Novel application of /sup 31/P NMR spectroscopy to the analysis of organic groups containing -OH, -NH and -SH functionalities in coal extracts and condensates
Over one hundred model organic compound including phenols, aliphatic alcohols, aromatic acids, aliphatic acids, amines, and thiols have been derivatized with two members of a phospholane series of phosphorus-containing reagents, namely, ClPOCH/sub 2/CH/sub 2/O and ClPOCHMe/sub 2/CMe/sub 2/O. Measurement of proton-decoupled /sup 31/P chemical shifts of these derivatives reveals that, in general, the resonances fall into well-separated regions for derivatized classes of these organic compounds. Both phosphorus reagents were also tested on pyridine extracts of Illinois No. 6 coal, revealing the presence of various phenols, carboxylic acids, and aliphatic alcohols. Similar derivatization of a low-temperature pyrolysis condensate from Illinois No. 6 coal showed no detectable concentrations of carboxylic acids, a relatively small amount of aliphatic alcohols, but considerable quantities of a variety of phenols. The current scope and limitations of this NMR technique and its applicability to the quantitation of -OH, -SH, and -NH functionalities in organic solutions of coal-derived materials are discussed.
- Research Organization:
- Iowa State Univ., Ames (USA)
- OSTI ID:
- 5974805
- Report Number(s):
- CONF-870802-
- Journal Information:
- Prepr. Pap., Am. Chem. Soc., Div. Fuel Chem.; (United States), Vol. 32:3; Conference: 194. American Chemical Society national meeting, New Orleans, LA, USA, 30 Aug - 4 Sep 1987
- Country of Publication:
- United States
- Language:
- English
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Development of instrumental techniques for coal surface analysis: Functional group analysis in coal by /sup 31/ NMR spectroscopy: Quarterly report, 1 April 1988--30 June 1988
Development of instrumental techniques for coal surface analysis: Functional group analysis in coal by /sup 31/P NMR spectroscopy: Quarterly report, January 1, 1988--March 31, 1988
Related Subjects
37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
ALCOHOLS
NUCLEAR MAGNETIC RESONANCE
AMINES
AROMATICS
COAL EXTRACTS
QUALITATIVE CHEMICAL ANALYSIS
COAL LIQUIDS
CONDENSATES
ORGANIC ACIDS
PHENOLS
THIOLS
DERIVATIZATION
EXPERIMENTAL DATA
NMR SPECTRA
PHOSPHORUS 31
PHOSPHORUS COMPOUNDS
CHEMICAL ANALYSIS
CHEMICAL REACTIONS
DATA
FLUIDS
HYDROXY COMPOUNDS
INFORMATION
ISOTOPES
LIGHT NUCLEI
LIQUIDS
MAGNETIC RESONANCE
NUCLEI
NUMERICAL DATA
ODD-EVEN NUCLEI
ORGANIC COMPOUNDS
ORGANIC SULFUR COMPOUNDS
PHOSPHORUS ISOTOPES
RESONANCE
SPECTRA
STABLE ISOTOPES
010600* - Coal
Lignite
& Peat- Properties & Composition
400102 - Chemical & Spectral Procedures