EN ISO 1628-5:2015

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.Kunststoffe - Bestimmung der Viskosität von Polymeren in verdünnter Lösung durch ein Kapillarviscosimeter - Teil 5: Thermoplastische Polyester(TP) Homopolymere und Copolymere (ISO 1628-5:1998)Plastiques - Détermination de la viscosité des polymères en solution diluée à l'aide de viscosimètres à capillaires - Partie 5: Homopolymères et copolymères des polyesters thermoplastiques (TP) (ISO 1628-5:1998)Plastics - Determination of the viscosity of polymers in dilute solution using capillary viscometers - Part 5: Thermoplastic polyester (TP) homopolymers and copolymers (ISO 1628-5:1998)83.080.20PlastomeriThermoplastic materialsICS:Ta slovenski standard je istoveten z:EN ISO 1628-5:2015SIST EN ISO 1628-5:2015en,de01-junij-2015SIST EN ISO 1628-5:2015SLOVENSKI
STANDARD
EUROPEAN STANDARD NORME EUROPÉENNE EUROPÄISCHE NORM
EN ISO 1628-5
March 2015 ICS 83.080.20 English Version
Plastics - Determination of the viscosity of polymers in dilute solution using capillary viscometers - Part 5: Thermoplastic polyester (TP) homopolymers and copolymers (ISO 1628-5:1998)
Plastiques - Détermination de la viscosité des polymères en solution diluée à l'aide de viscosimètres à capillaires - Partie 5: Homopolymères et copolymères des polyesters thermoplastiques (TP) (ISO 1628-5:1998)
Kunststoffe - Bestimmung der Viskosität von Polymeren in verdünnter Lösung durch ein Kapillarviscosimeter - Teil 5: Thermoplastische Polyester(TP) Homopolymere und Copolymere (ISO 1628-5:1998) This European Standard was approved by CEN on 1 March 2015.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and United Kingdom.
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B-1000 Brussels © 2015 CEN All rights of exploitation in any form and by any means reserved worldwide for CEN national Members. Ref. No. EN ISO 1628-5:2015 ESIST EN ISO 1628-5:2015

AReference numberISO 1628-5:1998(E)INTERNATIONALSTANDARDISO1628-5Second edition1998-03-15Plastics — Determination of the viscosity ofpolymers in dilute solution using capillaryviscometers —Part 5:Thermoplastic polyester (TP) homopolymersand copolymersPlastiques — Détermination de la viscosité des polymères en solutiondiluée à l'aide de viscosimètres à capillaires —Partie 5: Homopolymères et copolymères des polyestersthermoplastiques (TP)SIST EN ISO 1628-5:2015

ISO 1628-5:1998(E)©
ISO 1998All rights reserved. Unless otherwise specified, no part of this publication may be reproducedor utilized in any form or by any means, electronic or mechanical, including photocopying andmicrofilm, without permission in writing from the publisher.International Organization for StandardizationCase postale 56 · CH-1211 Genève 20 · SwitzerlandInternetcentral@iso.chX.400c=ch; a=400net; p=iso; o=isocs; s=centralPrinted in SwitzerlandiiForewordISO (the International Organization for Standardization) is a worldwidefederation of national standards bodies (ISO member bodies). The work ofpreparing International Standards is normally carried out through ISOtechnical committees. Each member body interested in a subject for whicha technical committee has been established has the right to be representedon that committee. International organizations, governmental and non-governmental, in liaison with ISO, also take part in the work. ISOcollaborates closely with the International Electrotechnical Commission(IEC) on all matters of electrotechnical standardization.Draft International Standards adopted by the technical committees arecirculated to the member bodies for voting. Publication as an InternationalStandard requires approval by at least 75 % of the member bodies castinga vote.International Standard ISO 1628-5 was prepared by Technical CommitteeISO/TC 61, Plastics, Subcommittee SC 9, Thermoplastic materials.This second edition cancels and replaces the first edition(ISO 1628-5:1986), which has been technically revised.ISO 1628 consists of the following parts, under the general title Plastics —Determination of the viscosity of polymers in dilute solution using capillaryviscometers:—Part 1: General principles—Part 2: Poly(vinyl chloride) resins—Part 3: Polyethylenes and polypropylenes—Part 4: Polycarbonate (PC) moulding and extrusion materials—Part 5: Thermoplastic polyester (TP) homopolymers and copolymers—Part 6: Methyl methacrylate polymersAnnex A of this part of ISO 1628 is for information only.SIST EN ISO 1628-5:2015

INTERNATIONAL STANDARD
© ISOISO 1628-5:1998(E)1Plastics — Determination of the viscosity of polymers indilute solution using capillary viscometers —Part 5:Thermoplastic polyester (TP) homopolymers and copolymers1ScopeThis part of ISO 1628 specifies a method for the determination of the viscosity number (also referred toas “reduced viscosity”) of dilute solutions of thermoplastic polyesters (TPs) in certain specified solvents.The method is applicable to poly(ethylene terephthalate) (PET), poly(butylene terephthalate) (PBT),poly- (cyclohexylenedimethylene terephthalate) (PCT), and poly(ethylene naphthalate) (PEN), as well asto copolyesters and other polyesters, defined in ISO 7792-1, that are soluble in one of the specifiedsolvents under the specified conditions.The viscosity number is determined by the general procedure specified in ISO 1628-1, observing theparticular conditions specified in this part of ISO 1628.The determination of the viscosity number of a thermoplastic polyester provides a measure of therelative molecular mass of the polymer.2Normative referencesThe following standards contain provisions which, through reference in this text, constitute provisionsof this part of ISO 1628.
At the time of publication, the editions indicated were valid.
All standards aresubject to revision, and parties to agreements based on this part of ISO 1628 are encouraged toinvestigate the possibility of applying the most recent editions of the standards indicated below.Members of IEC and ISO maintain registers of current valid International Standards.ISO 1628-1:—1),
Plastics - Determination of the viscosity of polymers in dilute solution using capillaryviscometers - Part 1: General principles.ISO 3105:1994,
Glass capillary kinematic viscometers - Specifications and operating instructions.ISO 3451-2:1984,
Plastics - Determination of ash - Part 2: Polyalkylene terephthalates.ISO 7792-1:1997,
Plastics - Thermoplastic polyester (TP) moulding and extrusion materials - Part 1:Designation system and basis for specifications.________1)
To be published. (Revision of ISO 1628-1:1984)SIST EN ISO 1628-5:2015

ISO 1628-5:1998(E)© ISO23PrincipleThe times of flow of a solvent and a solution of resin in the solvent at a concentration of 0,005 g/ml aremeasured at 25 °C by conventional methods. The viscosity number is calculated from thesemeasurements and from the known concentration of the solution. Specific gravity difference and kineticenergy corrections are small in this method and are not applied.4SolventsWARNING - The solvents used are hazardous.
Avoid contact with the skin and inhalation of thevapours.4.1Phenol/1,2-dichlorobenzeneWeigh out 1 part by mass of phenol (analytical grade) and dissolve in 1 part by mass of 1,2-dichlorobenzene (analytical grade). Work to an accuracy of 1 % or better in the weighings.4.2Phenol/1,1,2,2-tetrachloroethaneWeigh out 6 parts by mass of phenol (analytical grade) and dissolve in 4 parts by mass of 1,1,2,2-tetrachloroethane (analytical grade), or weigh out 1 part by mass of phenol and dissolve in 1 part bymass of 1,1,2,2-tetrachloroethane. Work to an accuracy of 1 % or better in the weighings.4.3o-Chlorophenol, analytical grade.4.4m-Cresol, meeting the following specifications:appearance:
clear and colorless;m-cresol content:
99 % (m/m) min.;o-cresol content:
0,3 % (m/m) max.;water content:
0,1 % (m/m) max.NOTE - A solvent of the required purity can be obtained by distillation of chemically pure m-cresol,preferably in vacuo, pressure compensation being effected with nitrogen in order to avoid oxidation.The purity of the solvent may be checked by gas chromatography.4.5Dichloroacetic acid, analytical grade.4.6Phenol/2,4,6-trichlorophenolWeight out 6 parts by mass of phenol (analytical grade) and dissolve in 4 parts by mass of 2,4,6-trichlorophenol (analytical grade).NOTE - 2,4,6-trichlorophenol of the required purity can be obtained by distillation of chemically pure2,4,6-trichlorophenol.4.7Storage of the solventsProtect the solvents from light by storing them, for example, in stoppered brown-glass bottles.SIST EN ISO 1628-5:2015

© ISOISO 1628-5:1998(E)35Apparatus5.1Mill, to reduce the sample to a grain size of about 0,5 mm.5.2Volumetric flask, of capacity 100 ml, fitted with a ground-glass stopper.5.3 Conical flask, of capacity 150 ml, fitted with a ground-glass stopper.5.4Burette, graduated in divisions of 0,1 ml.5.5Steam bath, or other means to heat the contents of a flask to 90 to 100 °C.5.6Oil bath, capable of being controlled at 135 to 140 °C, or other means to heat the contents of a flaskto that temperature range.5.7Magnetic stirrer, or other equipment to continuously agitate the contents of a stoppered flask.5.8Thermostatic bath, capable of being maintained at 25 + 0,05 °C.5.9Viscometer, suspended-level Ubbelohde type, size No. 1B, 1C or 2, in accordance with ISO 3105.Other types of viscometer listed in ISO 3105 may be used, provided that the results are equivalent tothose of the Ubbelohde viscometers specified above.
However, in cases of dispute, Ubbelohdeviscometers shall be used.5.10Stainless-steel sieve, with a nominal aperture size of 63 to 90 µm, or sintered-glass filter funnelwith 40 to 100 µm pore diameter.5.11Analytical balance, accurate to 0,1 mg.5.12Stopwatch, accurate to 0,1 s.5.13Vacuum dryer, capable of being maintained at about 130 °C under vacuum.6Solvent and solution6.1Selection of the solvent6.1.1The value of the viscosity number of a saturated polyester depends on the solvent used. Sixdifferent solvents are described in this part of ISO 1628:
phenol/1,2-dichlorobenzene (4.1),phenol/1,1,2,2-tetrachloroethane (4.2), o-chlorophenol (4.3), m-cresol (4.4), dichloroacetic acid (4.5) andphenol/2,4,6-trichlorophenol (4.6).The flow times of the solvents shall be determined at least once each day that they are used (see 7.2). Ifthe flow time of a solvent differs by more than 1 % from the initial value at the time of preparation, thesolvents shall be discarded and fresh solvent prepared.The solvent or solvents to be used for a particular saturated polyester are specified below.6.1.2For PET, use phenol/1,2-dichlorobenzene (50/50), phenol/1,1,2,2-tetrachloroethane (50/50 or60/40), o-chlorophenol or dichloroacetic acid as solvent.SIST EN ISO 1628-5:2015

ISO 1628-5:1998(E)© ISO4NOTE - Equations for the interconversion of viscosity number determined in these four solvents arepresented in annex A, subclause A.3.1.6.1.3For PBT and corresponding copolyesters, use phenol/1,1,2,2-tetrachloroethane (50/50 or 60/40),o-chlorophenol, m-cresol, phenol/1,2-dichlorobenzene (50/50) or dichloroacetic acid as solvent.NOTE - Equations for the interconversion of viscosity number determined in these four solvents arepresented in annex A, subclause A.3.2.6.1.4For PCT, use phenol/1,1,2,2-tetrachloroethane (60/40) as solvent.6.1.5For amorphous PEN, use phenol/1,1,2,2-tetrachloroethane (60/40) as solvent and for crystallinePEN use phenol/2,4,6-trichlorophenol (60/40).6.1.6For other TP homopolymers and copolymers, m-cresol is the recommended solvent.6.2Determination of inorganic materials or other additives in the sampleContents of inorganic materials or other additives exceeding 0,5 % (m/m) each shall be taken intoaccount in the preparation of the test solution (6.4).6.2.1Determination of the content of inorganic materialsIf the sample contains inorganic materials, such as fillers or glass fibres, determine the content inaccordance with ISO 3451-2.6.2.2Determination of the content of other additivesIf the sample contains other additives, such as polyalkenes or flame retardants, determine the content inan appropriate way.
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