1、Designation: D2669 06 (Reapproved 2012)1Standard Test Method forApparent Viscosity of Petroleum Waxes Compounded withAdditives (Hot Melts)1This standard is issued under the fixed designation D2669; the number immediately following the designation indicates the year oforiginal adoption or, in the cas
2、e of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTEAdded mercury caveat editorially in April 2012.1. Scope1.1 This test method covers the determinati
3、on of the appar-ent viscosity of petroleum waxes compounded with additives(hot melts). It applies to fluid hot melts having apparentviscosities up to about 20 Pas at temperatures up to 175C(347F).NOTE 1For petroleum waxes and their blends having low apparentviscosities, below about 15 mPas, Test Met
4、hod D445, is especiallyapplicable.1.2 The values stated in SI units shall be regarded as thestandard. One pascal second (Pas) = 1000 centipoises (cP).One millipascal second (mPas) = 1 centipoise (cgs units).1.3 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material tha
5、t can causecentral nervous system, kidney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebs
6、itehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. I
7、t 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:2D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and
8、Calculation of Dynamic Viscos-ity)E1 Specification for ASTM Liquid-in-Glass ThermometersE180 Practice for Determining the Precision of ASTMMethods for Analysis and Testing of Industrial and Spe-cialty Chemicals33. Terminology3.1 Definitions:3.1.1 viscositythe ratio of shear stress to shear rate.Visc
9、osity of a liquid is a measure of the internal friction of theliquid in motion. The unit of dynamic viscosity is the pascalsecond. For a Newtonian liquid, the viscosity is constant at allshear rates. For a non-Newtonian liquid, viscosity will varydepending on shear rate.3.1.2 viscosity, apparentthe
10、viscosity determined by thismethod, expressed in pascal seconds. Its value may vary withthe spindle and rotational speed selected because many hotmelts are non-Newtonian.4. Summary of Test Method4.1 Approximately 800 g of sample are melted on a hotplate or in an oven. An 800-mL glass beaker which is
11、 jacketedwith an electric heating mantle is filled with the melted sampleto a level of about 25 mm (1 in.) from its top. The viscometer,with attached spindle and guard, is properly positioned. Stir-ring is begun and continued while the temperature of thesample is brought to slightly above the highes
12、t desired testtemperature. Heating is discontinued and stirring is maintaineduntil the sample cools to the chosen temperature. At this time,stirring is stopped and the apparent viscosity is determined.Additional determinations are made over a range of tempera-tures as the sample cools. Results of te
13、mperature and apparentviscosity determinations are plotted on semilog paper, andvalues at any particular temperature are determined from thecurve.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.
14、10.0A on Physical/Chemical Properties.Current edition approved April 15, 2012. Published April 2012. Originallyapproved in 1967. Last previous edition approved in 2006 as D266906. DOI:10.1520/D2669-06(2012)E01.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Custo
15、mer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.1Copyright ASTM International, 100 Barr Harbor Drive, PO
16、 Box C700, West Conshohocken, PA 19428-2959, United States.5. Significance and Use5.1 This test distinguishes between hot melts having differ-ent apparent viscosities. It is believed that apparent viscositydetermined by this procedure is related to flow performance inapplication machinery operating
17、under conditions of low shearrate. Apparent viscosity as determined by this method may notcorrelate well with end use applications where high shear ratesare encountered.5.2 Materials of the type described in this procedure may bequite non-Newtonian and as such the apparent viscosity will bea functio
18、n of shear rate under the conditions of test. Althoughthe viscometer described in this test generally operates underconditions of relatively low shear rate, differences in sheareffect can exist depending upon the spindle and rotationalspeed conditions selected for the test program. Maximumcorrelatio
19、n between laboratories, therefore, depends upon test-ing under conditions of equivalent shear.6. Apparatus6.1 ViscometerBrookfield Synchro-Lectric Viscometer,Models LVF or LVT with numbers 1, 2, 3, and 4 stainless steelspindles and V-shaped stand with leveling screws.6.2 Glass Beaker, 800-mL Griffin
20、 standard form.6.3 Glass Heating Mantle, for 800-mL beaker.6.4 Autotransformer, variable.46.5 Thermometers,ASTM Precision Thermometer 88C hav-ing a range from 10 to 200C or Thermometer 88F having arange from 50 to 392F as prescribed in Specification E1 aresuitable.6.6 Laboratory Stirrer Motor, varia
21、ble speed.6.7 Propeller and Shaft, stainless steel 51 mm (2 in.) indiameter, three blades to fit 7.9 by 475-mm (516 by 18-in.)stainless steel shaft.6.8 Hot Plate, with continuously adjustable temperaturecontrol.6.9 Laboratory Jack, scissors-type.6.10 Ring Stands and Clamps, for mounting stirrer andt
22、hermometer.6.11 Semilog Graph Paper, two cycles.7. Procedure7.1 Selection of SpindleFrom the estimated viscosity ofthe sample and Table A1.1, select a spindle size and speedcombination that preferably will produce readings within therange recommended by the manufacturer. Attach the spindle tothe vis
23、cometer, with guard attached and mount the instrumenton its stand.NOTE 2Care must be taken while storing and handling the spindle. Itshould be protected from dust, corrosive deposits, and mechanical abuse.Avoid touching the calibrated section of the spindle with the hands.Thoroughly clean it and the
24、 guard after each use.7.2 Preparation of SampleIn a suitable container, meltapproximately 800 g representative of the sample to be testedon a hot plate or in an oven. Bring the temperature of thesample to 120 to 150C (250 to 300F) and stir to ensurehomogeneity, taking care not to whip air into the m
25、eltedsample. Fill the 800-ml test beaker with the melted sample toa level about 25 mm (1 in.) from the top. Place the filled beakerinto the heating mantle which is supported by the laboratoryjack in its lowered position. Connect the heating mantle to theautotransformer which, in turn, is connected t
26、o the proper acsupply. Connect the viscometer to its proper ac supply. Positionthe viscometer with spindle and guard attached, the stirrer, andthermometer as shown in Figs. A1.1 and A1.2. Mount thethermometer so that the center of its bulb is in the samehorizontal plane as the center of the test sec
27、tion of the spindle,and spaced approximately the same distance as the guard fromthe spindle, about 13 mm (12 in.). Position the stirring propellerabout midway between the bottom of the guard and the bottomof the beaker. Position the complete assembly so that the testportion of the spindle is spaced
28、approximately 19 mm (34 in.)from the side of the beaker when the beaker containing thesample is in the operating position. Raise the beaker containingthe sample by means of the laboratory jack so that the spindleis covered to about 6 mm (14 in.) below its immersion mark.Adjust the stirrer speed to g
29、ive maximum agitation of the testsample without permitting vortex or air bubble inclusion.Apply heat to the sample by adjusting the autotransformer, andraise its temperature to about 5C (10F) above the highest testtemperature. Maintain stirring throughout the heating cycle,being careful to prevent a
30、ir entrainment in the sample.NOTE 3As the temperature of the sample increases, its liquid levelwill approach the immersion mark on the spindle. Be careful to preventthe sample level from rising above the immersion mark on the spindle.Final immersion adjustment shall be made just before viscometer re
31、adingsare determined.7.3 Viscosity DeterminationWhen the temperature of thesample reaches 5C (10F) above the highest test temperature,shut off the autotransformer, start the viscometer motor, andcontinue stirring. The temperature of the sample will begin tolower, and when it becomes 0.5C (1F) above
32、the intendedtest temperature, stop the stirrer, but continue the spindlerotation. Wait 5 s, and readjust the viscometer to the immersionmark on the spindle. Allow the spindle to make three completeadditional rotations. Engage the pointer clutch, and stop theviscometer motor when the pointer is in vi
33、ew. Record the dialreading. Restart the viscometer motor, release the clutch, makethree additional spindle revolutions, engage the clutch, andstop the viscometer motor when the pointer is in view. Recordthe second dial reading, and repeat the above operation toobtain a total of three readings which
34、should be completedwithin a period of about 1 min. During this time the tempera-ture of the sample should fall no lower than 0.5C (1F) belowthe intended test temperature. Record the three test readingsand the test temperature. Immediately after the final reading,start the stirrer motor and viscomete
35、r with the clutch engaged.Permit the temperature of the sample to drop about 15C(25F), and repeat the same procedure at a lower temperature.Continue this sequence to produce dial readings at four or moredifferent temperatures, each spaced approximately 15C (25F)lower than the preceding test temperat
36、ure.4The sole source of supply of the apparatus known to the committee at this timeis the Variac Type W5 MT, IET Labs, Inc. 534 Main Street, Westbury, NY 11590.If you are aware of alternative suppliers, please provide this information to ASTMInternational Headquarters. Your comments will receive car
37、eful consideration at ameeting of the responsible technical committee,1which you may attend.D2669 06 (2012)12NOTE 4The range of test temperatures shall include all temperaturesat which apparent viscosity values are desired. Minor vertical adjustmentsof the spindle may be required to maintain its pro
38、per immersion as thevolume of the sample decreases with lower temperatures.8. Calculation8.1 Determine the averages of the three scale readings madefor each test temperature. Calculate the apparent viscosities, inpascal seconds or millipascal seconds, by multiplying theaverage viscometer scale readi
39、ng for each test temperature bythe factor indicated in Table A1.1 for the spindle and speedcombination used.8.2 Plot the apparent viscosity values obtained on the logscale, and the corresponding test temperatures on the linearscale of appropriate semilog paper. From the plot, determinethe apparent v
40、iscosity of the sample at any temperature withinthe range of the test temperatures.9. Report9.1 Report the apparent viscosity at a given temperaturewith the spindle number and speed used to obtain the data as:Apparent viscosity, 325 mPas at 120C (1)No. 2 spindle, 30 rpm!10. Precision and Bias10.1 Th
41、e composition of a hot melt influences the precisionto be expected when testing different types of samples. Thefollowing data should be used to judge the acceptability ofresults (95 % probability) for four different types of hot meltsaccording to the concept of precision as given in Practice E180.10
42、.2 Duplicate results should be considered suspect if theydiffer by more than the following amounts for each of the fourtypes listed: below:10.2.1 High-Viscosity Sample, M1-65-20:58 weight % of a 68C (155F) melting point wax.42 weight % of an ethylene-vinyl acetate copolymer con-taining 27 to 29 % vi
43、nyl acetate and having a melt index offrom 12 to 18.Viscosity,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)11 200 121 (250) 1900 24007500 134 (275) 1200 17005100 149 (300) 660 150010.2.2 Medium-Viscosity Sample, MI-65-21:72 weight % of a 61C (142F) melting point wax.28 weight % of the
44、 same copolymer used in sample MI-65-20.Viscosity,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)1200 121 (250) 81 240840 134 (275) 63 150610 149 (300) 47 12010.2.3 Low-Viscosity Sample, MI-65-22:96.3 weight % of a 77C (170F) melting point microcrys-talline wax.2.7 weight % of butyl rub
45、ber.Viscosity,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)68 121 (250) 15 3252 134 (275) 11 2941 149 (300) 7.9 2210.2.4 Low-Viscosity Sample, MI-65-23:80 weight % of a 68C (154F) melting point wax.20 weight % of a 5000 molecular weight polyethylenehaving a melting point from 107 to 1
46、11C (224 to 232F), aspecific gravity of 0.92 and a typical viscosity at 140C of 4Pas.Viscosity,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)25 121 (250) 1.9 4.420 134 (275) 1.2 4.016 149 (300) 1.5 3.810.3 BiasThe procedure in this test method has no biasbecause the value of apparent v
47、iscosity can be defined only interms of a test method.11. Keywords11.1 apparent viscosity; hot melts; petroleum waxes; waxesANNEX(Mandatory Information)A1. SELECTION OF SPINDLE AND PREPARATION OF SAMPLEA1.1 Table A1.1 lists spindle size and spindle speed, Fig.A1.1 and Fig. A1.2 present a top and sid
48、e view of the testapparatus.D2669 06 (2012)13TABLE A1.1 Viscometer Spindle Number-Speed-Maximum Viscosity RelationshipSpindle NumberSpindle Speed, rpm60 30 12 6125101. Multiplication factor viscosity, max, mPas 100520010500251000502. Multiplication factor viscosity, max, mPas 50020100040250010050002
49、003. Multiplication factor viscosity, max, mPas 2000100400020010 00050020 00010004. Multiplication factor viscosity, max, mPas 10 000 20 000 50 000 100 000FIG. A1.1 Viscosity Test Apparatus, Side ViewD2669 06 (2012)14ASTM 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 validity of any such patent rights, and the riskof infringement o
