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TitlePilot scale chromatographic separation of poly unsaturated ethyl esters using liquefied gases and supercritical fluids
Publication TypeConference Paper
Year of Publication2012
AuthorsTallon, S.J., Montanes F., Mitchell K., and Rose P.
Conference NameAIChE 2012 - 2012 AIChE Annual Meeting, Conference Proceedings
Date Published2012
AbstractThis paper describes the scale-up, development and commissioning of a pilot scale preparative chromatography plant suitable for use with liquefied gases and supercritical fluids as the mobile phase, including the use of flammable gases. The pilot plant has 2 by 10L columns capable of operation up to 350 bar pressure and 85°C temperature. The columns can be operated in series or independently, and in single or semi-continuous automated operation. A UV-Vis detection system is used, and up to 4 fractions can be separately recovered. A co-solvent gradient can also be applied. A laboratory scale process for separation of the polyunsaturated fatty acids EPA and DHA from mixtures of ethyl esters derived from fish and algal sources has been developed, and a comparison of results between laboratory and pilot scale is given. Very good separation, exceeding 90% concentration of EPA and DHA, and very good recovery was able to be achieved in a single pass operation using CO2 as the mobile phase and a silica column. Conditions were optimised over the range 150 to 250 bar pressure, temperatures from 40 to 60°C, and using a range of ethyl ester and CO2 flow rates. Results were able to be reproduced on the pilot scale using loadings between 10g and 100g of ethyl esters.

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