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Mass Spectral Study Of Organic Sulfur In The Polymeric Matrix Of Coal Technical Report December 1 1992 February 28 1993
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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.
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Book Synopsis La musique du diable, ou le mercure galant dévalisé by :
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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.
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.
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 Annual Index by :
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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 Government Reports Announcements & Index by :
Download or read book Government Reports Announcements & Index written by and published by . This book was released on 1993 with total page 790 pages. Available in PDF, EPUB and Kindle. Book excerpt:
Book Synopsis VHF EPR Analysis of Organic Sulfur in Coal. Final Technical Report, September 1, 1991--August 31, 1992 by :
Download or read book VHF EPR Analysis of Organic Sulfur in Coal. Final Technical Report, September 1, 1991--August 31, 1992 written by and published by . This book was released on 1992 with total page 21 pages. Available in PDF, EPUB and Kindle. Book excerpt: The development of very High Frequency Electron Paramagnetic Resonance (VHF-EPR) into an analytical technique that holds great promise for the non-destructive determination of the amount and structure of organic sulfur in both native and desulfurized coal advanced considerably during the past year. The VHF-EPR spectrometer built with funds from the CRSC is one of two operating near 96 GHz, and the only such instrument in the United States. Earlier work has shown that W-band spectra of Illinois coals and separated macerals shows good sensitivity to forms of organic sulfur present. This work has been extended to improve the use of W-band spectra to provide quantitative as well as qualitative information regarding different sulfur species and, in collaboration with other researchers, their fate during various desulfurizing techniques. A key approach is to synthesize various model compounds, both those from known precursors and those made as sulfurized chars, and to compare their respective W-band spectra (1) with each other, (2) with the predictions of theoretical models, and (3) with the W-band spectra of coal specimens. The quantitative measurement of aromatic sulfur in these compounds has improved as different methods of calibration and indexing are evaluated. Work is also being conducted on apparent variations in spectral line-shapes on evacuation of coal samples. Corroborations of many aspects of W-band organic sulfur interpretation in both raw and desulfurized coals as well as in model compounds are also being carried out by microanalysis and by high-temperature mass spectroscopy. The determination of populations of groups or species of aromatic sulfur molecules is being refined. Especially promising are methods to improve discrimination by differing saturation rates, and by second-derivative spectra.
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 VHF EPR Analysis of Organic Sulfur in Coal. Technical Report, December 1, 1991--February 29, 1992 by :
Download or read book VHF EPR Analysis of Organic Sulfur in Coal. Technical Report, December 1, 1991--February 29, 1992 written by and published by . This book was released on 1992 with total page 19 pages. Available in PDF, EPUB and Kindle. Book excerpt: This is a report of the second quarter of a two-year investigation exploiting electron paramagnetic resonance (EPR), especially novel, very high frequency (VHF) spectroscopy techniques and instrumentation (the only high-modulation W-band EPR spectrometer in the world) developed earlier by these authors, to conduct further qualitative and quantitative studies of heteroatomic organic molecules in coal with particular emphasis on sulfur. New model compounds have been prepared in EPR-active forms and surveyed with X-band EPR. Previous W-band (96 GHz) VHF-EPR work is being extended to studies of these new model compounds as well as to a variety of coal and desulfurized coal samples. Typically, the model compounds under investigation and their analogues are found in coals as stable free radicals which give rise to an EPR signal.
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 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 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: The overall goal of this study is to improve the understanding of sulfur in coals/chars via the use of combined advanced nondestructive and advanced destructive methods of sulfur analysis. This study combines selective oxidation, analytical pyrolysis, and sulfur X-ray Absorption Near Edge Structure Spectroscopy (XANES) analysis. Samples with a wide variety of sulfur contents, (0.63%--4.40%) have been prepared for use in this study. This includes steam gasification chars, oxidized coals and desulfurized coals as well of the original unaltered coals. Mild pyrolysis and XANES data shows that the sulfur chemistry of gasification chars is significantly different from that of the original coals. Mild pyrolysis of the samples that were oxidized with peroxyacetic acid showed that the level of simple thiophene structures observed in the pyrolysis products declines with increasing levels of oxidation. Sulfur XANES spectra of treated samples showed various effects depending on the treatment severity. The XANES spectra of less severely treated samples were similar, although not identical, to the untreated coal spectra. XANES of gasification chars indicated conversion of pyrite to pyrrhotite, removal of organic sulfide sulfur and dissolution of soluble inorganic sulfur species during gasification. Mild oxidation with peroxyacetic acid results in preferential oxidation of sulfide forms before thiophene forms but increasing oxidation severity leads to virtually all sulfur species being oxidized. Good agreement between W-band EPR and XANES data for aromatic sulfur contents were obtained. The TPR analysis of coal indicated that organic sulfur was present as alkyl-aryl sulfide, aryl-aryl sulfides, simple thiophenes and condensed thiophenes. TPR shows that non-thiophenic compounds are removed by PAA oxidation, and that the longer the oxidation is performed the greater is the removal of non-thiophenic sulfur structures.
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