如题,AfPS GS 2014:01 PAK这个方法有净化步骤
3.1.2 Column chromatography extraction step
For some polymers (e.g. plastic or rubber products), especially those that dissolve well in
toluene under the described extraction conditions, it is necessary to clean the extract using
adsorption chromatography on silica gel.
For this purpose, a clean-up column with “Hahnschliff” (“stopcock”) (approx. 220 mm x 15 mm)
is filled with glass wool, 4 g of silica gel and 1 cm of sodium sulfate.
The silica gel is deactivated beforehand by adding 10% water (the corresponding volume of
water is added to the silica gel in a glass flask, and the mixture is homogenised on the rotary
evaporator for 1 h at standard pressure and room temperature. The silica gel can then be stored
in the sealed glass flask at room temperature).
The packed column is conditioned with 10 ml of petroleum ether.
The aliquot of toluene extract is then evaporated to a volume of approx. 1 ml on the rotary
evaporator and poured into the column. The pointed flask is rinsed out with approx. 20 ml of
eluent, which is then also transferred to the clean-up column. Elution is performed with 50 ml of
petroleum ether. The collected petroleum ether eluate is amended with 1 ml of toluene and
evaporated to a volume of approx. 1 ml under a nitrogen stream (e.g. on the TurboVap). This is
then made up to a defined volume with toluene, and the extract is analysed by
gc-MS.
我完全采用这个净化对样品进行净化处理,发现完全没有起到净化的效果,有使用为个标准的版友可以提出大家讨论下。