1、Designation: D8020 15Standard Test Method forFreeze-Thaw Viscosity Stability of Water-Based Inks and InkVehicles1This standard is issued under the fixed designation D8020; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 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 a procedure for evaluating theeffect of freeze-thaw cycling on the properties of water-basedi
3、nks and ink vehicles.1.2 This test is based on a similar standard test for coatings;Test Method D2243.1.3 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns,
4、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 Documents2.1 ASTM Standards:2D2243 Test Method for Freeze-Thaw Resistance
5、of Water-Borne CoatingsD2196 Test Methods for Rheological Properties of Non-Newtonian Materials by Rotational ViscometerD4212 Test Method for Viscosity by Dip-Type ViscosityCupsE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory St
6、udy toDetermine the Precision of a Test Method3. Summary of Test Method3.1 The waterborne ink or ink vehicle is placed into two237-mL plastic jars. One jar is stored at room temperature,while the other jar is subjected to cycles of freezing andthawing. After cycling, the ink or ink vehicle is examin
7、ed forchanges in viscosity and uniformity.4. Significance and Use4.1 When waterborne inks and ink vehicles are shippedduring cold weather, these materials may experience cycles offreezing and thawing. This can damage the material renderingit unusable.4.2 Cycles of freezing and thawing can cause more
8、 damageto waterborne inks or ink vehicles than when the inks or inkvehicles are subjected to steady freezing.5. Apparatus5.1 Test Chamber, a suitable cabinet, room, or enclosurespace large enough to contain the specimens to be testedpermitting at least 25 mm (1 in.) of air space between the sidesof
9、adjacent jars and capable of being maintained continuouslyat a temperature of 18C (0F).NOTE 1Although a variation of the test chamber temperature of 62C(3.5F) is allowed, the test chamber temperature should be maintained asnear 18C (0F) as practicable and the amount of variation should berecorded an
10、d reported.5.2 Viscometer, a dip-type viscosity cup as described in TestMethod D4212 or a Brookfield type viscometer as described inTest Methods D2196.5.3 Recirculating Water Bath, capable of maintaining atemperature of 25 6 1C (77 61.8F).5.4 Cylindrical Container, with a capacity of 0.5-L (1-pt),85
11、 mm (338 in.) diameter to contain the test specimen duringtesting.5.5 Spatula.6. Sampling and Test Specimens6.1 Ensure that the bulk sample from which the jars arefilled is well stirred and uniform, the containers used are clean,and the lids are applied promptly to the jars to preventevaporation los
12、ses. Prepare two specimens for testing by filling0.5-L plastic jars with 400 mL of the ink or ink vehicle.Identify one as the test specimen and the other as the controlspecimen.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications
13、 and is the direct responsibility ofSubcommittee D01.37 on Ink Vehicles.Current edition approved Dec. 1, 2015. Published January 2016. DOI: 10.1520/D8020-15.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of AS
14、TMStandards volume information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States17. Procedure7.1 Stir the specimen by hand and measure its viscosity inaccordance with Test
15、 Methods D4212 or D2196.7.2 Store the control specimen at room temperature.7.3 Place the test specimen in the chamber maintained at18C (0F) in such a manner that it does not touch the wallsor bottom of the chamber and air circulates around it freely.Placing jars on racks that raise them off the bott
16、om of thechamber or upon pieces of insulating board resting on thebottom is suggested. In the case of several test specimens,maintain a minimum of 25 mm (1 in.) of air space betweenadjacent jars and between jars and the chamber walls.7.4 Remove the test specimen from the chamber after 17 h.Place it
17、adjacent to the control specimen and allow it to standfor 5 h undisturbed at room temperature, followed by2hinarecirculating water bath for a complete freeze-thaw cycle of24 h.7.5 Examine both the test and control specimens for anyevidence of settling, gelation, and coagulation.7.6 Stir the test and
18、 control ink or ink vehicle by hand usinga spatula. Stir carefully so as to avoid air entrainment andfoam. Measure the viscosities in accordance with Test MethodsD4212 or D2196. Record the temperature at which the viscos-ity is measured.7.7 Repeat 7.2 7.6 for two additional freeze-thaw cycles,or as
19、many as agreed on between cooperating laboratories orbuyer and seller. If any test specimen more than doubles inviscosity compared to the control the test is stopped.8. Interpretation of Results8.1 The cycle is considered passed if the viscosity of the testspecimen is less than double the viscosity
20、of the control and thetest specimen does not exhibit coagulation or gelation. If theviscosity of the test specimen more than doubles, the test isstopped and the specimen fails. If a test specimen passes threecycles, it is considered freeze-thaw stable.9. Report9.1 Report the following information:9.
21、1.1 The condition of the ink or ink vehicle in the jar inaccordance with 7.5 after each cycle.9.1.2 The change in viscosity between the test and controlinks or ink vehicles in accordance with 7.6.9.1.3 The number of cycles passed by the test specimen.10. Precision and Bias310.1 The precision of this
22、 test method is based on aninterlaboratory study of ASTM D8020, Test Method forFreeze-Thaw Viscosity Stability of Water-Based Inks and InkVehicles, conducted in 2013. A total of six laboratories testedfive different samples, using two methods. Every “test result”represents an individual determinatio
23、n, and one participant wasasked to report duplicate test results. Practice E691 wasfollowed for the design and analysis of the data; the details aregiven in ASTM Research Report RR:D01-1180.10.1.1 Repeatability (r)The difference between repetitiveresults obtained by the same operator in a given labo
24、ratoryapplying the same test method with the same apparatus underconstant operating conditions on identical test material withinshort intervals of time would in the long run, in the normal andcorrect operation of the test method, exceed the followingvalues only in one case in 20.10.1.1.1 Repeatabili
25、ty can be interpreted as maximum dif-ference between two results, obtained under repeatabilityconditions, that is accepted as plausible due to random causesunder normal and correct operation of the test mehtod.10.1.1.2 Repeatability limits are listed in Tables 1-8.10.1.2 Reproducibility (R)The diffe
26、rence between twosingle and independent results obtained by different operatorsapplying the same test method in different laboratories usingdifferent apparatus on identical test material would, in the longrun, in the normal and correct operation of the test method,exceed the following values only in
27、 one case in 20.10.1.2.1 Reproducibility can be interpreted as maximumdifference between two results, obtained under reproducibilityconditions, that is accepted as plausible due to random causesunder normal and correct operation of the test method.10.1.2.2 Reproducibility limits are listed in Tables
28、 1-8.10.1.3 The above terms (repeatability limit and reproduc-ibility limit) are used as specified in Practice E177.10.1.4 Any judgment in accordance with statements 10.1.1and 10.1.2 would normally have an approximate 95 % prob-ability of being correct, however the precision statistics ob-tained in
29、this ILS must not be treated as exact mathematical3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1180. ContactASTM CustomerService at serviceastm.org.TABLE 1 Brookfield Viscosity (cps)InitialMaterialAverageARepeatabilitySta
30、ndardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXsrSRrRControl 1 316.050 5.485 44.682 15.358 125.109Control 2 340.633 6.928 57.275 19.399 160.370Control 3 321.300 6.351 43.168 17.782 120.871Control 4 318.133 6.351 41.722 17.782 116.822Control 5 316.383 2.021 51.93
31、8 5.658 145.426AThe average of the laboratories calculated averages, when duplicates were reported.D8020 152quantities which are applicable to all circumstances and uses.The limited number of materials tested and laboratories report-ing results guarantees that there will be times when differencesgre
32、ater than predicted by the ILS results will arise, sometimeswith considerably greater or smaller frequency than the 95 %probability limit would imply. The repeatability limit and thereproducibility limit should be considered as general guides,and the associated probability of 95 % as only a roughind
33、icator of what can be expected.10.2 BiasAt the time of the study, there was no acceptedreference material suitable for determining the bias of this testmethod, therefore no statement on bias is being made.TABLE 2 Brookfield Viscosity (cps)After 1 CycleMaterialAverageARepeatabilityStandardDeviationRe
34、producibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXsrSRrRControl 1 299.033 9.815 37.637 27.482 105.384Test 1 283.883 6.640 41.566 18.591 116.384Control 2 315.867 6.351 31.108 17.782 87.103Test 2 338.717 3.753 37.497 10.508 104.992Control 3 311.050 6.640 36.289 18.591 101.609Test 3
35、342.633 4.619 35.549 12.933 99.538Control 4 301.783 10.104 32.286 28.290 90.400Test 4 352.550 3.753 35.062 10.508 98.175Control 5 301.283 1.443 30.219 4.041 84.613Test 5 419.717 2.598 74.624 7.275 208.947AThe average of the laboratories calculated averages, when duplicates were reported.TABLE 3 Broo
36、kfield Viscosity (cps)After 2 CyclesMaterialAverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXsrSRrRControl 1 306.633 2.598 46.984 7.275 131.555Test 1 305.633 0.000 49.440 0.000 138.433Control 2 320.550 1.443 40.122 4.041 112.343Test 2 365.2
37、17 3.753 42.159 10.508 118.044Control 3 312.717 0.866 38.818 2.425 108.691Test 3 397.633 1.732 69.054 4.850 193.351Control 4 305.050 3.753 37.384 10.508 104.676Test 4 411.550 1.443 69.273 4.041 193.964Control 5 312.133 2.887 38.025 8.083 106.470Test 5 551.533 14.722 128.407 41.223 359.541AThe averag
38、e of the laboratories calculated averages, when duplicates were reported.TABLE 4 Brookfield Viscosity (cps)After 3 cyclesMaterialAverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXsrSRrRControl 1 310.967 2.309 54.256 6.466 151.916Test 1 316.5
39、50 2.021 50.095 5.658 140.267Control 2 328.383 5.485 46.462 15.358 130.092Test 2 383.717 7.794 48.622 21.824 136.140Control 3 319.800 1.155 49.092 3.233 137.458Test 3 426.217 3.753 60.506 10.508 169.415Control 4 314.633 0.577 47.073 1.617 131.805Test 4 467.300 9.815 79.299 27.482 222.037Control 5 31
40、9.967 1.732 46.271 4.850 129.559Test 5 615.633 14.434 110.186 40.415 308.520AThe average of the laboratories calculated averages, when duplicates were reported.D8020 15310.3 The precision statement was determined through sta-tistical examination of 245 test results, reported by 6laboratories, on 5 s
41、amples plus 5 controls.10.4 To judge the equivalency of two test results, it isrecommended to choose the material closest in characteristicsto the test material.11. Keywords11.1 freeze-thaw resistance; resistance to low-temperaturecyclingTABLE 5 Standard Zahn (sec)InitialMaterialAverageARepeatabilit
42、yStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXsrSRrRControl 1 18.808 0.318 1.161 0.889 3.249Control 2 19.275 0.202 1.232 0.566 3.450Control 3 18.850 0.404 1.968 1.132 5.510Control 4 18.817 0.289 1.746 0.808 4.888Control 5 18.992 0.202 1.251 0.566 3.503AThe
43、average of the laboratories calculated averages, when duplicates were reported.TABLE 6 Standard Zahn (sec)After 1 CycleMaterialAverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXsrSRrRControl 1 18.533 0.346 0.989 0.970 2.770Test 1 18.267 0.00
44、0 1.662 0.000 4.654Control 2 19.350 0.231 1.118 0.647 3.130Test 2 19.875 0.202 1.211 0.566 3.390Control 3 18.692 0.433 1.183 1.212 3.313Test 3 20.783 0.404 1.420 1.132 3.975Control 4 18.358 0.260 1.189 0.727 3.330Test 4 21.250 0.000 1.961 0.000 5.492Control 5 19.200 0.058 0.757 0.162 2.121Test 5 22.
45、992 0.318 3.613 0.889 10.118AThe average of the laboratories calculated averages, when duplicates were reported.TABLE 7 Standard Zahn (sec)After 2 CyclesMaterialAverageARepeatabilityStandardDeviationReproducibilityStandardDeviationRepeatabilityLimitReproducibilityLimitXsrSRrRControl 1 18.450 0.520 1
46、.344 1.455 3.763Test 1 19.133 0.635 2.228 1.778 6.239Control 2 19.192 0.375 1.985 1.051 5.558Test 2 21.450 0.404 1.610 1.132 4.508Control 3 19.158 0.548 1.725 1.536 4.831Test 3 22.883 0.981 1.725 2.748 4.830Control 4 19.442 0.202 1.714 0.566 4.800Test 4 23.025 1.068 1.726 2.991 4.832Control 5 19.217
47、 0.520 1.500 1.455 4.199Test 5 27.300 1.328 3.478 3.718 9.737AThe average of the laboratories calculated averages, when duplicates were reported.D8020 154ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard.
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