1、Designation: D 1601 99 (Reapproved 2004)Standard Test Method forDilute Solution Viscosity of Ethylene Polymers1This standard is issued under the fixed designation D 1601; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、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 covers the determination of the dilutesolution viscosity of ethylene polymers at 135C. It is appli-
3、cable to a reasonably 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)
4、.1.2 The values as stated 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 t
5、he applica-bility of 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 D 1601 and are included for information only.2. Referenced Documents2.1 ASTM Standards:2D 8
6、6 Method for Distillation of Petroleum Products atAtmospheric PressureD 445 Test Method for Kinematic Viscosity of Transparentand Opaque LiquidsD 883 Terminology Relating to PlasticsD 1600 Terminology for Abbreviated Terms Relating toPlasticsD 4020 Specification for Ultra-High-Molecular WeightPolyet
7、hylene Molding and Extrusion MaterialsE 1 Specification for ASTM 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 Viscosity NumberPart 3: Polyethylenesand
8、 Polypropylenes3. Terminology3.1 Units, symbols, and abbreviations used in this testmethod are those recommended in IEEE/ASTM SI 10 andTerminologies D 883 and D 1600 (see also Appendix X4).4. Significance and Use4.1 The knowledge of dilute solution viscosity serves as anadditional tool in characteri
9、zing 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 charac-terizations.4.2 Satisfacto
10、ry 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 manufacturing pro-cesses. Hence, its co
11、rrelation 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 viscosity may be of questionablevalue
12、where ethylene polymers are known or suspected tocontain colorants, carbon black, low molecular weight hydro-carbons, fillers, or other additives.4.4 The measurement of dilute solution viscosity of ethyl-ene polymers presents problems not ordinarily encountered inviscosimetry. Ethylene polymers are
13、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 Plasticsand is the direct respon
14、sibility of Subcommittee D20.70 on Analytical Methods(Section D20.70.05).Current edition approved July 1, 2004. Published July 2004. Originally approvedin 1958. Last previous edition approved in 1999 as D 1601 - 99.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM
15、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 10036.1*A Summary of Changes section appears
16、at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.test if the correct solution concentration is to be maintained.This test has no significance unless the sample is completelysoluble.4.5 The solution viscosity
17、 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 viscometer, solvent, or temperatureother than specified is used
18、, 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.5.4 Viscometer, Ubbelohde No. 1, calibrated for kineticenergy co
19、rrection 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 D 445.5.7 ThermometerAn ASTM High Softening Point Ther-mometer having a range from 30 to 200C, and
20、conforming tothe requirements for Thermometer 16C in Specification E 1.6. 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 treatmen
21、tremoves naphthalene, tetrahydronaphthalene, and oxy com-pounds, particularly peroxides.6.1.2 The redistilled product shall conform to the followingrequirements when tested in accordance with Method D 86:Standard DistillationASTMMethod D 86Initial boiling point 190C min10 mL 191C min20 mL 192C min80
22、 mL 194C max90 mL 195C maxDry point 196C maxNOTE 4While 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 the decahydronaph-thalene, add 0.2 % Tetr
23、akis methylene 3-(38,58-di-tert-butyl-48-hydroxphenyl) propionate methane to inhibit oxidationduring 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 tha
24、tdiscolor or smoke with prolonged heating.NOTE 5Silicone heat-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
25、store in a clean amber bottle.7.2 Cleaning the ViscometerClean the viscometer thor-oughly as follows: fill with cleaning solution, let stand over-night, empty and rinse several times with distilled water, thenrinse with acetone and purge with dry nitrogen.7.3 Solution PreparationWeigh 20 to 30 mg of
26、 theUHMWPE (see Note 6) into the Erlenmeyer flask. Add thedecahydronaphthalene 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
27、 150C 6 2C. Continue stirring at 150C 6 2C for1 h, with the 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
28、 Place the clean viscometer into the constant-temperature bath. Fill the viscometer with decahydronaphtha-lene, and allow it and the solvent to equilibrate at 135 6 0.1C.Measure the flow time of the solvent, to, three times, andaverage the results. The viscometer may have to be cleaned ifreplicate m
29、easurements of flow time differ by more than 0.3 s(see 7.4.3). Remove the decahydronaphthalene from the vis-cometer with vacuum and thoroughly rinse the viscometer withxylene at 110 to 120C or decahydronaphthalene at 135C.Remove the xylene or decahydronaphthalene with vacuum andaspirate dry air or n
30、itrogen to dry the viscometer (2 or 3 min).It is essential that the viscometer be completely 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
31、, in triplicate, and average theresults.7.4.3 Between uses, clean the viscometer by rinsing withhot xylene or decahydronaphthalene, drying with air or nitro-gen, and storing filled with hot decahydronaphthalene. Ifsolvent flow time changes by more than 0.3 s, or if difficulty isencountered in obtain
32、ing 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, it shall first be dried in a vacuum oven at 60C for 2 h.NOTE 7Filling of the viscometer is made easier by th
33、e use of a glassfunnel warmed with a heating mantle. This helps to prevent the UHMWPEsolution from precipitating.4Glassware used in this test method should be tested in accordance with theprocedures described in the National Institute of Standards and Technology CircularNo. C-434, “Testing of Glass
34、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., Linde Silicones Div., New York, NY, have beenfound satisfactory for this purpose.D 1601 99 (2004)28. Ca
35、lculation8.1 Calculate the relative solution viscosity as follows:hr5 ts k/ts!/to 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 threemeasur
36、ements).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 moreconcentrations, dependi
37、ng on whether it is desired to obtainrelative, inherent, or intrinsic 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. P
38、recision and Bias10.1 Table 1 is based on a round robin conducted in 1997 inaccordance with Practice E 691, 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 ma
39、terial.NOTE 8Caution: The explanations of r and R (10.1.1-10.1.4) are 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 teste
40、d in the round robin and are unlikely to be representative ofother lots, formulations, conditions, materials, or laboratories. Users ofthis test method should apply the principles outlined in Practice E 691 togenerate data specific to their materials and laboratory (or betweenlaboratories). The prin
41、ciples of 10.1.1-10.1.4 would then be valid for suchdata.10.1.1 Concept 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
42、 the criti-cal difference between two test results for the same material,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
43、 interval representing thecritical difference between two test results 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 fo
44、r that material.10.1.4 Any judgement in accordance with 10.1.2 and 10.1.3would 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; inherentviscosi
45、ty (logarithmic viscosity number); intrinsic viscosity(limiting viscosity number); reduced viscosity (viscosity num-ber); relative viscosity; specific viscosity; viscosity ratioAPPENDIXES(Nonmandatory Information)X1. PROCEDURE FROM PREVIOUS VERSION (D 1601 86 (1991)e1) DATING BACK TO 1957X1.1 If it
46、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
47、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 approximateweights to 6 0.0002 g:Specimen 1 0.09 to 0.11 gSpecimen 2 0.18 to 0.22 gSpecimen 3 0.2
48、8 to 0.32 gSpecimen 4 0.38 to 0.42 gNOTE X1.2The intrinsic viscosity (limiting viscosity number) mayalso be measured using successive dilutions of only one, or duplicate,solutions. This has the advantage of requiring that only one polymerspecimen be weighed. Dilutions to the solution of this specime
49、n in theviscometer are a time-saving device. The technique is as follows: Weighone, or a duplicate, specimen of 0.38 to 0.42 g to an accuracy of 60.0002TABLE 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 the indicated material. It isobtained by first pooling the within-laboratory standard deviations of the testresults from all of the participating laboratories.Sr5 $ s1!21 s2!21 sR!2% /n 1
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