1、Designation: D4603 03 (Reapproved 2011)1Standard 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
2、adoption or, in the 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.1NOTEReapproved with editorial change to 6.5 in November 2011.1. Scope1.1 This t
3、est method is for the determination of the inherentviscosity of poly(ethylene terephthalate) (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 mixtur
4、e will require a different procedure.1.2 The inherent viscosity values obtained 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 f
5、or informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to
6、use. Specific hazardsstatements are given in Section 8.NOTE 1This test method and ISO 1628-5 are similar but not techni-cally equivalent. This ISO standard gives an option of solvents for PET.Solvent specified in this ASTM test method is one of the options in theISO method. ISO also uses Type 1C Ubb
7、elohde viscometer, rather than the1B, and reports viscosity number, rather than inherent viscosity.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D446 Specifications and Operating Instruction
8、s for GlassCapillary Kinematic ViscometersD1972 Practice for Generic Marking of Plastic ProductsD5225 Test Method for Measuring Solution Viscosity ofPolymers with a Differential ViscometerE1 Specification for ASTM Liquid-in-Glass ThermometersIEEE/ASTM SI-10 Practice for Use of the InternationalSyste
9、m of Units (SI)E691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:ISO 1628-5 Determination of the Viscosity of Polymers inDilute Solution Using Capillary ViscometersPart 5:Thermoplastic Polyester (TP) homopolymers and Copo-lymers.32.3 NIS
10、T Standard:C 602 Testing of Glass Volumetric Apparatus43. Terminology3.1 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 numb
11、er)defined by the equation given in 11.1.3.2.2 PETas outlined 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 k
12、nown polymer concentration andthe flow time of the pure solvent in a capillary viscometer at afixed temperature. The inherent viscosity value is calculatedfrom the flow time values.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcom
13、mittee D20.70 on Analytical Methods(D20.70.05).Current edition approved Nov. 15, 2011. Published April 2012. Originallyapproved in 1986. Last previous edition approved in 2003 as D4603 03. DOI:10.1520/D4603-03R11E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM
14、 Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Available from Na
15、tional Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 The inherent viscosity is relat
16、able to the compositionand molecular weight of a polyester resin. It must be controlledso that the processability and end 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
17、 Holder.6.3 Electric Timer, readable to 0.1 s, as described in TestMethod D445.6.4 Constant Temperature Bath, control label at 30C(86F) 6 0.01C (0.02F).6.5 Kinematic Viscosity Thermometer ASTM 118 (for use at30C), conforming to Specification E1. Thermometric devicessuch as liquid-in-glass thermomete
18、rs, resistance temperaturedetectors, thermistors and thermocouples with equal or betteraccuracies within the temperature 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 F
19、lasks and Stoppers, 50-mL capacity, con-forming to the standards of accuracy in NIST Circular No.C 602.6.9 Analytical 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 st
20、eelscreen.6.14 Drying Oven, for equipment.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall 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 Chemica
21、l Societywhere such specifications are available.5Other grades arepermitted to be used, providing it is first ascertained 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 % m
22、ixture (0.5 % moisture maximum, protected in sucha manner as to maintain this maximum level). Protect PETagainst the 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
23、-bis-(isoethyl mercaptoacetate).67.3 Reagent Grade Methylene Chloride and Acetone, rins-ing solvents.7.4 Chromic Acid, 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 tox
24、ic and require care inhandling. Make reference to the material safety data sheetsavailable from the suppliers of these 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
25、Obtain the material safety data sheets for methylenechloride, acetone, and the chromic acid solution used forcleaning 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 inertm
26、aterial such as titanium dioxide or glass fiber, determine theamount of inert material accurately by a procedure suitable 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 sa
27、mple in an oven for a suggestedminimum of2hat65C (149F) 6 5C (9F) or until aconstant weight of 6 0.1 % is reached. Moisture picked upfrom ambient humidity will weigh 0.30 % and is negligible inthis procedure. (See Note 2.)NOTE 2Use a suitable technical method to determine moisture con-tent.9.3 If th
28、e sample is difficult to dissolve, reduce the samplesize by grinding it to a 20-mesh screen size in a Wiley Mill orother size reduction technique. Avoid overheating the sampleduring the grinding operation. It is possible to maintain a lowtemperature by grinding in the presence of dry ice or liquidni
29、trogen. Grind a 15 to 20- g sample, representative of theentire lot being tested. It is likely that drying is necessary afterthe dry ice grinding step.10. Procedure10.1 Accurately weigh between 0.2475 and 0.2525 g (accu-rate to 60.0002 g) of sample into a clean, dry 50-mLvolumetric flask. If the sam
30、ple contains more than 0.5 % inertmaterial, weigh the amount of sample necessary to give thespecified amount of PET.10.2 Place a TFE-fluorocarbon plastic-coated stirring barinto the flask and add approximately 25 mL of solvent. Prepareone flask without any sample present. Cap the flasks.10.3 Place t
31、he flasks in steel beakers and place on amagnetic hot plate which has been preheated to 110C (230F)6 10C (18F). Heat the flasks for 15 min while stirring.Remove flasks and inspect for undissolved PET. If a sampledoes not dissolve completely, extend the stirring time for up to30 more min while inspec
32、ting the sample at 10-min intervals.If the sample fails to dissolve completely at this time, thisprocedure is not applicable.10.4 When the samples have completely dissolved, removethe flasks from the hot plate and allow them to cool to5Reagent Chemicals, American Chemical Society Specifications, Ame
33、ricanChemical Society, Washington, DC. For suggestions on the testing 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. (US
34、PC), Rockville,MD.6Available from M inherent viscosity; poly-(ethylene terephthalate); PET; solution viscosityASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised
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37、u 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, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual
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