1、Designation: D1823 95 (Reapproved 2009)D1823 16Standard 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
2、adoption 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. Scope Scope*1.1 This test method covers the measurement of plastisol and orga
3、nosol viscosity at high shear rates by means of an extrusionviscometer.1.2 Apparent viscosity at low shear rates is covered in Test Method D1824.1.3 The values stated in SI units are to be regarded as standard. The values in parentheses are given for information only.1.4 This standard does not purpo
4、rt to address the safety concerns associated with its use. It is the responsibility of the userof this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations priorto use.NOTE 1This test method resembles ISO 4575-1985 in title only. The
5、 content is significantly different.standard and ISO 4575-2007 address the samesubject matter, but differ in technical content.2. Referenced Documents2.1 ASTM Standards:2D1475 Test Method For Density of Liquid Coatings, Inks, and Related ProductsD1755 Specification for Poly(Vinyl Chloride) ResinsD18
6、24 Test Method for Apparent Viscosity of Plastisols and Organosols at Low Shear RatesE1 Specification for ASTM Liquid-in-Glass ThermometersE691 Practice for Conducting an Interlaboratory Study to Determine the Precision of a Test Method2.2 ISO Standard:ISO 4575-1985ISO 4575-2007 Poly Vinyl Chloride
7、PastesDetermination ofApparent Viscosity Using the Severs Rheometer33. Summary of Test Method3.1 The sample is conditioned to the proper temperature, placed into an extrusion chamber, and extruded under standardconditions. The viscosity is calculated from the extrusion pressure and the rate of flow
8、through the orifice.4. Significance and Use4.1 The suitability of a dispersion resin for any given application is dependent upon its viscosity characteristics.4.2 The extrusion viscosity defines the flow behavior of a plastisol or organosol under high shear. This viscosity relates to theconditions e
9、ncountered in mixing, pumping, knife coating, roller coating, and spraying processes.5. Apparatus5.1 Extrusion Rheometer.45.2 Orifice, 3.17 6 0.13 mm (0.125 6 0.005 in.) inside diameter and 50 6 1.0 mm (1.97 6 0.04 in.) long.1 This test method is under the jurisdiction of ASTM Committee D20 on Plast
10、ics and is the direct responsibility of Subcommittee D20.15 on Thermoplastic Materials(Section D20.15.08).Current edition approved Oct. 1, 2009May 1, 2016. Published January 2010May 2016. Originally approved in 1961. Last previous edition approved in 20012009 asD1823 95 (2001).(2009). DOI: 10.1520/D
11、1823-95R09.10.1520/D1823-16.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Available from American Nationa
12、l Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.4 The sole source of supply of the Burrell Severs, Model A-120 known to the committee at this time is Burrell Corp., 2223 Fifth Ave., Pittsburgh, PA 15219. If you areaware of alternative suppliers, please
13、 provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1 which you may attend.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of
14、 what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered
15、 the official document.*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 States15.3 Sample Containers, Tin Cans, or Glass Jars, 1-pt (500-mL) capacity.5.4 Paper Cups, 8-oz (250-m
16、L) capacity.5.5 Nitrogen Cylinder, equipped with pressure regulator and gage.5.6 ThermometerASTM Solvents Distillation Thermometer having a range from 2 to +52C (28 to 126F) and conformingto the requirements for Thermometer 37C as prescribed in Specification E1. Use of temperature measuring devices
17、such asliquid-in-glass thermometers, thermocouples, or platinum resistance thermometers having equivalent or better accuracy andprecision, while covering the temperature range of Thermometer 37C shall be permitted. (WarningThermometers referenced inSpecification E1 contain mercury, mercury thallium
18、eutectic alloy, or toluene or other suitable liquid colored with a permanent reddye. Mercury has been designated by EPAand many state agencies as a hazardous material that can cause central nervous system,kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to mat
19、erials. Caution should be takenwhen handling mercury and mercury containing products. See the applicable product Safety Data Sheet (SDS) for details andEPAs website- http:/www.epa.gov/mercury/faq.htm - for additional information. Users should be aware that selling mercuryand/or mercury containing pr
20、oducts into your state may be prohibited by state law. )5.7 Timer.6. Conditioning6.1 Maintain the plastisol or organosol samples at 236 1C (73 6 2 F) and 50 6 5 %10 % relative humidity at all times aftermixing and throughout the period of viscosity determinations.7. Procedure7.1 Set Up RheometerAtta
21、ch the pressure regulator to the nitrogen tank. Connect the nitrogen supply to the rheometer bymeans of the copper tubing. Do not use oxygen or liquid pressure sources (Note 2). Set the three-way quick-acting valve to theIN position. Regulate the tank pressure to give 1.04 MPa (150 psi) pressure to
22、the instrument. Do not use input or line pressureover 1.38 MPa (200 psi). Insert the medium-size orifice (approximately 3.2 mm (18 in.) inside diameter) in the orifice retainingcap, with the orifice and the barrel, then screw the cap solidly in place. Mount the barrel in the instrument.NOTE 2Air may
23、 be used instead of nitrogen.7.2 Weigh four empty paper cups for each sample to be tested. Record tare weight of each cup to the nearest 0.1 g. Fill the barrelwith 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 a
24、nd 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 the instrument) to 0.069 MPa (10 psi) pressure. Open the three-wayquick-acting valve to the OUTposition and allow the mix to e
25、xtrude into an unweighed paper cup for 10 s.Adjust the gage pressureback to 0.069 MPa (10 psi).7.5 Quickly place a preweighed and labeled paper cup under the nozzle and at the same time start the timer. Collect the extrudateuntil approximately 50 g of sample have entered the cup. Simultaneously remo
26、ve the cup and stop the timer, again placing theunweighed cup under the nozzle. (Use a maximum flow time of 200 s for extremely viscous samples.)7.6 Push the three-way quick-acting valve to the IN position to turn off the nitrogen supply to the chamber.7.7 Record the extrudate weight to the nearest
27、0.1 g and efflux time to the nearest second.7.8 Increase the gage pressure to 0.28 MPa (40 psi) and repeat 7.4 7.7. Increase to 0.48 MPa (70 psi) and repeat. Make a fourthdetermination at 0.69 MPa (100 psi). Report the exact efflux time for each determination.After all tests have been completed, tur
28、noff the nitrogen supply at the tank. Release the pressure in the instrument by pulling the three-way valve to the OUT position.7.9 Clean the orifice between runs using pipe cleaners that have been wetted with mineral spirits.Take care that the inner surfaceof the orifice does not become scratched.
29、After rinsing with mineral spirits, dry the orifice in air.8. Calculation8.1 Calculate the shear stress, shear rate, and viscosity as follows: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,
30、s21 54W/3.1416R3 DT (2)D1823 162where:W = weight of material effluxed, g,D = density of the sample, determined in accordance with Test Method D1475, except convert lb/gal to g/mL, andT = efflux time, s.NOTE 3The preferred practice is to determine both the density and efflux time on deaerated materia
31、l. If the efflux time of undeaerated material isspecifically desired, the determination of density on an undeaerated sample may also be desirable.Viscosity,pascal seconds5shear stress/shear rate!3106 (3)if shear stress is in MPa.Viscosity,poises5shear stress/shear rate!36.8953104if shear stress is i
32、n 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 stress, in pascals (orpounds-force p
33、er 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 obtained at 100 psi together with the shear rate and shear stress, for example: “Viscosityat a shear stress of Z psi and a shea
34、r rate of Y s1 = X poises.” The most information will be gained, however, by a plot of shear rate versus shear stressand would typify a true flow curve. In all cases where only one value is to be reported, the test must be run at each pressure in the order indicated inthe procedure.10. Precision and
35、 Bias510.1 Tables 1-4 are based on a round robin5 conducted in 1983 involving six PVC dispersion resins tested by four laboratoriesat extrusion pressures of 10, 40, 70, and 100 psi. For each resin, all the samples were prepared at one source, but the individualplastisols were prepared according to M
36、ethod D1755 at the laboratories which tested them. Each test result consisted of oneindividual determination at the stated extrusion pressure. Each laboratory obtained 5 test results for each resin at each extrusionpressure. (WarningThe following explanations of r and R (10.2 10.2.3) are only intend
37、ed to present a meaningful way ofconsidering the approximate precision of this test method. With data from only four laboratories, the between-laboratories results,in particular, should be viewed with extreme caution! The data in Tables 1-4 should not be rigorously applied to acceptance orrejection
38、of material, as those data are specific to the round robin and may not be representative of other lots, conditions, materials,or laboratories. Users of this test method should apply the principles outlined in Practice E691 to generate data specific to theirlaboratory and materials, or between specif
39、ic laboratories. The principles of 10.2 10.2.3 would then be valid for such data.)10.2 Concept of r and RIf Sr and SR were calculated from a large enough body of data, and for test results consisting of onedetermination per test result.10.2.1 Repeatability Limit, rIn comparing two test results for t
40、he same material, obtained by the same operator using the sameequipment on the same day, the two test results should be judged not equivalent if they differ by more than the r value for thatmaterial.5 Supporting data have been filed at ASTM International Headquarters and may be obtained by requestin
41、g Research Report RR: RR:D20-1137.TABLE 1 Precision of Viscosity Data at 10 psi Extrusion PressureResinAverageViscosity(Poises)Values expressed as % of the Averager A R B r C R DIV 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
42、13.7 33.6 38.5VI 221.25 9.4 9.8 26.3 27.3A r is the within-laboratory coefficient of variation of the average.B R is the between-laboratories coefficient of variation of the average.C r is the within-laboratory repeatability Limit ( = 2.8 r).D R is the between-laboratories reproducibility Limit ( =
43、2.8 R).D1823 16310.2.2 Reproducibility Limit, RIn comparing two test results for the same material, obtained by different operators usingdifferent equipment in different laboratories on different days, the two test results should be judged not equivalent if they differby more than the R value for th
44、at material.10.2.3 Any judgment in accordance with 10.2.1 or 10.2.2 would have an approximate 95 % (0.95) probability of being correct.10.3 There are no recognized standards by which to estimate bias of this test method.11. Keywords11.1 apparent viscosity; extrusion viscometer; high shear rate visco
45、metry; PVC organosol; PVC plastisolTABLE 2 Precision of Viscosity Data at 40 psi Extrusion PressureResinAverageViscosity(Poises)Values expressed as % of the Averager A R B r C R DV 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
46、.5 11.1 15.4 31.0VI 211.80 5.9 8.7 16.5 24.3A r is the within-laboratory coefficient of variation of the average.B R is the between-laboratories coefficient of variation of the average.C r is the within-laboratory repeatability Limit ( = 2.8 r).D R is the between-laboratories reproducibility Limit (
47、 = 2.8 R).TABLE 3 Precision of Viscosity Data at 70 psi Extrusion PressureResinAverageViscosity(Poises)Values expressed as % of the Averager A R B r C R DV 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 233.9
48、5 6.6 13.8 18.5 38.5A r is the within-laboratory coefficient of variation of the average.B R is the between-laboratories coefficient of variation of the average.C r is the within-laboratory repeatability Limit ( = 2.8 r).D R is the between-laboratories reproducibility Limit ( = 2.8 R).TABLE 4 Precis
49、ion of Viscosity Data at 100 psi ExtrusionPressureResinAverageViscosity(Poises)Values expressed as % of the Averager A R B r C R DV 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 39.9A r is the within-laboratory coefficient of variation of the average.B R is the between-laboratories coefficient of variation of the average.C r is the within-laboratory repeatability Limit ( = 2.8 r).D R is the between-laboratories
