1、Designation: D1823 95 (Reapproved 2009)Standard Test Method forApparent Viscosity of Plastisols and Organosols at HighShear Rates by Extrusion Viscometer1This standard is issued under the fixed designation D1823; the number immediately following the designation indicates the year oforiginal adoption
2、 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.1. Scope1.1 This test method covers the measurement of plastisoland organosol viscosity
3、at high shear rates by means of anextrusion viscometer.1.2 Apparent viscosity at low shear rates is covered in TestMethod D1824.1.3 The values stated in SI units are to be regarded asstandard. The values in parentheses are given for informationonly.1.4 This standard does not purport to address the s
4、afetyconcerns associated with its use. It is the responsibility of theuser of this standard to establish appropriate safety and healthpractices and determine the applicability of regulatory limita-tions prior to use.NOTE 1This test method resembles ISO 4575-1985 in title only. Thecontent is signific
5、antly different.2. Referenced Documents2.1 ASTM Standards:2D1475 Test Method For Density of Liquid Coatings, Inks,and Related ProductsD1755 Specification for Poly(Vinyl Chloride) ResinsD1824 Test Method forApparent Viscosity of Plastisols andOrganosols at Low Shear RatesE1 Specification for ASTM Liq
6、uid-in-Glass ThermometersE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method2.2 ISO Standard:ISO 4575-1985 Poly Vinyl Chloride PastesDetermination of Apparent Viscosity Using the SeversRheometer33. Summary of Test Method3.1 The sample is conditioned to th
7、e proper temperature,placed into an extrusion chamber, and extruded under standardconditions. The viscosity is calculated from the extrusionpressure and the rate of flow through the orifice.4. Significance and Use4.1 The suitability of a dispersion resin for any givenapplication is dependent upon it
8、s viscosity characteristics.4.2 The extrusion viscosity defines the flow behavior of aplastisol or organosol under high shear. This viscosity relates tothe conditions encountered in mixing, pumping, knife coating,roller coating, and spraying processes.5. Apparatus5.1 Extrusion Rheometer.45.2 Orifice
9、, 3.17 6 0.13 mm (0.125 6 0.005 in.) insidediameter and 50 6 1.0 mm (1.97 6 0.04 in.) long.5.3 Sample Containers, Tin Cans, or Glass Jars, 1-pt(500-mL) capacity.5.4 Paper Cups, 8-oz (250-mL) capacity.5.5 Nitrogen Cylinder, equipped with pressure regulator andgage.5.6 ThermometerASTM Solvents Distill
10、ation Thermom-eter having a range from 2 to +52C (28 to 126F) andconforming to the requirements for Thermometer 37C asprescribed in Specification E1. Use of temperature measuringdevices such as liquid-in-glass thermometers, thermocouples,or platinum resistance thermometers having equivalent orbetter
11、 accuracy and precision, while covering the temperaturerange of Thermometer 37C shall be permitted.5.7 Timer.6. Conditioning6.1 Maintain the plastisol or organosol samples at 236 1C(73 6 2 F) and 50 6 5 % relative humidity at all times aftermixing and throughout the period of viscosity determination
12、s.1This test method is under the jurisdiction ofASTM Committee D20 on Plasticsand is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials(Section D20.15.08).Current edition approved Oct. 1, 2009. Published January 2010. Originallyapproved in 1961. Last previous edition approve
13、d in 2001 as D1823 95 (2001).DOI: 10.1520/D1823-95R09.2For 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 onthe ASTM website.3Availa
14、ble from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4The sole source of supply of the Burrell Severs, Model A-120 known to thecommittee at this time is Burrell Corp., 2223 Fifth Ave., Pittsburgh, PA 15219. Ifyou are aware of alterna
15、tive suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-
16、2959, United States.7. Procedure7.1 Set Up RheometerAttach the pressure regulator to thenitrogen tank. Connect the nitrogen supply to the rheometer bymeans of the copper tubing. Do not use oxygen or liquidpressure sources (Note 2). Set the three-way quick-acting valveto the IN position. Regulate the
17、 tank pressure to give 1.04 MPa(150 psi) pressure to the instrument. Do not use input or linepressure over 1.38 MPa (200 psi). Insert the medium-sizeorifice (approximately 3.2 mm (18 in.) inside diameter) in theorifice retaining cap, with the orifice and the barrel, then screwthe cap solidly in plac
18、e. Mount the barrel in the instrument.NOTE 2Air may be used instead of nitrogen.7.2 Weigh four empty paper cups for each sample to betested. Record tare weight of each cup to the nearest 0.1 g. Fillthe barrel with the sample to be tested to within 13 mm (12 in.)from the top of the barrel. Measure th
19、e sample temperature.7.3 Insert the top air cap and gasket into the air cap ring,screw it in place on top of the barrel, and connect the air supplyquick-connector.7.4 Set the rheometer regulator gage (on the right side of theinstrument) to 0.069 MPa (10 psi) pressure. Open the three-way quick-acting
20、 valve to the OUT position and allow the mixto extrude into an unweighed paper cup for 10 s. Adjust thegage pressure back to 0.069 MPa (10 psi).7.5 Quickly place a preweighed and labeled paper cup underthe nozzle and at the same time start the timer. Collect theextrudate until approximately 50 g of
21、sample have entered thecup. Simultaneously remove the cup and stop the timer, againplacing the unweighed cup under the nozzle. (Use a maximumflow time of 200 s for extremely viscous samples.)7.6 Push the three-way quick-acting valve to the IN positionto turn off the nitrogen supply to the chamber.7.
22、7 Record the extrudate weight to the nearest 0.1 g andefflux time to the nearest second.7.8 Increase the gage pressure to 0.28 MPa (40 psi) andrepeat 7.4-7.7. Increase to 0.48 MPa (70 psi) and repeat. Makea fourth determination at 0.69 MPa (100 psi). Report the exactefflux time for each determinatio
23、n. After all tests have beencompleted, turn off the nitrogen supply at the tank. Release thepressure in the instrument by pulling the three-way valve to theOUT position.7.9 Clean the orifice between runs using pipe cleaners thathave been wetted with mineral spirits. Take care that the innersurface o
24、f the orifice does not become scratched. After rinsingwith mineral spirits, dry the orifice in air.8. Calculation8.1 Calculate the shear stress, shear rate, and viscosity asfollows:Shear stress, MPa or psi!5PR/2L (1)where:P = pressure in rheometer, MPa (or psi),R = radius of orifice, cm (in.), andL
25、= length of orifice, cm (in.)Shear rate, s215 4W/3.1416R3DT (2)where:W = weight of material effluxed, g,D = density of the sample, determined in accordance withTest Method D1475, except convert lb/gal to g/mL,andT = efflux time, s.NOTE 3The preferred practice is to determine both the density andeffl
26、ux time on deaerated material. If the efflux time of undeaeratedmaterial is specifically desired, the determination of density on anundeaerated sample may also be desirable.Viscosity, pascal seconds 5shear stress/shear rate!3106if shear stress is in MPa. (3)Viscosity, poises 5shear stress/shear rate
27、!36.895 3 104if shear stress is in psi.9. Report9.1 The report shall include the following:9.1.1 Complete sample identification,9.1.2 Test temperature as measured in,9.1.3 Conditioning time, and9.1.4 Extrusion viscosity, in pascal seconds (or poises);shear rate, in reciprocal seconds; and shear stre
28、ss, in pascals (orpounds-force per square inch), for each of the four pressures(0.069, 0.28, 0.48, and 0.69 MPa (or 10, 40, 70, and 100 psi).NOTE 4If only one viscosity is to be reported, report the data obtainedat 100 psi together with the shear rate and shear stress, for example:“Viscosity at a sh
29、ear stress of Z psi and a shear rate of Y s1= X poises.”The most information will be gained, however, by a plot of shear rateversus shear stress and would typify a true flow curve. In all cases whereonly one value is to be reported, the test must be run at each pressure inthe order indicated in the
30、procedure.10. Precision and Bias510.1 Tables 1-4 are based on a round robin5conducted in1983 involving six PVC dispersion resins tested by fourlaboratories at extrusion pressures of 10, 40, 70, and 100 psi.For each resin, all the samples were prepared at one source, butthe individual plastisols were
31、 prepared according to MethodD1755 at the laboratories which tested them. Each test resultconsisted of one individual determination at the stated extru-sion pressure. Each laboratory obtained 5 test results for eachresin at each extrusion pressure. (WarningThe followingexplanations of r and R (10.2-
32、10.2.3) are only intended topresent a meaningful way of considering the approximateprecision of this test method. With data from only fourlaboratories, the between-laboratories results, in particular,should be viewed with extreme caution! The data in Tables 1-4should not be rigorously applied to acc
33、eptance or rejection ofmaterial, as those data are specific to the round robin and maynot be representative of other lots, conditions, materials, orlaboratories. Users of this test method should apply theprinciples outlined in Practice E691 to generate data specific totheir laboratory and materials,
34、 or between specific laboratories.The principles of 10.2-10.2.3 would then be valid for suchdata.)5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D20-1137.D1823 95 (2009)210.2 Concept of r and RIf Srand SRwere calculated froma
35、large enough body of data, and for test results consisting ofone determination per test result.10.2.1 Repeatability Limit, rIn comparing two test resultsfor the same material, obtained by the same operator using thesame equipment on the same day, the two test results should bejudged not equivalent i
36、f they differ by more than the r value forthat material.10.2.2 Reproducibility Limit, RIn comparing two testresults for the same material, obtained by different operatorsusing different equipment in different laboratories on differentdays, the two test results should be judged not equivalent ifthey
37、differ by more than the R value for that material.10.2.3 Any judgment in accordance with 10.2.1 or 10.2.2would have an approximate 95 % (0.95) probability of beingcorrect.10.3 There are no recognized standards by which to esti-mate bias of this test method.11. Keywords11.1 apparent viscosity; extrus
38、ion viscometer; high shearrate viscometry; PVC organosol; PVC plastisolASTM 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 that determination of the validity of
39、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 five years andif not revised, either reapproved or withdrawn. Your comments are
40、 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 committee, which you may attend. If you feel that your comments have not rece
41、ived 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) o
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43、/).TABLE 1 Precision of Viscosity Data at 10 psi ExtrusionPressureResinAverageViscosity(Poises)Values expressed as % of the AveragenrAnRBrCRDIV 79.95 10.5 18.3 29.4 51.1V 81.05 7.0 25.8 19.6 72.2I 87.95 7.1 11.9 19.9 33.4III 99.90 6.1 8.6 17.1 24.1II 121.55 12.0 13.7 33.6 38.5VI 221.25 9.4 9.8 26.3
44、27.3Anr is the within-laboratory coefficient of variation of the average.BnR is the between-laboratories coefficient of variation of the average.Cr is the within-laboratory repeatability Limit ( = 2.8 nr).DR is the between-laboratories reproducibility Limit ( = 2.8 nR).TABLE 2 Precision of Viscosity
45、 Data at 40 psi ExtrusionPressureResinAverageViscosity(Poises)Values expressed as % of the AveragenrAnRBrCRDV 86.30 7.3 10.2 20.4 28.6IV 129.85 11.9 24.2 33.3 67.7II 130.90 9.9 21.8 27.7 61.2I 147.00 7.4 9.6 20.7 26.9III 184.20 5.5 11.1 15.4 31.0VI 211.80 5.9 8.7 16.5 24.3Anr is the within-laborator
46、y coefficient of variation of the average.BnR is the between-laboratories coefficient of variation of the average.Cr is the within-laboratory repeatability Limit ( = 2.8 nr).DR is the between-laboratories reproducibility Limit ( = 2.8 nR).TABLE 3 Precision of Viscosity Data at 70 psi ExtrusionPressu
47、reResinAverageViscosity(Poises)Values expressed as % of the AveragenrAnRBrCRDV 79.10 7.6 11.1 21.3 31.2II 119.50 4.9 6.4 13.7 18.0IV 139.85 11.9 24.3 33.3 68.1I 150.50 7.6 16.5 21.3 46.3VI 182.40 5.9 10.3 16.5 28.7III 233.95 6.6 13.8 18.5 38.5Anr is the within-laboratory coefficient of variation of
48、the average.BnR is the between-laboratories coefficient of variation of the average.Cr is the within-laboratory repeatability Limit ( = 2.8 nr).DR is the between-laboratories reproducibility Limit ( = 2.8 nR).TABLE 4 Precision of Viscosity Data at 100 psi ExtrusionPressureResinAverageViscosity(Poise
49、s)Values expressed as % of the AveragenrAnRBrCRDV 70.20 6.6 10.8 18.5 30.3II 107.50 5.3 7.3 14.8 20.6IV 130.80 6.3 16.5 17.6 46.2I 134.35 12.4 24.2 34.7 67.7VI 153.05 5.0 10.1 14.0 28.4III 249.05 7.4 14.3 20.7 39.9Anr is the within-laboratory coefficient of variation of the average.BnR is the between-laboratories coefficient of variation of the average.Cr is the within-laboratory repeatability Limit ( = 2.8 nr).DR is the between-laboratories reproducibility Limit ( = 2.8 nR).D1823 95 (2009)3
