commiss regul ec march amend regul eec determin commun method analysi wine commiss european commun regard treati establish european commun regard council regul ec common organis market wine amend regul ec subparagraph articl thereof annex commiss regul eec amend regul ec describ analysi method analysi method malic acid suitabl measur low level found wine develop valid recognis intern criteria intern vine wine offic adopt descript method gener assembl june method determin carbon isotop ratio wine ethanol ethanol obtain ferment grape must concentr grape must rectifi concentr grape must develop valid recognis intern criteria intern vine wine offic adopt descript method gener assembl method ensur control wine qualiti authent prevent disput caus applic accur test method enrich mixtur sugar origin acidif wine malic acid exist method dosag malic acid annex regul eec supplement descript procedur determin low level descript isotop method carbon ethanol ad measur provid regul accord opinion manag committe wine adopt regul articl annex regul eec amend chapter quot malic acid quot point replac annex hereto chapter annex ii hereto ad articl regul enter forc seventh dai public offici journal european union regul bind entireti directli applic member state brussel march commiss franz fischler member commiss oj oj oj oj annex quot dosag malic acid malic acid wine low level field applic method appli dosag enzymat mean malic acid wine level mg principl principl method point format nadh introduct cuvett mg malic acid proport quantiti malat present measur basi increas absorb wavelength nm reagent malic acid solut reagent point apparatu apparatu point prepar sampl point procedur procedur point introduct measur cuvett mg malic acid introduct ml malic acid solut displac equival volum water valu obtain decreas mg intern valid tabl summaris intern valid file method determin dosag malic acid addit mg isom gt tabl gt quot annex ii quot determin isotop mass spectrometri ratio wine ethanol ethanol obtain ferment must concentr must rectifi concentr must field applic method enabl measur isotop ratio wine ethanol ethanol obtain ferment product vine must concentr must rectifi concentr must refer standard iso accuraci trueness precis measur method result basic method determin repeat reproduc standard measur method pdb vienna pee dee belemnit rpdb method annex regul detect enrich grape must concentr grape must rectifi concentr grape must wine applic nuclear magnet reson deuterium snif nmr term definit ratio carbon carbon isotop sampl carbon content express part permil snif nmr fraction natur isotop studi nuclear magnet reson pdb vienna pee dee belemnit pdb primari refer materi measur natur variat carbon isotop content consist calcium carbon cretac belemnit guard pee dee format south carolina usa isotop ratio rpdb pdb reserv exhaust long time remain primari refer express natur variat carbon isotop content refer materi intern atom energi agenc iaea vienna austria calibr isotop indic natur occur carbon convention express relat pdb mass charg ratio principl photosynthesi assimil carbon dioxid plant occur principl form metabol metabol calvin cycl metabol hatch slack photosynthesi mechan present type isotop fraction product plant sugar alcohol deriv ferment higher level carbon similar product plant plant includ vine sugar beet belong group sugar cane maiz belong group measur carbon content enabl detect evalu sugar origin sugar cane maiz isoglucos ad grape product grape must wine inform carbon content combin obtain snif nmr enabl ad quantiti mixtur sugar alcohol deriv plant determin carbon content determin carbon dioxid produc complet combust sampl abund principl isotopom mass result combin isotop determin ionic current measur collector mass isotop spectromet contribut isotopom disregard low level ionic current correct contribut calcul current intens measur take rel abund account craig correct comparison refer calibr intern refer pdb permit calcul carbon content rel scale reagent materi consum depend apparatu point laboratori system gener base element analys system equip introduct sampl seal metal capsul inject liquid sampl septum syring depend type instrument refer materi reagent consum refer materi iaea gt tabl gt irmm geel institut refer materi measur gt tabl gt standard work sampl ratio calibr intern refer materi indic list consum continu flow system helium analysi ca oxygen analysi ca carbon dioxid analysi secondari refer ga carbon content ca oxid reagent furnac combust system copper oxid element analysi ca desicc elimin water produc combust anhydron element analysi magnesium perchlor ca apparatus equip water elimin system cryogen trap select permeabl capillari apparatu equip isotop ratio mass spectromet irm isotop ratio mass spectromet irm capabl determin rel content natur occur ga intern accuraci permil express rel point intern accuraci defin differ measur sampl mass spectromet measur isotop ratio gener equip tripl collector simultan measur intens isotop ratio mass spectromet equip dual inlet altern measur unknown sampl refer sampl integr system carri quantit combust sampl separ carbon dioxid combust product measur mass spectromet combust apparatu combust apparatu quantit convert ethanol carbon dioxid elimin combust product includ water isotop fraction apparatu continu flow system integr mass spectrometri apparatu point separ combust system point apparatu permit accuraci point continu flow system compris element analys ga chromatograph onlin combust system laboratori equip need system equip introduct sampl contain metal capsul calibr microsyring micropipett tip balanc μg accuraci tweezer encapsul tin capsul liquid sampl tin capsul solid sampl note order reduc risk evapor ethanol sampl absorb materi chromosorb mesh capsul verifi mean measur sampl signific quantifi carbon affect result laboratori equip need element analys equip liquid injector case combust chromatographi prepar system syring liquid flask equip airtight close system inert septa laboratori equip list exampl replac equip equival perform depend type combust mass spectrometri apparatu laboratori separ prepar system sampl carbon dioxid result combust sampl analys refer sampl collect bulb dual inlet spectromet isotop analysi combust apparatus literatur close combust system fill circul oxygen element analys helium oxygen flow seal glass bulb fill copper oxid oxid agent prepar sampl test ethanol extract wine isotop test carri distil wine point method snif nmr case grape must concentr grape must rectifi concentr grape must sugar ferment ethanol point method procedur step prepar carri signific ethanol loss evapor chang isotop composit sampl descript refer procedur gener ethanol sampl combust commerci autom combust system method ensur ethanol sampl convert carbon dioxid loss ethanol evapor prepar carbon dioxid isotop analysi experiment procedur base element analys place sampl capsul capsul tweezer prepar trai clean size capsul tweezer introduc amount liquid capsul micropipett note mg absolut ethanol mg distil alcohol strength obtain mg carbon quantiti distil calcul basi quantiti carbon sensit mass spectrometri apparatu close capsul tweezer capsul complet seal discard capsul prepar capsul prepar sampl place capsul place trai automat sampler element analys capsul carefulli identifi serial number systemat place capsul work refer begin end sampl seri regularli insert control sampl sampl seri check adjust element analysi mass spectrometri apparatu adjust temperatur element analys furnac helium oxygen flow optim combust sampl check element analysi mass spectrometri system leak check ionic current adjust mass spectromet measur ionic current check system control sampl start measur sampl carri seri measur sampl automat sampler element analys chromatograph introduc turn carbon dioxid sampl combust elut mass spectromet measur ionic current interfac comput record ionic current calcul sampl point calcul purpos method measur isotop ratio ofethanol extract wine product deriv grape ferment isotop ratiocan express deviat work refer isotop deviat carbon calcul delta scale thousand compar result obtain sampl measur work refer previous calibr basi primari intern refer pdb valu express relat work refer csam ref permil rsam rref rref rsam rref isotop ratio sampl carbon dioxid refer ga valu express relat pdb csam pdb permil csam ref cref pdb csam ref cref pdb cref pdb previous determin isotop deviat work refer pdb small variat occur measur line due instrument condit case valu sampl correct differ measur standard work sampl true previous calibr pdb comparison intern refer materi measur standard work sampl variat correct appli result obtain sampl assum linear standard work sampl measur begin end sampl seri correct calcul sampl linear interpol qualiti assur control check work refer differ permil admiss spectrometri apparatu set check adjust sampl check differ result capsul measur success permil final result sampl averag capsul deviat greater permil measur repeat check correct measur base ionic current proport quantiti carbon inject element analys standard condit ionic current constant sampl analys signific deviat indic ethanol evapor imperfect seal capsul instabl element analys mass spectromet perform characterist method accuraci initi collabor studi point carri distil alcohol vinou origin cane beet alcohol mixtur alcohol origin studi account distil procedur inform interlaboratori studi wine point seri profici test point isotop measur consid result show satisfactori condit measur snif nmr distil system produc signific variat determin wine ethanol accuraci paramet observ wine ident obtain joint studi distil point joint studi distil year interlaboratori test number laboratori number sampl sampl doubl blind comparison analyt ethanol gt tabl gt gt tabl gt interlaboratori studi wine alcohol year interlaboratori test number laboratori distil wine measur wine ethanol measur alcohol sampl number sampl white wine asv white wine asv alcohol strength analyt ethanol gt tabl gt distil system particip laboratori isotop determin carri singl laboratori number distil return particip reveal aberr valu valu differ significantli averag valu variat result compar repeat varianc sr joint studi distil point result exercis carri monitor profici perform isotop test decemb intern profici test determin isotop measur wine alcohol distil asv regularli organis result enabl particip laboratori check qualiti analys statist result permit appreci variat measur condit reproduc estim paramet varianc limit reproduc result obtain determin wine distil ethanol summaris tabl gt tabl gt number particip laboratori limit repeat reproduc basi data interlaboratori test tabl limit repeat reproduc establish method includ distil stage limit repeat limit reproduc quot