1、Designation: D 1823 95 (Reapproved 2001)Standard Test Method forApparent Viscosity of Plastisols and Organosols at HighShear Rates by Extrusion Viscometer1This standard is issued under the fixed designation D 1823; the number immediately following the designation indicates the year oforiginal adopti
2、on or, in the 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. Scope1.1 This test method covers the measurement of plastisoland organosol viscosi
3、ty at high shear rates by means of anextrusion viscometer.1.2 Apparent viscosity at low shear rates is covered in TestMethod D 1824.1.3 The values stated in SI units are to be regarded as thestandard. The values in parentheses are given for informationonly.1.4 This standard does not purport to addre
4、ss the safetyconcerns 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 standard resembles ISO 4575-1985 in title only. Thecontent is sig
5、nificantly different.2. Referenced Documents2.1 ASTM Standards:D 1475 Test Method for Density of Liquid Coatings, Inks,and Related Products2D 1755 Specification for Poly(Vinyl Chloride) Resins3D 1824 Test Method for Apparent Viscosity of Plastisolsand Organosols at Low Shear Rate by Brookfield Visco
6、m-eter3E1 Specification for ASTM Thermometers4E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method52.2 ISO Standard:ISO 4575-1985: Poly Vinyl Chloride PastesDetermination of Apparent Viscosity Using the SeversRheometer63. Summary of Test Method3.1 The sam
7、ple is conditioned to the 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 givenapplicat
8、ion is dependent upon its 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 Extrusio
9、n Rheometer.75.2 Orifice, 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.1This test m
10、ethod 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 March 15, 1995. Published May 1995. Originallypublished as D 1823 61 T. Last previous edition D 1823 90.This
11、edition contains changes in Sections 1, 2, and 11 to include an ISOequivalency statement, to reference a low shear rate test method, and to includeKeywords.2Annual Book of ASTM Standards, Vol 06.01.3Annual Book of ASTM Standards, Vol 08.01.4Annual Book of ASTM Standards, Vol 14.03.5Annual Book of AS
12、TM Standards, Vol 14.02.6Available from American National Standards Institute, 11 W. 42nd St., 13thFloor, New York, NY 10036.7Burrell Severs, ModelA-120, or equivalent, has been found satisfactory for thispurpose. The Burrell Severs, ModelA-120 is available from the Burrell Corp., 2223Fifth Ave., Pi
13、ttsburgh, PA 15219.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5.6 ThermometerASTM Solvents Distillation Thermom-eter having a range from 2 to +52C (28 to 126F) andconforming to the requirements for Thermometer 37C asprescribed i
14、n Specification E1.5.7 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 determinations.7. Procedure7.1 Set Up RheometerAttach the pressure regulator to thenitrogen t
15、ank. 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 tank pressure to give 1.04 MPa(150 psi) pressure to the instrument. Do not use input or linepress
16、ure 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 place. Mount the barrel in the instrument.NOTE 2Air may be used instead of nitrogen.7.2 Weigh four emp
17、ty 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 the sample temperature.7.3 Insert the top air cap and gasket into the air cap ring,screw it in place
18、 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 valve to the OUT position and allow the mixto extrude into an unweighed paper cup for 10 s. Adjus
19、t 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 sample have entered thecup. Simultaneously remove the cup and stop the timer, againplacing the unw
20、eighed 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.7.7 Record the extrudate weight to the nearest 0.1 g andefflux time to the nearest second.7.8 Increa
21、se 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 determination. After all tests have beencompleted, turn off the nitrogen supply at the tank. Release thepressu
22、re 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 of the orifice does not become scratched. After rinsingwith mineral spirits, dry the orifice in air
23、.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 = length of orifice, cm (in.)Shear rate, s215 4W/3.1416R3DT (2)where:W = weight of material efflux
24、ed, g,D = density of the sample, determined in accordance withTest Method D 1475, except convert lb/gal to g/mL,andT = efflux time, s.NOTE 3The preferred practice is to determine both the density andefflux time on deaerated material. If the efflux time of undeaeratedmaterial is specifically desired,
25、 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!36.895 3 104if shear stress is in psi.9. Report9.1 The report shall include the following:9.1.1
26、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 stress, in pascals (orpounds-force per square inch), for each of the four pressures(0.069, 0.28, 0.48
27、, 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 shear stress of Z psi and a shear rate of Y s1= X poises.”The most information will be gained, howe
28、ver, 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 procedure.10. Precision and Bias810.1 Tables 1-4 are based on a round robin8conducted in1983 invo
29、lving 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 prepared according to MethodD 1755 at the laboratories which tested them. Each test resultconsis
30、ted of one individual determination at the stated extru-sion pressure. Each laboratory obtained 5 test results for eachresin at each extrusion pressure.NOTE 5Caution: The following explanations of r and R (10.2-10.2.3)are only intended to present a meaningful way of considering the8Supporting data a
31、re available from ASTM Headquarters. Request RR: D20-1137.D 1823 95 (2001)2approximate precision of this test method. With data from only fourlaboratories, the between-laboratories results, in particular, should beviewed with extreme caution! The data in Tables 1-4 should not berigorously applied to
32、 acceptance or rejection of material, as those data arespecific to the round robin and may not be representative of other lots,conditions, materials, or laboratories. Users of this test method shouldapply the principles outlined in Practice E 691 to generate data specific totheir laboratory and mate
33、rials, or between specific laboratories. Theprinciples of 10.2-10.2.3 would then be valid for such data.10.2 Concept of r and RIf Srand SRwere calculated froma large enough body of data, and for test results consisting ofone determination per test result.10.2.1 Repeatability Limit, rIn comparing two
34、 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 if they differ by more than the r value forthat material.10.2.2 Reproducibility Limit, RIn comparing two testresults for the same material, o
35、btained by different operatorsusing different equipment in different laboratories on differentdays, the two test results should be judged not equivalent ifthey 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 % (0.9
36、5) 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; extrusion viscometer; high shearrate viscometry; PVC organosol; PVC plastisolASTM International takes no position respecting the validity of any p
37、atent rights asserted in connection with any item mentionedin this standard. Users 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 revisi
38、on 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 invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your co
39、mments will receive careful consideration at a meeting of theresponsible technical 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 copyrigh
40、ted 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
41、-mail); or through the ASTM website(www.astm.org).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 12
42、1.55 12.0 13.7 33.6 38.5VI 221.25 9.4 9.8 26.3 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 L
43、imit ( = 2.8 nR).TABLE 2 Precision of Viscosity 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.
44、80 5.9 8.7 16.5 24.3Anr 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 3 Precis
45、ion of Viscosity Data at 70 psi ExtrusionPressureResinAverageViscosity(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
46、 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 4 Precision of Viscosity Data at 100 p
47、si ExtrusionPressureResinAverageViscosity(Poises)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).D 1823 95 (2001)3
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