1、Designation: D1601 18Standard Test Method forDilute Solution Viscosity of Ethylene Polymers1This standard is issued under the fixed designation D1601; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revision. A num
2、ber 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 covers the determination of the dilutesolution viscosity of ethylene polymers at 135C. It is appli-cable to a reasonably
3、 wide spectrum of ethylene polymershaving densities from 0.910 to 0.970 g/cm2. Directions aregiven for the determination of relative viscosity (viscosityratio), inherent viscosity (logarithmic viscosity number), andintrinsic viscosity (limiting viscosity number).1.2 The values as stated in SI units
4、are to be regarded as thestandard.1.3 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, health, and environmental practices and deter-mine the applicability of r
5、egulatory limitations prior to use.1.3.1 WarningMercury 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
6、mercuryand mercury containing products. See 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 bylaw.NOTE 1This standard is equivalent to ISO 1628-3.NOTE
7、2Appendix X1 Appendix X3 contain material from theprevious version of Test Method D1601 and are included for informationonly.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDe
8、velopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-
9、ity)D446 Specifications and Operating Instructions for GlassCapillary Kinematic ViscometersD883 Terminology Relating to PlasticsD1600 Terminology forAbbreviated Terms Relating to Plas-ticsD4020 Specification for Ultra-High-Molecular-Weight Poly-ethylene Molding and Extrusion MaterialsE2251 Specifica
10、tion for Liquid-in-Glass ASTM Thermom-eters with Low-Hazard Precision LiquidsE2935 Practice for Conducting Equivalence Testing inLaboratory ApplicationsIEEE/ASTM SI-10 Standard for Use of the InternationalSystem of Units (SI): The Modern Metric System2.2 ISO Standards:3ISO 1628-3 PlasticsDeterminati
11、on of Viscosity Numberand Limiting Viscosity NumberPart 3: Polyethylenesand Polypropylenes3. Terminology3.1 Units, symbols, and abbreviations used in this testmethod are those recommended in IEEE/ASTM SI-10 andTerminologies D883 and D1600.4. Significance and Use4.1 The knowledge of dilute solution v
12、iscosity serves as anadditional tool in characterizing ethylene polymers. Viscositydata alone is potentially a limited value in predicting theprocessing behavior of the polymer. However, when used inconjunction with other flow and physical property values, thesolution viscosity of ethylene polymers
13、contributes to charac-terizing the material.1This test method is under the jurisdiction of ASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods(Section D20.70.05).Current edition approved May 1, 2018. Published June 2018. Originallyapproved in 1
14、958. Last previous edition approved in 2012 as D1601 - 12. DOI:10.1520/D1601-18.2For 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 standards Document Summary page
15、onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.*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 St
16、atesThis international standard 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 T
17、rade (TBT) Committee.14.2 Satisfactory correlation between solution viscosity andcertain other properties is possible from polymers of a singlemanufacturing process. The solution viscosity test is notsensitive to some molecular configurational patterns that occuramong polymers from different manufac
18、turing processes.Hence, its correlation with other properties of polymers pro-duced by different processes, by even one manufacturer, islimited without structural characterization.4.3 The viscosity of polymer solutions has the potential tobe drastically affected by the presence of known or unknownad
19、ditives in the sample. The use of solution viscosity datawhere ethylene polymers are known or suspected to containcolorants, carbon black, low molecular weight hydrocarbons,fillers, or other additives needs to be considered.4.4 The measurement of dilute solution viscosity of ethyl-ene polymers prese
20、nts problems not ordinarily encountered inviscosimetry. Ethylene polymers are not soluble at roomtemperature in any known solvent. Some of the higher densitymaterials are insoluble below 100C. Extreme care must beexercised in transferring the solution to the viscometer for thetest if the correct sol
21、ution concentration is to be maintained.This test has no significance unless the sample is completelysoluble.4.5 The solution viscosity is a function of the root-mean-square size of the polymer molecules in solution. It is knownthat the solvent selected and the temperature of the determina-tion have
22、 an effect on the root-mean-square size of theparticles. Hence, where a viscometer, solvent, or temperatureother than specified in this standard is used, the data is likelynot comparable to that obtained by this procedure.5. Apparatus5.1 Burets, (specifications).5.2 Erlenmeyer flask, 250 mL with sto
23、pper.5.3 Constant Temperature Bath, capable of maintaining 1356 l0.1C.5.4 Viscometer, Ubbelohde Size No. 1, calibrated for kineticenergy correction constant.NOTE 3Other types of viscometers may be used provided they can beshown to agree with the type specified.5.5 Oven, maintained at 140 6 5C.5.6 Ti
24、mer, as specified in 4.5 of Test Method D445.5.7 ThermometerAn ASTM High Softening Point Ther-mometer having a range from 30 to 200C, and conforming tothe requirements for Thermometer 16C in Specification E2251.Thermometric devices such as resistance temperature detectors(RTDs), having accuracies eq
25、ual to or better than Thermometer16C in the specified temperature range are also appropriate foruse.6. Reagents and Materials6.1 SolventDecahydronaphthalene (Decalin) CAS # 97-17-8, practical grade, purified and redistilled, as follows:6.1.1 The solvent shall be purified by percolation through100 to
26、 200 mesh commercial grade silica gel. This treatmentremoves naphthalene, tetrahydronaphthalene, and oxycompounds, particularly peroxides.NOTE 4While use of other solvents, such as tetrahydronaphthalene orxylene, may sometimes be advantageous, they will generally yielddifferent values for solution v
27、iscosities.6.1.2 Immediately after redistillation of thedecahydronaphthalene, add 0.2 % Tetrakis methylene 3-(3,5-di-tert-butyl-4-hydroxphenyl) propionate methane to inhibitoxidation during the viscosity determination.6.2 Heat Transfer MediumAny liquid heat transfer me-dium that will not appreciably
28、 affect the accuracy of the test isrecommended. Use caution when using fluids that discolor orsmoke with prolonged heating.NOTE 5Silicone heat-transfer fluids are adequate for this use4.7. Procedure7.1 Decahydronaphthalene PreparationAdd 0.2 %weight/volume stabilizer (Irganox 1010 or equivalent), to
29、 thedecahydronaphthalene, stir to dissolve, filter before use, andstore in a clean amber bottle.7.2 Cleaning the ViscometerClean the viscometer thor-oughly as follows: fill with appropriate cleaning solution, letstand overnight, empty and rinse several times with distilledwater, then rinse with acet
30、one and purge with dry nitrogen.7.3 Solution Preparation:7.3.1 Polyolefins other than UHMWPEThe polymer con-centration that gives a relative viscosity of the solution between1.2 and 2.0. Weigh an appropriate amount of polymer to thenearest 0.0001 g into the Erlenmeyer flask. Typically anappropriate
31、weight is between 0.1 and 0.5 g, depending on themolecular weight Add 100 mL of decahydronaphthalene atroom temperature. Heat the flask, with stirring, to 150C 62C. Continue stirring at 150C 6 2C for 1 h, with the flasklightly stoppered. Examine the flask to see if undissolvedpolyolefin remains. If
32、so, heat an additional 15 min andreexamine. Heat for an additional 15 min, if necessary, but donot heat longer than 2 h total.7.3.2 UHMWPEWeigh 20 to 30 mg of the UHMWPE (seeNote 6) into an appropriate flask. Add the decahydronaphtha-lene at room temperature, using a burette to measure inmilliliters
33、 a volume equal to 4.5 times the UHMWPE weight inmilligrams (for example, 26 mg of UHMWPE and 117 ml ofdecahydronaphthalene). Heat the flask, with stirring, to 150C6 2C. Continue stirring at 150C 6 2C for 1 h, with the flasklightly stoppered. Examine the flask to see if undissolvedUHMWPE remains. If
34、 so, heat an additional 15 min andreexamine. Heat for an additional 15 min, if necessary, but donot heat longer than 2 h total.7.4 Viscosity Measurement:7.4.1 Place the clean viscometer into the constant-temperature bath. Fill the viscometer withdecahydronaphthalene, and allow it and the solvent to
35、equili-brate at 135 6 0.1C. Measure the flow time of the solvent, to,4The silicone fluids available from the Dow Corning Corp., Midland, MI, orfrom the Union Carbide Corp., Linde Silicones Div., New York, NY, have beenfound satisfactory for this purpose.D1601 182three times, and average the results.
36、 The viscometer needs to becleaned if replicate measurements of flow time differ by morethan 0.3 s (see 7.4.3). Remove the decahydronaphthalene fromthe viscometer and thoroughly rinse the viscometer with xyleneat 110 to 120C or decahydronaphthalene at 135C. Removethe xylene or decahydronaphthalene a
37、nd aspirate dry air ornitrogen to dry the viscometer (2 or 3 min). If needed, rinse theviscometer with a lower boiling nonpolar solvent to enhancedrying. It is essential that the viscometer be completely dry.7.4.2 Transfer the hot (150C) polymer solution to theviscometer with sufficient quantity to
38、fill to the mark (see Note7), allow to equilibrate at 135C 6 0.1C, and measure theflow time of the solution, ts, in triplicate, and average theresults.7.4.3 Between uses, clean the viscometer by rinsing withhot xylene or decahydronaphthalene, drying with air ornitrogen, and storing filled with hot d
39、ecahydronaphthalene. Ifsolvent flow time changes by more than 0.3 s, or if difficulty isencountered in obtaining reproducible flow times with anysolution or solvent, clean the viscometer with cleaning solutionas described in 7.2.NOTE 6If the UHMWPE is suspected to contain moisture or othervolatiles,
40、 it shall first be dried in a vacuum oven at 60C for 2 h.NOTE 7Filling of the viscometer is made easier by the use of a glassfunnel warmed with a heating mantle. This helps to prevent the UHMWPEsolution from precipitating. Stainless steel mesh folded into a cone may beused to filter the solutions du
41、ring loading.8. Calculation8.1 Calculate the relative solution viscosity as follows:r5 ts2 k/ts2!/to2 k/to2! (1)where:k = kinetic energy correction constant for the particularviscometer used,ts= flow time of solution at 135C (average of threemeasurements), andto= flow time of pure solvent at 135C (a
42、verage of threemeasurements).9. Report9.1 Report the following information:9.1.1 Complete identification of the material tested includ-ing type, source, manufacturers code numbers, and tradename.9.1.2 Conditioning procedure used, if any.9.1.3 The relative viscosity (viscosity ratio) of one or moreco
43、ncentrations, depending on whether it is desired to obtainrelative, inherent, or intrinsic viscosity (viscosity ratio, loga-rithmic viscosity number, or limiting viscosity number).9.1.4 The intrinsic viscosity (limiting viscosity number),when desired, to three significant figures.10. Precision and B
44、ias10.1 Table 1 is based on a round robin conducted in 1997 inaccordance with Practice E691, involving two materials testedby six laboratories. One laboratory distributed the two com-mercial UHMWPE samples chosen for the evaluation. Eachlaboratory obtained six test results for each material.(Warning
45、The explanations of r and R (10.1.1 10.1.4) areonly intended to present a meaningful way of considering theapproximate precision of this test method. The data in Table 1should not be applied to acceptance or rejection of materials, asthese data apply only to the materials tested in the round robinan
46、d are unlikely to be representative of other lots, formulations,conditions, materials, or laboratories. Users of this test methodshould apply the principles outlined in Practice E691 togenerate data specific to their materials and laboratory (orbetween laboratories). The principles of 10.1.1 10.1.4
47、wouldthen be valid for such data.)10.1.1 Concept of r and R in Table 1If Srand SRhavebeen calculated from a large enough body of data, and for testresults from testing one sample for each test result, then thefollowing applies:10.1.2 Repeatability Limit, rThe value below which theabsolute difference
48、 between two individual test results obtainedunder repeatability conditions may be expected to occur with aprobability of approximately 0.95 (95 %).10.1.3 Reproducibility Limit, RThe value below which theabsolute difference between two individual test results obtainedunder reproducibility conditions
49、 may be expected to occur witha probability of approximately 0.95 (95 %).10.1.4 When required, conducting equivalence testing onnumerical data from two sources shall be conducted in accor-dance with E2935 or any known method for judging theequivalence of two means, for example, a t-test.10.2 BiasThere are no recognized standards by which toestimate bias of this method.11. Keywords11.1 dilute solution viscosity; ethylene polymers; inherentviscosity (logarithmic viscosity number); intrinsic viscosity(limiting viscosity number);
