1、Designation: D 6267 05Standard Test Method forApparent Viscosity of Hydrocarbon Resins at ElevatedTemperatures1This standard is issued under the fixed designation D 6267; 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 (e) 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 viscositie
3、sup 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 SI units are to be regarded as th
4、estandard. The values given in parentheses are for informationonly.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 practices and determine the ap
5、plica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 6440 Terminology Relating to Hydrocarbon ResinsE1 Specification for ASTM Liquid-in-Glass ThermometersE 691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3. Te
6、rminology3.1 The definitions in Terminology D 6440 are applicable tothis test method.3.2 Definition Specific to This Standard:3.3 apparent viscosity, nof a hydrocarbon resin, theviscosity determined by this test method, expressed in milli-pascal seconds.3.3.1 DiscussionIts value may vary with the sp
7、indle androtational speed selected.4. Summary of Test Method4.1 The viscometer described in this test method can beused to determine the apparent viscosity of hydrocarbon resinsat elevated temperatures. Apparent viscosity is determinedunder temperature equilibrium conditions using a rotatingspindle
8、type viscometer. The torque on a spindle rotating in athermostatted sample holder containing a small amount 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 m
9、easure the apparentviscosity of hydrocarbon resins at elevated temperatures.Elevated temperature viscosity 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
10、 a function of shear rate under the conditions oftest. Although the viscometer described in this test methodoperates under conditions of relatively low shear rate, shearrate depends on the spindle and rotational speed selected for adetermination; therefore, comparisons between apparent vis-cosity va
11、lues should be made only for measurements madewith similar viscometers under conditions of equivalent shearrate.5.3 Approximate shear rates using various spindles areshown in Table A1.1 in Annex A1 to this procedure.6. Apparatus6.1 Rotational Viscometerrotating-spindle type with lev-eling stand.6.2
12、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. Replace the spindle extensionif it is bent.Avoid touching the calibrated section of the spindlewith ha
13、nds. Clean the spindle and sample chamber thoroughlyafter each use. A recommended cleaning procedure is includedin the procedure.)1This test method is under the jurisdiction of ASTM Committee D01 on Paintand Related Coatings, Materials , andApplications and is the direct responsibility ofSubcommitte
14、e D01.38 on Hydrocarbon Resins.Current edition approved Jan. 1, 2005. Published February 2005. Originallyapproved in 1998. Last previous edition approved in 1998 as D 6267 98.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For
15、 Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.3 Temperature Controller, Thermocontainer (a heater forthe sample cha
16、mber), and Sample Chamber, designed for usewith the viscometer in 6.1, complete with locating ring,leveling screws, safety guard, spindle extension, insulating cap,alignment bracket, cooling plug (optional) and extracting tool.The precision temperature controller shall provide controlaccuracy of 61.
17、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 Assemble the apparatus according to the manufacturersinstructions.8. Calibration8.1 A digital viscometer should be zeroed according to themanu
18、facturers instructions. For a dial-reading viscometer, nozero adjustment is required, since experience has shown thatthe zero point will not vary due to changes in the spring.NOTE 2The viscometer and spindles are precision equipment andshould be kept from undue shock and mishandling. Physical damage
19、 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. When operating normally, the reading in air will be stable and havefree oscillation about the zero point.8.2 The calibration of the inst
20、rument may be verified usingstandard reference fluids. Suitable fluids are available innominal viscosities up to 15 000 mPas at 149C (300F). Theprocedure for instrument calibration using standard referencefluids shall be that described by this test method. Resultsobtained using standard reference fl
21、uids should not deviatefrom the nominal viscosity by more than the following amount:=a21 b2(1)where “a” is 1 % of the full measurement range under theconditions of the test, and “b” is 1 % of the nominal viscosityof the calibration fluid. If the results deviate by more than thisvalue, the instrument
22、 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 8.3.2.8.3.1 Place enough silicone oil (or other high-boiling mate-rial that is liquid under the conditions of the determination) inthe sample con
23、tainer to permit immersion of the appropriateASTM thermometer to the proper depth. Suitable thermom-eters are shown in Table 1 in accordance with SpecificationE1. Adjust the thermal controller setpoint to provide thedesired temperature.8.3.2 Insert the thermometer through the insulating cover ofthe
24、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 each testtem
25、perature 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 Table A1.1, Annex A1; sel
26、ect a viscometer andspindle combination that will produce readings in the desiredrange.NOTE 4Use only spindles shown to be appropriate for the viscometerto be used.9.1.1 Where more than one spindle is available for the rangeselected, choose the spindle that produces a display or dialreading between
27、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. If the reading
28、 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 on-scale rea
29、dings 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, which when melt
30、ed will be equivalent to the testvolume (see Table 2), into the sample chamber. Insert thesample chamber into the thermocontainer, preheated to thedesired test temperature.NOTE 6Use a fresh sample for each temperature for which adetermination is to be made. The sample should be uniform in appearance
31、and 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 shaft(note left-handed thread). With the vi
32、scometer aligned andleveled, lower the entire assembly until the spindle touches thesample in the chamber. Do not force the spindle into thesample, since this may result in bending the spindle extensionTABLE 1 Suitable ASTM ThermometersTemperatureRangeImmersionmmScaleError,maxASTMThermometerNumber90
33、C - 170C 51 0.2C 35C-6294F - 338F 51 0.5F 35F-62145C - 206C 76 0.4C 100C-68TABLE 2 Sample Size GuidelineSpindleApproximateVolume, mLApproximate SampleWeight, gSC 4-18 8.0 6.4SC 4-21 8.0 6.4SC 4-27 10.5 6.4SC 4-28 11.5 9.2SC 4-29 13.0 10.4SC 4-31 10.0 8.0SC 4-34 9.5 7.6D6267052or causing it to detach
34、 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 mm(116 in.) above the horizontal surface of the locating ring,making contact with th
35、e 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 insulatingcap over the sample chamber inlet.9.4 Viscosity DeterminationEnsure tha
36、t 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 is indi-cated, typically after about 10 to 15 min., turn off theviscometer, remove the insulating cap, and i
37、nspect 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. Continue spindle rotation for 15 minafter apparent equilibrium. Increase the
38、 spindle speed tomaximize the reading at the test temperature. For digitalviscometers, record the display reading. For dial-reading vis-cometers, engage the pointer clutch and stop the viscometermotor when the pointer is in view. Record the dial reading. Fordigital viscometers, record the display re
39、ading. Repeat thisoperation until 3 consecutive readings differ by no more than0.5 scale units (or 0.5 % of the viscosity value for a direct-reading viscometer.) (WarningThe spindle extension linkshould not come in contact with the insulating cap whenrotating. The rotating spindle must not come in c
40、ontact with theinside 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 thermocontainer using theextracting tool and
41、 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 chamber usingan appropriate solvent. Care
42、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 reading bythe appropriate factor taken fr
43、om either the instrument instruc-tion manual or Table A1.2 in the Annex A1. Repeat this foreach 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. Report
44、11.1 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 Table A1.1 (or the equiva-lent) for the appropri
45、ate 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 reprod
46、ucibility, SR and R, as specified in Practice E 691,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; Brookfield
47、 viscometer; rotationalviscometer; thermosel; viscosity3Supporting data are available from ASTM International Headquarters. RequestRR: D011109.TABLE 3 Interlaboratory Precision Study ResultsMaterial Average, cP Sr SR r RStandard Oil 4657.3 23.0 58.2 64.4 162.9Resin A, Temperature 1 9657.6 191.6 925.
48、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 19.9D6267053ANNEX(Mandatory Information)A1. V
49、ISCOMETER RANGE DATA AND VISCOMETER-SPINDLE FACTORSA1.1 Table A1.1 and Table A1.2 illustrate viscometer rangedata and viscometer-spindle factors.NOTE A1.1For each range, the first number represents the minimumrecommended measurable viscosity (10 % of the lowest full scale of eachviscometer).TABLE A1.1 Viscometer Range DataLV Series ViscometersViscosity Range (cP)Spindle LVT LVF 5XLVTShearRate(sec1)SampleVolume(ml)SC4-18 5-10 000 5-500 25-50 000 1.32NA8.0SC4-31 5-100 000 50-5 000 250-250 000 0.34N 10.0SC4-34 100-200 000 100-10 000
