BS EN 14105 Fat and oil derivatives - Fatty Acid Methyl Esters (FAME) - Determination of free and total glycerol and mono-, di-, triglyceride contents
3 Reagents
Use only reagents of recognized analytical grade, unless otherwise specified.
3.1 N-methyl-N-trimethysilyltrifluoroacetamide (MSTFA)
3.2 Pyridine, max. 0.1 % water, stored on molecular sieve
NOTE Pyridine silyl grade (3.10) can also be used.
3.3 Tetrahydrofurane (THF)
3.4 n-Heptane
3.5 Glycerol
3.6 1,2,4-Butanetriol
3.7 1-Glyceryl monononadecanoate (Mono C19)
3.8 1-3 Glyceryl dinonadecanoate (Di C38)
3.9 Glyceryl trinonadecanoate (Tri C57)
3.10 Pyridine, silyl grade
4 Apparatus
Usual laboratory apparatus and, in particular, the following.
4.1 Gas chromatograph, equipped with an on-column injector or equivalent device, a temperature-programmable oven and a flame ionization detector.
4.2 Capillary column, capable of being programmed up to 400 °C ("high temperature" type) for which the following characteristics are advised:
100 % dimethylpolysiloxane or 95 % dimethyl-5 % diphenylpolysiloxane stationary phase;
length 15 m;
internal diameter 0,32 mm;
film thickness 0,1 µ m.
4.3 Volumetric flask, 50 ml capacity
4.4 Volumetric flasks, 20 ml capacity
4.5 Volumetric flasks, 10 ml capacity
4.6 Screw-cap vials with PTFE-faced septa, 10 ml capacity
4.7 Precision pipette, 1 ml capacity
4.8 Microsyringe, 100 µl capacity
4.9 Microsyringe, 500 µl capacity
4.10 Microsyringe, 5 µl or 10 µl capacity specially designed for on-column operation
4.11 Graduated cylinder, 10 ml capacity
4.12 Analytical balance, with an accuracy of +/- 0.1 mg
4.13 Carrier gas, hydrogen or helium
4.14 Auxiliary gases, such as air, hydrogen and nitrogen