1、Designation: D2669 16Standard 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 case of revision, the
2、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.1. Scope*1.1 This test method covers the determination of the appar-ent viscosity of petroleum waxes compounded with addit
3、ives(hot melts). It applies to fluid hot melts having apparentviscosities up to about 20 Pas at temperatures up to 175 C(347 F).NOTE 1For petroleum waxes and their blends having low apparentviscosities, below about 15 mPas, Test Method D445, is especiallyapplicable.1.2 The values stated in SI units
4、shall be regarded as thestandard.1.2.1 ExceptionAlternative units in parentheses are forinformation purposes only.NOTE 2One Pascal second (Pas) = 1000 centipoises (cP). One milli-Pascal second (mPas) = 1 centipoise (cgs units).1.3 WARNINGMercury has been designated by manyregulatory agencies as a ha
5、zardous material that 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
6、details and EPAswebsitehttp:/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, associ
7、ated 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:2D445 Test Method for Kinematic Viscosity of Transparentand
8、Opaque Liquids (and Calculation of Dynamic Viscos-ity)3. Terminology3.1 Definitions:3.1.1 viscosity, nthe ratio of shear stress to shear rate.Viscosity 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,
9、 the viscosity is constant at allshear rates. For a non-Newtonian liquid, viscosity will varydepending on shear rate.3.1.2 viscosity, apparent, nthe viscosity determined bythis method, expressed in Pascal seconds. Its value may varywith the spindle and rotational speed selected because manyhot melts
10、 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 container is filled with themelted sample to a level of about 25 mm (1 in.) from its topand placed in a temperature bath. The viscometer, withattached spindle and guar
11、d, is positioned in the test specimen.Stirring is begun and continued while the temperature of thesample is brought to slightly above the highest desired testtemperature. Heating is discontinued and stirring is maintaineduntil the sample cools to the chosen temperature. At this time,stirring is stop
12、ped and the apparent viscosity is determined.Additional determinations are made over a range of tempera-tures as the sample cools. Results of temperature and apparent1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct
13、 responsibility ofSubcommittee D02.10.0A on Physical/Chemical Properties.Current edition approved June 1, 2016. Published July 2016. Originally approvedin 1967. Last previous edition approved in 2012 as D2669 06 (2012)1. DOI:10.1520/D2669-16.2For referenced ASTM standards, visit the ASTM website, ww
14、w.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.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, P
15、O Box C700, West Conshohocken, PA 19428-2959. United States1viscosity determinations are plotted on semilog paper, andvalues at any particular temperature are determined from thecurve.5. Significance and Use5.1 This test distinguishes between hot melts having differ-ent apparent viscosities. It is b
16、elieved that apparent viscositydetermined by this procedure is related to flow performance inapplication machinery operating 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 Ma
17、terials of the type described in this procedure may bequite non-Newtonian and as such the apparent viscosity will bea function of shear rate under the conditions of test. Althoughthe viscometer described in this test generally operates underconditions of relatively low shear rate, differences in she
18、areffect can exist depending upon the spindle and rotationalspeed conditions selected for the test program. Maximumcorrelation between laboratories, therefore, depends upon test-ing under conditions of equivalent shear.6. Apparatus6.1 Viscometer, RotationalThe essential instrumentationrequired provi
19、ding the minimum rotational viscometer analyti-cal capability includes:6.1.1 A drive motor, to supply a unidirectional displacementto the specimen at a rate between 0.5 r min and 60 r minconstant to 61%.6.1.2 A force sensor to measure the torque developed by thespecimen to within 1 %.6.1.3 A couplin
20、g shaft, or other means to transmit therotation displacement from the motor to the specimen.NOTE 3It is helpful to have a mark on the shaft to indicate appropriatetest fluid level.6.1.4 A rotational element, spindle or tool, composed ofstainless steel or other insulating material, to fix the specime
21、nbetween the draft shaft and a stationary position of the typeshown in Fig. 1.NOTE 4Each spindle typically covers a range of about 2 decades ofviscosity. The spindle is selected so that the measured viscosity is between10 % and 90 % of the range of that spindle.6.1.5 A specimen container to contain
22、800 mL of the testspecimen during testing.NOTE 5A low form, glass Griffin beaker has been found suitable forthis purpose.6.1.6 A data collection device, to provide a means ofacquiring, storing, and displaying measured or calculatedsignals, or both. The minimum output signals required forrotational v
23、iscosity are torque, rotational speed, temperatureand time.NOTE 6Manual observation and recoding of data are acceptable6.1.7 A stand to support, level and adjust the height of thedrive motor, shaft and spindle.6.1.8 Auxiliary instrumentation considered useful in con-ducting this method includes:6.1.
24、8.1 A level to indicate the vertical plumb of the drivemotor, shaft and spindle.6.1.8.2 A guard to protect the rotational element frommechanical damage.6.2 A temperature bath and controller to provide a con-trolled isothermal temperature environment for the specimenover the temperature range of 100
25、C to 175 C constant towithin 61 C.NOTE 7A glass heating mantle of suitable size for the container andan autotransformer have been found suitable for this purpose.6.3 A temperature sensor or temperature measuring deviceto provide an indication of the specimen temperature over therange of 100 C to 200
26、 C to within 60.1 C.6.4 Laboratory Stirrer Motor, variable speed.6.5 Propeller and Shaft, stainless steel 51 mm (2 in.) indiameter, three blades to fit 7.9 mm by 475 mm (516 in. by18 in.) stainless steel shaft.6.6 Hot Plate, with continuously adjustable temperaturecontrol.6.7 Laboratory Jack, scisso
27、rs-type.6.8 Ring Stands and Clamps, for mounting stirrer andtemperature measuring device.6.9 Semilog Graph Paper, two cycles.FIG. 1 Spindle ConfigurationD2669 1627. Procedure7.1 Selection of SpindleFrom the estimated viscosity ofthe sample and Table 1, select a spindle size and speedcombination that
28、 will produce readings within the range of10 % to 90 % full scale. Attach the spindle to the viscometer,with guard attached and mount the instrument on its stand.NOTE 8Care must be taken while storing and handling the spindle. Itshould be protected from dust, corrosive deposits, and mechanical abuse
29、.Avoid touching the calibrated section of the spindle with the hands.Thoroughly clean it and the 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
30、 120 C to 150 C (250 F to 300 F) and stir toensure homogeneity, taking care not to whip air into the meltedsample.7.2.1 Fill the 800 mL container with the melted sample toa level about 25 mm (1 in.) from the top. Place the filledcontainer into the temperature bath so that it is supported in itsposit
31、ion. Position the viscometer with spindle and guardattached, the stirrer, and temperature sensor as shown in Fig. 2and Fig. 3. Mount the temperature sensor so that it is in thesame horizontal plane as the center of the test section of thespindle, and spaced approximately the same distance as theguar
32、d from the spindle, about 13 mm (12 in.). Position thestirring propeller about midway between the bottom of theguard and the bottom of the container. Position the viscometerassembly so that the test portion of the spindle is spacedapproximately 19 mm (34 in.) from the side of the containerwhen in th
33、e operating position. Raise the container with thesample so that the spindle is covered to about 6 mm (14 in.)below its immersion mark. Adjust the stirrer speed to givemaximum agitation of the test sample without permittingvortex or air bubble inclusion. Apply heat to the temperaturebath and raise i
34、ts temperature to about 5 C (10 F) above thehighest operator selected test temperature. Maintain stirringthroughout the heating cycle, being careful to prevent airentrainment in the sample.NOTE 9As the temperature of the sample increases, its liquid levelwill approach the immersion mark on the spind
35、le. Be careful to preventthe sample level from rising above the immersion mark on the spindle.Final immersion adjustment shall be made just before viscometer readingsare determined.7.3 Viscosity Determination:7.3.1 When the temperature of the sample reaches 5 C(10 F) above the highest test temperatu
36、re, shut off the tem-perature bath, start the viscometer motor, and continue stirring.7.3.2 The temperature of the sample will begin to lower, andwhen it becomes 0.5 C (1 F) above the intended testtemperature, stop the stirrer, but continue the spindle rotation.Wait 5 s, and readjust the viscometer
37、to the immersion mark onthe spindle.7.3.3 Allow the spindle to make three complete additionalrotations. Record the torque reading.7.3.4 Make three additional spindle revolutions. Record thesecond torque reading.7.3.5 Repeat 7.3.4 to obtain a total of three readings, whichshould be completed within a
38、 period of about 1 min. Duringthis time, the temperature of the sample should fall no lowerthan 0.5 C (1 F) below the intended test temperature. Recordthe three test readings and the test temperature.7.3.6 Immediately after the final reading, start the stirrermotor and maintain the viscometer rotati
39、on.7.3.7 Permit the temperature of the sample to drop about15 C (25 F), and repeat 7.3.3 to 7.3.6 at a lower temperature.Continue this sequence to produce dial readings at four or moredifferent temperatures, each spaced approximately 15 C(25 F) lower than the preceding test temperature.NOTE 10The ra
40、nge of test temperatures shall include all temperaturesat which apparent viscosity values are desired. Minor vertical adjustmentsof the spindle may be required to maintain its proper immersion as thevolume of the sample decreases with lower temperatures.8. Calculation8.1 Determine the averages of th
41、e three scale readings madefor each test temperature. Calculate the apparent viscosities, inPascal seconds or milliPascal seconds.8.2 Plot the apparent viscosity values obtained on thelogarithmic scale, and the corresponding test temperatures onthe linear scale of appropriate semilog paper. From the
42、 plot,determine the apparent viscosity of the sample at any tempera-ture within the range of the test temperatures.9. Report9.1 Report the apparent viscosity at a given temperaturewith the spindle identification and speed used to obtain the dataas:Apparent viscosity is 325 mPas at 120 C using a No.
43、2 spindle and 30 r min.10. Precision and Bias10.1 The 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 melts.TABLE 1 Visco
44、meter Spindle Dimensions, Speed, Viscosity RelationshipSpindle No. Nominal Diameter,Amm Nominal Length,BmmMaximum Viscosity, mPasat 60 r/min at 30 r/min at 12 r/min at 6 r/min1 19 65 100 200 500 10002 10 54 500 1000 2500 50003 5.9 43 200 4000 10 000 20 0004 3.2 31 10 000 20 000 50 000 100 000ADinFig
45、. 1.BLinFig. 1.D2669 163FIG. 2 Viscosity Test Apparatus, Side ViewFIG. 3 Viscosity Test Apparatus, Top ViewD2669 16410.2 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
46、% by mass ofa 68 C (155 F) melting point wax.42 % by mass of an ethylene-vinyl acetate copolymercontaining 27 % to 29 % vinyl acetate and having a melt indexof from 12 to 18.Viscosity,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)11 200 121 (250) 1900 24007500 134 (275) 1200 17005100 1
47、49 (300) 660 150010.2.2 Medium-Viscosity Sample, MI-65-21: 72 % by massof a 61 C (142 F) melting point wax.28 % by mass of the same copolymer used in sampleMI-65-20.Viscosity,mPasTemperature, Repeatability,mPasReproducibility,mPasC (F)1200 121 (250) 81 240840 134 (275) 63 150610 149 (300) 47 12010.2
48、.3 Low-Viscosity Sample, MI-65-22: 96.3 % by mass ofa 77 C (170 F) melting point microcrystalline wax.2.7 % by mass of butyl rubber.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 %
49、 by mass of a68 C (154 F) melting point wax.20 % by mass of a 5000 g mol molecular weight polyeth-ylene having a melting point from 107 C to 111 C (224 F to232 F), a specific gravity of 0.92 and a typical viscosity at140 C of 4 Pas.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 viscosity can be defined only interms of a
