Development of on-line liquid chromatograph-inductively coupled plasma-atomic emission spectrometer for the analysis of trace organically bound metals and metalloids in coal derived products
Included in this thesis is a review of separations of organically bound metals by LC and a review of specific metal detectors as applied to LC. Coal-derived material has been separated into acid, base and neutral fractions; oil asphaltene and asphaltol fractions and functionality divided fractions. Metal distributions in each fraction after acid digestion are reported as well as possible interpretations of the metal analysis. A series of fractions were collected from a preparative size exclusion separation of a CHCl/sub 3/-soluble SRC on BioBeads S-X4. After removal of the solvent the samples were digested using H/sub 2/SO/sub 4//H/sub 2/O/sub 2/. Plots of metal content versus elution volume provided metal specific detection. The development of the LC-ICP interface provided simultaneous on-line detection for metal species separated by effective molecular size. A new spray chamber to facilitate the analysis in organic solvents of relatively high volatility was developed. It also served as the interface between the LC and the ICP. Detection limits in toluene are comparable to those found in aqueous off-line operation of ICP-AES. Discussions are included concerning the requirements of computer based data output and examples of the output developed are presented. Demonstration of the LC-ICP interface is achieved by size separation of three synthetic mixtures. Two of the mixtures are iron and silicon organometallic species with different ligands attached; while, the third mixture consists of 20 different metals in essentially the same ligand environment.
- OSTI ID:
- 5668202
- Resource Relation:
- Other Information: Thesis (Ph. D.)
- Country of Publication:
- United States
- Language:
- English
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Related Subjects
COAL LIQUIDS
SEPARATION PROCESSES
ORGANOMETALLIC COMPOUNDS
LIQUID COLUMN CHROMATOGRAPHY
ON-LINE MEASUREMENT SYSTEMS
ASPHALTENES
COMPUTERS
ELEMENTS
IRON
LIGANDS
METALS
PYRIDINE
SEMIMETALS
SILICON
SRC PROCESS
TRACE AMOUNTS
ASPHALTS
AZINES
BITUMENS
CHROMATOGRAPHY
FLUIDS
HETEROCYCLIC COMPOUNDS
LIQUIDS
ON-LINE SYSTEMS
ORGANIC COMPOUNDS
ORGANIC NITROGEN COMPOUNDS
OTHER ORGANIC COMPOUNDS
PYRIDINES
TAR
TRANSITION ELEMENTS
010600* - Coal
Lignite
& Peat- Properties & Composition
010500 - Coal
Lignite
& Peat- Products & By-Products