ANNEX XIU.K.DETERMINATION OF VOLATILE HALOGENATED SOLVENTS CONTENT OF OLIVE OIL
4.PROCEDUREU.K.
4.1.Exactly weigh around 3 g of oil in a glass flask (not to be reused); hermetically seal it. Place it in a thermostat at 70 °C for one hour. Using a syringe carefully remove 0,2 to 0,5 ml of the head space. Inject this into the column of the gas chromatography apparatus regulated as follows:U.K.
injector temperature: 150 °C,
column temperature: 70 to 80 °C,
detector temperature: 200 to 250 °C.
Other temperatures may also be used provided the results remain equivalent.
4.2.Reference solutions: prepare standard solutions using refined olive oil with no trace of solvents with concentrations ranging from 0,05 to 1 ppm (mg/kg) and corresponding to the presumed content of the sample. The halogenated solvents may be diluted using pentane.U.K.
4.3.Quantitative assessment: correlate the surfaces or the elevations of the peaks of the sample and of the standard solution of the concentration presumed closest. If the deviation is greater than 10 % the analysis must be repeated in comparison with another standard solution until the deviation is within 10 %. The content is determined on the basis of the average of the elementary injections.U.K.
4.4.Expression of results: in ppm (mg/kg). The detection limit for the method is 0,01 mg/kg.U.K.