By Carter Litchfield

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M e a s u r e a b s o r p t i o n a t 520 n m . Glycerol R e a c t w i t h K O H or L i A l H 4. R e c o v e r glycerol a n d a d d i n t e r n a l s t a n d a r d such as b u t a n e - l , 4 - d i o l . A n a l y z e free alcohols or t h e i r a c e t a t e or t r i m e t h y l s i l y l e t h e r d e r i v a t i v e s . G a s - l i q u i d chromatography M e t h y l esters A d d i n t e r n a l s t a n d a r d such as t r i h e p t a d e c a n o i n or m e t h y l p e n t a d e c a n o a t e .

The internal standard should be a glyceryl, methyl, or other ester of a C 1 2 - C 2 4 acid that will undergo the same chemical reactions as the sample during methyl ester preparation. The methyl ester derived from the standard must not overlap any GLC peak from the original sample; hence proper choice requires prior knowledge of the fatty acids present. Triglycerides or methyl esters of odd-carbon fatty acids such as 13:0, 15:0, 17:0, and 21:0 are frequently selected as convenient standards which are commercially available in 99% purity.

The major problem in preparing such derivatives for analytical work is to obtain quantitative conversion of the original material to the expected end product without significant by-product formation. When conversion approaches 9 9 % , as in hydrogénation and acetylation reactions, then derivative formation sometimes offers decided analytical advantages. However, when yields fall below 9 5 % , as in mercaptan addition and ozonization, then analysis of the original sample is definitely preferable to using the derivatized form.

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Analysis of Triglycerides by Carter Litchfield
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