1、Designation: D1601 12Standard 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) (see AppendixX4).1.2 The values as st
4、ated in SI units 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 and health practices and determine the applica-bility of
5、regulatory limitations prior to use.NOTE 1This test method is technically equivalent to ISO 1628-3.NOTE 2Appendix X1-Appendix X3 contain material from the previ-ous version of Test Method D1601 and are included for information only.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Disti
6、llation of Petroleum Products atAtmospheric PressureD445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D883 Terminology Relating to PlasticsD1600 Terminology forAbbreviated Terms Relating to Plas-ticsD4020 Specification for Ultra-High-Mol
7、ecular-Weight Poly-ethylene Molding and Extrusion MaterialsE1 Specification for ASTM Liquid-in-Glass ThermometersIEEE/ASTM SI-10 Standard for Use of the InternationalSystem of Units (SI): The Modern Metric System2.2 ISO Standards:3ISO 1628-3 PlasticsDetermination of Viscosity Numberand Limiting Visc
8、osity 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 (see also Appendix X4).4. Significance and Use4.1 The knowledge of dilute solution viscosity serves
9、as anadditional tool in characterizing ethylene polymers. Viscositydata alone may be of limited value in predicting the processingbehavior of the polymer. However, when used in conjunctionwith other flow and physical property values, the solutionviscosity of ethylene polymers may contribute to their
10、 charac-terizations.4.2 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 mayoccur among polymers from different manuf
11、acturing pro-cesses. Hence, its correlation with other properties of polymersproduced by different processes, by even one manufacturer,may be limited.4.3 The viscosity of polymer solutions may be drasticallyaffected by the presence of known or unknown additives in thesample. The use of solution visc
12、osity may be of questionablevalue where ethylene polymers are known or suspected tocontain colorants, carbon black, low molecular weighthydrocarbons, fillers, or other additives.4.4 The measurement of dilute solution viscosity of ethyl-ene polymers presents problems not ordinarily encountered invisc
13、osimetry. 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 the1This test method is under the jurisdiction of ASTM Committee D20 on
14、Plasticsand is the direct responsibility of Subcommittee D20.70 on Analytical Methods(Section D20.70.05).Current edition approved Aug. 1, 2012. Published September 2012. Originallyapproved in 1958. Last previous edition approved in 2004 as D1601 - 99(2004).DOI: 10.1520/D1601-12.2For referenced ASTM
15、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 onthe ASTM website.3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th F
16、loor, 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 States1test if the correct solution concentration is to be maintained.This test has no significance unl
17、ess 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 an effect on the root-mean-square size of theparticles. Hence, where a v
18、iscometer, solvent, or temperatureother than specified is used, data may not be comparable to thatobtained by this procedure.5. Apparatus5.1 Volumetric Flasks, 100-mL, grade EXAX or better.45.2 Transfer Pipets, Grade EXAX or better.45.3 Constant Temperature Bath, capable of maintaining 1356 l0.1C.5.
19、4 Viscometer, Ubbelohde 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 Timer, as specified in 4.5 of Test Method D445.5.7 ThermometerAn ASTM High Soft
20、ening Point Ther-mometer having a range from 30 to 200C, and conforming tothe requirements for Thermometer 16C in Specification E1.Thermometric devices such as resistance temperature detectors(RTDs), having accuracies equal to or better than Thermometer16C in the specified temperature range are also
21、 appropriate foruse.6. Reagents and Materials6.1 SolventDecahydronaphthalene, practical grade, puri-fied and redistilled, as follows:6.1.1 The solvent shall be purified by percolation through100 to 200 mesh commercial grade silica gel. This treatmentremoves naphthalene, tetrahydronaphthalene, and ox
22、ycompounds, particularly peroxides.6.1.2 The redistilled product shall conform to the followingrequirements when tested in accordance with Method D86:Standard DistillationASTMMethod D86Initial boiling point 190C min10 mL 191C min20 mL 192C min80 mL 194C max90 mL 195C maxDry point 196C maxNOTE 4While
23、 use of other solvents, such as tetrahydronaphthalene orxylene, may sometimes be advantageous, they will generally yielddifferent values for solution viscosities.6.1.3 Immediately after redistillation of thedecahydronaphthalene, add 0.2 % Tetrakis methylene 3-(3,5-di-tert-butyl-4-hydroxphenyl) propi
24、onate methane to inhibitoxidation during the viscosity determination.6.2 Heat Transfer MediumAny liquid heat transfer me-dium that will not appreciably affect the accuracy of the testmay be used. Care should be exercised in using fluids thatdiscolor or smoke with prolonged heating.NOTE 5Silicone hea
25、t-transfer fluids are adequate for this use5.7. Procedure7.1 Decahydronaphthalene PreparationAdd 0.2 %weight/volume stabilizer (Irganox 1010 or equivalent), to thedecahydronaphthalene, stir to dissolve, filter through fast filterpaper, and store in a clean amber bottle.7.2 Cleaning the ViscometerCle
26、an the viscometer thor-oughly as follows: fill with cleaning solution, let standovernight, empty and rinse several times with distilled water,then rinse with acetone and purge with dry nitrogen.7.3 Solution PreparationWeigh 20 to 30 mg of the UH-MWPE (see Note 6) into the Erlenmeyer flask. Add thede
27、cahydronaphthalene at room temperature, using a burette tomeasure in milliliters a volume equal to 4.5 times the UHM-WPE weight in milligrams (for example, 26 mg of UHMWPEand 117 ml of decahydronaphthalene). Heat the flask, withstirring, to 150C 6 2C. Continue stirring at 150C 6 2C for1 h, with the
28、flask lightly stoppered. Examine the flask to seeif undissolved UHMWPE remains. If so, heat an additional 15min and reexamine. Heat for an additional 15 min, if necessary,but do not heat longer than 2 h total.7.4 Viscosity Measurement:7.4.1 Place the clean viscometer into the constant-temperature ba
29、th. Fill the viscometer withdecahydronaphthalene, and allow it and the solvent to equili-brate at 135 6 0.1C. Measure the flow time of the solvent, to,three times, and average the results. The viscometer may haveto be cleaned if replicate measurements of flow time differ bymore than 0.3 s (see 7.4.3
30、). Remove the decahydronaphthalenefrom the viscometer with vacuum and thoroughly rinse theviscometer with xylene at 110 to 120C or decahydronaphtha-lene at 135C. Remove the xylene or decahydronaphthalenewith vacuum and aspirate dry air or nitrogen to dry theviscometer (2 or 3 min). It is essential t
31、hat the viscometer becompletely dry.7.4.2 Transfer the hot (150C) polymer solution to theviscometer with sufficient quantity to 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, c
32、lean the viscometer by rinsing withhot xylene or decahydronaphthalene, drying with air ornitrogen, and storing filled with hot decahydronaphthalene. Ifsolvent flow time changes by more than 0.3 s, or if difficulty is4Glassware used in this test method should be tested in accordance with theprocedure
33、s described in the National Institute of Standards and Technology CircularNo. C-434, “Testing of Glass Volumetric Apparatus,” and should not exceed thelimits of accuracy set forth in the circular.5The silicone fluids available from the Dow Corning Corp., Midland, MI, orfrom the Union Carbide Corp.,
34、Linde Silicones Div., New York, NY, have beenfound satisfactory for this purpose.D1601 122encountered 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 othervolatile
35、s, 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.8. Calculation8.1 Calculate the relative solution viscosity as follows:hr5 t
36、s2 k/ts!/to2 k/to! (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 (average of threemeasurements).9. Report9.1 Report the following information:9.1.1 Complete
37、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 moreconcentrations, depending on whether it is desired to obtainrelative, inherent, or intrinsic
38、 viscosity (viscosity ratio, loga-rithmic viscosity number, or limiting viscosity number) (seeAppendix X4).9.1.4 The intrinsic viscosity (limiting viscosity number),when desired, to three significant figures (see Appendix X4).10. Precision and Bias10.1 Table 1 is based on a round robin conducted in
39、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.NOTE 8Caution: The explanations of r and R (10.1.1-10.1.4) are
40、onlyintended to present a meaningful way of considering the approximateprecision of this test method. The data in Table 1 should not be applied toacceptance or rejection of materials, as these data apply only to thematerials tested in the round robin and are unlikely to be representative ofother lot
41、s, formulations, conditions, materials, or laboratories. Users ofthis test method should apply the principles outlined in Practice E691 togenerate data specific to their materials and laboratory (or betweenlaboratories). The principles of 10.1.1-10.1.4 would then be valid for suchdata.10.1.1 Concept
42、 of r and R in Table 1If Srand SRhave beencalculated from a large enough body of data, and for test resultsfrom testing one sample for each test result, then the followingapplies:10.1.2 Repeatabilityr is the interval representing the criti-cal difference between two test results for the same materia
43、l,obtained by the same operator using the same equipment on thesame day in the same laboratory. Two test results shall bejudged not equivalent if they differ by more than the r value forthe material.10.1.3 ReproducibilityR is the interval representing thecritical difference between two test results
44、for the samematerial, obtained by different operators using different equip-ment in different laboratories, not necessarily on the same day.Two test results shall be judged not equivalent if they differ bymore than the R value for that material.10.1.4 Any judgement in accordance with 10.1.2 and 10.1
45、.3would have an approximate 95 % (0.95) probability of beingcorrect.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 viscosi
46、ty number); reduced viscosity (viscosity num-ber); relative viscosity; specific viscosity; viscosity ratioTABLE 1 Relative Solution ViscosityMaterial Average SrASRBrCRDUHMWPE No. 1 1.454 0.015 0.049 0.042 0.136UHMWPE No. 2 1.653 0.017 0.048 0.047 0.136ASr= within-laboratory standard deviation for th
47、e indicated material. It is obtainedby first pooling the within-laboratory standard deviations of the test results from allof the participating laboratories.Sr5 f h ss1d21ss2d21ssRd2j/n g1/2BSR= between-laboratory reproducibility, expressed as standard deviation:SR5 f Sr21SL2g1/2where SL= standard d
48、eviation of laboratory means.Cr = within-laboratory critical interval between two test results = 2.8 Sr.DR = between laboratories critical interval between two test results = 2.8 SR.D1601 123APPENDIXES(Nonmandatory Information)X1. PROCEDURE FROM PREVIOUS VERSION (D1601 86 (1991)1) DATING BACK TO 195
49、7X1.1 If it is desired to determine only the relative viscosity(viscosity ratio) or the inherent viscosity (logarithmic viscositynumber), weigh one specimen of 0.18 to 0.226 0.0002 g andtransfer it quantitatively to a 100-mL volumetric flask whichhas been purged with nitrogen.NOTE X1.1Usually the determination of relative or inherent viscosity(viscosity ratio or logarithmic viscosity number) may suffice.X1.2 To determine the intrinsic viscosity (limiting viscositynumber), weigh four specimens of the following approximatewei
