1、Designation: D4603 18Standard Test Method forDetermining Inherent Viscosity of Poly(EthyleneTerephthalate) (PET) by Glass Capillary Viscometer1This standard is issued under the fixed designation D4603; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope*1.1 This test method is for the determination of the inherentviscosity of poly(ethylene te
3、rephthalate) (PET) soluble at0.50 % concentration in a 60/40 phenol/1,1,2,2-tetrachloroethane solution by means of a glass capillary vis-cometer. Highly crystalline forms of PET that are not soluble inthis solvent mixture will require a different procedure.1.2 The inherent viscosity values obtained
4、by this testmethod are comparable with those obtained using differentialviscometry described in Test Method D5225.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafet
5、y concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.Specific hazards statements are given in Section 8.1.4.1 War
6、ningMercury has been designated by manyregulatory agencies as a hazardous material that can causeserious medical issues. Mercury, or its vapor, has beendemonstrated to be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercuryand mercury containing products. See
7、the applicable productSafety Data Sheet (SDS) for additional information. Usersshould be aware that selling mercury and/or mercury contain-ing products into your state or country may be prohibited bylawNOTE 1This standard and ISO 1628-5 address the same subjectmatter, but differ in technical content
8、. This ISO standard gives an optionof solvents for PET. Solvent specified in this ASTM test method is one ofthe options in the ISO method. ISO also uses Type 1C Ubbelohdeviscometer, rather than the 1B, and reports viscosity number, rather thaninherent viscosity.1.5 This international standard was de
9、veloped in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced D
10、ocuments2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D446 Specifications and Operating Instructions for GlassCapillary Kinematic ViscometersD1972 Practice for Generic Marking of Plastic Products(Withdrawn 2014)3D
11、5225 Test Method for Measuring Solution Viscosity ofPolymers with a Differential ViscometerE2251 Specification for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision LiquidsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE2935 Practice for Co
12、nducting Equivalence Testing inLaboratory ApplicationsIEEE/ASTM SI-10 Practice for Use of the InternationalSystem of Units (SI)2.2 ISO Standard:ISO 1628-5 Determination of the Viscosity of Polymers inDilute Solution Using Capillary ViscometersPart 5:Thermoplastic Polyester (TP) homopolymers and Copo
13、-lymers.42.3 NIST Standard:C 602 Testing of Glass Volumetric Apparatus51This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods(D20.70.05).Current edition approved May 1, 2018. Published June 2018. Orig
14、inallyapproved in 1986. Last previous edition approved in 2011 as D4603 03(2011)1.DOI: 10.1520/D4603-18.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standard
15、s Document Summary page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.4Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.5Available from National Institute of Standard
16、s and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international stan
17、dard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.13. Te
18、rminology3.1 Units, symbols, and abbreviations used in this testmethod are those recommended in Practice IEEE/ASTMSI-10.3.2 Definitions of Terms Specific to This Standard:3.2.1 inherent viscosity (also known as the logarithmicviscosity number)defined by the equation given in 11.1.3.2.2 PETas outline
19、d in Practice D1972. The PET acro-nym may be used to avoid trademark infringement and tocomply with various state or federal laws.4. Summary of Test Method4.1 The inherent viscosity is determined by measuring theflow time of a solution of known polymer concentration andthe flow time of the pure solv
20、ent in a capillary viscometer at afixed temperature. The inherent viscosity value is calculatedfrom the flow time values.5. Significance and Use5.1 The inherent viscosity is relatable to the compositionand molecular weight of a polyester resin. It must be controlledso that the processability and end
21、 properties of the resin remainin a desired range.6. Apparatus6.1 Cannon Ubbelohde Type 1B Viscometer, as described inSpecifications and Operating Instructions D446.6.2 Viscometer Holder.6.3 Electric Timer, readable to 0.1 s, as described in TestMethod D445.6.4 Constant Temperature Bath, control lab
22、el at 30C(86F) 6 0.01C (0.02F).6.5 Kinematic Viscosity Thermometer ASTM 118 (for use at30C), conforming to Specification E2251. Thermometricdevices such as liquid-in-glass thermometers, resistance tem-perature detectors, thermistors and thermocouples with equalor better accuracies within the tempera
23、ture range involved,may be used.6.6 Temperature Controllable Magnetic Stirring Hot Plate.6.7 TFE-Fluorocarbon Plastic-Coated Stirring Bars and aMagnetic Bar Retriever.6.8 Volumetric Flasks and Stoppers, 50-mL capacity, con-forming to the standards of accuracy in NIST Circular No.C 602.6.9 Analytical
24、 Balance, with readout to 0.0001 g.6.10 Borosilicate Funnels.6.11 Stainless Steel Filter Screening, 325-mesh or finer.6.12 Aspirator.6.13 Wiley Mill Grinder, with 20-mesh stainless steelscreen.6.14 Drying Oven, for equipment.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shal
25、l beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Societywhere such specifications are available.6Other grades arepermitted to be used, providing it is first ascerta
26、ined that thereagent is of sufficiently high purity to permit its use withoutlessening the accuracy of the determination.7.2 Phenol/1,1,2,2-tetrachloroethane Solution, 60/40weight % mixture (0.5 % moisture maximum, protected in sucha manner as to maintain this maximum level). Protect PETagainst the
27、degradation which has been found to occasionallyoccur during the heating stage in 10.3 through the addition ofa hydrogen chloride scavenger to the solvent, such as 0.2weight % n-octyl-bis-(isoethyl mercaptoacetate).77.3 Reagent Grade Methylene Chloride and Acetone, rins-ing solvents.7.4 Chromic Acid
28、, cleaning solution.8. Hazards8.1 The solvent used in this procedure is a mixture of 60weight % phenol and 40 weight % 1,1,2,2-tetrachloroethane.Both compounds and the mixture are toxic and require care inhandling. Make reference to the material safety data sheetsavailable from the suppliers of thes
29、e compounds for dealingwith the hazards they present. In addition to using a hood foradequate ventilation in handling these materials, protectionagainst skin contact is essential.8.2 Obtain the material safety data sheets for methylenechloride, acetone, and the chromic acid solution used forcleaning
30、 the testing equipment from their suppliers. Consultthe material safety data sheets before using the materials.9. Conditioning9.1 If the sample of PET contains 0.5 % or more of inertmaterial such as titanium dioxide or glass fiber, determine theamount of inert material accurately by a procedure suit
31、able forthe type of inert material present.9.2 If the sample is suspected of being wet (in excess of themoisture level derived from exposure to ambient humidityconditions), dry the sample in an oven for a suggestedminimum of2hat65C (149F) 6 5C (9F) or until aconstant weight of 6 0.1 % is reached. Mo
32、isture picked upfrom ambient humidity will weigh 0.30 % and is negligible inthis procedure. (See Note 2.)NOTE 2Use a suitable technical method to determine moisturecontent.6Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the t
33、esting of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.7Available from M inherent viscosity; poly-(e
34、thylene terephthalate); PET; solution viscositySUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard since the last issue(D4603 03(2011)1) that may impact the use of this standard. (May 1, 2018)(1) Permissive language sweep entire document.(2) Updated ISO e
35、quivalency statement in Note 1.(3) Added Mercury thermometer caveat to 1.4.1.(4) Replaced E1 reference with E2251 in 2.1 and 6.5.(5) Updated Section 13 precision and bias language.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item m
36、entionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committ
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38、ing of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, P
39、O Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org). Permission rights to photocopy the standard may also be secured from the Copyright Clearance Center, 222Rosewood Drive, Danvers, MA 01923, Tel: (978) 646-2600; http:/ data are available from ASTM Headquarters. Request RR:D20-1132.D4603 184
