Identification and cleavage of breakable single bonds by selective oxidation, reduction and hydrolysis. Quarterly report No. 2, January 1-March 31, 1979
The objective of this project is to determine the structure of bituminous coal with emphasis on the crosslinks and breakable single bonds. During this past quarter, a new gel permeation chromatography system using pyridine as solvent was installed and calibrated. Pyridine dissolved some coal fractions that were only partly soluble in tetrahydrofuran, but the sensitivity of the detector was lower with pyridine because its index of refraction was closer to that of coal products. Acetylation, methylation, trimethylsilylation, and decyldimethylsilylation of the pyridine soluble, toluene-insoluble (asphaltol) fraction of Illinois No. 6 coal extract and of products obtained from that extract were conducted to increase solubilities for NMR studies. This effort was only partially successful, and new NMR data on aromatic and aliphatic hydrogen and carbon contents are presented and conclusions are discussed. Cleavage of the asphaltol fraction was carried out by slow addition of sodium dissolved in ammonia and butylamine. Field ionization mass spectroscopy on the sodium-cleaved asphaltol and its methylation products show that this technique is unsuitable for these coal fractions. A new preparation of black acids from NaOCl oxidation of pyridine-extracted coal contained more aromatic carbon and less aliphatic and carboxyl carbon than a similar product discussed under an earlier contract. Treatment of the asphaltol fraction with bases resulted in 12 to 50% of the asphaltol becoming soluble in ether or alcohol. 10 references, 2 figures, 5 tables.
- Research Organization:
- SRI International, Menlo Park, CA (USA)
- DOE Contract Number:
- AC22-78ET11423
- OSTI ID:
- 6335326
- Report Number(s):
- DOE/ET/11423-T13; ON: DE85003867
- Resource Relation:
- Other Information: Portions are illegible in microfiche products
- Country of Publication:
- United States
- Language:
- English
Similar Records
Identification and cleavage of breakable single bonds by selective oxidation, reduction, and hydrolysis. Quarterly report No. 1, October 1-December 31, 1978
Identification and cleavage of breakable single bonds by selective oxidation, reduction, and hydrolysis. Quarterly report No. 13, October 1-December 31, 1981
Related Subjects
BITUMINOUS COAL
STRUCTURAL CHEMICAL ANALYSIS
COAL EXTRACTS
NMR SPECTRA
ACETYLATION
AMINES
ASPHALTENES
CALIBRATION
CHEMICAL BONDS
CHROMATOGRAPHY
EXPERIMENTAL DATA
FRACTIONATION
MASS SPECTROSCOPY
METHYLATION
OXIDATION
PYRIDINE
RESEARCH PROGRAMS
SOLVENT EXTRACTION
TETRAHYDROFURAN
ACYLATION
ASPHALTS
AZINES
BITUMENS
BLACK COAL
CARBONACEOUS MATERIALS
CHEMICAL REACTIONS
COAL
DATA
ENERGY SOURCES
EXTRACTION
FOSSIL FUELS
FUELS
FURANS
HETEROCYCLIC COMPOUNDS
INFORMATION
MATERIALS
NUMERICAL DATA
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
ORGANIC OXYGEN COMPOUNDS
OTHER ORGANIC COMPOUNDS
PYRIDINES
SEPARATION PROCESSES
SPECTRA
SPECTROSCOPY
TAR
010600* - Coal
Lignite
& Peat- Properties & Composition