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Mass Spectral Study Of Organic Sulfur In The Polymeric Matrix Of Coal Quarterly Technical Report March 1 1993 May 31 1993
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Book Synopsis Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. [Quarterly] Technical Report, March 1, 1993--May 31, 1993 by :
Download or read book Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. [Quarterly] Technical Report, March 1, 1993--May 31, 1993 written by and published by . This book was released on 1993 with total page 11 pages. Available in PDF, EPUB and Kindle. Book excerpt: This report reviews the seventh quarter progress of a two year project to examine the chemical environment of organic sulfur in the polymeric matrix of Illinois coal by laser desorption ion trap mass spectrometry. This project is attempting to develop new laser desorption-ionization schemes for coal which preserve the polymeric matrix. From work this quarter, we have concluded that ultraviolet matrix assisted laser desorption is not an appropriate method to volatilize high molecular weight material extracted from coal. However, we have found that direct 355 nm laser desorption of neat samples of pyridine extracts from Illinois No. 6 coal gives what appears to be intact molecular ions. Direct laser desorption of the extract using both IR and UV wavelengths produces a distribution of ions between 150 and 1500 amu, with a peak near 500 amu. Work is continuing into the final quarter of this project to obtain such spectra from separated coal macerals and from various other coals.
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 Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. [Quarterly] Technical Report, March 1, 1992--May 31, 1992 by :
Download or read book Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. [Quarterly] Technical Report, March 1, 1992--May 31, 1992 written by and published by . This book was released on 1992 with total page 14 pages. Available in PDF, EPUB and Kindle. Book excerpt: This report reviews the progress of a project to examine the chemical environment of organic sulfur in the polymeric matrix of Illinois coal by laser desorption ion trap mass spectrometry. This project is developing new laser desorption-ionization schemes for coal which preserve the polymeric matrix. It will compare mass spectra of whole coal with its separated macerals and will analyze organic sulfur in the polymeric matrix of coal by collision induced dissociation and high resolution mass spectrometry. A laser desorption mass spectrum of a trial polymer is shown to demonstrate the advantage of this technique over more traditional electron impact ionization mass spectrometry. A preliminary mass spectrum of THF extracts from a Herrin No. 6 (IBC 101) coal sample is also shown which contains low molecular weight fragments in the 60 to 250 amu region. Efforts are presently underway to obtain higher molecular weight ions from coal samples by optimizing the laser desorption conditions, improving the solvent extraction technique, and extending the mass range of the ion trap.
Download or read book のこる生命の日々 written by and published by . This book was released on 1967 with total page 316 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. Technical Report, December 1, 1992--February 28, 1993 by :
Download or read book Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. Technical Report, December 1, 1992--February 28, 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: This report reviews the sixth quarter progress of a two year project to examine the chemical environment of organic sulfur in the polymeric matrix of Illinois coal by laser desorption ion trap mass spectrometry. This project is attempting to develop new laser desorption-ionization schemes for coal which preserve the polymeric matrix. During this quarter, we extended experiments utilizing ultraviolet matrix assisted laser desorption ionization to the examination of solvent extracts of coal. Regardless of the matrix compound, concentration, or laser wavelength chosen, only carbon cluster ions were observed in the mass spectra. During the next quarter, we will attempt to apply laser desorption of neutral compounds followed chemical ionization to form intact molecular ions from the polymeric component of coal.
Book Synopsis Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. [Quarterly] Technical Report, December 1, 1991--February 29, 1992 by :
Download or read book Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. [Quarterly] Technical Report, December 1, 1991--February 29, 1992 written by and published by . This book was released on 1992 with total page 11 pages. Available in PDF, EPUB and Kindle. Book excerpt: This report reviews the second quarter progress of a new project to examine the chemical environment of organic sulfur in the polymeric matrix of Illinois coal by laser desorption mass spectrometry inside a modified ion trap mass spectrometer. This project is developing new laser desorption and ionization schemes for coal which preserve the polymeric matrix, will compare mass spectra of whole coal with its separated macerals, and will analyze organic sulfur in the polymeric matrix of coal.
Book Synopsis La musique du diable, ou le mercure galant dévalisé by :
Download or read book La musique du diable, ou le mercure galant dévalisé written by and published by . This book was released on 1711 with total page pages. Available in PDF, EPUB and Kindle. Book excerpt:
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 199? with total page 1140 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. Technical Report, September 1--November 30, 1991 by :
Download or read book Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal. Technical Report, September 1--November 30, 1991 written by and published by . This book was released on 1991 with total page 6 pages. Available in PDF, EPUB and Kindle. Book excerpt: These experiments will examine the chemical environment of organic sulfur in the polymeric matrix of Illinois coal by novel mass spectrometric techniques: High molecular weight ions from the polymeric coal matrix will be formed by laser desorption and photoionization of powdered coal samples. These ions will be subsequently injected into an ion trap mass spectrometer for single and multiple mass analysis for the identification of sulfur containing moieties in the polymeric matrix. Furthermore, comparison of the mass spectra of various separated macerals with that of whole coal will be made to determine whether chemical modification occurs during the separation process.
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 1994-02 with total page 868 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal by :
Download or read book Mass Spectral Study of Organic Sulfur in the Polymeric Matrix of Coal written by and published by . This book was released on 1991 with total page 6 pages. Available in PDF, EPUB and Kindle. Book excerpt: These experiments will examine the chemical environment of organic sulfur in the polymeric matrix of Illinois coal by novel mass spectrometric techniques: High molecular weight ions from the polymeric coal matrix will be formed by laser desorption and photoionization of powdered coal samples. These ions will be subsequently injected into an ion trap mass spectrometer for single and multiple mass analysis for the identification of sulfur containing moieties in the polymeric matrix. Furthermore, comparison of the mass spectra of various separated macerals with that of whole coal will be made to determine whether chemical modification occurs during the separation process.
Book Synopsis Analysis of Organic Sulfur and Nitrogen in Coal Via Tandem Degradation Methods. [Quarterly] Technical Report, March 1--May 31, 1993 by :
Download or read book Analysis of Organic Sulfur and Nitrogen in Coal Via Tandem Degradation Methods. [Quarterly] Technical Report, March 1--May 31, 1993 written by and published by . This book was released on 1993 with total page 21 pages. Available in PDF, EPUB and Kindle. Book excerpt: There is need for alternative methods for determining the nature of organic sulfur and nitrogen compounds in coal. In our research, we apply chemical and thermal degradation techniques to render coal amenable to standard gas chromatography characterization. Standard density gradient centrifugation successfully isolated vitrinite from the IBC101 coal, whereas the multi-step high resolution method was required to isolate liptinite and inertinite macerals, which are minority constituents. Analytical pyrolysis-gas chromatography, operating with either the sulfur selective flame photometric detector (py-GC-PFD) or a mass spectrometer (py-GC/MS), provides distinctive organosulfur ''fingerprints'' for all coal, asphaltene and maceral samples analyzed to date. PY-GC/MS permits ready differentiation of asphaltenes from low and high rank coals. Of the two pyrolysis techniques, py-GC-FPD is simpler and less expensive, and is the recommended method for situations in which sulfur content is the prime concern. Both py-GC methods are superior to oxidative degradation techniques in that they are permit direct, one-step micro-scale analysis, requiring only a minimum of sample preparation. Distinctive chromatographic profiles are also achieved using the methylated dichromate oxidation products of coals, asphaltenes and macerals, but the extensive wet chemical preparation required is a serious disadvantage. Reasonable matches for the expected masses of alkylthiophene carboxylic acid derivatives have been found in the direct probe, low voltage, high resolution mass spectral data set collected on the methylated dichromate oxidation products of the sulfur-rich Spanish lignite sample, providing an additional line of evidence confirming the presence of such compounds.
Book Synopsis VHF EPR Analysis of Organic Sulfur in Coal. [Quarterly] Technical Report, March 1, 1993--May 31, 1993 by :
Download or read book VHF EPR Analysis of Organic Sulfur in Coal. [Quarterly] Technical Report, March 1, 1993--May 31, 1993 written by and published by . This book was released on 1993 with total page 15 pages. Available in PDF, EPUB and Kindle. Book excerpt: One important goal of this project is the development of methods to analyze the Very High Frequency Electron Paramagnetic Resonance (VHF EPR) spectra from Illinois coals in order to determine the concentration of organic sulfur in them. In this third Quarter, the axially symmetric model for the simulation of VHF EPR coal spectra was refined for routine quantitative percent sulfur determination. The computer modeling technique which we have developed makes use of a sophisticated multi-dimensional simplex strategy for optimization. The percent sulfur determined from VHF-EPR of sporinite, vitrinite, and two blends of these macerals (from Illinois Herrin No. 6) show excellent linear correlation with far less reliable, time consuming, and difficult techniques.
Book Synopsis Vhf EPR Analysis of Organic Sulfur in Coal. [Quarterly] Technical Report, March 1, 1992--May 31, 1992 by :
Download or read book Vhf EPR Analysis of Organic Sulfur in Coal. [Quarterly] Technical Report, March 1, 1992--May 31, 1992 written by and published by . This book was released on 1992 with total page 17 pages. Available in PDF, EPUB and Kindle. Book excerpt: This third quarterly report of the project's first year reports that, consonant with our research goals, we have refined the quantitative measurement of organic sulfur in coals, and extended this technique to analysis of treated and desulfurized coals, using either low temperature pyrolysis in our labs, or other techniques as supplied by DOE-PETC. The evolution of the central carbon and downfield sulfur peak amplitudes vs pyrolysis temperature support both the hypothesis of increase in aromatic carbon radicals and the evolution of some sulfur, even at low temperatures. The examination of evacuation effects, and differentiation of species by microwave power saturation levels and second derivative W-band detection also continued. Finally, model sulfur-containing carbonaceous solids -- chars from sucrose or cellulose, and various model sulfur compounds (elemental, mono- and di-thiophenic, and thiosulfidal) - are under development. Already, the W-band spectra of some of these char models show striking similarities to those of whole and treated coals. The further development of these models in conjunction with all other aspects of this program are progressing steadily toward the goal of better quantitative md qualitative differentiation of aromatic heteroatoms in coal.
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 Analyzing Organic Sulfur in Coal by :
Download or read book Analyzing Organic Sulfur in Coal written by and published by . This book was released on 1994 with total page 33 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis Vhf EPR Quantitation and Speciation of Organic Sulfur in Coal. [Quarterly] Technical Report, December 1, 1993--February 28, 1994 by :
Download or read book Vhf EPR Quantitation and Speciation of Organic Sulfur in Coal. [Quarterly] Technical Report, December 1, 1993--February 28, 1994 written by and published by . This book was released on 1994 with total page 17 pages. Available in PDF, EPUB and Kindle. Book excerpt: The existence of free electrons in coals' natural site offers a great attraction for Electron Paramagnetic Resonance (EPR) analysis to aid in the study of the structure and composition of coal. This direct and non-destructive approach to coal analysis has been hindered by the problem of resolution using the conventional 9.5 GHz EPR spectrometers. In the past few years, we have developed techniques including W-band Very High Frequency EPR spectroscopy as a means of determining the quantity and structure of organic sulfur in native and desulfurized coals. The state of the art 95 GHz (W-band) EPR spectrometer which we have constructed shows a well resolved spectrum including the interaction between unpaired electrons and the heteroatom like sulfur. The spectra also provide quantitative as well as qualitative information regarding different sulfur species. In collaboration with researchers at the University of Kentucky, we are also analyzing the result of desulfurization techniques on the presence of various sulfur species in coal. In the past, we have tried to synthesize various model compounds comparing their W-band spectra with other models, the predictions of theoretical models, and with the W-band spectra of coal specimens. In this quarter, we have been concentrating our efforts on developing a new standard protocol in handling and preparing the coal samples for EPR measurements to provide a quantitative comparison between the EPR spectra of coal in the natural state and desulfurized. Ten coal samples, both native and desulfurized, have been provided to us. These samples have been run in both laboratories. The simulation of coal EPR spectra has been carried out using several mathematical models. EPR results now are being compared with XANES data.
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