1、Designation: D 7271 06Standard Test Method forViscoelastic Properties of Paste Ink Vehicle Using anOscillatory Rheometer1This standard is issued under the fixed designation D 7271; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, th
2、e 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 procedure for determiningthe viscoelastic properties of printing ink vehicles b
3、y measur-ing the G, G”, and tan delta using a controlled strain cone andplate oscillatory rheometer.1.2 This test method provides the flexibility of using severaldifferent types of rheometers to determine viscoelastic proper-ties in ink vehicles.1.3 This test method is not intended for systems that
4、arevolatile at procedure temperatures as evaporation may occureffectively changing the percent solids before testing is finishedand significantly altering the rheology.1.4 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.5 This
5、 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 the applica-bility of regulatory limitations prior to use.2. Referenced Documents
6、2.1 ASTM Standards:2E 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Terminology3.1 Definitions:33.1.1 frequency sweep test, nmost rheometers have pro-grams specific for their instrument.3.1.1.1 DiscussionThe user provides a specified geom-etry, fre
7、quency range, strain % or oscillatory stress andtemperature of the test. This test will produce the data requiredfor this method.3.1.2 G, nthe elastic (storage) modulus obtained from anoscillatory test represents the energy stored during each fre-quency cycle, where the stress is divided by the corr
8、espondinglinear elastic strain.3.1.3 G”, nthe viscous (loss) modulus obtained from anoscillatory test represents the amount of energy lost duringeach frequency cycle or the imaginary part of the complexmodulus (for shear).3.1.4 geometry, nthe cone used in the test.3.1.5 shear strain, nrelative defor
9、mation in shear; termoften abbreviated to shear.3.1.6 shear stress, nthe component of stress parallel to(tangential to) the area considered.3.1.7 strain, nthe measurement of deformation relative toa reference configuration.3.1.8 tan delta(d), nthe ratio of G” (viscous modulus) toG (elastic modulus).
10、3.1.9 viscoelasticity, nthe phenomena exhibited by a liq-uid when energy is applied and once the force is released, theliquid recovers towards its original state by means of storedenergy.4. Summary of Test Method4.1 Apply the ink vehicle to the plate of a rheometer.4.2 Select the geometry (cone) and
11、 set to the required gap tothe plate.4.3 Remove the excess vehicle with the ink spatula.4.4 Set the required temperature, strain or stress and fre-quency range for the frequency sweep. (Most rheometers havea test sequence that can be pre-prepared.)4.5 Allow five minutes for temperature calibration a
12、nd thevehicle to relax to its lowest energy state.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.37 on Ink VehiclesCurrent edition approved June 1, 2006. Published June 20
13、06.2For 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.3Many of the definitions came wholly or in part from “An I
14、ntroduction toRheology,” H.A. Barnes, J.F. Hutton, and K. Walters, Elesevier, 1989.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.NOTE 1Do not run a pre-shear sequence as this may affect results.4.6 Start the frequency sweep test.5.
15、 Significance and Use5.1 This test method has found acceptance in the litho-graphic ink industry in predicting rheological behavior of avehicle under press conditions caused by extrusion, shear-thinning rollers and dot gain recovery.5.2 This test method is restricted within the torque limita-tions a
16、nd strain resolution of the rheometer used.5.3 Results may not be reproducible if the vehicle is nothomogenous.6. Apparatus6.1 Oscillatory Rheometer, capable of over 400 Newtons offorce, running at the required frequency range, and controllingstrain in the 5 to 10 % range, as well as computer and so
17、ftwarecapable of running this test.6.2 Cone, preferably two cm and 2 (if the viscosity of thevehicle is too high for this geometry, other geometries may beused by agreement between customer and supplier).6.3 Spatula, non-abrasive to administer vehicle to the in-strument.7. Reagents and Materials7.1
18、Cleaning solvent.7.2 Lint free rags or tissue.8. Calibration and Standardization8.1 Calibrate the instrument using the procedure recom-mended by the manufacturer.9. Conditioning9.1 Since paste ink vehicles are shear thinning, care isneeded to ensure the test sample has not been sheared bystirring or
19、 kneading prior to testing.9.2 Allow vehicle to sit a minimum of five minutes if thevehicle has experienced shear forces before testing.10. Procedure10.1 After the instrument has been calibrated and cleaned,separate the geometry to administer approximately1gofvehicle (or sufficient amount to complet
20、ely fill geometry gap)to the center of the bottom plate.NOTE 2Do not leave air bubbles in the vehicle. If air-bubbles exist orsample does not fill entire geometry gap, either re-administer the sampleor carefully try to eliminate them with the spatula.10.2 Set the cone and plate to the required gap.
21、Many of therheometers will do this automatically.10.3 Using the spatula, carefully trim around cone anyexcess vehicle that may have been pushed from under the cone.10.4 Allow the vehicle to equilibrate to 25C (or requiredtemperature) for five minutes. (This is the test temperature thatshould be prog
22、rammed into the instrument prior to starting.)NOTE 3This method suggests that no pre-shear sequence is run. Thischanges the rheology of the sample and though the pre-shear sequencemay be reproducible, the resulting data is tampered by the pre-shear.10.5 Open the Frequency Sweep Test on the computera
23、ttached to the instrument.10.6 The frequency range should be 0.1 to 1.0 Hz inlogarithmic ramp mode. Set the number of readings to 20 in adecade.10.7 The strain should be 5 to 10 %. (If this instrument is acontrolled-strain rheometer, set the strain at 5 %.)10.8 Start the test as per instructions for
24、 the operationprocedure of the rheometer.10.9 The results will be over the entire frequency rangetested. The only results of interest for this method will be at 1.0Hz.10.10 Record the G, G”, and tan delta at 1.0 Hz.10.11 Clean the instrument.11. Report11.1 Report test data along with temperature, ge
25、ometry size,and frequency.12. Precision and Bias12.1 PrecisionAn interlaboratory study of the rheologicaldata of two varnishes, one resin solution and one lithographicprinting ink were run by 13 rheometers in eight laboratories.12.1.1 The precision estimates here are based on one analystin each labo
26、ratory performing duplicate determinations on eachof the samples.12.1.2 Practice E 691 was used in developing these preci-sion statements.12.2 Repeatability (Within-Laboratory)The 95 % repeat-ability of each sample is recorded in Table 1. The averagedeviation from average is 2.76 %.12.3 Reproducibil
27、ity (Multilaboratory)The 95 % repro-ducibility of each sample is recorded in Table 2. The averagedeviation from average is 4.66 %.12.4 BiasThe procedure in this test method has no biasbecause there is no standard calibration fluid for this testmethod.13. Keywords13.1 frequency sweep; G; G”; oscillat
28、ory rheometer; print-ing ink vehicles; rheology; tan delta; viscosityD7271062ASTM 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 validi
29、ty 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, either reapproved or withdrawn. Your commen
30、ts are 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 no
31、t received 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 cop
32、ies) 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-mail); or through the ASTM website(www.astm.org).TABLE 1 RepeatibilityAverage Repeatability % from AverageVarnish AG 6933.5 106.2 1.53G” 15548.5 326.0 2.
33、10tan delta 2.2 0.0 0.0Varnish BG 11677.3 279.5 2.39G” 20191.5 347.1 1.72tan delta 1.7 0.0 0.0Resin SolutionG 2617.1 147.1 5.62G” 6541.6 285.2 4.36tan delta 2.5 0.2 8.0InkG 3215.0 93.9 2.92G” 5372.6 241.5 4.50tan delta 1.7 0.0 0.0TABLE 2 ReproducibilityAverage Reproducibility % from AverageVarnish AG 6933.5 372.4 5.37G” 15548.5 877.1 5.64tan delta 2.2 0.0 0.0Varnish BG 11677.3 581.1 4.98G” 20191.5 856.8 4.24tan delta 1.7 0.0 0.0Resin SolutionG 2617.1 233.5 8.92G” 6541.6 433.7 6.62tan delta 2.5 0.2 8.0InkG 3215.0 211.3 6.57G” 5372.6 300.1 5.59tan delta 1.7 0.0 0.0D7271063
