidic water through stationary phase activated aluminum oxide. Poppy seed samples were collected from 13 provinces and
35 different sowing fields of Turkey. The determined morphine contents in poppy seeds were ranged between (9.73 to 37.46) &mu / g/g. Any study was not found in the literatures on determination of total phenolic in poppy seed. In this study, the optimum condition for extraction of polyphenols in poppy
seeds was determined and then, total phenolic values were obtained in three different colours seeds by spectrophotometric method. At the end of experiments the total phenolic contents in white, yellow and blue colours
poppy seed were found to be 4.44, 3.05 and 3.67 mg/g respectively.
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Limestone Decay In Historic Monuments And Consolidation With Nanodispersive Calcium Hydroxide SolutionsCaner, Evin 01 March 2011 (has links) (PDF)
Exposure to atmospheric conditions results of deterioration in historic monuments. and their stones. Limestone conservation presents many problems that have to be investigated in detail. In this study, limestone deterioration and development of its conservation treatments were investigated through examination of the statues carved from karstic limestones in Nemrut Dag Monument. The decay mechanisms that had major roles in their deterioration during two thousand years of exposure to atmospheric conditions and the development of their conservation treatments involved several types of analyses that were carried out in the field and in the laboratory. Exposed surfaces of limestones having karstic veins, interior crack surfaces were examined and compared with relatively undeteriorated interior parts. Similar limestones from the geological formations nearby were artificially deteriorated by salt crystallization and were also examined for comparison. Standard physical and physicomechanical tests, petrographical analysis, XRD, SEM-EDX and FTIR were used during those examinations. Swelling nature of clays in limestones and their control were quantified by CEC measurements.
The micro structure of limestone was observed to be composed of micritic calcite with karstic veins of sparitic calcite crystals. Some karstic zones were found to be preferred sites of dissolution and precipitation of calcium carbonate where swelling action of clays and widening of cracks occurred. Iron oxides that moved through those zones, as well as biological activity were also found to contribute to those phenomena. Preparation of high concentrations of nanodispersive calcium hydroxide solutions was achieved for the conservation treatments of the deteriorated limestone. Success of treatments with nanodispersive Ca(OH)2 solutions targeted to the decay zones were discussed in terms of their ability to control the swelling action of clays, carbonation of nanodispersive solution, and improvement in the physicomechanical properties of treated limestone.
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Performance Analysis Of Drilling Fluid Liquid LubricantsSonmez, Ahmet 01 September 2011 (has links) (PDF)
Excessive torque is one of the most important problems in oil/gas drilling industry. Friction between wellbore/casing and drill string causes excessive torque. This study discusses performance analysis of drilling fluid lubricants, which are used as friction reducers in well-bore. Three different types of commercial chemical lubricants, which are fatty acid and glycerid based, triglycerid and vegetable oil based and polypropylene glycol based, diesel oil, and crude oil, which consists of different API gravity, paraffin and asphaltene value samples, were selected for the analysis.
In the analysis, different lubricant compositions with the mixture of commercial chemical lubricants, crude oil and diesel oil, which were added to water based lignosulfonate mud, are tested on metal-metal contact surface by Ofite Lubricity Tester to determine the best lubricity/cost ratio of lubricant compositions.
Moreover, effects of the lubricants on mud rheology and API fluid loss of mud, foam forming potential and cheesing/greasing of the lubricants and the influence of mud properties on lubricants (calcium, salt, pH and mud density) are examined.
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Epoxidation Reactions Of Small Alkenes On Catalytic SurfacesKurnaz, Emine 01 November 2011 (has links) (PDF)
Propylene epoxidation reaction was investigated on catalytic surfaces of chlorinated
copper(I) oxide and ruthenium(IV) oxide using periodic density functional theory
(DFT). Cu2O(001) and (110) surface of RuO2 was selected to generate chlorinated
surfaces to be used in the study. Besides epoxidation, other reactions that compete
with epoxidation were also studied such as formations of allyl-radical, acrolein,
acetone on chlorinated Cu2O(001) and formations of propionaldehyde, allyl-radical
and acetone on chlorinated RuO2(110) surface. Path of each reaction was
determined by CI-NEB method and transition state analyses. Generally accepted
stable surface intermediate mechanism was utilized in reactions to final products.
The surface intermediate favorable on the surfaces in this study was determined to
be the intermediate that is not preferable on metallic surfaces under low oxygen.
On chlorinated Cu2O(001) surface, formation of propylene oxide, acetone and
acrolein have higher probability than gas phase allyl-radical since the desorption
energy of allyl-radical was calculated to be 70kcal/mol which is a relatively high
value. In fact it is desirable since gas phase allyl-radical is known to be the
precursor of combustion products. On chlorinated RuO2(110) surface, desorption Propylene epoxidation reaction was investigated on catalytic surfaces of chlorinated
copper(I) oxide and ruthenium(IV) oxide using periodic density functional theory
(DFT). Cu2O(001) and (110) surface of RuO2 was selected to generate chlorinated
surfaces to be used in the study. Besides epoxidation, other reactions that compete
with epoxidation were also studied such as formations of allyl-radical, acrolein,
acetone on chlorinated Cu2O(001) and formations of propionaldehyde, allyl-radical
and acetone on chlorinated RuO2(110) surface. Path of each reaction was
determined by CI-NEB method and transition state analyses. Generally accepted
stable surface intermediate mechanism was utilized in reactions to final products.
The surface intermediate favorable on the surfaces in this study was determined to
be the intermediate that is not preferable on metallic surfaces under low oxygen.
On chlorinated Cu2O(001) surface, formation of propylene oxide, acetone and
acrolein have higher probability than gas phase allyl-radical since the desorption
energy of allyl-radical was calculated to be 70kcal/mol which is a relatively high
value. In fact it is desirable since gas phase allyl-radical is known to be the
precursor of combustion products. On chlorinated RuO2(110) surface, desorption
observed to be possible on chlorinated RuO2(110) surface but not possible on
chlorinated Cu2O(001). When activation barriers and desorption energies of all
possible reactions are compared on chlorinated RuO2(110) surface / gas phase
propylene oxide generated directly seems as the preferable product with allylradical
although it was computed to have high desorption energy.
Comparison of activation barriers obtained in this study on chlorinated Cu2O(001)
with the barriers of nonchlorinated surface revealed chlorine slightly increases the
activation barrier of unwanted allylic hydrogen stripping and hence slightly
decreases the probability of occurance. When chlorine is placed closer to reaction
site, activation barrier of allylic hydrogen stripping reaction increases further. The
effect of chlorine might be electronic since the charge of oxygen at reaction site
slightly becomes less negative when the place of chlorine gets closer to the reaction
site on the surface. Similar comparison between chlorinated and nonchlorinated
RuO2(110) surfaces revealed that chlorine addition does not improve the surface
toward propylene oxide formation, rather it is detrimental as chlorine addition
caused a decrease in unwanted allylic hydrogen stripping reaction.
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Preparation Of Silica Coated Cobalt Ferrite Magnetic Nanoparticles For The Purification Of Histidine-tagged ProteinsAygar, Gulfem 01 October 2011 (has links) (PDF)
The magnetic separation approach has several advantages compared with conventional separation methods / it can be performed directly in crude samples containing suspended solid materials without pretreatment, and can easily isolate some biomolecules from aqueous systems in the presence of magnetic gradient fields. This thesis focused on the development of new class of magnetic separation material particularly useful for the separation of histidine-tagged proteins from the complex matrixes through the use of imidazole side chains of histidine molecules. For that reason surface modified cobalt ferrite nanoparticles which contain Ni-NTA affinity group were synthesized. Firstly, cobalt ferrite nanoparticles with a narrow size distribution were prepared in aqueous solution using the controlled coprecipitation method. In order to obtain small size of agglomerates two different dispersants, oleic acid and sodium chloride, were tried. After obtaining the best dispersant and optimum experimental conditions, ultrasonic bath was used in order to decrease the size of agglomerates. Then, they were coated with silica and this was followed by surface modification of these nanoparticles by amine in order to add functional groups on silica shell. Next, &ndash / COOH functional groups were added to silica coated cobalt ferrite magnetic nanoparticles through the NH2 groups. After that N&alpha / ,N&alpha / -Bis(carboxymethyl)-L-lysine hydrate, NTA, was attached to carboxyl side of the structure. Finally, nanoparticles were labeled with Ni (II) ions. The size of the magnetic nanoparticles and their agglomerates were determined by FE-SEM images, particle size analyzer, and zeta potential analyzer (zeta-sizer). Vibrational sample magnetometer (VSM) was used to measure the magnetic behavior of cobalt ferrite and silica coated cobalt ferrite magnetic nanoparticles. Surface modifications of magnetic nanoparticles were followed by FT-IR measurements. ICP-OES was used to find the amount of Ni (II) ion concentration that was attached to the magnetic nanoparticle.
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Carbon Nanotube ProductionHocaoglu, Caner 01 November 2011 (has links) (PDF)
Carbon nanotubes (CNTs), allotropes of carbon with a cylindrical nanostructure, are one of the most attractive research subjects for scientists and industry because of their extraordinary chemical, electrical, optical, mechanical and thermal properties, and their wide range of potential application areas. Mainly, there are two types of carbon nanotubes: single-walled carbon nanotubes (SWNTs) and multi-walled carbon nanotubes (MWNTs).
The most commonly used methods for carbon nanotube production are arc discharge, laser ablation, and chemical vapor deposition (CVD). In the CVD method, CNTs are produced from thermal decomposition of the carbon-containing molecules on a suitable transition metal catalyst. CVD method enables large scale production of high-quality CNTs with low cost compared to other methods. The growth and morphology of CNTs can be controlled by adjusting the reaction parameters.
In this study, Co and Mo impregnated CaCO3 catalysts were synthesized at different Co:Mo weight ratios and calcined at different temperatures. XRD results showed that there was mainly CaCO3 compound in the catalysts calcined at 500º / C whereas the catalysts calcined at 700 and 750 º / C were mainly composed of CaO and Ca(OH)2 compounds. In addition to these, CaMoO4, CoO, CoMoO4 and Mo2C were the other solid phases mainly observed in all catalysts.
The production of CNTs was performed by chemical vapor deposition of acetylene at a temperature range of 500-700
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Silica Coating Of Monodisperse Hydrophobic Magnetite Nanoparticles Through Reverse Microemulsion TechniquesErgul, Zeynep 01 January 2012 (has links) (PDF)
Magnetic nanoparticles find broad applications in biomedical field such as drug delivery, hyperthermia and magnetic resonance imaging (MRI). For these applications magnetic nanoparticles need to be coated with suitable materials which are soluble, biocompatible and nontoxic. Among these materials, silica is
the most often used coating material. This thesis is focused on preparation of silica coated iron oxide magnetic nanoparticles. Magnetic iron oxide nanoparticles are synthesized by thermal decomposition method. In the presence of iron acetylacetonate Fe(acac)3, a high boiling point organic solvent and a reducing
agent, particle sizes ranging from about 5 nm to 7 nm were obtained. Nanoparticles were characterized by transmission electron microscopy (TEM). The obtained nanoparticles were coated with ultra thin silica shell via reverse microemulsion method. The influence of the amount of Igepal CO-520, NH4OH
and TEOS was studied systematically and their amounts were optimized to yield monodisperse and well defined particles. The size of the silica coated magnetic nanoparticles and their agglomerates were determined by TEM images and particle size analyzer (zeta sizer). X-Ray photoelectron spectroscopy (XPS) was used to confirm the presence of silica whenever the coating could not be seen by TEM measurements. Magnetic nanoparticles having 4-6 nm thickness of silica shell were obtained. The results showed that the amount of surfactant Igepal CO-520 played an important role in the reaction system.
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Separation Of Arsenite And Arsenate Species From Water By Charged Ultrafiltration MembranesAysegul, Sezdi 01 June 2012 (has links) (PDF)
Arsenic is found in drinking waters in many countries and since maximum allowable concentration is as low as 10 µ / g/L, there are many research efforts to separate it from water. Membrane methods are used more and more widely in separation operations in recent years.
Arsenic is mainly present in water as arsenite [As(III)] and arsenate [As(V)]. As pH of water changes, molecular formulas of As(III) and As(V) change. In this study, the performance of different ultrafiltration membranes for arsenic removal from water was investigated at different pH values, different feed concentrations and presence of other anions (SO42-, HPO42-, NO3-, Cl-). Donnan exclusion effect on separation was discussed since distribution of arsenite and arsenate anions change in water due to change in pH of the solution.
Experiments were conducted via batch and continuous modes. For continuous ultrafiltration experiments, 30 kDa of polysulfone and 20 kDa of polyether sulfone membranes were used. Batch ultrafiltration experiments were performed with the usage of 3 kDa of regenerated cellulose membrane.
Higher retention values for As(V) were obtained compared to retention values of As(III). When membranes&rsquo / performances were investigated, it was seen that highest As(V) removal was observed with the usage of polysulfone membrane. Increase in feed concentration and presence of other anions caused decrement in separation.
Hydride Generation Atomic Absorption Spectrometry was used to perform analyses. Hydride generator part was designed, constructed and optimized to obtain reliable and accurate absorbance values.
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Preparation Of Functional Surfaces Using Zeolite Nanocrystals For Biosensor And Biomedical ApplicationsKirdeciler, Salih Kaan 01 July 2012 (has links) (PDF)
Zeolites are crystalline aluminosilicates which have highly ordered pore structures and high surface area. Also the tailorable surface properties, high ion-exchange capability, high chemical, thermal, and mechanical strength make these particles an important candidate for various application such as sensors, catalysis, dielectric materials, separation, and membrane technologies. Although zeolites have these unique properties, applications where zeolites are integrated into devices according to their application areas, are limited due to the powder form of the material.
The purpose of the current study was to investigate the effect of zeolite nanoparticles on conductometric biosensor performance and cell viability measurements. Firstly, zeolite attachment on silicon surfaces was investigated by attaching silicalite and zeolite A nanoparticles onto the silicon substrates by direct attachment methodology in a closely packed monolayer form with perfect orientation and full coverage without using any chemical linker. Furthermore, the ability to pattern these zeolite crystals on silicon substrates with electron beam lithography and photolithography techniques was investigated. With the combination of electron beam lithography and direct attachment methodology, zeolite patterns were produced with feature sizes as small as a single silicalite nanoparticle thick line, that is approximately 500 nm. This approach has the ability of patterning very small features on silicon substrate, but the drawback is the long patterning time and lack of electron beam stability during long pattern formation process. Accordingly, it is almost impossible to form large patterns with electron beam lithography systems.
Afterwards, to have full control on surfaces with differentiated areas on solid substrates, patterns of one type of zeolite crystals was formed on the monolayer of another type of zeolite layer with electron beam lithography for the first time. The same closed packed and highly oriented silicalite patterns were successfully formed on zeolite A monolayers and vice versa.
Then photolithography technique was combined with direct attachment methodology to overcome the problem of the lack of total patterned area. With this technique, it was possible to pattern the whole silicon wafer in a couple of seconds, however the feature size of the zeolite patterns was limited with the infrastructures of the mask fabricated for photolithography studies. In this particular study, zeolite lines patterns with a minimum of 5 µ / m thickness were prepared and the total patterned area was kept constant at 1 cm2. Similar to what was obtained by electron beam lithography study, zeolite A patterns were formed on silicalite monolayers with the minimum feature size of 5 µ / m and vice versa.
In the second part of the study, zeolite films were prepared on the transducers of conductometric biosensors using dip coating technique and named as Zeolite Coated Transducers (ZCT). Electrodes prepared using a mixture of zeolite and enzyme solution and then subjected to casting using glutaraldehyde were called Zeolite Membrane Transducers (ZMT). The operational and storage stabilities were determined to be in an acceptable range using ZCTs for conductometric urea biosensors. It was observed that using electrodes fabricated by the ZCT technique enhanced the biosensor signals up to two times and showed a rapid response after the addition of urea to the medium when it was compared with Standard Membrane Transducers (SMT). This enhancement can be explained by the lack of GA layer on top of the film, which acts as a diffusion barrier and inhibits the activity of the enzyme. On the second part of this conductometric biosensor study, effect of zeolite modification with methyl viologen (MV) and silver nanoparticles (Ag+ and Ag0), as well as the effect of changing Si/Al ratio was investigated with three different zeolite Beta particles which have Si/Al ratios of 40, 50, and 60. There were no significant effect of MV modification on ZMTs and there was no response observed with Ag+ and Ag0 modified zeolites. However, it was observed that conductometric responses increased with increasing Si/Al ratio for ZMTs. This behavior can be due to an increased hydrophobicity and/or the increasing acidic strength with the increasing Si/Al ratio within the zeolite crystals. Also ZCTs showed higher responses with respect to both SMTs and ZMTs. When compared with SMTs and ZMTs, ZCTs had higher reproducibility due to the controlled thickness of zeolite thin film by dip coating, and the controlled amount of enzyme adsorbed on this film.
In the third part of the study, effect of zeolites on cell proliferation with MG63 osteoblast cells and NIH3T3 fibroblast cells were investigated. For that purpose, zeolite A, silicalite, and calcined forms of these zeolites were patterned with photolithography technique onto silicon wafers. Three different patterns prepared for this particular study, which has 0.125cm2, 0.08825cm2, and 0.04167cm2 zeolite patterned areas on 1 cm2 samples. In that way, not only the zeolite type and effect of calcination of zeolites, but also the effect of zeolite amount on MG63 osteoblast cells and NIH3T3 fibroblast cells were investigated.
Silicalite coated samples were observed to have higher amount of cells than zeolite A coated samples after 24, 48, and 72 hours of incubation. This may be referred to the hydrophilic/hydrophobic properties, surface charge, and/or particle size of zeolites. Also it is observed that higher zeolite amount on samples resulted in an increase in the number of cells attached to the samples.
There was also a significant increase in the number of cells upon using calcined silicalite samples. Accordingly, it can be hypothesized that zeolite pores result in an enhancement of protein adsorption and proliferation, even if this only occurs at the pore openings. On the other hand, there was no positive effect of calcining zeolite A. This result was expected since there is no structure directing agent used in synthesis procedure of zeolite A, which again supports the fact that pores might have some role in cell attachment.
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Hydrogen Generation From Conventional Fuels Over Mesoporous Mixed Oxide Catalysts Under Time Interrupted Reaction ConditionsCan, Mukaddes 01 April 2011 (has links) (PDF)
In this study, catalytic activity of the Co and/or Pb-SBA-15 mesoporous catalysts in methane partial oxidation reaction was investigated. By using sol-gel, incipient wetness impregnation and post grafting method, SBA-15 samples are incorporated with Co and/or Pb at different weight loadings to provide a controlled geometry in nanometer scale. The characterization of the synthesized samples was done by XRD, N2 adsorption isotherms, FTIR, TEM images, Raman and XPS analysis. In the present study also, gas phase methane partial oxidation modeling and the synthesizing of mesoporous SBA-15 silica with different pore sizes were investigated.
For the samples prepared by sol-gel method, XRD analysis showedthat cobalt exists in the form of Co3O4and Pb exist in the form of PbO. BET surface areas of the Co loaded catalysts are in the range of 479.5-640.1 m2/g. However, in Pb loaded samples, higher metal loading decrease the surface area up to 4.63 m2/g. Considering the both Co and Pb containing bi-metallic samples, TEM and BET results revealed that the ordered hexagonal mesostructure was fully destroyed.
The samples prepared by incipient wetness impregnation and post grafting method characterized by using BET, TEM, Raman and XPS analysis. According to the BET results all the samples show ordered mesostructure in agreement with TEM results for all Co and/or SBA-15 mesoporous samples. TEM results also revealed that, the Co(5%) Pb(5%)-SBA-15 catalyst prepared by incipient wetness impregnation method possess big cobalt and lead oxide crystallines on the mesoporous structure. Raman analysis results indicated that cobalt exist in Co3O4 form. According to XPS results all samples containing cobalt include Co3O4.
The partial oxidation of methane was carried out in a fixed bed flow-type reactor in a temperature range of 50&ndash / 850° / C under atmospheric pressure.According to the reaction test results, the 0.5%Rh-Co-SBA15 catalyst shows the highest methane conversion (82%) and H2 selectivity. The non-precious metal show lower reactivities, addition of Pb to the Co-SBA-15 catalyst increases the catalytic activity and decrease the H2 production temperature.
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