commiss regul ec march amend regul eec characterist oliv oil oliv residu oil relev method analysi council regul eec tariff statist nomenclatur common custom tariff commiss european commun regard treati establish european commun regard council regul eec septemb establish common organ market oil fat amend regul ec articl thereof regard council regul eec juli tariff statist nomenclatur common custom tariff amend commiss regul ec articl thereof commiss regul eec amend regul ec defin characterist oliv oil oliv residu oil relev method analysi regul eec amend addit note chapter combin nomenclatur contain annex regul eec develop research characterist oliv oil defin regul eec amend ensur puriti product market relev method analysi defin experi adjust method determin trilinolein content addit order continu process harmon intern standard laid intern oliv oil council limit characterist oliv oil oliv residu oil adjust characterist oliv oil refer requir amend addit note chapter combin nomenclatur period adjust standard introduct mean need appli avoid disturb trade entri forc regul defer approxim month provis made oil packag prior entri forc dispos limit period regul eec eec annex xiv amend addit note amend measur provid regul accord opinion manag committe oil fat adopt regul articl regul eec amend articl indent ad determin stigmastadien method set annex xvii annex amend accord annex hereto articl addit note chapter combin nomenclatur contain annex regul eec replac text set annex ii hereto articl regul enter forc dai public offici journal european commun appli oliv oil oliv residu oil packag prior date entri forc market end month entri forc regul bind entireti directli applic member state brussel march commiss franz fischler member commiss annex summari annex regul eec titl ad annex xvii determin stigmastadien veget oil annex replac tabl text annex characterist oliv oil gt tabl gt gt tabl gt note annex viii replac note order permit clear separ trilinolein peak adjac peak interf substanc lampant virgin oil crude oliv residu oil purifi accord method absorb ìl undilut oil silica column liquid solid extract type sep pac silica cartridg water part elut triglycerid ml anhydr hexan hplc second dry elut product nitrogen flow dissolv isopropanol acton ml inject ìl hplc fatti acid composit oil check ensur purif accuraci rang analysi method adopt annex xvii ad annex xvii method determin stigmastadien veget oil purpos determin stigmastadien veget oil low concentr hydrocarbon virgin oliv oil crude oliv residu oil scope standard appli veget oil measur reliabl content hydrocarbon li mg kg method suit detect presenc refin veget oil oliv oliv residu sunflow palm virgin oliv oil refin oil contain stigmastadien virgin oil principl isol unsaponifi matter separ steroid hydrocarbon fraction column chromatographi silica gel analysi capillari ga chromatographi apparatu ml flask suitabl reflux condens separ funnel ml capac ml round bottom flask rotari evapor glass chromatographi column cm intern diamet cm length teflon tap plug glass wool fibr sinter glass disc bottom prepar silica gel column pour hexan chromatographi column depth approxim cm fill slurri silica gel hexan ml hexan portion settl finish settl appli slight vibrat add anhydr sodium sulphat height approxim cm final elut excess hexan ga chromatograph flame ioniz detector split cold column injector oven programm fuse silica capillari column ga chromatographi mm intern diamet length coat phenylmethylsilicon phase mm film thick note column similar lower polar integr record possibl vallei vallei integr mode ml microsyring ga chromatographi cement needl electr heat mantl hot place reagent reagent analyt grade water distil water water equival puriti hexan mixtur alkan bp interv distil rectifi column note solvent distil remov impur ethanol anhydr sodium sulphat alcohol potassium hydroxid solut add ml water potassium hydroxid stir dissolv mixtur ethanol ml note alcohol potash turn brown stand prepar freshli dai stopper dark glass bottl silica gel column chromatographi mesh merck refer similar note silica gel directli contain treatment batch silica gel show low activ result bad chromatograph separ circumst silica gel treat activ silica gel heat minimum hour heat place silica gel desicc gel cool transfer silica gel stopper flask add water shake lump powder flow freeli batch silica gel result chromatogram interf peak silica gel treat altern extra pure silica gel merck refer stock solut ppm cholesta dien sigma puriti hexan mg ml standard solut cholesta dien hexan concentr ppm obtain dilut solut note solut stabl period month solut nonacosan hexan concentr approxim ppm carrier ga chromatographi helium hydrogen puriti auxiliari gase flame ioniz detector hydrogen puriti purifi air procedur prepar unsaponifi matter weigh oil ml flask add ml standard solut cholesta dien ìg ml alcohol potash fit reflux condens heat slight boil minut remov flask sampl heat solut cool slightli cool complet sampl set add ml water transfer solut separ funnel aid ml hexan shake mixtur vigor second separ note emuls produc rapidli disappear add small quantiti ethanol transfer aqueou phase beneath separ funnel extract ml hexan run lower phase wash hexan extract combin separ funnel time ml time mixtur ethanol water neutral ph reach pass hexan solut anhydr sodium sulphat wash ml hexan evapor rotari evapor reduc pressur dryness separ steroid hydrocarbon fraction residu fraction column aid ml portion hexan run sampl column allow solut level drop top sodium sulphat start chromatograph elut hexan flow rate ml min approxim discard ml eluat collect ml fraction collect transfer fraction ml round bottom flask note fraction satur hydrocarbon figur fraction steroid elut squalen relat compound achiev good separ satur steroid hydrocarbon optim fraction volum requir volum fraction adjust fraction analys peak repres satur hydrocarbon low figur intens standard peak low volum reduc complet separ compon fraction unnecessari overlap peak gc analysi gc condit ajust optim volum fraction gener need good separ exist compon presenc larg peak approxim minut lower retent time standard due squalen indic bad separ evapor fraction rotari evapor reduc pressur dryness immedi dissolv residu ml hexan solut refriger analysi note residu dry room temperatur obtain solvent ad solut refriger ga chromatographi work condit split inject injector temperatur detector temperatur integr record paramet integr fix give correct assess area vallei vallei integr mode recommend sensit time minimum attenu amount solut inject ìl oven program temperatur initi minut rise minut injector flow divid carrier helium hydrogen kpa pressur condit adjust accord characterist chromatograph column give chromatogram meet requir intern standard peak approxim minut time intern standard peak full scale ga chromatograph system check inject mixtur stock solut cholestadien nonacosan solut cholesta dien peak nonacosan figur occur action undertaken reduc oven temperatur polar column peak identif intern standard peak appear approxim minut stigmastadien rel retent time approxim figur stigmastadien occur small quantiti isom elut singl chromatograph peak column polar show high resolv power isom small peak close stigmasta dien figur order ensur stigmastadien elut peak advis replac column polar wider intern diamet note stigmastadien refer obtain analysi refin veget oil amount sampl stigmastadien origin promin easili identifi peak quantit analysi stigmastadien content determin formula gt tabl gt area stigmastadien peak peak resolv isom sum area peak ac area intern standard cholestadien mc mass standard ad microgram mass oil gram detect limit mg kg figur ga chromatogram obtain oliv oil sampl analys fuse silica capillari column mm intern diamet coat phenylmethylsilicon ìm film thick fraction ml virgin oil spike standard fraction ml oliv oil mg kg stigmastadien fraction ml small proport fraction figur ga chromatogram obtain refin oliv oil sampl analys db column show isom stigmastadien annex ii head no cover oil deriv sole treatment oliv analyt characterist acid sterol composit tabl fatti acid composit percentag total fatti acid gt tabl gt tabl ii sterol composit percentag total sterol gt tabl gt head no cover chemic alter oliv oil esterifi oliv oil mixtur oliv oil oil presenc esterifi oliv oil oil ascertain method set annex vi regul eec subhead cover oliv oil defin section ii obtain sole mechan physic mean condit thermal condit lead deterior oil undergon treatment wash decant centrifug filtrat oil deriv oliv solvent fall head purpos subhead virgin lampant oliv oil acid mean oliv oil wax content exceed mg kg erythrodiol uvaol content exceed content satur fatti acid posit triglycerid exceed sum transol isom exceed sum translinol translinolen isom exceed characterist peroxid number lower meq kg content volatil halogen solvent lower mg kg lower mg kg solvent extinct coeffici lower treatment oil activ alumina higher point fact oil free fatti acid content express oleic acid passag activ alumina accord method set annex ix regul eec extinct coeffici higher neutral decolor laboratori accord method set annex xiii aforement regul characterist extinct coeffici higher extinct coeffici variat delta nm region higher higher gt tabl gt organolept characterist includ detect defect exceed limit accept panel test score lower accord annex xii regul eec content stigmastadien exceed mg kg ii purpos subhead virgin oil mean oliv oil characterist acid content express oleic acid exceed peroxid number exceed meq kg wax content exceed mg kg content volatil halogen solvent exceed mg kg exceed mg kg solvent extinct coeffici higher treatment oil activ alumina higher extinct coeffici variat delta nm region higher organolept characterist includ detect defect limit accept panel test score lower accord annex xii regul eec erythradiol uvaol content exceed ij content satur fatti acid posit triglycerid exceed sum transol isom exceed sum translinolen translinol isom exceed content stigmastadien exceed mg kg subhead cover oliv oil obtain treatment oliv oil fall subhead blend virgin oliv oil characterist acid content express oleic acid exceed wax content exceed mg kg extinct coeffici higher extinct coeffici variat aek nm region higher erythrodiol uvaol content exceed content satur fatti acid posit triglycerid exceed sum transol isom exceed sum translinol translinolen isom exceed purpos subhead quot crude oil quot mean oil oliv residu oil characterist acid content express oleic acid lower erythrodiol uvaol content lower content satur fatti acid posit triglycerid exceed sum transol isom exceed sum translinol translinolen isom exceed subhead cover oil obtain treatment oil fall subhead blend virgin oliv oil oil characterist oil refer addit note oil fall subhead content satur fatti acid posit triglycerid exceed sum transol isom lower sum translinol translinolen isom lower subhead cover residu result treatment fatti substanc oil iodin index determin accord method laid annex xvi regul eec lower higher residu result treatment fatti substanc oil iodin index higher lower peak area repres retent volum betasitosterol determin accord annex regul eec total sterol peak area analyt method determin characterist product refer laid annex regul eec