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Advanced Nmr Approaches In The Characterization Of Coal Final Technical Report September 1 1990 August 31 1993
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Book Synopsis Advanced NMR Approaches in the Characterization of Coal. Final Technical Report, September 1, 1990--August 31, 1993 by :
Download or read book Advanced NMR Approaches in the Characterization of Coal. Final Technical Report, September 1, 1990--August 31, 1993 written by and published by . This book was released on 1993 with total page 18 pages. Available in PDF, EPUB and Kindle. Book excerpt: This project addressed two main goals and one much smaller one. The main goals were (1) to improve the significance, reliability and information content in high-resolution NMR (nuclear magnetic resonance) characterization of coal samples and (2) to develop chemically informative NMR imaging techniques for coal. The minor goal was to explore advanced features of dynamic nuclear polarization (DNP) as a technique for coal characterization; this included the development of two DNP probes and the examination of DNP characteristics of various carbonaceous samples, including coals. 13C NMR advances for coal depended on large-sample MAS devices, employing either cross-polarization (CP) or direct polarization (DP) approaches. CP and DP spin dynamics and their relationships to quantitation and spin counting were elucidated. 1H NMR studies, based on CRAMPS, dipolar dephasing and saturation with perdeuteropyridine, led to a 1H NMR-based elucidation of chemical functionality in coal. 1H and 13C NMR imaging techniques, based on magic-angle spinning and rotating magnetic field gradients, were developed for introducing chemical shift information (hence, chemical detail) into the spatial imaging of coal. The TREV multiple-pulse sequence was found to be useful in the 1H CRAMPS imaging of samples like coal.
Download or read book Energy Research Abstracts written by and published by . This book was released on 1995 with total page 782 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Advanced NMR Approaches in the Characterization of Coal. [Quarterly] Report No. 12, [April--June 1993]. by :
Download or read book Advanced NMR Approaches in the Characterization of Coal. [Quarterly] Report No. 12, [April--June 1993]. written by and published by . This book was released on 1993 with total page 3 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Advanced NMR Approaches in the Characterization of Coal. [Quarterly] Report by :
Download or read book Advanced NMR Approaches in the Characterization of Coal. [Quarterly] Report written by and published by . This book was released on 1992 with total page 2 pages. Available in PDF, EPUB and Kindle. Book excerpt: The paper submitted earlier on the use of (bicyclo[3.2.1]4pyrrolidino-N-methyl-octan-8-one triflate) (13CO-123) as a 13C intensity standard was accepted for publication. Subsequently, 13CO-321 was used in this manner for quantitative 13C CP-MAS NMR analysis (including spin counting) of Argonne Premium coals. The cross-polarization time constants, T{sub CH}, and the rotating-frame proton spin-lattice relaxation times, T{sub 1p}{sup H}, were determined for each major peak of each coal via a combination of variable contact-time and variable spin-lock (T{sub 1p}{sup H}) experiments. Two or three components of rotating-frame 1H relaxation decay and two or three components of T{sub CH} behavior were observed for each major 13C peak of each coal. These data were used to determine the number of carbon atoms detected in each coal; these values are in the range between 77% and 87% of the amount of carbon known to be in each coal from elemental analysis data, except for Pocahontas No. 3, for which only 50% of the carbon was detected. In an attempt to use 1H CRAMPS to elucidate chemical functionality in coal, pyridine-saturated samples of the Argonne Premium coals were examined in detail in terms of their 1H CRAMPS NMR spectra. These spectra were deconvoluted to yield relative concentrations for individual peaks.
Book Synopsis Government Reports Annual Index by :
Download or read book Government Reports Annual Index written by and published by . This book was released on 1995 with total page 1686 pages. Available in PDF, EPUB and Kindle. Book excerpt: Sections 1-2. Keyword Index.--Section 3. Personal author index.--Section 4. Corporate author index.-- Section 5. Contract/grant number index, NTIS order/report number index 1-E.--Section 6. NTIS order/report number index F-Z.
Book Synopsis Advanced NMR Approaches in the Characterization of Coal by :
Download or read book Advanced NMR Approaches in the Characterization of Coal written by and published by . This book was released on 1992 with total page 2 pages. Available in PDF, EPUB and Kindle. Book excerpt: The paper submitted earlier on the use of (bicyclo[3.2.1]4pyrrolidino-N-methyl-octan-8-one triflate) ([sup 13]CO-123) as a [sup 13]C intensity standard was accepted for publication. Subsequently, [sup 13]CO-321 was used in this manner for quantitative [sup 13]C CP-MAS NMR analysis (including spin counting) of Argonne Premium coals. The cross-polarization time constants, T[sub CH], and the rotating-frame proton spin-lattice relaxation times, T[sub 1p][sup H], were determined for each major peak of each coal via a combination of variable contact-time and variable spin-lock (T[sub 1p][sup H]) experiments. Two or three components of rotating-frame [sup 1]H relaxation decay and two or three components of T[sub CH] behavior were observed for each major [sup 13]C peak of each coal. These data were used to determine the number of carbon atoms detected in each coal; these values are in the range between 77% and 87% of the amount of carbon known to be in each coal from elemental analysis data, except for Pocahontas No. 3, for which only 50% of the carbon was detected. In an attempt to use [sup 1]H CRAMPS to elucidate chemical functionality in coal, pyridine-saturated samples of the Argonne Premium coals were examined in detail in terms of their [sup 1]H CRAMPS NMR spectra. These spectra were deconvoluted to yield relative concentrations for individual peaks.
Book Synopsis Advanced NMR Approaches in the Characterization of Coal. [Quarterly] Report by :
Download or read book Advanced NMR Approaches in the Characterization of Coal. [Quarterly] Report written by and published by . This book was released on 1992 with total page 3 pages. Available in PDF, EPUB and Kindle. Book excerpt: A considerable effort in this project during the past few months has been focussed on the development of 1H and 13C NMR imaging techniques to yield spatially-resolved chemical shift (structure) information on coal. In order to yield the chemical shift information, a solid-state NMR imaging technique must include magic-angle spinning, so rotating gradient capabilities are indicated. A 13C MAS imaging probe and a 1H MAS imaging probe and the circuitry necessary for rotating gradients have been designed and constructed. The 1H system has already produced promising preliminary results, which are briefly described in this report.
Book Synopsis Government Reports Announcements & Index by :
Download or read book Government Reports Announcements & Index written by and published by . This book was released on 1994 with total page 876 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Download or read book Fossil Energy Update written by and published by . This book was released on 1982 with total page 952 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Analysis of Organic Sulfur and Nitrogen in Coal Via Tandem Degradation Methods. Final Technical Report, September 1, 1992--August 31, 1993 by :
Download or read book Analysis of Organic Sulfur and Nitrogen in Coal Via Tandem Degradation Methods. Final Technical Report, September 1, 1992--August 31, 1993 written by and published by . This book was released on 1993 with total page 35 pages. Available in PDF, EPUB and Kindle. Book excerpt: The principal impediment to the molecular characterization of organic sulfur and nitrogen in coal is the polymeric nature of coal's molecular structure, rendering coal insoluble and impossible to analyze by the necessary gas chromatographic (GC) methods. In this research, the authors apply chemical and thermal degradation techniques to render coal amenable to standard GC characterization. IBC101 floated coal was oxidized with sodium dichromate in five sequential steps. The SIC ratio in the residues decreases markedly with each successive step. It appears the method is effectively mobilizing the organic sulfur. The NIC ratio shows little change. In the GC/MS analysis of the dichromate oxidation products, alkylmethoxy-thiophene carboxylic acids (ATCA) were found to be major organosulfur compounds. Their relative concentrations also drop markedly with each oxidation step, while the concentration of benzene derivatives progressively increases. It is hypothesized the thiophenic moieties are located on the exterior surfaces of the coal structure, while the core is more aromatic. Using analytical micropyrolysis-gas chromatography with a sulfur-selective flame photometric detector (py-GC-FPD), it is possible to easily see a full distribution of organic sulfur forms in a one-step analysis. The predominance of alkylthiophenes in the pyrolyzates lends support to the recognition of thiophenic compounds in the dichromate oxidation products. The thiophene concentrations in pyrolyzates are directly proportional to bulk organic sulfur values. However, thiophene distributions in Illinois Basin coals are remarkably similar, regardless of organic sulfur content. It is possible to distinguish Illinois Basin coals from foreign coals on the basis of thiophene distributions. The py-GC method has an advantage over oxidative degradation techniques in that it permits direct, one-step micro-scale analysis, requiring only a minimum of sample preparation.
Book Synopsis The Use of Solid-state NMR Techniques for the Analysis of Water in Coal and the Effect of Different Coal Drying Techniques on the Structure and Reactivity of Coal. Quarterly Report, June 1--August 31, 1993 by :
Download or read book The Use of Solid-state NMR Techniques for the Analysis of Water in Coal and the Effect of Different Coal Drying Techniques on the Structure and Reactivity of Coal. Quarterly Report, June 1--August 31, 1993 written by and published by . This book was released on 1993 with total page 7 pages. Available in PDF, EPUB and Kindle. Book excerpt: One area for improvement in the economics of coal liquefaction is coal drying, particularly for the lower rank coals. However, there is considerable evidence to show that drying has a detrimental effect on the liquefaction behavior of coals. Regarding the liquefaction of coal, there does not appear to have been any systematic study of the methods of coal drying on coal structure and the role water plays in enhancing or lessening coal reactivity toward liquefaction. To conduct this study two coals, the North Dakota Beulah Zap lignite and the Utah Blind Canyon coals were chosen. These coals represent a low and high rank coal, respectively. In addition, the Beulah Zap lignite has a high moisture content whereas the Blind Canyon coal (hvA) bituminous has a very low moisture content. The overall objectives of this study are to develop a nuclear magnetic resonance (NMR) method for measuring the water in coal, to measure the changes in coal structure that occur during coal drying, to determine what effect water has on retrograde/condensation reactions, and to determine the mechanism by which water may impact coal reactivity toward liquefaction. Different methods of drying are being investigated to determine if drying can be accomplished without destroying coal reactivity toward liquefaction. The objectives for this quarterly report period were (1) to measure the volumetric swelling ratio for initial and chemically-dried coals and (2) to conduct preliminary experiments concerning the exchange of water in coal with deuterium oxide (D2O).
Book Synopsis Advanced NMR-based Techniques for Pore Structure Analysis of Coal. Quarterly Report No. 6, January 1, 1993--March 31, 1993 by :
Download or read book Advanced NMR-based Techniques for Pore Structure Analysis of Coal. Quarterly Report No. 6, January 1, 1993--March 31, 1993 written by and published by . This book was released on 1993 with total page 18 pages. Available in PDF, EPUB and Kindle. Book excerpt: One of the main problems in coal utilization is the inability to properly characterize its complex pore structure. Coals typically have micro/ultra-micro pores but they also exhibit meso and macroporosity. Conventional pore size techniques (adsorption/condensation, mercury porosimetry) are limited because of this broad pore size range, microporosity, reactive nature of coal, samples must be completely dried, and network/percolation effects. Small angle scattering is limited because it probes both open and closed pores. Although one would not expect any single technique to provide a satisfactory description of a coal's structure, it is apparent that better techniques are necessary. Small angle scattering could be improved by combining scattering and adsorption measurements. Also, the measurement of NMR parameters of various gas phase and adsorbed phase NMR active probes can provide pore structure information. We will investigate the dependence of the common NMR parameters such as chemical shifts and relaxation times of several different nuclei and compounds on the pore structure of model microporous solids, carbons, and coals. In particular, we will study the interaction between several small molecules (129Xe, 3He, 2H2, 14N2, 14NH3, 15N2, 13CH4, 13CO2) and the pore surfaces in coals.
Book Synopsis Advanced NMR-based Techniques for Pore Structure Analysis of Coal. Quarterly Report No. 7, April 1, 1993--June 31, 1993 by :
Download or read book Advanced NMR-based Techniques for Pore Structure Analysis of Coal. Quarterly Report No. 7, April 1, 1993--June 31, 1993 written by and published by . This book was released on 1993 with total page 12 pages. Available in PDF, EPUB and Kindle. Book excerpt: One of the main problems in coal utilization is the inability to properly characterize its complex pore structure. Coals typically have micro/ultramicro pores but they also exhibit meso and macroporosity. Conventional pore size techniques (adsorption/condensation, mercury porosimetry) are limited because of this broad pore size range, microporosity, reactive nature of coal, samples must be completely dried, and network/percolation effects. Small angle scattering is limited because it probes both open and closed pores. Although one would not expect any single technique to provide a satisfactory description of a coal's structure, it is apparent that better techniques are necessary. Small angle scattering could be improved by combining scattering and adsorption measurements. Also, the measurement of NMR parameters of various gas phase and adsorbed phase NMR active probes can provide pore structure information. We will investigate the dependence of the common NMR parameters such as chemical shifts and relaxation times of several different nuclei and compounds on the pore structure of model microporous solids, carbons, and coals. In particular, we will study the interaction between several small molecules (129Xe, 3He, 2H2, 14N2, 14NH3, 15N2, 13CH4, 13CO2) and the pore surfaces in coals.
Book Synopsis Advanced Coal Characterization by Nuclear Magnetic Resonance (NMR) by : Jeffrey R. Harmer
Download or read book Advanced Coal Characterization by Nuclear Magnetic Resonance (NMR) written by Jeffrey R. Harmer and published by . This book was released on 1999 with total page 357 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Two Dimensional NMR and NMR Relaxation Studies of Coal Structure. Progress Report, October 1, 1993--December 31, 1993 by :
Download or read book Two Dimensional NMR and NMR Relaxation Studies of Coal Structure. Progress Report, October 1, 1993--December 31, 1993 written by and published by . This book was released on 1993 with total page 40 pages. Available in PDF, EPUB and Kindle. Book excerpt: Four major areas of inquiry are being pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups that determine the reactivity of coals. Special attention is being paid to methods that are compatible with the very high magic angle sample spinning rates needed for operation at the high magnetic field strengths available today. Polarization inversion methods utilizing the difference in heat capacities of small groups of spins are particularly promising. Methods combining proton-proton spin diffusion with 13C CPMAS readout are being developed to determine the connectivity of functional groups in coals in a high sensitivity relay type of experiment. Additional work is aimed at delineating the role of methyl group rotation in the proton NMR relaxation behavior of coals.
Book Synopsis Two Dimensional NMR and NMR Relaxation Studies of Coal Structure. Progress Report, January 1, 1993--March 31, 1993 by :
Download or read book Two Dimensional NMR and NMR Relaxation Studies of Coal Structure. Progress Report, January 1, 1993--March 31, 1993 written by and published by . This book was released on 1993 with total page 17 pages. Available in PDF, EPUB and Kindle. Book excerpt: This report covers the progress made on the title project for the project period. Four major areas of inquiry are being pursued. Advanced solid state NMR methods are being developed to assay the distribution of the various important functional groups that determine the reactivity of coals. Special attention is being paid to methods that are compatible with the very high magic angle sample spinning rates needed for operation at the high magnetic field strengths available today. Polarization inversion methods utilizing the difference in heat capacities of small groups of spins are particularly promising. Methods combining proton-proton spin diffusion with 13C CPMAS readout are being developed to determine the connectivity of functional groups in coals in a high sensitivity relay type of experiment. Additional work is aimed at delineating the role of methyl group rotation in the proton NMR relaxation behavior of coals.
Book Synopsis Advanced Solids NMR Studies of Coal Structure and Chemistry. Progress Report, September 1, 1995--February 28, 1996 by :
Download or read book Advanced Solids NMR Studies of Coal Structure and Chemistry. Progress Report, September 1, 1995--February 28, 1996 written by and published by . This book was released on 1996 with total page 22 pages. Available in PDF, EPUB and Kindle. Book excerpt: This report covers the progress made on the title project for the project period. The study of coal chemical structure is a vital component of research efforts to develop better chemical utilization of coals, and for furthering our basic understanding of coal geochemistry. In this grant we are addressing several structural questions pertaining to coals with advances in state of the art solids NMR methods. Our goals are twofold. First, we are interested in developing new methods that will enable us to measure important structural parameters in whole coals not directly accessible by other techniques. In parallel with these efforts we will apply these NMR methods in a study of the chemical differences between gas-sourcing and oil-sourcing coals. The NMR methods work will specifically focus on determination of the number and types of methylene groups, determination of the number and types of methine groups, identification of carbons adjacent to nitrogen and sites with exchangeable protons, and methods to more finely characterize the distribution of hydrogen in coals. We will also develop NMR methods for probing coal macropore structure using hyperpolarized 129Xe as a probe, and study the molecular dynamics of what appear to be mobile, CH2 rich, long chain hydrocarbons. The motivation for investigating these specific structural features of coals arises from their relevance to the chemical reactivity of some types of coals. The coals to be studied and contrasted include oil-prone coals from Australia and Indonesia, those comprising the Argonne Premium Coal Sample bank, and other relevant samples.
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