1、BRITISH STANDARD BS EN 13991:2003 Derivatives from coal pyrolysis Coal tar based oils: creosotes Specifications and test methods The European Standard EN 13991:2003 has the status of a British Standard ICS 71.100.50; 75.140 BS EN 13991:2003 This British Standard, was published under the authority of
2、 the Standards Policy and Strategy Committee on 22 October 2003 BSI 22 October 2003 ISBN 0 580 42788 9 National foreword This British Standard is the official English language version of EN 13991:2003. The UK participation in its preparation was entrusted to Technical Committee CII/56, Derivatives f
3、rom coal pyrolysis, 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 international or European publications referred to in this document may be found in the BSI C
4、atalogue under the section entitled “International Standards Correspondence Index”, or by using the “Search” facility of the BSI Electronic Catalogue or of British Standards Online. This publication does not purport to include all the necessary provisions of a contract. Users are responsible for its
5、 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 committee any enquiries on the interpretation, or proposals for change, and keep the UK interest
6、s 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 EN title page, pages 2 to 15 and a back cover. The BSI copyright notice displayed in this document indicates when the
7、document was last issued. Amendments issued since publication Amd. No. Date CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISCHENORM EN13991 August2003 ICS71.100.50;75.140 Englishversion DerivativesfromcoalpyrolysisCoaltarbasedoils:creosotes Specificationsandtestmethods Produitsdrivsdelapyrolyseduchar
8、bonHuilesde goudrondehouille:CrosotesSpcificationsetmthodes dessai DerivatederKohlenpyrolyseleausSteinkohlenteer: KreosotAnforderungenundPrfverfahren ThisEuropeanStandardwasapprovedbyCENon2July2003. CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingth
9、isEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoanyCENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherl
10、anguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustria,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Hungary,Iceland,Ireland,Italy,Luxembour
11、g,Malta,Netherlands,Norway,Portugal,Slovakia,Spain,Sweden,SwitzerlandandUn ited Kingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Brussels 2003CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwidef
12、orCENnationalMembers. Ref.No.EN13991:2003EEN13991:2003(E) 2 Contents page Foreword3 1 Scope 4 2 Normativereferences 4 3 Termsanddefinitions. .4 4 Sampling.4 5 Specificationsandtestmethods. .4 AnnexA (normative) Determinationofthecrystallizationtemperatureofcoaltaroil 6 AnnexB (normative) Determinati
13、onofthedistillationrangeofcoaltaroil8 AnnexC (informative) Warningtouse 14 Bibliography 15EN13991:2003(E) 3 Foreword Thisdocument(EN13991:2003)hasbeenpreparedbyTechnicalCommitteeCEN/TC317,“Derivativesfromcoal pyrolysis“,thesecretariatofwhichisheldbyIBN. ThisEuropeanStandardshallbegiventhestatusofana
14、tionalstandard,eitherbypublicationofanidenticaltextor byendorsement,atthelatestbyFebruary2004,andconflictingnationalstandardsshallbewithdrawnatthelatest byFebruary2004. AnnexesAandBarenormative.AnnexCisinformative. AccordingtotheCEN/CENELECInternalRegulations,thenationalstandardsorganizationsofthefo
15、llowing countriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic,Denmark,Finland, France,Germany,Greece,Hungary,Iceland,Ireland,Italy,Luxembourg,Malta,Netherlands,Norway,Portugal, Slovakia,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN13991:2003(E) 4 1Scope ThisEuropeanStandard
16、givesthespecificationsandthetestmethodsforcreosotesforindustrialwood preservation. Differentgradesofcreosoteareuseddependingonthedesiredpropertiesofthetreatedwood. WARNING TheuseofthisEuropeanStandardmayinvolvehazardousmaterials,operationsand equipment.Thisstandardcannotaddressallofthesafetyimplicat
17、ionsassociatedwithitsuse.Itisthe responsibilityoftheuserofthisstandardtoestablishappropriatehealthandsafetypracticesandassess theapplicabilityofregulatorylimitationspriortouse.ThewarningstousearecoveredinannexC. 2 Normativereferences ThisEuropeanStandardincorporatesbydatedorundatedreference,provisio
18、nsfromotherpublications.These normativereferencesarecitedattheappropriateplacesinthetextandthepublicationsarelistedhereafter.For datedreferences,subsequentamendmentstoorrevisionsofanyofthesepublicationsapplytothisEuropean Standardonlywhenincorporatedinitbyamendmentorrevision.Forundatedreferencesthel
19、atesteditionofthe publicationreferredtoapplies(includingamendments). EN10141,WoodpreservativesCreosoteandcreosotedtimberMethodsofsamplingandanalysis Part1:Procedureforsamplingcreosote . EN10143,WoodpreservativesCreosoteandcreosotedtimberMethodsofsamplingandanalysis Part3:Determinationofthebenzo a py
20、renecontentofcreosote . EN10144,WoodpreservativesCreosoteandcreosotedtimberMethodsofsamplingandanalysis Part4:Determinationofthewaterextractablephenolscontentofcreosote . EN12303:2000, CoaltarbasedoilsTerminology . BS144:1997,Coaltarcreosoteforwoodpreservation. ENISO2719, DeterminationofflashpointPe
21、nskyMartensclosedcupmethod(ISO2719:2002) ISO386, LiquidinglasslaboratorythermometersPrinciplesofdesign,constructionanduse. ISO760, DeterminationofwaterKarlFischermethod(Generalmethod). 3 Termsanddefinitions ForthepurposesofthisEuropeanStandard,thefollowingtermsanddefinitionsgiveninEN12303:2000apply.
22、 4Sampling Samplingofcreosotesandpreparationofsamples. SamplesfortheassessmentoftheparameterslistedinTable1shallbetakeninaccordancewithEN10141. 5 Specificationsandtestmethods SpecificationsforcreosotegradeA,B,CandtherelevanttestmethodsaregiveninTable1.EN13991:2003(E) 5 Table1Specificationsforcreosot
23、egradeA,BandC Parameters GradeA GradeB GradeC TestMethod Density(kg/m 3 )at20/4C 1,0401,150 1,0201,150 1,0301,170 BS144annexB Watercontent(m/m)% max.1 max.1 max.1 ISO760 a Crystallizationtemperature(C) max.23 max.23 max.50 AnnexA Waterextractablephenols(m/m)% max.3 max.3 max.3 EN10144 Insolublematte
24、rintoluene(m/m)% max.0.4 max.0.4 max.0.4 BS144annexG Boilingrange(volume)% annexB Distillateto235C max.10 max.20 Distillateto300C 2040 4060 max.10 Distillateto355C 5575 min.70 min.65 Benzo a pyrenecontent(mg/kg) max.500 max.50 max.50 EN10143 Flashpoint(C) min.61 min.61 min.61 ENISO2719 a Asanalterna
25、tive,thedistillationmethodofISO3733canbeused. NOTE1 GradeAisintendedfortreatmentoftimberbypressureimpregnation. GradeBisalsointendedforpressureimpregnation.IncontrasttogradeA,thedistillationresidueislowered inordertoreducethebenzoapyrenecontent.Itisespeciallysuitablefortreatmentofpolesforoverhead po
26、werandtelecommunicationlines,andforstructuraltimberswherebleedinginservicecanoccur. GradeCexcludesthelowerboilingfractionallowableintheothertypesofcreosoteandbecauseofthelow volatilityareductioninodourisachieved. NOTE2 Alltypesofcreosotesaresuitableforthehotandcoldopentankprocess. NOTE3 Creosoteinus
27、eshouldnotcontainmorethan3%ofwater. NOTE4 Thedensityisdeterminedatatemperatureabovethecrystallizationtemperature.Foreach degreeCelsiusabove20C,afixedvalueof0.7kg/m 3 isaddedtothedensityreading.EN13991:2003(E) 6 Annex A (normative) Determinationofthecrystallizationtemperatureofcoaltaroil A.1Scope Thi
28、smethoddescribestheprocedureforthedeterminationofthecrystallizationtemperatureofcoaltaroilandis applicabletocreosote,carbolineum,carbonblackfeedstock,fluxingoilsandothercoaltarbasedoils. A.2Sampling SamplingshallfollowtheproceduresdescribedinEN10141. A.3 Apparatus:anexampleoftheapparatusisgiveninFig
29、ureA.1 A.3.1 Porcelaindish,topdiameter(105 5)mm,height(60 5)mm,capacityca.300ml. A.3.2 Porcelaindish,flatshape,diameter(250 10)mm,capacityca.2000ml. A.3.3 Electricheatingplate,(5001000)W. A.3.4 Thermometer,(0100)C,graduatedin0,5CasdescribedinISO386. A.3.5 Metalsupportring. A.4Procedure Heatthesample
30、untilcompletelyfreeofcrystals.Thetemperatureshallbeatleast10Cabovethespecified maximumcrystallizationtemperature. Pour(150 5)mlofthesopreparedoilintothesmallporcelaindish. Placethedishwithoilonthesupportringinthelargerdishandfillthelatterwithwateratatemperature about10Clowerthanthespecifiedmaximumcr
31、ystallizationtemperature. Thewatersurfaceshallbe(10 2)mmabovetheoilsurfaceinthesmallerdish. Stirtheoilgentlywiththethermometer,theoilshallbecrystalfreeatthetemperatureindicatedinTable1. Ifitisrequiredtoknowthecrystallizationtemperature,repeatthedeterminationwithwateratalowertemperature. Usesomeicewh
32、ennecessary. Thetemperatureatwhichcrystalformationstartsisthecrystallizationtemperature.EN13991:2003(E) 7 A.5 Testreport Thetestreportshallatleastincludethefollowing: typeoftaroil; referencesofsample; thereferencetothisEuropeanStandard; thedateofdetermination; thenameoftheoperator; theresultofthedet
33、ermination,(PassorFail),thecrystallizationtemperatureifrequired,expressedindegrees Celsius; anyparticularpointsobservedinthecourseofthesamplingprocedureandthetestprocedure. Key 1 Coaltaroil 2W a t e r 3 Thermometer 4 Metalsupportring FigureA.1DeterminationofthecrystallizationtemperatureEN13991:2003(
34、E) 8 Annex B (normative) Determinationofthedistillationrangeofcoaltaroil B.1Scope Thismethodspecifiesrequirementsforcomponentsofanapparatususedinthedeterminationofthedistillation characteristicsofcoaltaroil.Thismethodisapplicabletocreosotes,carbolineum,carbonblackfeedstock,fluxing oilsandotherscoalt
35、arbasedoils. B.2Sampling SamplingshallfollowtheproceduresdescribedinEN10141. B.3Apparatus B.3.1 DistillationflaskasspecifiedinFigureB.1. B.3.2 CondensertubeasspecifiedinFigureB.2. B.3.3 DistillationcabinetasshowninFigureB.3. B.3.4 (0360)Cthermometer,graduatedin1Cdivisions,certifiedasinISO386. B.3.5
36、100mlmeasuringcylinder,scaleca.(140150)mm,calibratedin1mldivisions. B.3.6 Tripodorretortstandandring. B.3.7 (160x160)mmgauze,withoutasbestos. B.3.8 Corks,beads. B.3.9 Spiritlamporequivalentheatsource. B.3.10 Bunsenburner,orhotplate(700W,opencoiland25 B.4 Preparingthedistillation 100mlofpreparedoilar
37、eusedinthedistillation.Sinceabout2mlsticktotheinnerwallwhentheoilispouredout ofthemeasuringcylinder,102mlofoilaremeasuredoutandthenplacedinthedistillationflaskwithafewbeads. Thedistillationflaskissealedwithadrilledbungwhichholdsthethermometer.Careshallbetakentoensurethat thebungisfirmlyseatedandthet
38、hermometervertical.Thereshallbenooilontheneckoftheflaskoronthe thermometer.Thethermometershallreachintotheflasksothatthemercurybulbis12mmto13mmabovethe surfaceoftheliquid.Thethermometershallnotbemovedduringdistillation.Twogauzesupportsonthetripodare usedwhenheatingbygasorequivalent,andonegauzeontheh
39、otplatewhenheatingbyelectricity.Theclean measuringcylinderisplacedunderthecondensertubeoutlet.EN13991:2003(E) 9 B.5 Method(seeFiguresB.4B.5) Thedistillationflaskisfirstheatedgentlyusingasmallflameoralowheatsettingonthehotplate,inorderto preventbumpingandfoamingofthewaterwhichisalwayspresent.Whenthew
40、aterhasevaporated,theoilstarts toboilgently.Theheatshouldbecontrolledsuchthatthefirstdropofoilfallsintothemeasuringcylinderafter5to amaximumof15minutes.Thedistillationshouldthenproceedsothat12dropsfallintothemeasuringcylinder everysecond.Ifsoliddepositsforminthecondensertubetheyshouldbeliquefiedbyge
41、ntlyheating,e.g.byusing thespiritlamp.Assoonasthethermometershowsthetemperaturegiveninthespecification,theamountcollected inthemeasuringcylinderismeasured. Theamountsmeasuredinmlcorrespondtothepercentagesinvolume%. NOTE Forcomparisonanalyses,theeffectofbarometricpressureshouldbetakenintoconsideratio
42、n(cf.ASTMD24673). Precision Repeatability:2,0vol.%absolutefortheindividualfraction. Reproducibility:4,0vol.%absolutefortheindividualfraction. B.6 Testreport Thetestreportshallatleastincludethefollowing: typeoftaroil; referenceofsample; thereferencetothisEuropeanStandard; thedateofdetermination; then
43、ameoftheoperator; theresultofdetermination; anyparticularpointsobservedinthecourseofthesamplingprocedureandthetestprocedure.EN13991:2003(E) 10 Dimensionsinmillimeters Key a=200 5,0 e=10 0,5 b=135 1,5 f=22 1,0 c=93 1,5 =73 2,0 d=86 1,5 (indegrees) FigureB.1Distillationflask Dimensionsinmillimeters Key a
