1、SAE Technical Standards Board Rules provide that: “This report is published by SAE to advance the state of technical and engineering sciences. The use of this report is entirelyvoluntary, and its applicability and suitability for any particular use, including any patent infringement arising therefro
2、m, is the sole responsibility of the user.”SAE reviews each technical report at least every five years at which time it may be reaffirmed, revised, or cancelled. SAE invites your written comments and suggestions.QUESTIONS REGARDING THIS DOCUMENT: (412) 772-8512 FAX: (412) 776-0243TO PLACE A DOCUMENT
3、 ORDER; (412) 776-4970 FAX: (412) 776-0790SAE WEB ADDRESS http:/www.sae.orgCopyright 1995 Society of Automotive Engineers, Inc.All rights reserved. Printed in U.S.A.SURFACEVEHICLE400 Commonwealth Drive, Warrendale, PA 15096-0001RECOMMENDEDPRACTICESubmitted for recognition as an American National Sta
4、ndardJ1524REV.AUG95Issued 1985-06Revised 1995-08Superseding J1524 NOV88(R) METHOD OF VISCOSITY TEST FOR AUTOMOTIVE TYPE ADHESIVES, SEALERS, AND DEADENERS1. ScopeThis SAE Recommended Practice contains a series of test methods for use in measuring theviscosity of automotive-type adhesives, sealers, an
5、d deadeners.The test methods which are contained in this document are as follows:1.1 Brookfield Method1.2 Castor-Severs Rheometer or Pressure Flowmeter1.3 Penetrometer1.4 Capillary Rheometer1.5 Plate Rheometers2. References2.1 Applicable DocumentsThe following publications form a part of this specif
6、ication to the extent specifiedherein.2.1.1 ANSI/ASME PUBLICATIONAvailable from ANSI, 11 West 42nd Street, New York, NY 10036-8002.ANSI/ASME B40.1Pressure Gauge2.1.2 ASTM PUBLICATIONSAvailable from ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959.ASTM D 5Needle PenetrometerASTM D 217Con
7、e PenetrometerASTMD1823Standard Test Method for Apparent Viscosity of Plastisols and Organosols at High ShearRates by Extrusion ViscometerASTMD1824Standard Test Method for Apparent Viscosity of Plastisols and Organosols at Low ShearRatesASTMD2196Standard Test Methods for Rheological Properties of No
8、n-Newtonian Materials byRotational (Brookfield) ViscometerASTM D 2240DurometerCOPYRIGHT Society of Automotive Engineers, Inc.Licensed by Information Handling ServicesSAE J1524 Revised AUG95-2-ASTMD3364Standard Test Method for Flow Rates for Poly(Vinyl Chloride) and Rheologically UnstableThermoplasti
9、csASTMD3835Standard Test Method for Determination of Properties of Polymeric Materials by Means ofa Capillary RheometerASTMD4440Standard Practice for Rheological Measurement of Polymer Melts Using DynamicMechanical Procedures3. Principle of MethodsThe viscosity of a material is a measurement of the
10、shear stress that must be appliedbefore a change of form (shear rate) can be accomplished. For the purpose of this test method, however,viscosity refers to a finished product parameter that is quantified in various ways and used by the automotiveindustry as a means of identifying and assigning a min
11、imum and maximum value for the applicationcharacteristics of a material.The use of these values should be tempered by the knowledge that the numbers generated are quality controlaids and may not fully address the plant-to-plant variations encountered in application systems.Each piece of equipment is
12、 best suited to a particular viscosity and shear rate range, although there are nosharp viscosity demarcations between the various viscometers. Each method has its own idiosyncrasies andlimitations and therefore must be evaluated with the particular material being tested. The rheometers (1.4 and1.5)
13、 have the ability to compare results under a range of conditions, and thus determine the sensitivity of thematerial to shear rate, shear history, and temperature. The following suggestions are intended as generalguidelines for use of these viscosity measuring devices. They may be used outside the su
14、ggested ranges ifdesired.Generally, a Brookfield viscometer is used for low viscosity materials in the 0.025 to 200 Pas (Pas = 1000cP) range with limited shear thinning. The pressure flowmeter is usually used for materials with viscosities upto 80 Pas at 50 s1. Since these materials are highly shear
15、 thinning they may exceed 1000 Pas at 1 s1. Thepenetrometer is used for very high viscosity materials such as putties and highly gelled compounds.The capillary rheometer is used for materials from 1 to 10 000 Pas at shear rates from 10 to 50 000 s1. Theplate rheometers are used for materials from 0.
16、025 to 1000 Pas at shear rates from 107 to 200 s1.4. Sample Temperature ConditioningPrior to the actual viscosity measurement, the sample to be testedmust be conditioned thermally.4.1 As Received ViscosityUnless specified otherwise, as received viscosity shall refer to material stored at“room temper
17、ature“ and tested at 23 C 1 C (75 F 2 F) and 50% 5% R.H.4.2 Aged ViscosityAged viscosity refers to a value obtained by subjecting a sample prior to testing to aspecified temperature for 72 h. The sample is then conditioned to 23 C 1 C and the viscosity is measured.The size of the sample to be tested
18、 should be 500 mL (1 pt). Samples smaller than this conditioned at elevatedtemperatures may give different results.5. Sample Mechanical ConditioningPrior to the actual viscosity measurement, the sample to be tested mustbe conditioned mechanically.5.1 Conditioning Method AUnagitatedUnagitated testing
19、 refers to the transfer of materials from the shippingcontainer to the testing apparatus with the minimum amount of agitation. This viscosity is supposed to beindicative of a compound in its shipping container prior to use. The tester should be aware that the very act ofremoving a sample for test ca
20、n affect the rheology of thixotropic materials and, in so doing, may substantiallyalter the value measured.COPYRIGHT Society of Automotive Engineers, Inc.Licensed by Information Handling ServicesSAE J1524 Revised AUG95-3-5.2 Conditioning Method BModerate AgitationModerate agitation of a sample is ac
21、hieved by stirring a500mL sample 50 stirs in 60 s with a 25 x 150 mm (1 x 6 in) steel bladed spatula. This agitation can also beused to assure the uniform 23 C necessary for testing.5.3 Conditioning Method CGrease WorkingGrease working refers to subjecting a sample to 150 cycles,unless otherwise spe
22、cified, in a standard mechanical grease-worker, as outlined in ASTM D 217.5.4 Conditioning Method DPre-shearSteady shear rheometers including Brookfield and Plate devicesallow the sample to be pre-sheared at a fixed shear rate for a known time before testing. Ten s1 for 10 min isa suggested conditio
23、n.6. Brookfield Method6.1 ApplicationThis procedure is used to determine the viscosity of adhesives, sprayable sound deadeners,and thin body sealers. The values obtained are expressed in Pas (Pas = 1000 cP) and are a measure of theresistance a rotating spindle encounters when immersed in the compoun
24、d to be tested. Due to secondaryflows, this method provides only relative values for shear thinning materials. Refer to ASTM D 1824 and ASTMD 2196 for additional details and reproducibility data.6.2 EquipmentCommercially available Brookfield Viscometer Figure 1, or equivalent.6.3 ProcedureTest equip
25、ment and sample shall be maintained at 23 C 1 C.6.3.1 Set viscometer at specified rpm.6.3.2 Attach specified spindle.6.3.3 Lower viscometer into 500 mL of test material so that the groove cut in the spindle is flush with the fluidslevel.6.3.4 Level the viscometer.6.3.5 Depress the clutch, turn on th
26、e viscometer, and release the clutch. Take the reading and record the timeafter the indicator has stabilized or after a specified time, typically 60 s. (When measuring thixotropicmaterials at specific times, other than stable readings, it will be necessary to test separate samples in orderto obtain
27、reproducible values.)6.3.6 Use conversion table to convert to centipoise.6.3.7 Take the average of three readings and report the viscosity, spindle, rpm, time of recording, and the model ofthe viscometer used.6.3.8 Repeat the procedure at a second rpm, and note extent of shear thinning. (Note that B
28、rookfield results area relative measure for thixotropic or shear thinning materials.)COPYRIGHT Society of Automotive Engineers, Inc.Licensed by Information Handling ServicesSAE J1524 Revised AUG95-4-FIGURE 1BROOKFIELD VISCOMETERCOPYRIGHT Society of Automotive Engineers, Inc.Licensed by Information H
29、andling ServicesSAE J1524 Revised AUG95-5-7. Castor-Severs Method/Pressure Flowmeter Method7.1 ApplicationThis procedure is used to determine the viscosity of adhesives, sealers, and sprayable sounddeadeners. The values obtained are expressed in seconds and are a measurement of the time needed toext
30、rude a specified mass (20 g) through a specified orifice at a specified pressure. These values can beconverted to apparent viscosity in centipoise at a specified shear rate using the capillary rheometer procedureas in ASTM D 3835 or ASTM D 1823. If this step is taken, it is recommended to repeat the
31、 procedure at threepressures with at least two orifices to obtain a measure of shear thinning and thixotropy.7.2 Equipment7.2.1 Rheometer as shown in Figure 2.7.2.2 Orifices are as follows in Table 1:Other orifices should be used if the data is to be analyzed by plotting viscosity versus shear rate.
32、 A minimumof two orifices is recommended to observe thixotropic behavior. The length should be a minimum of 10 timesthe diameter. The dimensions should meet the accuracy requirements specified in ASTM D 3835 6.1.3.7.2.3 Air supply, 700 kPa (100 psi).7.2.4 Pressure gauge, 700 kPa (100 psi) 1% (ANSI/A
33、SME B40.1-1985 Grade 1A or better).7.2.5 Pressure regulator and water/oil extractor for air line.7.2.6 Pipe cleaners for cleaning the orifice.7.2.7 Stop watch or other timing device calibrated in tenths of seconds.7.2.8 Balance, double beam type or equivalent, sensitivity to 0.01 g.7.2.9 Mechanical
34、convection oven capable of maintaining a temperature of 1 C (2 F), or alternate meanswhere temperature conditioning is specified.7.2.10 Weight per gallon cup, or other means to determine density within 1%.TABLE 1RHEOMETER ORIFICESNo.mm (in)Diametermm (in)Lengthmm (in)TypicalUseLimits1 1.32 (0.052) 1
35、3.5 (0.531) Sprayable Readings less than 10 s, use BrookfieldMethod2 2.64 (0.104) 13.5 (0.531) Pumpable Readings less than 10 s, use orifice 13 3.18 (0.125) 51.0 (2.008) Deadeners Readings less than 10 s, use orifice 2COPYRIGHT Society of Automotive Engineers, Inc.Licensed by Information Handling Se
36、rvicesSAE J1524 Revised AUG95-6-FIGURE 2RHEOMETERCOPYRIGHT Society of Automotive Engineers, Inc.Licensed by Information Handling ServicesSAE J1524 Revised AUG95-7-7.3 Procedure7.3.1 Fill the clean, dry, sealer cup equipped with the specified orifice with the material to be tested. The materialshould
37、 be at 23 C 1 C unless otherwise specified. Care should be taken to avoid air entrapment and toallow enough room for the plunger.7.3.2 Adjust line pressure to 276 kPa (40 psi), unless otherwise specified. Open air valve and extrude materialthrough orifice until entrapped air is eliminated. Shut air
38、valve. When plotting viscosity versus shear rateusing the equations from ASTM D 1823, it is desirable to repeat this procedure at four pressures. Therecommended pressures are 69, 276, 483, and 690 kPa (10, 40, 70, and 100 psi).7.3.3 Place a paper on the balance, tare and add specified weight (20 g).
39、7.3.4 Open air valve and start timer when the material touches the paper on the weighing pan.7.3.5 When 20 g of sealer has accumulated on the balance pan, stop the timer, close the air valve, and open thepressure relief valve.7.3.6 Take the average of three readings and report the number of seconds,
40、 pressure, and orifice length anddiameter.8. Penetration Method8.1 ApplicationThis procedure is used to determine the viscosity of heavy-bodied sealers, extrudable and diecut deadeners. In this method, viscosity is a measurement of the depth of penetration by a cone or needle intothe material tested
41、 and is expressed in 0.1 mm of penetration.8.2 Equipment8.2.1 Commercially available penetrometer (Figure 3), as described in Table 2.8.2.2 Stop watch8.2.3 Weights to place on loading bar8.2.4 Penetration instruments (cone ASTM D 217 and needle ASTM D 5).8.2.5 SAMPLE CUP75 mm diameter by 60 mm depth
42、, or as specified.TABLE 2PENETRATION INSTRUMENTSNo. Penetrometer Typical Use Limits1 Cone ASTM D 217 Deadeners Readings less than 5 mm use Penetrometer No. 22 Needle ASTM D 5 Thumbable Materials Readings less than 5 mm use Durometerhardness ASTM D 2240COPYRIGHT Society of Automotive Engineers, Inc.L
43、icensed by Information Handling ServicesSAE J1524 Revised AUG95-8-FIGURE 3PENETROMETER8.3 ProcedureTest material at 23 C 1 C.8.3.1 Level penetrometer.8.3.2 Insert specified penetrating instrument into chuck.8.3.3 Set dial reading to zero.COPYRIGHT Society of Automotive Engineers, Inc.Licensed by Inf
44、ormation Handling ServicesSAE J1524 Revised AUG95-9-8.3.4 Add weight to loading bar, as needed, to achieve the specified moving load. Use a 150 g total weight,including rod and added weights, unless otherwise specified.8.3.5 Place the sample to be tested on the center of base plate.8.3.6 Adjust the
45、zeroed height of the penetrometer so that the point of the penetrating instrument is exactly incontact with the surface of the material to be tested.8.3.7 Release test rod by depressing the trigger and keep in this position for 5 s unless otherwise specified.8.3.8 At the end of the specified “drop“
46、period, release the trigger.8.3.9 Gently push the depth gage rod down as far as it will go and record the depth of penetration, units are in0.1mm.8.3.10 Take the average of three readings and report the depth of penetration, moving load, and penetration time.9. Capillary Rheometer Method9.1 Applicat
47、ionThis method is used to determine the viscosity versus shear rate characteristics of adhesives,sealers, and deadeners per ASTM D 3835 (ISO DIS11443). The basic test determines apparent viscosityversus apparent shear rate over a typical shear rate range of 100 to 50 000 s1. Various corrections areo
48、utlined in ASTM D 3835. The piston in barrel arrangement outlined in ASTM D 3835 is preferred for reachinghigh-shear rate, but the apparatus in Figure 2 and ASTM D 1823 is acceptable as a moderate shear ratescreening tool (10 to 100 s1). Round Robin results are reported in ASTM D 1823.9.2 Equipment9
49、.2.1 Capillary Rheometer per ASTM D 3835 (ISO DIS11443) and associated orifices (preferred).9.2.2 Castor Severs rheometer as in Figure 2 is an alternate with limited shear rate range. This rheometer willrequire a balance, a timer, and a means to determine density within 1%, and thus volumetric flow rate. Thiswill follow ASTM D 1823.9.2.3 A set of orifices chosen for the material as outlined in the ASTM specification. If a Bagley plot is notgenerated, then a length to diameter ratio of at least 10
