Development and application of analytical techniques to chemistry of donor solvent liquefaction. Quarterly progress report, October 1980-December 1980

Technical Report · Wed Apr 01 00:00:00 EST 1981

DOI:https://doi.org/10.2172/6544324· OSTI ID:6544324

Dorn, H. C.; Taylor, L. T.

The LC-ICP interface which can simultaneously detect (ICP) and speciate (LC) up to 34 elements at concentrations between 10 ppM and 0.5 ppB depending on the element and the matrix has been developed. A variety of organic matrices have been successfully used. Preliminary experiments using this interface have monitored 15 elements simultaneously (Al, Ca, Cd, Co, Cr, Cu, Fe, Hg, Mg, Mn, Mo, Ni, Ti, V and Zn). The mode of separation of process derived coal liquefaction solvents and Amax solvent refined coal has been size exclusion chromatography. The metals present in a process solvent obtained from the SRC Wilsonville, AL facility and metal distribution according to effective molecular size are presented. Very low levels of Mg, Mn, Ti, Cd and Hg are observed. Of the elements which were monitored, Cr surprisingly exhibits the largest concentration unlike the other coal-derived materials which have been examined via LC-ICP. The source of Cr in this case may well be from corrosion of the reactor equipment. Both Cr and Fe show a similar molecular size distribution with most of the material eluting near the totally excluded volume. Cu and Zn, on the other hand, show a much smaller size distribution with Cu having at least two groups of sized species; while, Zn appears to be incorporated in a relatively small number of single sized species. The remainder of the elements monitored did not show detectable peaks above ambient noise level. A moderately hydrotreated process solvent that had been previously separated into four distillation ranges: IBP (initial boiling point) -800/sup 0/F, 400 to 800/sup 0/F, 400 to 600/sup 0/F and 600 to 800/sup 0/F was subjected to SEC-ICP using pyridine as the eluting medium. Size exclusion chromatographic metallograms are presented for calcium, magnesium, titanium, iron, copper and zinc.

• Research Organization: Virginia Polytechnic Inst. and State Univ. (Virginia Tech), Blacksburg, VA (United States)
• Sponsoring Organization: USDOE
• DOE Contract Number: AC22-80PC30041
• OSTI ID: 6544324
• Report Number(s): DOE/PC/30041-T3
• Country of Publication: United States
• Language: English

Related Subjects

01 COAL, LIGNITE, AND PEAT
37 INORGANIC
ORGANIC
PHYSICAL AND ANALYTICAL CHEMISTRY
CADMIUM
LIQUID COLUMN CHROMATOGRAPHY
CALCIUM
CHROMIUM
COAL LIQUIDS
CHEMICAL ANALYSIS
COPPER
IRON
MAGNESIUM
MANGANESE
MERCURY
SOLVENT-REFINED COAL
TITANIUM
ZINC
COAL LIQUEFACTION
EMISSION SPECTROSCOPY
ORGANOMETALLIC COMPOUNDS
RESEARCH PROGRAMS
ALKALINE EARTH METALS
CHROMATOGRAPHY
ELEMENTS
FLUIDS
FUELS
LIQUEFACTION
LIQUIDS
METALS
ORGANIC COMPOUNDS
SEPARATION PROCESSES
SPECTROSCOPY
THERMOCHEMICAL PROCESSES
TRANSITION ELEMENTS
010405* - Coal
Lignite
& Peat- Hydrogenation & Liquefaction
010600 - Coal
Lignite
& Peat- Properties & Composition
400105 - Separation Procedures