1、Designation: D 6606 00 (Reapproved 2005)Standard Test Method forViscosity and Yield of Vehicles and Varnishes by the DukeViscometer1This standard is issued under the fixed designation D 6606; the number immediately following the designation indicates the year oforiginal adoption or, in the case of r
2、evision, 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 procedure for determiningthe viscosity of varnishes, ink vehicles, a
3、nd similar liquids thatare essentially nonvolatile and unreactive under ordinary roomconditions using the DukeAutomated high-shear rod and collarviscometer.21.2 The instrument in this test method is similar in principleto the falling-rod viscometer described in Test Method D 4040except that the coll
4、ar is motor driven and the range of availableshear stresses is considerably greater. This instrument iscapable of measured and extrapolated viscosity and yieldvalues provided the proper model is chosen for the givenapplication. See Section 6 for the ranges of specified models.1.3 The values stated i
5、n SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard does not purport to address all of thesafety concerns, if any, that may be associated with its use. Itis the responsibility of the user of this standard to establish anyappropriate
6、safety and health practices and determine theapplicability of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D 4040 Test Method for Rheological Properties of PastePrinting Inks and Vehicles by the Falling-Rod Viscometer3. Terminology3.1 Definitions Terms relative to t
7、his test method aredefined in Test Method D 4040 except for those found in 3.2.3.2 Definitions of Terms Specific to This Standard:3.2.1 yield value, nThe Lehmans yield value that isdefined as the stress at 2.5 s1.3.2.1.1 DiscussionThis value can be either extrapolatedor measured.3.2.2 shortness rati
8、o, na ratio to determine the shortnesscharacteristic of the fluid where SR = yield value/apparentviscosity.4. Summary of Test Method4.1 This automated test method is based upon accuratemeasurement of the force that is transferred at a knowntemperature into a stationary vertical rod as a fluid such a
9、sprinting ink/varnish moves through a precision measurementgap formed between the outside diameter of the rod and theinside diameter of collar of specific geometry as said collarmoves upward along the length of the rod at specifiedvelocities.4.2 The operator of the instrument and the customer mustag
10、ree on the preprogrammed test sequence, which is to be runfor a given material and the desired test temperature. Supervi-sory personnel should know the specifics of each prepro-grammed test sequence, how to change a given test sequence,and how to make a new test sequence.4.3 This test method provide
11、s actual measured test data offluids at specified shear rates, which can be programmed torelate. In addition to actual measured data, extrapolated datausing the “power law mathematical model” is provided thatcorrelates with manual testing methods as outlined in TestMethod D 4040.4.4 Specified test r
12、eference temperatures can range from 20to 40C. Allowable deviation from desired test referencetemperature could be specified differently in each test se-quence.Allowable programmable is within the range of 0.05 to0.4C.1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Rela
13、ted Coatings, Materials, andApplications and is the direct responsibility ofSubcommittee D01.37 on Ink Vehicles.Current edition approved Sept. 1, 2005. Published September 2005. Originallyapproved in 2000. Last previous edition approved in 2000 as D 6606 00.2The sole source of supply of an automated
14、 high shear rod and collar viscometerknown to the committee at this time is Duke Custom Systems, Inc., Pleasant View,TN. If you are aware of alternative suppliers, please provide this information toASTM International Headquarters. Your comments will receive careful consider-ation at a meeting of the
15、 responsible technical committee,1which you may attend.3For 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.1Copyr
16、ight ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 Actual direct measurements of apparent viscosity andstress at shear rates of interest can be useful in the practicalcontrol of ink viscosity during production and t
17、he specificationacceptance between supplier and purchaser.5.2 Use of the Duke automated viscometer provides directmeasurements for viscosity and yield value versus extrapolat-ing data points that may be far from the desired shear rates.6. Apparatus6.1 Table 1 describes each model of the Duke automat
18、edhigh shear rod and collar viscometer with the appropriateranges for the ink or varnish being tested.7. Materials7.1 ASTM Standard Viscosity Fluids(For calibration pur-poses only.) At approximately 100, 200, and 400 poise, spanthe practical range of the instrument without inducing self-heating erro
19、rs. The required fluids4are N4000 (100 poise at25C), S8000 (200 poise at 25C), and N15000 (400 poise at25C).7.2 Lint and Metal-Free Rags or Tissues of appropriatesize, so that they may be pulled or pushed completely throughthe collar in a single pass.7.3 Naphtha or other Low-Boiling Solvent in a was
20、h bottleor closed metal container.8. Hazards8.1 Warning: Solvents may be hazardous to the skin andeyes. In addition to other precautions, always wear protectivegloves and safety glasses during cleanup to avoid solventcontact with skin and eyes. See suppliers material safety datasheet for further inf
21、ormation on each solvent used.8.2 Instrument Warning: Never operate the instrument withthe rod installed without fluid in the collar.9. Preparation of Apparatus9.1 Set the viscometer up on a sturdy vibration-free benchcapable of supporting at least 6.75 sq. m.9.2 Locate the viscometer in an area fre
22、e of direct sunlightto prevent sun-induced heating inside the clear temperature-controlled enclosure.9.3 Level the viscometer by turning the adjustable feet up ordown until the spirit level is centered and the instrument is freefrom wobble.9.4 Clean the rod and collar thoroughly with tissues wettedw
23、ith naphtha or other appropriate solvent. Remove residualsolvent with clean dry tissue. Ensure rod and collar are free oflint or other particles from tissue or environment. Warning:Failure to clean instrument adequately will severely influenceresults.9.5 Ensure identification code on rod and collar
24、match.9.6 Properly install and lock into viscometer the rod withrod cup and collar in accordance with manufacturers recom-mendations.9.7 Plug in collar/sample temperature probe.9.8 Allow instrument to equilibrate at a desired test tem-perature.10. Calibration10.1 Ensure instrument is within calibrat
25、ion window byreading information contained in “Days to Next CalibrationWindow” on the computer screen.The number of days until thenext factory-authorized calibration is displayed whenever theinstrument is not in active use.10.2 Periodically check calibration as in Section 17.11. Sample Preparation11
26、.1 Transport sample to be tested to the test area andpreserve in a suitable clean closed container. Skin paper shouldbe used for oxidative fluids.11.2 Samples should be uniform dispersions or structuresthroughout. Samples to be tested should be free of bubbles,skin, or other debris. If variations in
27、 structure are suspected, thesample must be remixed until it is of uniform consistency.11.3 Fill pipet with the sample and place filled pipet into thetemperature-controlled enclosure of viscometer. Warning: Donot work the sample vigorously. Be sure to close the samplecontainer immediately after remo
28、ving the desired sample to betested.12. Conditioning12.1 The test sequence and reference temperatures areprogrammable and are protected by password security toprevent unauthorized changes from desired temperatures. The4The sole source of supply of the certified standard viscosity oil known to thecom
29、mittee at this time is Cannon Instrument Company, P.O. Box 16, State College,PA 16801. If you are aware of alternative suppliers, please provide this informationto ASTM International Headquarters. Your comments will receive careful consid-eration at a meeting of the responsible technical committee,1
30、which you may attend.TABLE 1 Performance Ranges For Each ModelModel Number Stress Range (Dynes/cm2)Viscosity RangePoise at 2500sec1Shear Rate Range(sec1)Temperature Range CD-2010 D-2010ED-2012 D-2012E751.031064 400 2.5 10,000 1940D-2020 D-2020ED-2022 D-2022E1502.0310610 800 2.5 10,000 1940D-2050 D-2
31、050ED-2052 D-2052E3005.0310620 1,600 2.5 7,500 1940D-2100 D-2100ED-2102 D-2102E600 10.0310740 3,200 2.5 7,500 1940D 6606 00 (2005)2reference temperature for this test method is 25.0 and theenclosure temperature for this test method is 24.95C.12.2 The pipet containing the sample should remain insidet
32、he temperature-controlled enclosure a minimum of one minutebefore the sample is placed on the rod. Samples are approxi-mately 2.2 ml and will quickly reach equilibrium.13. Procedure for Test Runs13.1 Allow instrument to equilibrate to desired test tempera-ture.13.2 Ensure sample to be tested, in pip
33、ette, is placed in itsholder inside the temperature-controlled enclosure.13.3 Select the desired test sequence from a list of prepro-grammed test sequences. (Press F1 key for list). See Section 18for details of test sequence specific to this test method.13.4 Start selected test sequence. (Press F2 k
34、ey.)13.5 Enter Test ID name. This is mandatory. (Name must beDOS compatible.) (Press Enter key.)13.6 Enter Operator ID (Optional). (Press Enter key.)13.7 Enter Formula ID (Optional). (Press Enter key.)13.8 Enter Batch ID (Optional). (Press Enter key.)13.9 Follow the instructions on computer screen.1
35、3.10 Open doors. Rod will start rotating once doors open.13.11 Place sample onto rotating rod just above the collar.Ensure sample is distributed completely around rotating rod.NOTE 1Do not place sample on upper 2 in. of the rod.13.12 Close doors. The rod will stop rotating.13.13 Press the Enter key
36、to proceed with the selected testsequence.13.14 No additional operator action is required until test iscompleted. The instrument will proceed automatically follow-ing preprogrammed specifications of the selected test se-quence. (Rates of shear and allowable temperature deviations.)13.15 After comple
37、tion of the test, the operator must re-move rod and collar assembly for cleaning.13.15.1 Open doors of temperature-controlled enclosure.13.15.2 Unplug collar/sample temperature sensor cable.13.15.3 Unlock collar assembly by pulling outwards oncollar on collar lock slide assembly.13.15.4 Unlock rod a
38、ssembly by pressing down on rod lockring. While rod lock ring is depressed, lift rod assemblyapproximately 12.3 mm. Release pressure on rod lock ring.13.15.5 With one hand on top and the other hand at bottomof rod, lift rod and collar assembly up through collar mount.Remove your hand from bottom of
39、rod long enough for bottomto clear collar mount.13.15.6 Take rod and collar assembly to designated cleanupstation.13.15.7 Before cleaning rod and collar assembly, if avail-able, insert secondary rod and collar assembly into the primaryposition in instrument by reversing steps 13.15.7-13.15.1.13.15.8
40、 Close doors on temperature-controlled enclosure.13.15.9 Return to cleanup station, the thoroughly clean rodand collar assembly using appropriate solvent and tissues orrags.13.15.10 Return clean rod and collar assembly totemperature-controlled enclosure. If secondary rod and collarare inserted, plac
41、e this rod and collar assembly on storage rackinside left side of enclosure. If secondary rod and collar are notinserted into instrument, replace this rod and collar assemblyinto primary position by reversing steps 13.15.7-13.15.1.13.16 Remove printout of test data from printer.13.17 Instrument is r
42、eady for next test.14. Test Data Available14.1 This instrument can provide these values for eachstroke of the test sequence performed: measured temperature,measured stress, measured rate of shear, measured grams, andelapsed seconds. The instrument can provide temperature-corrected measured stress an
43、d viscosity if the sequence was notperformed at exactly the desired reference temperature.14.2 In addition, this instrument can compute apparentviscosity at 2500 s1, extrapolated yield stress at 2.5 s1, andshortness factor. These values are derived from the Power LawModel.15. Report15.1 Report measu
44、red and apparent viscosity at 2,500 s1,measured yield stress at 2.5 s1, measured shortness factor,reference temperature, test sequence number, instrument modelnumber, and instrument serial number.16. Precision16.1 PrecisionAn interlaboratory study of this methodwas conducted in which a single operat
45、or in each of sevenlaboratories made one run consisting of four varnishes and oneink. The samples ranged in viscosity from 250 to 1200 P. Thevarnishes were of different rheological character to reflect arange of shortness ratios applicable to those seen in the graphicarts industry. The estimated sta
46、ndard deviations and degrees offreedom are given inTable 2. (Since the standard deviations areproportional to the test value, precision statements are made interms of percent of the observed value.) Based on thesestandard deviations, the following criteria should be used forjudging the acceptability
47、 of results at the 95 % confidencelevel.16.2 ReproducibilityTwo results, each the mean of resultsobtained on different days by operators in different laboratoriesshould be considered suspect if they differ more than theallowable differences indicated in Table 2.TABLE 2 Reproducibility Round Robin Re
48、sultsTest ResultsStandard Deviation% RelativeDegrees ofFreedomMaximumAllowableDifference, 6 %RelativeReproducibilityMeasured Viscosity at2500 s14.68 6 4.33Extrapolated Viscosityat 2500 s14.69 6 4.34Measured Yield Stressat 2.5 s15.26 6 4.86Measured ShortnessRatio6.79 6 6.28D 6606 00 (2005)317. Keywor
49、ds17.1 apparent viscosity; automated viscometers; falling-rodviscometers; non-Newtonian; power law model; rod and collarviscometers; shortness; vehicles; viscometers; viscosity; yieldvalueANNEXES(Mandatory Information)A1. CHECKING INSTRUMENT CALIBRATIONA1.1 Thoroughly clean rod and collar assembly usingappropriate solvent and tissues or rags.A1.2 Thoroughly clean all mechanicals inside temperature-controlled enclosure. Use appropriate solvents and tissues orrags. Remove all lint, dust, and visible particulate matter usinga vacuu
