1、Designation: D 4603 03Standard Test Method forDetermining Inherent Viscosity of Poly(EthyleneTerephthalate) (PET) by Glass Capillary Viscometer1This standard is issued under the fixed designation D 4603; the number immediately following the designation indicates the year oforiginal adoption or, in t
2、he case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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
3、 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 mixture will require a different procedure.1.2 The inherent viscosity values obtain
4、ed by this testmethod are comparable with those obtained using differentialviscometry described in Test Method D 5225.1.3 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 thes
5、afety 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 use. Specific hazardsstatements are given in Section 8.NOTE 1This test metho
6、d 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 Ubbelohde viscometer, rather than the1B, and reports viscosity number, rather t
7、han inherent viscosity.2. Referenced Documents2.1 ASTM Standards:D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and the Calculation of DynamicViscosity)2D 446 Specification for Operating Instructions for GlassCapillary Kinematic Viscometers2D 1972 Practice for Generic Ma
8、rking of Plastic Products3D 5225 Test Method for Measuring Solution Viscosity ofPolymers with a Differential Viscometer4E 1 Specification for ASTM Thermometers5E 380 Practice for Use of the International System of Units(SI)6E 691 Practice for Conducting an Interlaboratory Study toDetermine the Preci
9、sion of a Test Method62.2 ISO Standard:1628/51998 Determination of the Viscosity of Polymers inDilute Solution Using Capillary Viscometers - Part 5:Thermoplastic Polyester (TP) homopolymers and Copoly-mers.72.3 NIST Standard:C 602 Testing of Glass Volumetric Apparatus83. Terminology3.1 Units, symbol
10、s, and abbreviations used in this testmethod are those recommended in Practice E 380.3.2 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 outlined in Practice D 1972. The PET acro-
11、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 solvent in a capillary viscometer at a
12、fixed 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 Subcommittee D20.70 on Analytical Methods(D20.70.05).Current edition approved March 10, 2003. Publis
13、hed April 2003. Originallyapproved in 1986. Last previous edition approved in 1996 as D 4603 96.2Annual Book of ASTM Standards, Vol 05.01.3Annual Book of ASTM Standards, Vol 08.01.4Annual Book of ASTM Standards, Vol 08.03.5Annual Book of ASTM Standards, Vol 14.03.6Annual Book of ASTM Standards, Vol
14、14.02.7Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.8Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.1*A Summary of Changes section appears at the end of this stan
15、dard.Copyright 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 relatable to the compositionand molecular weight of a polyester resin. It must be controlledso that the processability and end p
16、roperties of the resin remainin a desired range.6. Apparatus6.1 Cannon Ubbelohde Type 1B Viscometer, as described inSpecifications and Operating Instructions D 446.6.2 Viscometer Holder.6.3 Electric Timer, readable to 0.1 s, as described in TestMethod D 445.6.4 Constant Temperature Bath, control lab
17、el at 30C86F 6 0.01C 0.02F.6.5 Kinematic Viscosity Thermometer ASTM 118 (for use at30C), conforming to Specification E 1.6.6 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 ca
18、pacity, 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 steelscreen.6.14 Drying Oven,
19、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 Chemical Societywhere such specific
20、ations are available.9Other 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 % mixture (0.5 % moisture maxim
21、um, 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-bis-(isoethyl mercaptoaceta
22、te).107.3 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 toxic and require care inhandl
23、ing. 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 Obtain the material safety
24、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 inertmaterial such as titanium di
25、oxide 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 sample in an oven for a sugge
26、stedminimum 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 the sample is difficult to dissol
27、ve, 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 liquidnitrogen. Grind a 15 to 20- g sam
28、ple, 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 sample contains more than 0.5 % in
29、ertmaterial, 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 the flasks in steel beakers and
30、place on amagnetic hot plate which has been preheated to 110C 230F6 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 inspecting the sample at 10-min intervals
31、.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 toapproximately room temperature. Remove the stirring barswith a magnetic retriever and wash the bar w
32、ith fresh solvent,9Reagent Chemicals, American Chemical Society Specifications, AmericanChemical 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
33、 States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.10Available from M inherent viscosity; poly-(ethylene terephthalate); PET; solution viscositySUMMARY OF CHANGESThis section identifies the location of selected changes to this test method. For the co
34、nvenience of the user,Committee D20 has highlighted those changes that may impact the use of this test method. This section may alsoinclude descriptions of the changes or reasons for the changes, or both.D 4603 03:(1) Deleted referenced document: Test Method D 4019 andadded ISO statement.(2) Editori
35、al changes including the removal of non-mandatorylanguage.D 4603 96:(1) This edition included a title change and revised precisionand bias statement.ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users
36、 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 committee and must be reviewed every f
37、ive years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical
38、 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, PO 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).D4603034
