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  • About
  • The Global ETD Search service is a free service for researchers to find electronic theses and dissertations. This service is provided by the Networked Digital Library of Theses and Dissertations.
    Our metadata is collected from universities around the world. If you manage a university/consortium/country archive and want to be added, details can be found on the NDLTD website.
101

Analysis of amino acids in food samples by high performance liquid chromatography using conductometric detection.

January 1999 (has links)
Poon Wai Mei Emily. / Thesis (M.Phil.)--Chinese University of Hong Kong, 1999. / Includes bibliographical references (leaves 74-81). / Abstracts in English and Chinese. / Chapter Chapter 1: --- Introduction --- p.1 / Chapter 1.1. --- Importance of amino acids --- p.1 / Chapter 1.1.1. --- Clinical samples --- p.1 / Chapter 1.1.2. --- Food samples --- p.2 / Chapter 1.2. --- Reviews of amino acid analysis --- p.6 / Chapter 1.2.1. --- Ion-exchange chromatography --- p.6 / Chapter 1.2.2. --- Gas chromatography --- p.6 / Chapter 1.2.3. --- Thin layer chromatography --- p.8 / Chapter 1.2.4. --- Flow injection analysis --- p.8 / Chapter 1.2.5. --- Liquid chromatography --- p.9 / Chapter 1.2.6. --- Capillary electrophoresis --- p.10 / Chapter 1.2.7. --- Methods of detecting amino acid without derivatization --- p.11 / Chapter 1.3. --- Determination of amino acids by reversed-phase ion-pair chromatography --- p.12 / Chapter 1.4. --- The objectives of the study --- p.15 / Chapter Chapter 2: --- Experimental --- p.16 / Chapter 2.1. --- Materials --- p.16 / Chapter 2.2. --- Apparatus --- p.16 / Chapter 2.3. --- Samples --- p.16 / Chapter 2.4. --- Procedures --- p.17 / Chapter 2.4.1. --- Preparation of amino acid standard solution (stock solutions) --- p.17 / Chapter 2.4.2. --- Method development --- p.17 / Chapter 2.4.3. --- Samples preparation --- p.18 / Chapter 2.4.4. --- Preparation of Dowex column --- p.18 / Chapter 2.4.5. --- Extraction of amino acids from samples --- p.19 / Chapter 2.4.6. --- Recovery test --- p.20 / Chapter Chapter 3: --- Results and Discussions --- p.21 / Chapter 3.1. --- Optimization --- p.21 / Chapter 3.1.1. --- pH --- p.21 / Chapter 3.1.2. --- Ion-interacting reagent --- p.22 / Chapter 3.1.3. --- Organic solvent --- p.29 / Chapter 3.1.4. --- Temperature --- p.34 / Chapter 3.1.5. --- Chromatographic conditions --- p.36 / Chapter 3.2. --- Application --- p.45 / Chapter 3.2.1. --- Precision of injection --- p.45 / Chapter 3.2.2. --- Accuracy of the method --- p.46 / Chapter 3.2.3. --- The concentration of amino acids in food samples --- p.50 / Chapter 3.2.3.1. --- Citrus fruits --- p.50 / Chapter 3.2.3.2. --- Orange juice drinks --- p.60 / Chapter 3.2.3.3. --- Chinese honey --- p.65 / Chapter 3.2.3.4. --- New Zealand honey --- p.67 / Chapter 3.2.3.5. --- Energy drinks --- p.70 / Chapter Chapter 4 : --- Conclusion --- p.72 / Chapter Chapter 5 : --- Bibliographies --- p.74 / Chapter 6. --- Appendices --- p.82 / Chapter 6.1. --- Table 1 : Ingredients of orange juice drinks --- p.82 / Chapter 6.2. --- Table 2 : Honey samples --- p.83 / Chapter 6.3. --- Table 3 : Ingredients of energy drinks --- p.83
102

An investigation into turbine blade tip leakage flows at high speeds

Saleh, Zainab Jabbar January 2015 (has links)
This investigation studies the leakage flows over the high pressure turbine blade tip at high speed flow conditions. There is an unavoidable gap between the un-shrouded blade tip and the engine casing in a turbine stage, where the pressure difference between the pressure and the suction surfaces of the blade gives rise to the development of leakage flows through this gap. These flows contribute to about one third of the aerodynamic losses in a turbine stage. In addition they expose the blade tip to a very high temperature and result in thermal damages which reduce the blade‟s operational life. Therefore any improvement on the tip design to reduce these flows has a significant impact on the engine‟s efficiency and turbine blade‟s operational life. At the engine operational condition, the leakage flows over the high pressure turbine blade tip are mostly transonic. On the other hand literature survey has shown that most of the studies on the tip leakage flows have been performed at low speed conditions and there are only a few experimental works on the transonic tip flows. This project aims to explore the tip leakage flows at high speed condition which is the real engine condition, both experimentally and computationally and establish a comprehensive understanding of these flows on different tip geometries. The effect of tip geometry was studied using the flat tip and the cavity tip models and the effect of in-service burnout on these two tip models was established using the radius-edge flat tip and the radius-edge cavity tip models. The experimental work was carried out in the transonic wind tunnel of Queen Mary University of London and the computational simulations were performed using RANS and URANS. As the flow approached each tip model it turned and accelerated around its leading edge in the same way as the flow turns around the leading edge of an aerofoil. In the case of the tip models with sharp edges the tip flow separated at the inlet to the tip gap. For the flat tip model the flow reattachment occurred further downstream whereas in the case of the cavity tip model the length of the pressure side rim was not sufficient for the reattachment to occur and the separated flow left the rim as a free shear layer. The cavity tip model was found to have a smaller effective tip gap and hence smaller discharge coefficient in comparison to the flat tip model. For the radius-edge tip models, no separation occurred at the inlet to the tip gap and the effective tip gap was found to be the same as the geometrical tip gap. Therefore it was concluded that the tip model with radius-edges had a larger effective tip gap and hence a greater discharge coefficient than the tip geometry with sharp edges. It was observed that in the case of the supersonic tip leakage flows, decreasing the pressure ratio PR (i.e. the ratio of the static pressure at the tip gap exit to the stagnation pressure at the inlet to the tip gap) increased the discharge coefficient Cd for the tip models with sharp edges but it decreased the Cd value in the case of the tip models with radius edges. The cavity tip model with sharp edges was found to have the smallest discharge coefficient and thus the best performance in reducing the tip leakage flows as compared to all the other tip models studied in this investigation.
103

Qualitative and quantitative analysis of aconitine alkaloids in Chinese medicinal materials by high performance liquid chromatography and atmospheric pressure ionization mass spectrometry.

January 1998 (has links)
by Kwok Chiu Nga. / Thesis (M.Phil.)--Chinese University of Hong Kong, 1998. / Includes bibliographical references (leaves 1-3 (4th gp.)). / Abstract also in Chinese. / TABLE OF CONTENTS --- p.i / ABSTRACT --- p.iv / 摘要 --- p.vi / LIST OF FIGURES --- p.vii / LIST OF TABLES --- p.x / ABBREVIATION --- p.xi / Chapter CHAPTER ONE --- RESEARCH BACKGROUND / Chapter 1.1 --- Introduction --- p.1 / Chapter 1.1.1 --- Alkaloids --- p.1 / Chapter 1.1.2 --- Diterpenoid alkaloids --- p.2 / Chapter 1.1.3 --- Aconitine-type alkaloids --- p.2 / Chapter 1.1.4 --- Toxicity --- p.4 / Chapter 1.1.5 --- Safety concerns --- p.4 / Chapter 1.2 --- Summary of the Previous Work --- p.8 / Chapter 1.3 --- Objectives and Outline of the Present Work --- p.13 / Chapter CHAPTER TWO --- INSTRUMENTATION AND EXPERIMENTAL / Chapter 2.1 --- Instrumentation --- p.15 / Chapter 2.1.1 --- High performance liquid chromatography (HPLC) --- p.15 / Chapter 2.1.2 --- Triple-stage quadrupole (TSQ) mass spectrometer --- p.17 / Chapter 2.1.2.1 --- Atmospheric pressure chemical ionization (APCI) --- p.17 / Chapter 2.1.2.2 --- Electrospray ionization (ESI) --- p.20 / Chapter 2.1.2.3 --- Quadrupole system --- p.20 / Chapter 2.1.2.4 --- Ion detection system --- p.22 / Chapter 2.1.2.5 --- Data system --- p.22 / Chapter 2.2 --- Experimental --- p.22 / Chapter 2.2.1 --- Sample and reagents --- p.22 / Chapter 2.2.2 --- Sample preparation --- p.23 / Chapter 2.2.3 --- High performance liquid chromatography conditions --- p.23 / Chapter 2.2.4 --- Mass spectrometry conditions --- p.25 / Chapter 2.2.4.1 --- Atmospheric pressure chemical ionization conditions --- p.25 / Chapter 2.2.4.2 --- Electrospray ionization conditions --- p.25 / Chapter CHAPTER THREE --- SELECTION AND OPTIMIZATION OF HPLC/MS METHOD / Chapter 3.1 --- Introduction --- p.26 / Chapter 3.2 --- Experimental --- p.29 / Chapter 3.3 --- Results and Discussion --- p.29 / Chapter 3.3.1 --- Triethylamine concentration --- p.31 / Chapter 3.3.2 --- Ammonium acetate concentration --- p.34 / Chapter 3.3.3 --- Acetic acid concentration --- p.37 / Chapter 3.3.4 --- HPLC/MS interface --- p.40 / Chapter 3.3.5 --- MS/MS conditions --- p.40 / Chapter 3.4 --- Conclusions --- p.43 / Chapter CHAPTER FOUR --- DETERMINATION OF ACONITINE-TYPE ALKALOIDS IN ACONITE ROOTS / Chapter 4.1 --- Introduction --- p.48 / Chapter 4.2 --- Experimental --- p.48 / Chapter 4.3 --- Results and Discussion --- p.50 / Chapter 4.3.1 --- Selection of internal standard --- p.50 / Chapter 4.3.2 --- Method validation --- p.50 / Chapter 4.3.2.1 --- Precision of measurement --- p.50 / Chapter 4.3.2.2 --- Accuracy of measurement --- p.50 / Chapter 4.3.2.3 --- Limits of detection and quantitation --- p.58 / Chapter 4.3.3 --- Determination of aconitine-type alkaloids in aconite roots --- p.58 / Chapter 4.4 --- Conclusions --- p.60 / Chapter CHAPTER FIVE --- CONCLUSIONS AND FUTURE WORK / Chapter 5.1 --- Conclusions --- p.67 / Chapter 5.2 --- Future Work --- p.68 / ACKNOWLEDGMENT --- p.A1 / APPENDIX --- p.A2 / REFERENCES --- p.R1
104

Crystal structure prediction at high pressures : stability, superconductivity and superionicity

Nelson, Joseph Richard January 2017 (has links)
The physical and chemical properties of materials are intimately related to their underlying crystal structure: the detailed arrangement of atoms and chemical bonds within. This thesis uses computational methods to predict crystal structure, with a particular focus on structures and stable phases that emerge at high pressure. We explore three distinct systems. We first apply the ab initio random structure searching (AIRSS) technique and density functional theory (DFT) calculations to investigate the high-pressure behaviour of beryllium, magnesium and calcium difluorides. We find that beryllium fluoride is extensively polymorphic at low pressures, and predict two new phases for this compound - the silica moganite and CaCl$_2$ structures - to be stable over the wide pressure range 12-57 GPa. For magnesium fluoride, our results show that the orthorhombic `O-I' TiO$_2$ structure ($Pbca$, $Z=8$) is stable for this compound between 40 and 44 GPa. Our searches find no new phases at the static-lattice level for calcium difluoride between 0 and 70 GPa; however, a phase with $P\overline{6}2m$ symmetry is energetically close to stability over this pressure range, and our calculations predict that this phase is stabilised at high temperature. The $P\overline{6}2m$ structure exhibits an unstable phonon mode at large volumes which may signal a transition to a superionic state at high temperatures. The Group-II difluorides are isoelectronic to a number of other AB$_2$-type compounds such as SiO$_2$ and TiO$_2$, and we discuss our results in light of these similarities. Compressed hydrogen sulfide (H$_2$S) has recently attracted experimental and theoretical interest due to the observation of high-temperature superconductivity in this compound ($T_c$ = 203 K) at high pressure (155 GPa). We use the AIRSS technique and DFT calculations to determine the stable phases and chemical stoichiometries formed in the hydrogen-sulfur system as a function of pressure. We find that this system supports numerous stable compounds: H$_3$S, H$_7$S$_3$, H$_2$S, H$_3$S$_2$, H$_4$S$_3$, H$_2$S$_3$ and HS$_2$, at various pressures. Working as part of a collaboration, our predicted H$_3$S and H$_4$S$_3$ structures are shown to be consistent with XRD data for this system, with H$_4$S$_3$ identified as a major decomposition product of H$_2$S in the lead-up to the superconducting state. Calcium and oxygen are two elements of generally high terrestrial and cosmic abundance, and we explore structures of calcium peroxide (CaO$_2$) in the pressure range 0-200 GPa. Stable structures for CaO$_2$ with $C2/c$, $I4/mcm$ and $P2_1/c$ symmetries emerge at pressures below 40 GPa, which we find are thermodynamically stable against decomposition into CaO and O$_2$. The stability of CaO$_2$ with respect to decomposition increases with pressure, with peak stability occurring at the CaO B1-B2 phase transition at 65 GPa. Phonon calculations using the quasiharmonic approximation show that CaO$_2$ is a stable oxide of calcium at mantle temperatures and pressures, highlighting a possible role for CaO$_2$ in planetary geochemistry, as a mineral redox buffer. We sketch the phase diagram for CaO$_2$, and find at least five new stable phases in the pressure/temperature ranges 0 $\leq P\leq$ 60 GPa, 0 $\leq T\leq$ 600 K, including two new candidates for the zero-pressure ground state structure.
105

First-principles studies of gas hydrates and clathrates under pressure

Teeratchanan, Pattanasak January 2018 (has links)
Gas hydrates are molecular host-guest mixtures where guest gas species are encapsulated in host water networks. They play an important role in gas storage in aqueous environments at relatively low pressures, and their stabilities are determined by weak interactions of the guest species with their respective host water frameworks. Thus, the size and the amount of the guest species vary, depending on the size of the empty space provided by the host water structures. The systems studied here are noble gas (He, Ne, Ar) and diatomic (H2) hydrates. Because of the similarity of the guests' sizes between the noble gases and the di-atomic gases, the noble gas hydrates act as simple models for the di-atomic gas hydrates. For example, He, Ne and H2 have approximately the same size. Density functional theory calculations are used to obtain the ground state formation enthalpies of each gas hydrate, as a function of host network, guest stoichiometry, and pressure. Dispersion effects are investigated by comparing various dispersion corrections in the exchange-correlation functionals (semi-local PBE, semi-empirical D2 pair correction, and non-local density functionals i.e. vdW-DF family). Results show that the predicted stability ranges of various phases agree qualitatively, although having quantitative difference, irrespective of the methods of the dispersion corrections in the exchange-correlation functionals. Additionally, it is shown in gas-water dimer interaction calculations that all DFT dispersion-corrected functionals overbind significantly than the interaction acquired by the coupled-cluster calculations, at the CCSD(T) level, which is commonly accepted to provide the most accurate estimation of the actual interaction energy. This could lead to an overestimation of the stability of the hydrate mixtures. Further study in the gas-water cluster indicates that less overbinding effect is found in the cluster than in the dimer. This implies that the overbinding energy caused by DFT might become less pronounce in the solid phase. Graph invariant topology and a program based on a graph theory are used to assign protons based on the 'ice rule' to fulfill the incomplete experimental structural data such as unknown/unclear positions of protons in the host water lattices. These methods help constructing host water networks for computational calculations. Several configurations of the host water structures are tested. Those configurations having lowest enthalpies are used as the host water networks in this research. Furthermore, the enthalpic spread between the configurations having the highest and the lowest enthalpy in the pure water ice network is very small (about 10 meV per water molecule). Nevertheless, it is still unclear to conclude that this protonic effect is also trivial in the gas-water compound. Therefore, this study also calculates the enthalpies of the gas-water mixtures having various proton configurations in the host water networks. Results indicate that very small enthalpic distributions among the proton configurations are found in the compounds as well. Furthermore, the enthalpic spread is almost constant as pressure increases. This suggests there is no pressure effect in the enthalpy gap amoung the proton distributions in both pure water ice and the gas-water compounds. Predicted stable phases for the noble gas compound systems are based on four host water networks, namely, ice Ih, II and Ic, and the novel host water network S!. The He-water system adopts ice Ih, II and Ic network upon increasing pressure. In the Ne-water system, a phase sequence of Sx/ice-Ih, II and Ic with a competitive hydrate phase in the S! host network at very low pressure is found. This is similar to the phase evolution of the H2-water system. For the Ar-water mixture, only a partially occupied hydrate in the Sx host network is found stable. This Sx phase becomes metastable if taking the traditional clathrates (sI and sII) into account. This result agrees very well with the experiment suggesting only two-third filling is found the large guest gases i.e. CO2. For the diatomic guest gas compound systems, the traditional clathrate structure (sII) that found to be existed experimentally in the H2-H2O system is also included in this study together with those four host water networks. Predicted phase stability sequence as elevated pressure is as follows: Sx, ice-Ih, II and Ic. This computationally prediction agrees very well with experiment. Results in this work suggest that the compound based on the traditional clathrate structure II (sII) host water framework is found to be metastable with respect to the decomposition constituents - in this case, they are pure water ice and the S!. The metastability of the hydrogen hydrates based on the sII structure might due to zero-point motions or other dynamic/entropic mechanisms uncovered in this research. Dynamic studies concerning the transition states of the hydrogen guest molecules in three competitive phases at very low pressure (less than 10 kbar), based on Sx, ice-Ih, and ice-II host water network, are considered. The energy barriers required by the hydrogen guest molecules in those three host frameworks are calculated by using Nudged Elastic Band (NEB) method. Results suggest that the hydrogen molecules are more mobile in the Sx than the other two host structures significantly. In the S! host water network, the energy barrier is about 25 meV/hydrogen molecule. This energy is about the room temperature suggesting that the hydrogen guest molecules are easily mobile in the Sx host water network if there is an empty site adjacent to them.
106

Effect of pressure on porous materials

McMonagle, Charles James January 2018 (has links)
Research to design and synthesise new porous materials is a rapidly growing field with thousands of new systems proposed every year due to their potential use in a multitude of application in a wide range of fields. Pressure is a powerful tool for the characterisation of structure-property relationships in these materials, the understanding of which is key to unlocking their full potential. In this thesis we investigate a range of porous materials at a range of pressures. Over time the chemical architecture and complexity of porous materials has increased. Although some systems display remarkable stability to high-pressures, which we generally think of as being above 1 GPa (10,000 bar), in general, the compressibility of porous materials have increased substantially over the last 10 years, rendering most unstable at GPa pressures. Here we present new methods for investigating porous materials at much more moderate pressures (100's of bar), alongside more traditional high-pressure methods (diamond anvil cell techniques), finishing with gas sorption studies in a molecular based porous material. Here, the design and development of a new moderate pressure sapphire capillary cell for the small molecule beamline I19 at the Diamond Light Source is described. This cell allowed access to pressures of more than 1000 bar regularly with a maximum operating pressure of 1500 bar with very precise pressure control (< 10 bar) on both increasing and decreasing pressure. This cell closes the gap between ambient pressure and the lowest pressures attainable using a diamond anvil cell (DAC), which is generally above 0.2 GPa (2000 bar). Along with the development of the sapphire capillary pressure cell, the compression to 1000 bar of the small organic sample molecule Hexamethylenetetramine (hexamine, C6H12N4) and its deuterated form (C6D12N4) was determined, demonstrating the precision possible using this cell. Solvent uptake into porous materials can induce large structural changes at 100's of bar. In the case of the Sc-based Metal-organic framework (MOF), Sc2BDC3 (BDC = 1,4-benzenedicarboxylate), we used the sapphire capillary pressure cell to study changes in the framework structure on the uptake of n-pentane and isopentane. This work shows how the shape and smaller size of n-pentane facilitated the swelling of the framework that could be used to explain the increase in stability of the MOF to applied pressure. The effect of pressure on the previously unreported Cu-framework bis[1-(4- pyridyl)butane-1,3-dione]copper(II) (CuPyr-I) was investigated using high-pressure single-crystal diffraction techniques (DAC). CuPyr-I was found to exhibit high-pressure and low-temperature phase transitions, a pressure induced Jahn- Teller switch (which was hydrostatic medium dependent), piezochromism, and negative linear compressibility. Although each of these phenomena has been reported numerous times in a range of materials, this is to the best of our knowledge the first example to have been observed within the same material. The final two chapters investigate the exceptional thermal, chemical, and mechanical stability of a porous molecular crystal system (PMC) prepared by the co-crystallisation of a cobalt phthalocyanine derivative and a fullerene (C 60 or C70). The stabilising fullerene is captured in the cavity between two phthalocyanines in a ball and socket arrangement. These PMCs retain their porous structure: on the evacuation of solvent of crystalisation; on heating to over 500 K; on prolonged immersion in boiling aqueous acid, base, and water; and at extreme pressures of up to 5.85 GPa, the first reported high-pressure study of a PMC. the reactive cobalt cation is accessible via the massive interconnected voids, (8 nm3), as demonstrated by the adsorption and binding of CO and O2 to the empty metal site using in situ crystallographic methods available at beamline I19, Diamond Light Source.
107

High-pressure studies on molecular systems at ambient and low temperatures

Cameron, Christopher Alistair January 2015 (has links)
Pressure and temperature are two environmental variables that are increasingly being exploited by solid-state researchers probing structure-property relationships in the crystalline state. Modern high-pressure apparatus is capable of generating many billions of Pascals in the laboratory, and therefore can produce significantly greater alterations to crystalline materials than changes in temperature, which can typically be varied by only a few thousand Kelvin. Many systems such as single-molecule magnets exhibit interesting properties under low-temperature regimes that can be substantially altered with pressure. The desire by investigators to perform analogous single-crystal X-ray diffraction studies has driven the development of new high-pressure apparatus and techniques designed to accommodate low-temperature environments. [Ni(en)3][NO3]2 undergoes a displacive phase transition from P6322 at ambient pressure to a lower symmetry P6122/P6522 structure between 0.82 and 0.87 GPa, which is characterized by a tripling of the unit cell c axis and the number of molecules per unit cell. The same transition has been previously observed at 108 K. The application of pressure leads to a general shortening of O···H hydrogen bonding interactions in the structure, with the greatest contraction (24%) occurring diagonally between stacks of Ni cation moieties and nitrate anions. A novel Turnbuckle Diamond Anvil Cell designed for high-pressure low-temperature single-crystal X-ray experiments on an open-flow cryostat has been calibrated using the previously reported phase transitions of five compounds: NH4H2PO4 (148 K), ferrocene (164 K), barbituric acid dihydrate (216 K), ammonium bromide (235 K), and potassium nitrite (264 K). From the observed thermal differentials between the reported and observed transition temperatures a linear calibration curve has been constructed that is applicable between ambient-temperature and 148 K. Low-temperature measurements using a thermocouple have been shown to vary significantly depending on the experimental setup for the insertion wire, whilst also adding undesirable thermal energy into the sample chamber which was largely independent of attachment configuration. High-pressure low-temperature single-crystal X-ray diffraction data of [Mn12O12(O2CMe)16(H2O)4] (known as Mn12OAc) reveals a pressure-induced expulsion of the crystallized acetic acid from the crystal structure and resolution of the Jahn-Teller axes disorder between ambient pressure and 0.87 GPa. These structural changes have been correlated with high-pressure magnetic data indicating the elimination of a slow-relaxing isomer over this pressure range. Further application of pressure to 2.02 GPa leads to the expansion of these Jahn-Teller axes, resulting in an enhancement of the slow-relaxing magnetic anisotropy as observed in the literature. Relaxation of pressure leads to a resolvation of the crystal structure and re-disordering of the Jahn-Teller axes, demonstrating that this structural-magnetic phenomenon is fully reversible with respect to pressure. The space group of the Prussian blue analogue Mn3[Cr(CN)6].15H2O has been re-evaluated as R-3m between ambient pressure and 2.07 GPa using high-pressure single-crystal X-ray and high-pressure neutron powder data. Reductions in metal-metal distances and gradual distortions of the Mn octahedral geometry have been correlated with previously reported increases in Tc and declines in ferrimagnetic moment in the same pressure range. Increasing the applied pressure to 2.97 GPa leads to partial amorphization and results in a loss of long-range magnetic order as shown by the literature. The application of pressure (1.8 GPa) to the structure of K2[Pt(CN)4]Br0.24.3.24H2O (KCP(Br)) causes a reduction in the Pt intra-chain and inter-chain distances, and results in an enhancement of the overall conductivity under these conditions as demonstrated in the literature. Almost no changes occur to the high-pressure crystal structure upon cooling to 4 K, except in the Pt-Pt intra-chain distances which converge and suppress the Peierls distortion known to occur at 4 K, resulting in a comparatively greater electrical conductivity under these conditions.
108

Application of high-pressure homogenization for the proximate analysis of meat and meat products by Fourier transform infrared (FTIR) spectroscopy

Dion, Bruno J. January 2000 (has links)
No description available.
109

Experimental investigation of molecular solids and vanadium at high pressure and temperature

Jenei, Zsolt January 2009 (has links)
Understanding high pressure effects on simple molecular system is of great interest for condensed matter science and geophysics. Accessing the static pressure and temperature regions found in planetary interiors is made possible by the development of the Diamond Anvil Cell technique. We developed a double sided resistive heating method for the membrane DAC operating in low pressure (&lt;0.5 mTorr) pressure environment requiring only 175 W input power to reach sample temperatures up to 1300 K. We applied this technique successfully to study molecular solids at high temperatures, such as H2, N2 and CO2. We made an attempt to determine the melting line of hydrogen and present data up to 26 GPa in agreement with literature. Raman spectroscopy of Nitrogen indicates a high stability of the ε molecular phase, while θ phase is only accessible via certain P, T paths. Studies of solid CO2 at high pressure and temperature lead to the discovery of a six-fold coordinated stishovite-like phase VI, obtained by isothermal compression of associated CO2-II above 50 GPa at 530-650 K, or by isobaric heating of CO2-III above 55 GPa. From our X-ray diffraction experiment on isothermally compressed H2O we report a coexistence of ice VII and symmetric ice X from the start of the transition pressure 40GPa to just below 100 GPa and a volume change of 4% across the transition. Vanadium, a transition metal undergoes a phase transition upon compression unlike other elements (Nb, Ta) from its group. We confirm the bcc phase transition to rhombohedral structure at 62 GPa under quasi hydrostatic compression in Ne pressure medium. Compression without pressure medium results in a much lower 30 GPa transition pressure at room temperature and 37 GPa at 425 K, pointing to a positive phase line between the bcc and rhombohedral crystalline phases.
110

Soot Measurements in High-pressure Diffusion Flames of Gaseous and Liquid Fuels

Intasopa, Gorngrit 30 May 2011 (has links)
Methane-air, ethane-air, and n-heptane-air over-ventilated co-flow laminar diffusion flames were studied up to pressures of 2.03, 1.52, and 0.51 MPa, respectively, to determine the effect of pressure on flame shape, soot concentration, and temperature. A spectral soot emission optical diagnostic method was used to obtain the spatially resolved soot formation and temperature data. In all cases, soot formation was enhanced by pressure, but the pressure sensitivity decreased as pressure was increased. The maximum fuel carbon conversion to soot, ηmax, was approximated by a power law dependence with the pressure exponent of 0.92 between 0.51 and 1.01 MPa, and 0.68 between 1.01 and 2.03 MPa with ηmax=9.5% at 2.03 MPa for methane-air flames. For ethane-air flames, the pressure exponent was 1.57 between 0.20 and 0.51 MPa, 1.08 between 0.51 and 1.01 MPa, and 0.58 between 1.01 and 1.52 MPa where ηmax=23% at 1.52 MPa. For nitrogen-diluted n-heptane-air flames, ηmax=6.5% at 0.51 MPa.

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