Techniques of solvent extraction of organic material from natural waters

Manual and automatic solvent extraction techniques were usedto concentrate organic material from natural waters. Field andlaboratory extractions were compared to determine the most probablemethod and best solvents for efficient concentration of organicmaterial from estuarine and sea waters.The large scale extraction processes utilizing extractors madefrom 55 gallon drums were operated both by manually moving perforatedmetal discs through the water and solvent for mixing and bybubbling air through the aqueous-solvent mixture. Resulting samplesproved large enough for the detection of short-chain fatty acids (carbonlength 1 through 10). Identification of organic constituents wasby gas chromatography-mass spectroscopy.Other portions of these samples were separated by columnchromatography with subsequent analysis by infrared, visible, ultraviolet,and mass spectroscopy. The proximity of the HanfordAtomic Product Operations to the collecting area caused some ofthe organics to be labeled with trace amounts of radionuclides.A counter-current pulse column extractor was used at seaaboard the Research Vessel YAQUINA. The organic solvent, hexone,used in this extraction was distilled before and after the extractionwith various fractions of solvent being kept for control. Theextraction was carried out under varying chemical and physicalconditions. The hexone was back-extracted into hydrochloric acid,sodium bicarbonate, or sodium hydroxide before analysis by flame-ionizationgas chromatography and mass spectroscopy. Other portionsof the product hexone were analyzed for total solid matterrecovered and carbon, hydrogen, and nitrogen content.Small intermediate scale extractions were carried out in thelaboratory using several solvents. Resulting organic material wasanalyzed by tandem gas chromatography-mass spectroscopy. Wherepossible, organic derivatives were prepared to aid in the identificationof the recovered organic material.The advantages and disadvantages of large scale extractionsand small laboratory procedures were discussed.