1、BRITISH STANDARD BS EN 13468:2001 Thermal insulating products for building equipment and industrial installations Determination of trace quantities of water soluble chloride, fluoride, silicate, sodium ions and pH The European Standard EN 13468:2001 has the status of a British Standard ICS 91.120.10
2、 91.100.60 NO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBS EN 13468:2001 This British Standard, having been prepared under the direction of the Engineering Sector Policy and Strategy Committee, was published under the authority of the Standards Policy and Strategy Committee
3、 on 09 November 2001 BSI 09 November 2001 ISBN 0 580 38620 1 National foreword This British Standard is the official English language version of EN 13468:2001. This British Standard, together with BS EN 13467:2001, BS EN 13469:2001, BS EN 13470:2001, BS EN 13471:2001 and BS EN 13472:2001, partially
4、supersedes BS 2972:1989. The UK participation in its preparation was entrusted by Technical Committee RHE/9, Thermal insulating materials, to Subcommittee RHE/9/4, Nomenclature and specifications, which has the responsibility to: A list of organizations represented on this subcommittee can be obtain
5、ed 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 Standards Catalogue under the section entitled “International Standards Correspondence Index”, or by using the “Find” fac
6、ility of the BSI Standards Electronic Catalogue. A British Standard does not purport to include 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 oblig
7、ations. aid enquirers to understand the text; present to the responsible European 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 d
8、ocument comprises a front cover, an inside front cover, the EN title page, pages 2 to 17 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 CommentsEUROPEANSTANDARD NORMEEUROPENNE EUROPISC
9、HENORM EN13468 September2001 ICS91.100.60 Englishversion Thermalinsulatingproductsforbuildingequipmentandindustrial installationsDeterminationoftracequantitiesofwatersoluble chloride,fluoride,silicate,sodiumionsandpH Produitsisolantsthermiquespourlquipementdubtiment etlesinstallationsindustriellesDt
10、erminationdesfaibles quantitsdionschlorure,fluorure,silicateetsodium solublesdansleauetmesuredupH WrmedmmstoffefrdieHaustechnikundfr betriebstechnischeAnlagenBestimmungdesGehaltsvon wasserlslichenChlorid,Fluorid,SilikatundNatrium IonenunddespHWertes ThisEuropeanStandardwasapprovedbyCENon18August2001
11、 CENmembersareboundtocomplywiththeCEN/CENELECInternalRegulationswhichstipulatetheconditionsforgivingthisEurope an Standardthestatusofanationalstandardwithoutanyalteration.Uptodatelistsandbibliographicalreferencesconcernings uchnational standardsmaybeobtainedonapplicationtotheManagementCentreortoany
12、CENmember. ThisEuropeanStandardexistsinthreeofficialversions(English,French,German).Aversioninanyotherlanguagemadebytra nslation undertheresponsibilityofaCENmemberintoitsownlanguageandnotifiedtotheManagementCentrehasthesamestatusasthe official versions. CENmembersarethenationalstandardsbodiesofAustr
13、ia,Belgium,CzechRepublic,Denmark,Finland,France,Germany,Greece, Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway,Portugal,Spain,Sweden,SwitzerlandandUnitedKingdom. EUROPEANCOMMITTEEFORSTANDARDIZATION COMITEUROPENDENORMALISATION EUROPISCHESKOMITEEFRNORMUNG ManagementCentre:ruedeStassart,36B1050Bru
14、ssels 2001CEN Allrightsofexploitationinanyformandbyanymeansreserved worldwideforCENnationalMembers. Ref.No.EN13468:2001EEN13468:2001(E) 2 Contents page Foreword .3 1 Scope4 2 Normativereferences 4 3 Termsanddefinitions . 4 4 Principle .4 5 Apparatus.4 6 Testspecimens 5 7 Procedure.6 8 Calculationand
15、expressionofresults . .9 9 Accuracyofmeasurement . 11 10 Testreport 11 AnnexA (normative) SpectrophotometricdeterminationoffluoridewithzirconiumSPADNS .13 AnnexB (informative) Generalinformationrelatedtotheuseofthisstandard.14 AnnexC (informative) Exampleofionchromatographyequipment .15 AnnexD (info
16、rmative) Exampleofborosilicateglassequipmenttoprepareleachingsolutionsfor thermalinsulatingproductsthatfloat . .16 Tables Table1Testtemperatureandleachingtime . 6 Table2 95%Confidenceintervalvalues . .11 Table3 Trueness .11EN13468:2001(E) 3 Foreword ThisEuropeanStandardhasbeenpreparedbyTechnicalComm
17、itteeCEN/TC88“Thermalinsulating materialsandproducts“,thesecretariatofwhichisheldbyDIN. ThisEuropeanStandardshallbegiventhestatusofanationalstandard,eitherbypublicationofan identicaltextorbyendorsement,atthelatestbyMarch2002,andconflictingnationalstandardsshallbe withdrawnatthelatestbyMarch2002. Thi
18、sEuropeanStandardisoneofaseriesofstandardswhichspecifytestmethodsfordetermining dimensionsandpropertiesofthermalinsulatingmaterialsandproducts.Itsupportsaseriesofproduct standardsforthermalinsulatingmaterialsandproductswhichderivefromtheCouncilDirectiveof21 December1988ontheapproximationoflaws,regul
19、ationsandadministrativeprovisionsoftheMember Statesrelatingtoconstructionproducts(Directive89/106/EEC)throughtheconsiderationoftheessential requirements. Thisstandardcontainsthefollowingnormativeannex: AnnexASpectrophotometricfluoridedeterminationofFluoridewithzirconiumSPADNS andthreeinformativeanne
20、xes: AnnexBGeneralinformationrelatedtotheuseofthisstandard AnnexCExampleofionchromatographyequipment AnnexDExampleofborosilicateglassequipmentforpreparationofleachingsolutionsforthermal insulatingproductsthatfloat ThisEuropeanStandardhasbeenpreparedforproductsusedtoinsulatebuildingequipmentand indus
21、trialinstallations,butitmayalsobeappliedtoproductsusedinotherareas. NoexistingEuropeanStandardissuperseded. ThisEuropeanStandardhasbeenpreparedunderamandategiventoCENbytheEuropean CommissionandtheEuropeanFreeTradeAssociation,andsupportsessentialrequirementsofEU Directive(s). AccordingtotheCEN/CENELE
22、CInternalRegulations,thenationalstandardsorganizationsofthe followingcountriesareboundtoimplementthisEuropeanStandard:Austria,Belgium,CzechRepublic, Denmark,Finland,France,Germany,Greece,Iceland,Ireland,Italy,Luxembourg,Netherlands,Norway, Portugal,Spain,Sweden,SwitzerlandandtheUnitedKingdom.EN13468
23、2001(E) 4 1 Scope Thisstandardspecifiestheequipmentandproceduresfordeterminingtracequantitiesofthewater solublechloride,fluoride,silicateandsodiumionsinanaqueousextractoftheproduct.Italsodescribes aprocedureforthedeterminationofthepHoftheaqueousextract.Thestandardisapplicabletothermal insulatingpro
24、ducts. NOTEThedeterminationoftheseparametersmayberelevantforthermalinsulatingproductsintendedfor applicationtostainlessausteniticsteelsurfaces.Thepresenceofchloride,fluoride,silicateandsodiumionsunder certainconditionsmayinfluencetheriskofstresscorrosioncracking.SeeinformativeannexBforfurtherinforma
25、tion . 2 Normativereferences ThisEuropeanStandardincorporates,bydatedorundatedreference,provisionsfromotherpublications. Thesenormativereferencesarecitedattheappropriateplacesinthetext,andthepublicationsarelisted hereafter.Fordatedreferences,subsequentamendmentstoorrevisionsofanyofthesepublications
26、applytothisEuropeanStandardonlywhenincorporatedinitbyamendmentorrevision.Thelatestedition ofthisundatedreferenceapplies(includingamendments). ISO101361, GlassandGlasswareAnalysesofextractsolutionsPart1:Determinationofsilicon dioxidebymolecularabsorptionspectrometry. ISO101362, GlassandGlasswareAnaly
27、sesofextractsolutionsPart2:Determinationofsodium oxideandpotassiumoxidebyflamespectrometricmethods. 3 Termsanddefinitions ThisEuropeanStandardcontainsnotermsanddefinitions. 4 Principle Testspecimensoftheinsulatingproductareboiledorheatedindeionizedwatertoleachoutsolubleions. Teststodeterminewatersol
28、ublechloride,fluoride,silicateandsodiumionsareperformedonaliquotsof thefilteredaqueousextract.ApHvalueisdeterminedononeofthealiquots. 5 Apparatus Allequipmentandworkinginstrumentsusedforthispurposemustbefreefromsolublechloride,fluoride, silicate,sodiumions,andgrease.Chloridefreesolventsshallbeusedto
29、cleanequipmentandworking instruments(avoidchlorinatedsolvents).Duringtheperformanceoftheanalyticprocedureextraneous sourcesoftheseionsshallbereducedoreliminated. 5.1 Preparationofaqueousextract 5.1.11000mlborosilicateglassflask; 5.1.2Watercondenser; 5.1.3Heater,complyingwiththerequirementsof7.2; 5.1
30、4Prewashedfilter,diameterofpores0,45 m; 5.1.5Corkborerhavingadiameterwhichenablestotakethespecifiedmassforthetestspecimen; 5.1.6Disposablegloves;EN13468:2001(E) 5 5.1.7Plasticbagorcontainer; 5.1.8Balance,permittingreadingto0,01g. 5.2 Analyses 5.2.1IonChromatographyequipment(IC).SeeinformativeannexC
31、forexampleofsuitableequipment; 5.2.2Titrationequipmentwithautomaticendpoint; 5.2.3AtomicAbsorptionSpectrophotometer(AAS); 5.2.4AtomicEmissionSpectrometerwithInductivelyCoupledPlasma(ICPAES); 5.2.5Spectrophotometer; 5.2.6pHmeter/millivoltmeter; 5.2.7Fluorideionselectiveelectrode. NOTEAnydeviceprovidi
32、ngthesameresultwithatleastthesameaccuracymaybeused. 5.3 Materials 5.3.1 deionizedwater,conductivitylessthan0,5 S/cm; 5.3.2 0,01Nsodiumcloride(NaCl); 5.3.3 0,01Nsilvernitrate(AgNO 3 ); 6 Testspecimens 6.1General Toensurethattheresultsarerepresentativeoftheproductcareshallbetakenthatthetestspecimens a
33、renotsubjectedtoanyoutsidecontamination. 6.2 Dimensionsoftestspecimens Takeouteachtestspecimenbyusingacorkboreratpositionsevenlydistributedoverthetotalsurfaceof afullsizeproduct.Toavoidcontaminationchloridefreeglovesmustbewornandthetestspecimenis placedinaclosedpolyethylenebag.Dependingontheproductf
34、amilytheweightofeachtestspecimen shallbeatleast7,5gor20g. 6.3 Numberoftestspecimens Thenumberoftestspecimensshallbeasspecifiedintherelevantproductstandard.Ifthenumberisnot specified,thenatleastthreetestspecimens(3weightsof7,5gor20g)shallbeused. NOTEIntheabsenceofaproductstandardoranyotherEuropeantec
35、hnicalspecificationthenumberofthetest specimensmaybeagreedbetweenparties. 6.4 Conditioningoftestspecimens Thetestspecimensshallbestoredforatleast6handnotmorethan24hat(235) C.Incaseofdis putetheyshallbestoredat(232) Cforthetimestatedintherelevantproductstandard.EN13468:2001(E) 6 7 Procedure 7.1 Testc
36、onditions Thetestshallbecarriedoutat(235) C. 7.2 Testprocedure 7.2.1 Preparationoftheleachingsolution Take(200,1)gor(7,50,05)gofthetestspecimen( m),asspecifiedintherelevantproductstandard andplaceitinthewidemouthglassflask.Add(4005)mldeionizedwater( V).Theflaskshallbeclosed withagroundinstopperandsh
37、akenuntilthetestspecimeniscompletelywettedandsubmerged.Ifthe testspecimenfloatsitshouldbeheldunderwater(example,seeinformativeannexD). Fixthewatercondensertotheflaskandelectricallyheatfor5minto10minuntiltheleachingsolution hasreachedthetesttemperature.Theleachingprocessshallbecontinued,underrefluxco
38、nditions,for thespecifiedtime. Dependingonthemaximumservicetemperaturespecifiedfortheproductthetesttemperatureand leachingtimeshallbechosenasspecifiedinTable1. Table1Testtemperatureandleachingtime Maximumservicetemperature C Testtemperature C Leachingtime h 100 (1001) 0,5 90to100 (901) 1,0 80to90 (8
39、01) 2,0 70to80 (701) 4,0 70 (601) 8,0 Removetheflaskwiththecondenser,fromtheheatandcoolfor10minto15minuntilthetemperature reachesroomtemperature,e.g.inawaterbath.Filtertheleachingsolution. Makea“blank“test,usingthesameprocedureasabove,butwithoutatestspecimenofinsulating product. Thefilteredsolutions
40、willsubsequentlybeusedfortheanalyses. NOTEOthertestmethodsthandecribedbelowmaybeusedifthesameresultwithatleastthesameaccuracyis obtained. 7.2.2 Chloridedetermination 7.2.2.1 General Oneofthefollowingmethodsshallbeusedonafreshaliquotofthefilteredsolution.Incaseofdispute themethoddecribedin7.2.2.2isth
41、ereferencemethod.Therepeatabilityofthemethodsiscalculatedas thestandarddeviationon10determinationstakenfromthesameleachingsolution.Thestandard deviationshallbesmallerthan0,5mg/kgforconcentrationssmallerthan8,3mg/kgandsmallerthan6% ofthemeanofthe10determinationsforconcentrationslargerthanorequalto8,3
42、mg/kg.EN13468:2001(E) 7 7.2.2.2 Ionchromatographicdetermination(IC) Theionchromatographicdeterminationofchlorideionsshallbecarriedoutinaccordancewiththe equipmentmanufacturersoperatinginstruction. 5mlofthefilteredsolutionisinjectedintothetestloopthroughadisposable,chloridefreefilter.The volumeofthet
43、estloopoftheICapparatusischosen(normally50 l). NOTEDependingonthekindofbindingand/orwaterproofingagent,mineralwoolproductsmayreleaseorganic contaminantsduringtheboilingprocesswhichmaycausepeaksthatareclosetothechloridepeaksintheion chromatogramme. AclearseparationoftestpeaksshallbeobtainedduringtheICdetermination. 7.2.2.3 AgNO 3 titration Thedeterminationofchlorideionsbypolarizationtitrationshallbeaccordingtothealternatingcurrentvol tagemethodwithamperometricindication. Precautionsshallbetakentoavoidinterferencefromotherions,e.g.fluoride. Thefollowingprocedureshallbeca
