Graduate Thesis Or Dissertation
 

Techniques of solvent extraction of organic material from natural waters

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  • Manual and automatic solvent extraction techniques were used to concentrate organic material from natural waters. Field and laboratory extractions were compared to determine the most probable method and best solvents for efficient concentration of organic material from estuarine and sea waters. The large scale extraction processes utilizing extractors made from 55 gallon drums were operated both by manually moving perforated metal discs through the water and solvent for mixing and by bubbling air through the aqueous-solvent mixture. Resulting samples proved large enough for the detection of short-chain fatty acids (carbon length 1 through 10). Identification of organic constituents was by gas chromatography-mass spectroscopy. Other portions of these samples were separated by column chromatography with subsequent analysis by infrared, visible, ultraviolet, and mass spectroscopy. The proximity of the Hanford Atomic Product Operations to the collecting area caused some of the organics to be labeled with trace amounts of radionuclides. A counter-current pulse column extractor was used at sea aboard the Research Vessel YAQUINA. The organic solvent, hexone, used in this extraction was distilled before and after the extraction with various fractions of solvent being kept for control. The extraction was carried out under varying chemical and physical conditions. The hexone was back-extracted into hydrochloric acid, sodium bicarbonate, or sodium hydroxide before analysis by flame-ionization gas chromatography and mass spectroscopy. Other portions of the product hexone were analyzed for total solid matter recovered and carbon, hydrogen, and nitrogen content. Small intermediate scale extractions were carried out in the laboratory using several solvents. Resulting organic material was analyzed by tandem gas chromatography-mass spectroscopy. Where possible, organic derivatives were prepared to aid in the identification of the recovered organic material. The advantages and disadvantages of large scale extractions and small laboratory procedures were discussed.
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