BS ISO 14714-2001 Essential oils and aromatic extracts - Determination of residual benzene content《香精油和芳族萃取物 残留苯含量测定》.pdf

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1、BRITISH STANDARD BS ISO 14714:1998 Essential Oils and aromatic extracts Determination of residual benzene content ICS 71.100.60; 71.040.40 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS ISO 14714:1998 This British Standard, having been prepared under the direction of the Co

2、nsumer Products and Services Sector Committee, was published under the authority of the Standards Committee and comes into effect on 15 September 2001 BSI 08-2001 ISBN 0 580 38315 6 National foreword This British Standard reproduces verbatim ISO 14714:1998 and implements it as the UK national standa

3、rd. The UK participation in its preparation was entrusted to Technical Committee AW/54, Essential Oils, which has the responsibility to: A list of organizations represented on this committee can be obtained on request to its secretary. Cross-references The British Standards which implement internati

4、onal or European publications referred to in this document may be found in the BSI Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” facility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include

5、all the necessary provisions of a contract. Users of British Standards are responsible for their correct application. Compliance with a British Standard does not of itself confer immunity from legal obligations. aid enquirers to understand the text; present to the responsible international/European

6、committee any enquiries on the interpretation, or proposals for change, and keep the UK interests informed; monitor related international and European developments and promulgate them in the UK. Summary of pages This document comprises a front cover, an inside front cover, the ISO title page, the IS

7、O foreword page, pages 1 to 5 and a back cover. The BSI copyright date displayed in this document indicates when the document was last issued. Amendments issued since publication Amd. No. Date CommentsA Referencenumbe r ISO14714:1998 (E) INTERNATIONAL STANDARD ISO 14714 Firstedition 19980801 Essenti

8、aloilsandaromaticextracts Determinationofresidualbenzenecontent HuilesessentiellesetextraitsaromatiquesDterminationdelateneuren benznersiduelISO14714:1998(E) OSI8991 Allirthgsserevr.delnUesstoiwrehsescepifi,detraponfothislbupictainomayebcudorperde turoziliynanidefoybromrynasnaem,celetrcinocemrocinah

9、a,lcniltohpgniducoypognidna .rehsilbupehtmorfgnitirwninoissimreptuohtiw,mliforcim noitazidradnatSrofnoitazinagrOlanoitanretnI 65elatsopesaC 02evneG1121HC dnalreztiwS tenretnI hc.osiosi dnalreztiwSnidetnirP ii Foreword ISO(theInternationalOrganizationforStandardization)isaworldwide federationofnation

10、alstandardsbodies(ISOmemberbodies).Theworkof preparingInternationalStandardsisnormallycarriedoutthroughISO technicalcommittees.Eachmemberbodyinterestedinasubjectforwhich atechnicalcommitteehasbeenestablishedhastherighttoberepresented onthatcommittee.Internationalorganizations,governmentalandnon gove

11、rnmental,inliaisonwithISO,alsotakepartinthework.ISO collaboratescloselywiththeInternationalElectrotechnicalCommission (IEC)onallmattersofelectrotechnicalstandardization. DraftInternationalStandardsadoptedbythetechnicalcommitteesare circulatedtothememberbodiesforvoting.PublicationasanInternational St

12、andardrequiresapprovalbyatleast75%ofthememberbodiescasting avote. InternationalStandardsaredraftedinaccordancewiththerulesgivenin theISO/IECDirectives,Part3. InternationalStandardISO14714waspreparedbyTechnicalCommittee ISO/TC54, Essentialoils . AnnexAofthisInternationalStandardisforinformationonly.I

13、NTERNATIONALSTANDARD OSI ISO14714:1998(E) 1 EssentialoilsandaromaticextractsDeterminationofresidual benzenecontent 1Scope ThisInternationalStandarddescribesamethodfordeterminingtheresidualtracesofbenzeneinessentialoilsand aromaticextracts,usingstaticheadspacegaschromatography. Itappliestoresidualcon

14、tentsofaround10 310 26 (10ppm)intheanalysedproduct. 2Normative references Thefollowingnormativedocumentscontainprovisionswhich,throughreferenceinthistext,constituteprovisionsof thisInternationalStandard.Fordatedreferences,subsequentamendmentsto,orrevisionsof,anyofthese publicationsdonotapply.However

15、,partiestoagreementsbasedonthisInternationalStandardareencouragedto investigatethepossibilityofapplyingthemostrecenteditionsofthenormativedocumentsindicatedbelow.For undatedreferences,thelatesteditionofthenormativedocumentreferredtoapplies.MembersofISOandIEC maintainregistersofcurrentlyvalidInternat

16、ionalStandards. ISO356, EssentialoilsPreparationoftestsamples. ISO7609, EssentialoilsAnalysisbygaschromatographyoncapillarycolumnsGeneralmethod. 3Principle Analysisbygaschromatographyofthestaticheadspaceonacapillarycolumn,eitherbyflameionizationdetector orbydetectionbymeansofmassspectrometry. Determ

17、inationofresidualbenzenecontentusingexternalstandardmethod(bycalibration). 4Reagents 4.1Referencesubstance :benzene,ofminimumpurity99%,asdeterminedbygaschromatography. 4.2Diethylphthalate ,freefromanytracesofbenzene,tobeverifiedundertestconditions.ISO14714:1998(E) OSI 2 5Apparatus 5.1Chromatograph,r

18、ecorderandintegrator SeeISO7609. 5.2 Capillarycolumn ,withthefollowingcharacteristics: length:30mto60m; internaldiameter:0,20mmto0,5mm; stationaryphase:methylsiliconetypeisrecommended. 5.3Flameionizationdetector or massdetector 5.4Headspacesamplingdevice ,fortheinjectionofheadspacevapours,comprising

19、either5.4.1or5.4.2. 5.4.1Gassyringesystem (manual),withleaktightlocks. 5.4.2Automaticinjectorequipment 6 Preparationoftestsample SeeISO356. 7Operating conditions 7.1 Chromatographicoperatingconditions 7.1.1 Injectortemperatureshallbe150 C. 7.1.2 Oventemperatureshallbemaintainedconstantatbetween40 Ca

20、nd60 Cfor15min,followedbyrapid temperatureprogrammingtoeluteanylessvolatileproduct. 7.1.3 Temperatureofflameionizationdetectorshallbebetween 200 Cand250 C. 7.1.4 Forflowrateofcarriergasandauxiliarygases,seeISO 7609. 7.2 Operatingconditionsforheadspacesamplingdevice 7.2.1 Thesampleshallbethermostatte

21、datatemperatureofbetw een70 Cand75 C. 7.2.2 Thistemperatureshallbemaintainedforaminimumof30min. 8 Quantitativeanalysismethod 8.1 Externalcalibrationcurve 8.1.1 Preparationofstandardsolutions Weighingtothenearest0,0001g,prepareastocksolutionofbenzeneinthediethylphthalate(4.2)containinga massfractiono

22、fbenzeneof1%.Bymeansofsuccessivegravimetricdilutions,preparearangeofstandardOSI ISO14714:1998(E) 3 solutionscontainingamassfractionofbenzeneofbetween1 310 26 and25 310 26 (1ppmand25ppm);i.e. 25 310 26 ,10 310 26 ,5 310 26 and1 310 26 (25ppm,10ppm,5ppmand1ppm). 8.1.2 Injectionofvapourphaseofstandards

23、olutions Thetestspecimenisplacedintheheadspacesamplingflask(5.4)andshallbe: identicalinallcases(calibrationandquantitativeanalysis); betweenonetenthandonehalfofthetotalvolumeoftheflask. 8.1.3 Plottingtheexternalcalibrationcurve Recordtheareasofthebenzenemarkersobtainedforthesuccessiveinjectionsintot

24、heheadspaceofthestandard solutions.Plotthecurveoftheareasasafunctionoftheconcentrations. 8.1.4 Validationoftheexternalcalibrationcurve Beforeeachanalysis,validatethecalibrationcurvebypreparing,byweighingafresh,abenzenesolutioncontaining amassfractionofbetween0and25 310 26 (25ppm).Injectionofthevapou

25、rphaseofthisvalidationsolution underthesameconditionsasusedforcalibrationshallgiveapointwhichisonthecalibrationcurve. Ifnot,itisnecessarytocarryoutacompletedeterminationofanewcalibrationcurve,withnewweighingandnew validation. 8.2Quantitative analysis 8.2.1Sample preparation Thetestspecimenofthesampl

26、eintheheadspaceflaskshallbeidenticaltotheoneusedforcalibration.Inthecase ofcontentsgreaterthanthefieldofthecalibrationcurve,carryoutadilutioninthesamesolvent. 8.2.2 Injectionofthesample Proceedinthesamewayasdescribedin8.1.2. 8.2.3 Determinationoftheresidualbenzenecontent Determinethebenzenecontentus

27、ingthecalibrationcurveplottedin8.1toreadoffthebenzenecontent correspondingtotheareaofthesampleanalysis,takingintoaccountanydilution. Ifamassspectrometerisused,theanalyticalmethodisthesame.Carryoutthecalibrationandquantitative analysisatleastonion78,visualizingthespectruminthechromatographicretention

28、zoneofthebenzene. NOTEUseofthemassdetectorisrecommendedifthereareproblemswiththeseparationoridentificationofthebenzene. 9Accuracy 9.1Interlaboratory test Aninterlaboratorytestorganizedin1991withtheparticipationofsevenlaboratoriesgavetheresultsshownin annexA,forinformationpurposes. 9.2Repeatability T

29、hedifferencebetweentwoindividualindependenttestresults,obtainedusingthesamemethodonanidentical materialsubjectedtothetestinthesamelaboratorybythesameoperatorusingthesameapparatusandwithina shorttimeinterval,willinnotmorethan5%ofcasesbegreaterthan6,5%.ISO14714:1998(E) OSI 4 9.3Reproducibility Thediff

30、erencebetweentwoindividualtestresults,obtainedusingthesamemethodonanidenticalmaterial undergoingthetestindifferentlaboratorieswithdifferentoperatorsusingdifferentapparatus,willinnotmorethan 5%ofcasesbegreaterthan13,50%. 10Test report SeeISO7609.OSI ISO14714:1998(E) 5 AnnexA (informative) Resultsofin

31、terlaboratorytests TableA.1 Valuesshouldbemultipliedby10 -6 (ppm) Numberof measurements Laboratories 123456 a) 7 7 7 6 6 5 5 5 5 4 2 1 1 _ 54 9,52 9,97 10,13 10,16 10,58 10,58 9,68 9,54 10,20 10,30 10,30 10,00 10,40 10,10 10,60 10,60 10,60 9,60 9,60 9,20 9,20 8,80 9,20 9,00 8,80 8,70 8,80 9,20 9,20

32、10,00 11,00 10,80 11,10 10,40 11,30 11,00 10,00 10,50 9,20 9,90 9,30 9,90 9,50 10,40 10,40 10,20 10,30 10,10 10,40 9,90 9,60 10,30 10,20 9,80 Results Minimum: Maximum: Mean: 9,52 10,58 10,02 10,00 10,60 10,34 8,70 9,60 9,11 10,00 11,30 10,68 9,20 9,90 9,58 9,50 10,40 9,95 9,60 10,40 10,12 Minimumdev

33、iation: Maximumdeviation: Maximum relativedeviation: 0,50 0,56 5,59% 0,34 0,26 3,33% 0,41 0,49 5,40% 0,68 0,62 6,35% 0,38 0,33 3,92% 0,45 0,45 4,52% 0,52 0,28 5,14% Variance: Repeatability standarddeviation: 0,18 0,42 0,05 0,22 0,09 0,30 0,23 0,48 0,14 0,38 0,41 0,64 0,07 0,27 Minimum: 8,70 Maximum:

34、11,30 Mean: 9,95 Minimumdeviation: 1,25=12,55% Maximumdeviation: 1,35=13,58% Variance: 0,41 Reproducibilitystandarddeviation:0,64 a)Thevaluesshownaretheminimaandmaximaofthesevenmeasurements.BS ISO 14714:1998 BSI 389 Chiswick High Road London W4 4AL BSI British Standards Institution BSI is the indepe

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