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Surface properties of photo-oxidized bituminous coals. Technical progress report, October--December 1995

Description: During this report period, polished blocks of coal containing 3--4 mm wide vitrain bands were prepared for contact angle measurements of fresh and photo-oxidized surfaces using the advancing-drop technique. Contact angles were measured on two of the coals collected for this study, (the Ohio No. 4a (DECS-33) and Lower Kittanning (PSOC-1562) seams) and the results added to those presented in the last quarterly report. Although the new data give additional variation to the sample set, they are consistent with the original observations, i.e., that contact angle is influenced by irradiation time and coal rank. Using the maximum change in contact angle measured between fresh and photo-oxidized surfaces, a linear decrease is observed with increasing rank resulting from 5 and 10 minutes of irradiation. The magnitude of the decrease in contact angle diminishes with increasing rank. Also during this period, an ultraviolet spotlight was evaluated as a means of irradiating powdered vitrain. This 100 watt, long wavelength (366 nm) ultraviolet lamp is to be used in place of the optical microscope system to establish the influence of surface photo-oxidation on the flotation characteristics of vitrain concentrates. A series of experiments was designed to determine the magnitude of change in the luminescence intensity (at 600 nm measured in the optical microscope) with exposure to the ultraviolet light with time for vitrinite from different rank coals. The authors have established that there is a significant decrease in luminescence intensity with time of exposure which diminishes slightly as rank increases. The ultraviolet light appears to provide a level of photo-oxidation that is a factor of 10 lower than that obtained with their optical microscope system.
Date: February 1, 1996
Creator: Mitchell, G.; Polat, H.; Davis, A. & Chander, S.
Partner: UNT Libraries Government Documents Department

Surface properties of photo-oxidized bituminous coals. Quarterly technical report, October 1, 1996--December 31, 1996

Description: During this reporting period, three vitrain concentrate samples crushed to -200 mesh were irradiated (photo-oxidized) for different time periods (0, 10, 50 and 100 min) using the BLAK-RAY ultraviolet lamp to obtain samples suitable for pyrolysis GC/MS. These samples will be used to investigate whether the levels of photo-oxidation induced with increasing UV irradiation can be detected and measured in bulk vitrains using the technique. The analyses have not been fully completed. Further, additional analysis of reflectance-mode FTIR results obtained from polished blocks of vitrain is currently under way. This evaluation involves calculating the second derivative of the spectra in an attempt to better identify the spectral regions of most significant change resulting from photo-oxidation. These analyses, along with final analytical tests that will destroy the irradiated surfaces, including electron microprobe analysis for near- surface oxygen concentration and x-ray mapping, and measurement of reflectance in oil immersion, are under way and will be completed by the end of February, 1997. During this report period we have begun the preparation of a manuscript tentatively entitled, ``Time Resolved C-NEXAFS Analysis of the Chemistry of Photochemical Alteration of Vitrinite. This publication will discuss our efforts in utilizing Scanning Transmission X-ray Microscopy as a tool to better define the kinetics of photo-oxidation or vitrinite from coals of three different ranks by measuring changes in regions near the carbon-edge absorption.
Date: February 1, 1997
Creator: Mitchell, G. & Davis, A.
Partner: UNT Libraries Government Documents Department

Maintenance of the coal sample bank and database. Quarterly progress report, April 1, 1996--June 30, 1996

Description: This five year project is intended to ensure the availability of well-characterized, high-quality coal samples for public and private coal research. It continues support of the DOE Coal Sample Bank and Database at The Pennsylvania State University. Eleven coal samples will be collected, processed, packaged, and analyzed, and a resulting database will be maintained. These samples and data, as well as 45 samples collected under previous contracts, will be distributed to DOE contractors and others performing coal research. Samples will be chosen to maintain a sample bank of 56 coals representing the major U.S. coal fields and a variety of coal ranks and compositions. In addition to standard analyses, liquefaction tests and organic geochemical analyses will be performed. The samples will be stored to minimize deterioration, and 10 samples will be monitored annually by proximate, sulfur forms, and gaseous oxygen analysis to evaluate their condition. This report reflects the level of effort described in the revised work statement submitted to DOE on February 2, 1996, setting out a reduction in effort following a cut in the level of funding of the project.
Date: July 29, 1996
Creator: Davis, A. & Glick, D.C.
Partner: UNT Libraries Government Documents Department

Maintenance of the Coal Sample Bank and Database. Quarterly technical progress report, January 1, 1996--March 31, 1996

Description: This five year project is intended to ensure the availability of well- characterized, high-quality coal samples for public and private coal research. It continues support of the DOE Coal Sample Bank and Database at The Pennsylvania State University. Eleven coal samples will be collected, processed, packaged, and analyzed, and a resulting database will be maintained. These samples and data, as well as 45 samples collected under previous contracts, will be distributed to DOE contractors and others performing coal research. Samples will be chosen to maintain a sample bank of 56 coals representing the major US coal fields and a variety of coal ranks and compositions. In addition to standard analyses, liquefaction tests and organic geochemical analyses will be performed. The samples will be stored to minimize deterioration, and 10 samples will be monitored annually by proximate, sulfur forms, and gaseous oxygen analysis to evaluate their condition. Technical progress is summarized for the following tasks: storage and inventory of samples; monitoring of sample quality; collection and processing of replacement samples; basic characterization of coal samples; liquefaction testing; organic geochemistry (nuclear magnetic resonance spectroscopy); distribution of coal samples to users; data entry; and distribution of data to users.
Date: April 25, 1996
Creator: Davis, A. & Glick, D.C.
Partner: UNT Libraries Government Documents Department

Maintenance of the Coal sample Bank and Database.

Description: This project provides coal samples and accompanying analytical data for research by DOE contractors and others. All 56 samples have been purged with argon before storage, and the 33 samples in the DECS series are heat-sealed in foil laminate bags and stored under refrigeration. Eleven DECS samples have been collected under the current contract. Basic characterization, standardized liquefaction analyses and organic geochemical analyses have been completed. Distribution of samples and data is continuing, with processing of samples being performed as needed. 133 samples, 291 data printouts, and individual data items from 4002 samples were distributed during the quarter.
Date: October 1, 1997
Creator: Davis, A. & Glick, D.C.
Partner: UNT Libraries Government Documents Department

Surface properties of photo-oxidized bituminous coals. Technical progress report, January--March 1996

Description: During this report period, a vitrinite concentrate from the mvb Splash Dam seam (DECS-30) was prepared and analyzed. Results show that the concentrate was 91 vol % vitrinite and that the sample has been adequately protected from oxidation under refrigerated storage in argon. The 9% level of contamination within the vitrinite resulted from the extreme friability of the coal and to the dispersion of fine grains of semifusinite and micrinite. Polished blocks containing vitrain bands that were prepared, irradiated in blue-light and employed in contact angle measurements were evaluated using specular reflectance-mode FT-IR for changes in functional group chemistry. Infrared spectra from unexposed areas of vitrinite and those irradiated for 1, 5 and 10 min for six coals ranging in rank from hvCb to mvb were obtained using a FTS 175 spectrometer with a Bio-Rad UMA 500 microscope accessory. Preliminary results demonstrate that photo-oxidation occurred during irradiation, becoming progressively more intense with increasing irradiation time; however, the magnitude of this change diminished with increasing rank. A relatively steady increase in the carbonyl region (1,800--1,650 cm{sup {minus}1}) and a decrease in the aliphatic region (2,950--2,850 cm{sup {minus}1}) of the spectra supports this observation and is similar to observations made in the past for natural weathering and laboratory oxidation of coals. A series of tests was initiated to photo-oxidize powdered vitrains using the BLAK-RAY ultraviolet lamp evaluated last quarter. Samples of four vitrinite concentrates were exposed to UV light for 10 mins per side. These and the corresponding whole-seam channel samples and raw vitrinite concentrates were submitted for initial microflotation tests which have not been completed at this time.
Date: December 31, 1996
Creator: Mitchell, G.; Davis, A. & Chander, S.
Partner: UNT Libraries Government Documents Department

Maintenance of the Coal Sample Bank and Database. Quarterly technical progress report, July 1, 1995--September 30, 1995

Description: This five year project is intended to ensure the availability of well- characterized, high-quality coal samples for public and private coal research. It continues support of the DOE Coal Sample Bank and Database at The Pennsylvania State University. Thirty coal samples will be collected, processed, packaged, and analyzed, and a resulting database will be maintained. These samples and data, as well as 26 samples collected under previous contracts, will be distributed to DOE contractors and others performing coal research. Samples will be chosen to maintain a sample bank of 56 coals representing the major US coal fields and a variety of coal ranks and compositions. In addition to standard analyses, liquefaction tests and organic geochemical analyses will be performed. The samples will be stored to minimize deterioration, and will be monitored annually by proximate, sulfur forms, and gaseous oxygen analysis to evaluate their condition. These samples will be used for additional research on the influence of changes in surface chemistry on surface properties, the influence of sample deterioration on liquefaction properties, and the mechanisms of coal oxidation. During the quarter, samples were distributed and inventory records were updated. The newly collected sample was added to the inventory records. One sample was collected from the main bituminous field of the Appalachian region during the quarter. Characterization of samples DECS-29 through -32, was accomplished. Product workup on the liquefaction components of DECS- 29, -31 and -32 was performed. The new sample (DECS-33) was processed promptly, and liquefaction testing was performed. Table 1 shows liquefaction product breakdown for 6 samples.
Date: February 13, 1996
Creator: Davis, A. & Glick, D.C.
Partner: UNT Libraries Government Documents Department

Surface properties of photo-oxidized bituminous coals. Technical progress report, July--September 1995

Description: During this report period, a new whole-seam channel sample (Ohio {number_sign}4a) was collected and analyzed, together with the Upper Banner and Splash Dam samples obtained last quarter. These additions bring to seven the number of coals obtained for this project and that range in rank from hvCb to mvb. Polished blocks of each coal containing 3-4 mm wide vitrain bands were prepared for contact angle measurements of fresh and photo-oxidized surfaces. An advancing-drop technique was used to measure contact angle. In this test a droplet of distilled water is grown initially on fresh surfaces and then moved across those irradiated in blue-light for 1, 5, and 10 minutes. The sequence of growth was recorded on video tape, and the change in contact angle measured relative to position at the air/water/surface interface. Contact angles were measured on five of the coals collected for this study, namely the Illinois {number_sign}6, Ohio {number_sign}4a, Lower Kittanning (PSOC-1563), Pittsburgh and Splash Dam seams. Preliminary results show that both coal rank and irradiation time influence surface wettability as measured by contact angle. With one exception, contact angle values decreased and remained low when the droplet advanced into an irradiated area. In most cases, one minute of irradiation resulted in only a slight decrease in contact angle, whereas after 5 and 10 minutes a more significant decrease was observed. The magnitude of change in contact angle values with degree of photo-oxidation decreased as rank increased, such that lower rank bituminous coals show the greatest change and medium volatile coal the least.
Date: November 1, 1995
Creator: Mitchell, G.; Polat, H.; Davis, A. & Chander, S.
Partner: UNT Libraries Government Documents Department

Maintenance of the coal sample bank and database. Quarterly technical progress report, January 1, 1995--March 31, 1995

Description: This project is concerned with the development of a coal database providing information to the public and private research sectors on 30 coal samples. The information from these samples, along with information previously collected on 26 samples, will be distributed to DOE contractors performing coal research.
Date: August 25, 1995
Creator: Davis, A. & Glick, D.C.
Partner: UNT Libraries Government Documents Department

Maintenance of the coal sample bank and database. Quarterly technical progress report, April 1, 1995 --June 30, 1995

Description: This five year project is intended to ensure the availability of well-characterized, high-quality coal samples for public and private coal research. It continues support of the DOE Coal Sample Bank and Database at The Pennsylvania State University. Thirty coal samples will be collected, processed, packaged, and analyzed, and a resulting database will be maintained. These samples and data, as well as 26 samples collected under previous contracts, will be distributed to DOE contractors and others performing coal research. Samples will be chosen to maintain a sample bank of 56 coals representing the major U.S. coal fields and a variety of coal ranks and compositions. In addition to standard analyses, liquefaction tests and organic geochemical analyses will be performed. The samples will be stored to minimize deterioration, and will be monitored annually by proximate, sulfur forms, and gaseous oxygen analysis to evaluate their condition. These samples will be used for additional research on the influence of changes in surface chemistry on surface properties, the influence of sample deterioration on liquefaction properties, and the mechanisms of coal oxidation. A revised work statement has been submitted to DOE, setting out a reduction in effort following a cut in the level of funding of the project.
Date: November 20, 1995
Creator: Davis, A. & Glick, D.C.
Partner: UNT Libraries Government Documents Department

Surface properties of photo-oxidized bituminous coals; Technical progress report, September--November 1993

Description: Five of the eight coals to be studied in this project have been selected on the basis of economic importance as well as geologic and chemical histories. Plans have been initiated to collect the first sample, a Pittsburgh seam coal from southwestern Pennsylvania. However, we have as yet not received permission from the mine to collect our working face sample. In addition, preliminary work was completed on development and testing of a procedure to photo-oxidize vitrinite containing coal blocks using the optical microscope.
Date: December 1, 1993
Creator: Mitchell, G. & Davis, A.
Partner: UNT Libraries Government Documents Department

Establishment and maintenance of a Coal Sample Bank and data base

Description: During the period 7/9/92-10/8/92 a total of 80 samples (30 DOE Sample Bank samples and 50 other Penn State samples) of various sizes, not including DECS-17, were distributed. Fifteen of these samples were provided to DOE contractors. Six orders for a total of 80 30-gram bags of DECS-17 have been filled. All of these bags have been distributed to DOE dispersed catalyst contractors or those approved by DOE to receive the samples. A total of 188 data printouts were distributed. In addition, 15 special data requests were fulfilled by either search/sort and printout or creation of a data disk, resulting in distribution of limited information on over 1089 samples. Several preliminary requests for Sample Bank and Data Base information and price quotations have also been handled.
Date: November 23, 1992
Creator: Davis, A.
Partner: UNT Libraries Government Documents Department

Establishment and maintenance of a Coal Sample Bank and data base. Project status report, July 9, 1992--October 8, 1992

Description: During the period 7/9/92-10/8/92 a total of 80 samples (30 DOE Sample Bank samples and 50 other Penn State samples) of various sizes, not including DECS-17, were distributed. Fifteen of these samples were provided to DOE contractors. Six orders for a total of 80 30-gram bags of DECS-17 have been filled. All of these bags have been distributed to DOE dispersed catalyst contractors or those approved by DOE to receive the samples. A total of 188 data printouts were distributed. In addition, 15 special data requests were fulfilled by either search/sort and printout or creation of a data disk, resulting in distribution of limited information on over 1089 samples. Several preliminary requests for Sample Bank and Data Base information and price quotations have also been handled.
Date: November 23, 1992
Creator: Davis, A.
Partner: UNT Libraries Government Documents Department

Establishment and maintenance of a coal sample bank and data base. Final report, April 8, 1988--September 28, 1993

Description: This DOE contract continued support for the DOE Coal Sample Bank and Data Base at Penn State. At the beginning of the contract, a new type of container was evaluated for long-term storage of coal samples ranging in quantity from a few grams to over 10 kg (22 lbs). Gieseler fluid behavior, oxidation of pyrite to sulfates, loss of heating value, and other properties were monitored over time. Based on preliminary results, these foil and polyethylene laminate bags were believed to be a significant improvement over the drums, buckets and cans previously used. Use of the bags was therefore instituted with DECS-1, the first sample collected under the contract. Twenty-two DECS samples were collected, ranging in rank from lignite to anthracite and representing the five most productive coal provinces of the US. Over 6500 containers of DECS samples were created under the contract and 750 containers of 34 PSOC samples are supported by the contract. Each sample was characterized by proximate and ultimate analysis, petrographic (vitrinite reflectance and maceral) analysis, physical and thermoplastic testing, and inorganic element analysis. The resulting data, and geologic data on each sample, were entered in a data base which can be used to produce a formatted five-page or one-page printout for each sample. An interactively operated data base can be searched, sorted or summarized to produce tables of selected data or to identify samples meeting a requestor`s criteria. During the period covered, 2,313 printouts, and 204 special data reports resulting in distribution of data on 34,086 samples, were provided on request.
Date: November 1, 1993
Creator: Davis, A. & Glick, D. C.
Partner: UNT Libraries Government Documents Department