1、Designation: D 2396 94 (Reapproved 2004)Standard Test Methods forPowder-Mix Time of Poly(Vinyl Chloride) (PVC) ResinsUsing a Torque Rheometer1This standard is issued under the fixed designation D 2396; the number immediately following the designation indicates the year oforiginal adoption or, in the
2、 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 These test methods cover the determination of thepowder-mix time of a general-purpose
3、poly(vinyl chloride)(PVC) resin.1.2 The values stated in SI units are to be regarded asstandard.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 p
4、ractices and determine the applica-bility of regulatory limitations prior to use.NOTE 1There is no ISO standard covering the primary subject ofthese ASTM test methods.2. Referenced Documents2.1 ASTM Standards:2D 883 Terminology Relating to PlasticsD 1600 Terminology for Abbreviated Terms Relating to
5、Plastics23. Terminology3.1 General:3.1.1 Definitions are in accordance with Terminology D 883and abbreviations are in accordance with Terminology D 1600unless otherwise indicated.4. Summary of Test Methods4.1 A sample of resin is heated and mixed in a bowl to thetest temperature. A measured amount o
6、f plasticizer is added tothe resin through a dispersing funnel. When the plasticizer isadded to the resin, the mix becomes wet and an increase inmotor torque is needed to maintain the same rotor speed.As themixing continues in the heated bowl, the plasticizer is absorbedinto the resin and the resin
7、granules become dry and free-flowing. When the mix reaches the dry and free-flowing state,its resistance to stirring decreases and the motor torque neededto maintain the same rotor speed decreases. By recording thechanges in motor torque with time, it is possible to measure thetime required for a re
8、sin to absorb a plasticizer.4.2 These test methods describe the use of two differentmixing heads that can be mounted on a torque rheometer toperform this test. Test results obtained with these mixing headsare compared in Section 14.4.2.1 A sigma mixing head is used in Test Method A.4.2.2 A planetary
9、 mixing head is used in Test Method B.5. Significance and Use5.1 The ability of PVC granules to accept a plasticizer andbecome a dry free-flowing powder is related to the internalpore structure of the resin, resin temperature, plasticizertemperature, and the plasticizer used. By choosing an appli-ca
10、ble plasticizer and maintaining a uniform temperature for theresin and plasticizer, it is possible to classify resins by howrapidly they absorb plasticizer. Resin suitability for a specificintensive mixing operation can be ascertained using these testmethods.6. Interferences6.1 ResinEach resin has a
11、 specific response in accepting aplasticizer. Differences in powder-mix time between resins canbe observed in the graph in the annex.6.2 PlasticizerPlasticizer viscosity directly affectspowder-mix time. Table 1 shows that an increase in diisodecylphthalate viscosity results in an increase in powder-
12、mix time.The data in Table 1 was generated in a single laboratory usingTest Method A.1These test methods are under the jurisdiction of ASTM Committee D20 onPlastics and are the direct responsibility of Subcommittee D20.15 on ThermoplasticMaterials.Current edition approved March 1, 2004. Published Ju
13、ne 2004. Originallyapproved in 1969. Last previous edition approved in 1999 as D 2396 - 94 (1999)e1.2For 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 Do
14、cument Summary page onthe ASTM website.TABLE 1 Powder-Mix Time of ASTM No. 1 ResinDIDP Viscosity,cP(millipascals-s)ABowlTemperature,CBMeanPowder-MixTime, sStandardDeviationNumber ofSamples111 85 435 . 2128 85 461 6.9 5147 85 479 . 2AViscosity was measured using a Brookfield RVF Viscometer, No. 1 spi
15、ndle, 20r/min, at 23C.BThe bowl temperature was measured at the thermocouple well.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 TemperatureThe temperature at which the test isperformed will affect the powder-mix time. A lower t
16、esttemperature will have a longer powder-mix time.NOTE 2It is also important to control the temperature of the plasti-cizer added to the resin. The powder-mix time can vary by as much as 3s for each degree Fahrenheit difference in plasticizer temperature, as seenin the graph in the annex.6.4 Equipme
17、ntDifferences between equipment can resultin differences in powder-mix times. To equate equipment, it issuggested that a specific powder-mix time be chosen and thatthe bowl temperature be adjusted to obtain the same time for allequipment. Table 2 shows the results from three laboratoriesusing this t
18、echnique to equate to a powder-mix time for ASTMNo. 1 resin using Test Method A to the value set by Laboratory1.6.5 Rotor SpeedObserved with the planetary mixing head(see Test Method B) was a decrease in dry time when the rotorspeed had been increased: 60 r/min 82C using DIDP = drytime of 868 s; and
19、 100 r/min 82C using DIDP = dry timeof 628 s.7. Apparatus7.1 Torque Rheometer.37.2 Sigma Mixer 650-mL,4or equivalent, and the disper-sion trough shown in Fig. 1 for plasticizer distribution. (ForTest Method A.)7.3 Planetary Mixer,5and the dispersion funnel shown inFig. 2 for plasticizer distribution
20、. (For Test Method B.)7.4 Balance, 0.1-g sensitivity.7.5 Container, 0.95 L size.7.6 Beaker, 400-mL.7.7 Funnel, for use with planetary mixer (see Test MethodB).7.8 Ruler, with metric scale.7.9 Paint Brush, 25.4 mm width.7.10 Thermometer, range of 40 to 100C with 0.2C divi-sions.7.11 Spatula.7.12 Visc
21、ometer, Brookfield RVF, or equivalent.8. Materials8.1 Poly(Vinyl Chloride) (PVC) Resin.8.2 Diisodecyl Phthalate Plasticizer.8.3 Clay.69. Safety Precautions9.1 Take care not to exceed the manufacturers recom-mended damping limit on the sigma mixer because of thedanger of bending the blades.9.2 Stop t
22、he mixer before cleaning the bowl and blades.10. Preparation of Torque Rheometer10.1 Electronic Plasti-Corder3Torque Rheometer:10.1.1 Adjust the torque rheometer so that the strip charttorque range reads 200 m-g at full scale.10.1.2 Set chart speed to 10 mm/min.10.1.3 Place pen on chart.10.1.4 Conne
23、ct the stock temperature measuring thermo-couple to the recorder and start the recorder.10.2 PL-20003Computerized Torque RheometerProgramthe PL-2000 Plasti-Corder3for the test conditions of:Order: (Run information)Operator: (Name)Date: (Current date)PL-Type: 2000Mixer Type: PlanetarySample: PVC (sou
24、rce)Plasticizer: DIDP (source)Mixer Temperature: 88CSpeed: 100 r/minMeas. Range: 500 mgZero Suppr: 0 %Damping: 1 sTest Time: 20 minSample Weight: 400.00 gPlasticizer Weight: 200.00 gNOTE 3When using equipment other than C. W. Brabender, refer tothe manufacturers suggested settings for their equipmen
25、t.11. Procedures11.1 Test Method A (Sigma Mixer):411.1.1 Attach the 650-mL oil (or electric) Sigma Mixer4tothe torque rheometer.11.1.2 Adjust the mixer-jacket temperature to 88 6 1C asmeasured at the thermocouple well.11.1.3 Set the mixer speed to 60 6 1 r/min.11.1.4 Weigh the resin and clay of the
26、following formulationinto the quart container and mix thoroughly with a spatula:Resin 225 6 0.1 gClay 40 6 0.1 gDIDP Plasticizer 124 6 0.1 g11.1.5 Wet the dispersion trough and the 400-mL beakerwith plasticizer and drain both for 1 min. Tare the prewettedbeaker and weigh 124 g of DIDP.NOTE 4The temp
27、erature and viscosity of the plasticizer is important(see 4.2 and section 4.3).11.1.6 With the mixer jacket at 88C and the mixer andrecorder running, remove the cover plate and add the PVC/claymix to the bowl. Replace bowl cover and continue mixing.3The C. W. Brabender PL 2000 Computerized Plasticor
28、der or ElectronicPlasticorder, a registered trademark of C. W. Brabender Instruments, Inc., 50 E.Wesley Street, South Hackensack, NJ 07606, or System 903, a registered trademarkof Haake Buchler Instruments, Inc., 244 Saddle River Road, Saddle Brook, NJ07662, or equivalents, have been found suitable
29、for this purpose.4Suitable equipment may be obtained from C. W. Brabender Instruments, Inc.,50 E. Wesley St., South Hackensack, NJ 07606, or Haake Buchler Instruments, Inc.,244 Saddle River Rd, Saddle Brook, NJ 07662.5C. W. Brabender Model 01-10-000, or equivalent, has been found suitable forthis pu
30、rpose.6Burgess No. 30, or equivalent, available from Burgess Pigment Co., Box 4146,Macon, GA 31208, has been found suitable for this purpose.TABLE 2 Interlaboratory Testing of ASTM No. 1 ResinLaboratory Powder-Mix Time, s Bowl Temperature, CA1 454 82.02 454 85.03 450 85.5AThe bowl temperature was me
31、asured at the thermocouple well.D 2396 94 (2004)211.1.7 After 4.5 min (or at a stock temperature of 88C)remove the cover plate and place the prewetted dispersiontrough over the bowl.11.1.8 At 5 min pour the DIDP evenly and quickly into thedispersion trough. Allow the beaker and trough to drain for 1
32、min. Remove the beaker and trough and replace the coverplate.11.1.9 Allow the ingredients to mix for at least 2 minbeyond the dry point. Turn off the mixer and recorder and cleanthe bowl.NOTE 5The mixer measuring head is best cleaned using a hose and avacuum cleaner to remove the bulk of the powder
33、from the bowl. Thebowl can then be opened, brushed, and blown clean. The walls of the bowland rotors should be wiped with a clean cloth. A drop of plasticizer placedbetween each rotor and back plate of the head will lubricate the rotors.11.1.10 For additional tests, repeat 11.1.4-11.1.9.11.2 Test Me
34、thod B (Planetary Mixer):511.2.1 Attach the Planetary Mixer to the torque rheometer.11.2.2 If the mixer is oil heated, make connections to theheating unit. Adjust the bowl temperature to 88 6 1C.11.2.3 Wet the dispersion funnel and the 400-mL beakerwith plasticizer and drain both for 1 min. Tare the
35、 prewettedbeaker and weigh 200 g DIDP.NOTE 6The temperature and viscosity of the plasticizer is important(see 6.2 and 6.3).11.2.4 Weigh 400 g PVC resin. Remove the bowl cover andadd the PVC resin. Replace the cover.NOTE 7If using the computerized torque rheometer, initiate thecomputer to calibrate t
36、he unit. Add the resin at the end of the calibration,and replace the cover and activate the test program.11.2.5 After mixing 4.5 min, place the prewetted dispersionfunnel in the slot on the bowl cover. After 5 min, pour theDIDP plasticizer into the dispersion funnel. Leave the funnel inplace until t
37、he end of the test.11.2.6 Allow the ingredients to mix for at least 2 minbeyond the dry point. Stop the mixer and vacuum the powderfrom the bowl and clean mixer components.11.2.7 For additional tests, repeat 11.2.3-11.2.6.12. Interpretation of Results12.1 Draw an average line (a line drawn through t
38、he middleof the oscillations) through the drop-off portion of the curvefrom the end of the lumpy stage to the dry point (see Fig. 3).12.2 Draw an average line (a line through the middle of theoscillations) through the section of the curve immediatelyfollowing the dry point (Fig. 3).12.3 Read the tim
39、e in seconds at the point at which theplasticizer was introduced (T1). Read the time in seconds at theintersection of the two lines from 12.1 and 12.2 (T2). SubtractT1from T2for the powder-mix time. Determine the powder-mix time to the nearest second.13. Report13.1 Report the following information:F
40、IG. 1 Distribution FunnelD 2396 94 (2004)313.1.1 Test method used, whether Test Method A (SigmaMixer4) or Test Method B (Planetary Mixer5),13.1.2 The poly(vinyl chloride) resin identification,13.1.3 The plasticizer or plasticizer blend used,13.1.4 The bowl temperature used in the test,13.1.5 The pow
41、der-mix time, as determined in Section 12,or the adsorption time from the computer printout.14. Precision and Bias14.1 Table 3 is the precision data obtained with this testmethod using ASTM #1 resin and the same DIDP plasticizer inthe same laboratory by a single operator on the same day. TheSigma4he
42、ad and Planetary5head were each maintained at88C. The sigma-head rotors were run at 60 r/min and theplanetary-mixer blade was run at 120 r/min.14.2 Table 3 is intended to compare the precision differencebetween Test Methods A and B and to provide the operatorwith a range of values that could be expe
43、cted using this testmethod.14.3 The concept of the “r” values (repeatability limits) inTable 3 is as follows:14.3.1 When comparing two test results for the samematerial, obtained by the same operator using the sameequipment on the same day, the two test results should bejudged not equivalent if they
44、 differ by more than the “r” valuefor that material.14.3.2 Any judgment in accordance with 14.3 would havean approximate 95 % (0.95) probability of being correct.14.4 Because of the interferences listed in Section 6 and theindividual procedural differences practiced by separate labora-tories, a roun
45、d robin was not performed. When a procedure hasbeen perfected to equate results between laboratories, aninterlaboratory precision will be developed.14.5 Bias is systematic error that contributes to the differ-ence between a test result and a true (or reference) value. Thereare no recognized standard
46、s on which to base an estimate ofbias for these test methods.15. Keywords15.1 poly(vinyl chloride); powder-mix time; torquerheometerFIG. 2 Planetary Mixer Dispersion FunnelTABLE 3 Precision of Test Methods A and B in a SingleLaboratoryTest MethodNumber ofTestsMean, Seconds Srr (Sr3 2.83)AB552082896.
47、01.617.04.5D 2396 94 (2004)4ANNEX(Mandatory Information)A1.See Fig. A1.1.FIG. 3 Powder-Mix ChartD 2396 94 (2004)5APPENDIX(Nonmandatory Information)X1.X1.1 Variations of plasticizer and bowl temperatures arerecommended where these changes would better classify aresin for the application. Such changes
48、 might be:X1.1.1 Another plasticizer or blend of plasticizers instead ofdiisodecyl phthalate, andX1.1.2 A bowl temperature lower than 88C would increasethe powder-mix time and highlight those resins having slowplasticizer absorption.NOTE 1circle = GP Resin O.square = GP Resin A.diamond = GP Resin P.
49、FIG. A1.1 Powder-Mix Time Versus DIDP TemperatureD 2396 94 (2004)6ASTM 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 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, eith
