1、Designation: D6267/D6267M 13Standard Test Method forApparent Viscosity of Hydrocarbon Resins at ElevatedTemperatures1This standard is issued under the fixed designation D6267/D6267M; the number immediately following the designation indicates theyear of original adoption or, in the case of revision,
2、the year of last revision. A number in parentheses indicates the year of lastreapproval. A superscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of the appar-ent viscosity of hydrocarbon resins having apparent
3、 viscositiesup to 2,000,000 millipascal seconds (mPas) (Note 1)attemperatures up to 300C 572F.NOTE 1The SI unit of (dynamic) viscosity is the pascal second. Thecentipoise (cP) is one millipascal second (mPas) and is frequently used asa viscosity unit.1.2 The values stated in either SI units or inch-
4、pound unitsare to be regarded separately as standard. The values stated ineach system may not be exact equivalents; therefore, eachsystem shall be used independently of the other. Combiningvalues from the two systems may result in non-conformancewith the standard.1.3 This standard does not purport t
5、o 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 Documents2.1 ASTM Standards:2D6440 Te
6、rminology Relating to Hydrocarbon ResinsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE1 Specification for ASTM Liquid-in-Glass Thermometers3. Terminology3.1 The definitions in Terminology D6440 are applicable tothis test method.3.2 Definition Specif
7、ic to This Standard:3.3 apparent viscosity, nof a hydrocarbon resin, the vis-cosity determined by this test method, expressed in millipascalseconds.3.3.1 DiscussionIts value may vary with the spindle androtational speed selected.4. Summary of Test Method4.1 The viscometer described in this test meth
8、od can beused to determine the apparent viscosity of hydrocarbon resinsat elevated temperatures. Apparent viscosity is determinedunder temperature equilibrium conditions using a rotatingspindle type viscometer. The torque on a spindle rotating in athermostatted sample holder containing a small amoun
9、t ofsample is used to measure the relative resistance to rotation. Afactor is applied to the torque reading to yield the viscosity inmPas.5. Significance and Use5.1 This test method is used to measure the apparentviscosity of hydrocarbon resins at elevated temperatures.Elevated temperature viscosity
10、 values of a hydrocarbon resinmay be related to the properties of coatings, adhesives and thelike, containing such a resin.5.2 For hydrocarbon resins, values of apparent viscositywill usually be a function of shear rate under the conditions oftest. Although the type of viscometer described in this t
11、estmethod operates under conditions of relatively low shear rate,shear rate depends on the spindle and rotational speed selectedfor a determination; therefore, comparisons between apparentviscosity values should be made only for measurements madewith similar viscometers under conditions of equivalen
12、t shearrate.6. Apparatus6.1 Rotational Viscometerrotating-spindle type with lev-eling stand.6.2 Viscometer Spindles, stainless steel. (WarningCaremust be taken in the storage and handling of spindles andassemblies. Protect them from scratches, dust, corrosion ordeposits, and mechanical abuse. Replac
13、e the spindle extensionif it is bent.Avoid touching the calibrated section of the spindle1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.34 on Pine Chemicals and Hydrocarbo
14、n Resins.Current edition approved Nov. 1, 2013. Published December 2013. Originallyapproved in 1998. Last previous edition approved in 2008 as D6267 08. DOI:10.1520/D6267_D6267M-13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.or
15、g. For Annual Book of ASTMStandards 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 States1with hands. Clean the spindle and sample chamber thoroughlyafter e
16、ach use. A recommended cleaning procedure is includedin the procedure.)6.3 Temperature Controller, Thermocontainer (a heater forthe sample chamber), and Sample Chamber, designed for usewith the viscometer in 6.1, complete with locating ring,leveling screws, safety guard, spindle extension, insulatin
17、g cap,alignment bracket, cooling plug (optional) and extracting tool.The precision temperature controller shall provide controlaccuracy of 61.0C or better through the range from 100 to150C 212 to 302F and 6 2.0C or better through the rangefrom 150 to 300C 302 to 572F.7. Assembly of Apparatus7.1 Asse
18、mble the apparatus according to the manufacturersinstructions.8. Calibration8.1 A digital viscometer should be zeroed according to themanufacturers instructions. For a dial-reading viscometer, nozero adjustment is required, since experience has shown thatthe zero point will not vary due to changes i
19、n the spring.NOTE 2The viscometer and spindles are precision equipment andshould be kept from undue shock and mishandling. Physical damage to theinstrument will often reveal itself as erratic or no oscillation of the readingwhen the instrument, with or without the spindle in place, is operated inair
20、. When operating normally, the reading in air will be stable and havefree oscillation about the zero point.8.2 The calibration of the instrument may be verified usingstandard reference fluids. Suitable fluids are available innominal viscosities up to 15 000 mPas at 149C 300F. Theprocedure for instru
21、ment calibration using standard referencefluids shall be that described by this test method. Resultsobtained using standard reference fluids should not deviatefrom the nominal viscosity by more than the following amount:=a21b2(1)where “a” is 1 % of the full measurement range under theconditions of t
22、he test, and “b” is 1 % of the nominal viscosityof the calibration fluid. If the results deviate by more than thisvalue, the instrument should be removed from use and re-paired.8.3 To check the controller and verify the calibration of thecontroller settings, use the procedure in 8.3.1 and 8.3.2.8.3.
23、1 Place enough silicone oil (or other high-boiling mate-rial that is liquid under the conditions of the determination) inthe sample container to permit immersion of the appropriateASTM thermometer to the proper depth. Suitable thermom-eters are shown in Table 1 in accordance with Specification E1.Te
24、mperature measuring devices such as RTDs, thermocouplesand liquid-in-glass thermometers with temperature range andaccuracy consistent with thermometers in Table 1 may be used.Adjust the thermal controller setpoint to provide the desiredtemperature.8.3.2 Insert the thermometer through the insulating
25、cover ofthe sample container, into the liquid, and hold it in place at thelevel required for proper immersion depth. Do not permit thethermometer bulb to rest on the bottom of the sample con-tainer. Adjust the thermal controller set point to provide thedesired temperature. Repeat this procedure for
26、each testtemperature desired.NOTE 3Particular care must be taken not to overflow the samplechamber when using the 100C, 76mm immersion thermometer, sincethe volume of the immersed stem is relatively large.9. Procedure9.1 Selection of SpindleFrom the estimated viscosity ofthe sample and the manufactu
27、rers instructions, select a vis-cometer and spindle combination that will produce readings inthe desired range.NOTE 4Use only spindles appropriate for the viscometer to be used.9.1.1 Where more than one spindle is available for the rangeselected, choose the spindle that produces a display or dialrea
28、ding between 10 and 100 % of full scale. The goal is toselect a combination whose range brackets the estimatedviscosity of the sample.NOTE 5Accuracy improves as the reading approaches 100 % of fullscale. If the reading is over 100 % of full scale, select a lower speed or asmaller spindle, or both. I
29、f the reading is under 10 % of full scale, selecta higher speed or a larger spindle, or both. Whenever possible, whenconducting multiple comparative tests, the same spindle/speed combina-tion should be used for all tests. When a test must be performed at severalspeeds, select a spindle that produces
30、 on-scale readings at all requiredspeeds. This may necessitate using a display or dial reading less than 10 %of full scale for some temperatures, which is acceptable as long as thereduced accuracy of such a reading is recognized.9.2 Preparation of SampleWeigh the amount of represen-tative sample, wh
31、ich when melted will be equivalent to thedesired test volume (see Table 2), into the sample chamber.Insert the sample chamber into the thermocontainer, preheatedto the desired test temperature.NOTE 6Use a fresh sample for each temperature for which adetermination is to be made. The sample should be
32、uniform in appearanceand free of foreign material.9.3 System Alignment and Spindle InsertionRaise theviscometer to clear the top of the thermocontainer. Connect thespindle extension to the spindle and to the coupling nut. Ifnecessary, connect the coupling nut to the viscometer shaftTABLE 1 Suitable
33、ASTM ThermometersTemperatureRangeImmersionmmScaleError,max90C - 170C 51 0.2C94F - 338F 51 0.5F145C - 206C 76 0.4CTABLE 2 Sample Size GuidelineSpindleApproximateVolume, mLApproximate SampleWeight, gSC 4-18 or equivalent 8.0 6.4SC 4-21 or equivalent 8.0 6.4SC 4-27 or equivalent 10.5 6.4SC 4-28 or equi
34、valent 11.5 9.2SC 4-29 or equivalent 13.0 10.4SC 4-31 or equivalent 10.0 8.0SC 4-34 or equivalent 9.5 7.6D6267/D6267M 132(note left-handed thread). With the viscometer aligned andleveled, lower the entire assembly until the spindle touches thesample in the chamber. Do not force the spindle into thes
35、ample, since this may result in bending the spindle extensionor causing it to detach from the spindle shaft.Allow the sampleto melt completely, but avoid prolonged heatingto minimizethermal and oxidative changes to the test material. Lower theassembly so that the tips of the alignment bracket are 2
36、mm116 in. above the horizontal surface of the locating ring,making contact with the vertical curve. A scribed line on theback of the vertical curve is the 2 mm 116 in. reference point.Do not forcibly displace the alignment bracket. Verify that theviscometer and thermocontainer are level. Place the i
37、nsulatingcap over the sample chamber inlet.9.4 Viscosity DeterminationEnsure that the material in thesample chamber is completely molten and that temperaturecontroller setting is proper. Turn on the viscometer, and allowthe spindle to rotate. When temperature equilibrium isindicated, typically after
38、 about 10 to 15 min., turn off theviscometer, remove the insulating cap, and inspect the liquidlevel on the spindle shaft. This level should be about 3 mm 18in. above the upper cone of the spindle. Do not overfill.Replace the insulating cap, and allow the unit to reestablishtemperature equilibrium.A
39、s needed, adjust the spindle speed tomaximize the on-scale reading at the test temperature. Con-tinue spindle rotation for 15 min after apparent equilibrium.For digital viscometers, record the display reading. For dial-reading viscometers, engage the pointer clutch and stop theviscometer motor when
40、the pointer is in view. Record the dialreading. Repeat this operation until 3 consecutive readingsdiffer by no more than 0.5 scale units (or 0.5 % of the viscosityvalue for a direct-reading viscometer.) (WarningThe spindleextension link should not come in contact with the insulatingcap when rotating
41、. The rotating spindle must not come incontact with the inside wall of the sample chamber.)9.5 Cleaning the ViscometerRemove the insulating capand turn off the motor. Unhook the spindle extension from thecoupling nut and remove the spindle from the sample chamber.Lift the sample chamber from the the
42、rmocontainer using theextracting tool and discard the sample in an appropriatemanner. With the sample chamber removed, (optionally) coolthe thermocontainer by inserting the cooling plug into thesample chamber well and circulating a cooling medium (tapwater) through it. Clean the spindle and sample c
43、hamber usingan appropriate solvent. Care must also be exercised to avoidscratching or deforming the spindles.10. Calculation10.1 Determine the average of the three acceptable scalereadings that differ by no more than 0.5 scale unit. If necessary,to convert to millipascal seconds, multiply the scale
44、reading bythe appropriate factor taken from the instrument instructionmanual. Repeat this for each temperature used.NOTE 7If desired, the viscosity at an intermediate temperature can becalculated by fitting 1/T versus log viscosity values to a straight line or byuse of curve-fitting software.11. Rep
45、ort11.1 Report the apparent melt viscosity at a given tempera-ture along with the instrument model, the spindle number, androtational speed.NOTE 8If it is desired to report the shear rate corresponding to theinstrument/spindle/speed combination, refer to the instrument instructionmanual for the appr
46、opriate calculation.12. Precision and Bias312.1 PrecisionAn interlaboratory study of the viscosity ofa standard oil at one temperature and the melt viscosity of threeresins each at 2 different temperatures was run in 1997 by 10laboratories. The precision, characterized by repeatability, sr, r,and re
47、producibility, SR and R, as specified in Practice E691,isshown in Table 3.12.2 BiasSince there is no accepted reference material,method or laboratory suitable for determining the bias for theprocedure in this test method, no statement on bias is beingmade.13. Keywords13.1 apparent viscosity; Brookfi
48、eld viscometer; rotationalviscometer; thermosel; viscosity3Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D01-1109. ContactASTM CustomerService at serviceastm.org.TABLE 3 Interlaboratory Precision Study ResultsMaterial Average,
49、cP Sr SR r RStandard Oil 4657.3 23.0 58.2 64.4 162.9Resin A, Temperature 1 9657.6 191.6 925.9 536.4 2592.6Resin A, Temperature 2 764.8 12.8 64.2 35.8 179.8Resin B, Temperature 1 1513.4 26.2 94.8 73.3 654.4Resin B, Temperature 2 480.2 6.6 31.5 18.4 88.3Resin C, Temperature 1 4420.0 58.6 172.8 164.2 438.8Resin C, Temperature 2 149.1 4.5 7.10 12.6 19.9D6267/D6267M 133ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users o
