1、Designation: D4889 04 (Reapproved 2011)D4889 15Standard Test Methods forPolyurethane Raw Materials: Determination of Viscosity ofCrude or Modified Isocyanates 1This standard is issued under the fixed designation D4889; the number immediately following the designation indicates the year oforiginal ad
2、option or, in the case 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.1. Scope Scope*1.1 These test methods (A and B) determine the viscosity of crude o
3、r modified isocyanates. They are applicable to productsderived from toluene diisocyanate, methylene-bis-(4-phenylmethyleneisocyanate), and polymethylene polyphenyldi(phenylisocyanate), and polymeric (methyleneisocyanates phenylisocyanate) (see Note 1).NOTE 1Test method A includes a procedure for mea
4、suring dynamic viscosity using a rotational Brookfield instrument. Test method B is simply areference to a general procedure for measuring kinematic viscosity using a Cannon-Fenske instrument, viscosity, D445.1.2 The values stated in SI units are to be regarded as standard.1.3 This standard does not
5、 purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific hazards statementsstatement,
6、see WarningsWarning at the end of 5.1 and 10.5.NOTE 2There is no known ISO equivalent to this standard.This standard is equivalent to ISO 3219 and ISO 3104.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynami
7、c Viscosity)D883 Terminology Relating to PlasticsE1E2251 Specification for ASTM Liquid-in-Glass ThermometersLiquid-in-Glass ASTM Thermometers with Low-HazardPrecision Liquids2.2 ISO Standards:3ISO 3104 Petroleum ProductsTransparent and Opaque LiquidsDetermination of Kinematic Viscosity and Calculati
8、on ofDynamic ViscosityISO 3219 PlasticsPolymers/Resins in the Liquid State or as Emulsions or DispersionsDetermination of Viscosity Using aRotational Viscometer with Defined Shear Rate3. Terminology3.1 DefinitionsFor definitions of terms used in these test methods see Terminology D883.4. Significanc
9、e and Use4.1 These test methods can be used for research or for quality control research, quality control, or specification tests tocharacterize isocyanates used in polyurethane products.4.2 Viscosity measures the resistance of a fluid to uniform continuous flow without turbulence or other forces.4.
10、3 Some isocyanates exhibit non-Newtonian behavior under certain conditions. Whenever possible, generate results forcomparison under the same conditions, that is, the same spindle/speed combination for Brookfieldrotational viscosity and the sametube size for Cannon-Fenskekinematic viscosity.1 These t
11、est methods are under the jurisdiction of ASTM Committee D20 on Plastics and are the direct responsibility of Subcommittee D20.22 on Cellular Materials -Plastics and Elastomers.Current edition approved Feb. 1, 2011May 1, 2015. Published March 2011June 2015. Originally approved in 1988. Last previous
12、 edition approved in 20042011 asD4889 - 04.D4889 - 04(2011). DOI: 10.1520/D4889-04R11.10.1520/D4889-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards
13、Document Summary page on the ASTM website.3 Available from Brookfield Engineering Laboratories, 240 Cushing St., Stoughton, MA 02072.American National Standards Institute (ANSI), 25 W. 43rd St., 4th Floor,New York, NY 10036, http:/www.ansi.org.This document is not an ASTM standard and is intended on
14、ly to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current vers
15、ionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Sampling5.1 Since organic isocyanate
16、s react with atmospheric moisture, take special precautions must be taken in sampling (see Warningat the end of this paragraph). Usual sampling methods (for example, sampling an open drum with a thief), even when carried outin sampling. Usual sampling methods, even when conducted rapidly, can cause
17、contamination of the sample with insoluble urea.Therefore, blanket the sample must be blanketed with dry air or nitrogen at all times. (WarningOrganic Diisocyanates areharmful when they are absorbed through the skin, or when eye, skin and respiratory irritants at concentrations above theoccupational
18、 exposure limit (TLV or PEL). Diisocyanates can cause skin and respiratory sensitization (asthma) in some people.Once sensitized, it is essential to limit further exposure to diisocyanates. Use a combination of engineering controls and personalprotective equipment, including respiratory, skin and ey
19、e protection, to prevent over-exposure to diisothe vapors are breathed.Provide adequate ventilation and protective gloves and wear eyeglasses.cyanates. Consult the product suppliersSafety Data Sheet(SDS) for more detailed information about potential health effects and other specific safety and handl
20、ing instructions for theproduct.)6. Test Conditions6.1 Since isocyanates react with moisture, keep laboratory humidity low, preferably about 50 % relative humidity. See Warningin 5.1.TEST METHOD ABROOKFIELDAROTATIONAL VISCOSITY7. Summary of Test Method7.1 The viscosity is measured at 25 6 0.3C with
21、a Brookfield viscometer, either Model LVF, LVT, RVF, or RVT.by determiningthe torque on a spindle rotating at constant speed in the liquid sample which is adjusted to 25 6 0.1C. Generation of comparativedata using this method requires agreement on the speed, spindle, temperature, time of rotation an
22、d torque range of the instrumentused.8. Interferences8.1 The temperature and container size are important factors in measuring Brookfield viscosity accurately. Deviation from theprescribed conditions will affect the accuracy of the results.8. Apparatus9.1 Brookfield Synchro-lectric Viscometers, 3 Mo
23、del LVF, LVT, RVF, or RVT is to be used. Calibrate the instrument periodicallywith Brookfield Engineering Laboratories 10 mPa s (cP) or 100 mPa s (cP) Viscosity Standard Fluids.9.2 Spindle No. 1, The No. 1 Spindles for the LV and RV instruments are different and, therefore, it is important to use th
24、ecorrect spindle type.8.1 Constant-Temperature Bath, Constant-Temperature Bath,capable of maintaining a temperature of 25 6 0.3C.25 6 0.1Cis to be used. Water, water and glycerin, or oil is used as the heating medium and the bath is to be provided with heating,circulating, and thermostatting devices
25、.8.2 Bath and Sample Thermometers, Bath and Sample Thermometers,graduated in 0.1C subdivisions and standardized for therange of use to the nearest 0.01C. An ASTM Saybolt Viscosity Thermometer having a range of 1927C and Thermometershaving ranges from 19 to 27C and 49 to 57C, as specified, and confor
26、ming to the requirements for Thermometer 17CThermometers S117C and S64C, respectively, as prescribed in Specification E1E2251 isare recommended.6 Any otherthermometric device of equal or better accuracy is also acceptable.8.3 Rotational Viscometer, Wide-Mouth 1-Quart Paint Cancapable of user defined
27、Alternatively, a 1-quart jar or a 600-mLbeaker can be used. speed and spindle combinations. An instrument that is capable of providing the shear rate is recommended.The calibration of the instrument is to be checked periodically by measuring the viscosity of NIST traceable standard fluids.9. Solvent
28、9.1 Cleaning Solventdichloromethane or acetone, reagent grade. Any solvent in which the isocyanate is completely miscibleis acceptable.10. Preparation of Sample10.1 The preparation of a homogeneous sample is of primary importance in viscosity measurements.Anon-uniform temperaturedistribution as well
29、 as the presence of air bubbles and traces of extraneous material are to be avoided. The sample must bethoroughly mixed and the temperature measured at several locations in the sample vessel before determining the viscosity.11. Preparation of Apparatus11.1 Follow the manufacturers instructions to se
30、t up the instrument and ensure that the viscometer is level.D4889 15212. Choice of Temperature12.1 Samples that are liquid and have a viscosity of less than 100 000 mPas(cP) at 25C are to be measured at 25C.12.2 In cases of interlaboratory studies and higher viscosity samples, all parties are to agr
31、ee upon a set measurementtemperature.13. Choice of Spindle and Rotational Speed13.1 Rotational Viscometers offer a variety of spindle size and rotational speeds. In the case of non-Newtonian liquids, changingthese factors will cause variation in the results obtained. In general, the following recomm
32、endations provide guidance for choosingthe spindle size and speed to be used for a specific sample.13.1.1 The combination chosen shall generate a torque value between 15 and 90% of full scale, or that specified by theinstrument manufacturer.13.1.1.1 If more than one speed/spindle combination will fu
33、lfill the requirement of 13.1.1, the combination with the higherspeed will provide higher accuracy and the combination with the lower speed will minimize certain types of non-Newtonianbehavior.13.1.1.2 There must be agreement between the testing laboratory and the submitter on the spindle/speed sele
34、ction.14. Procedure14.1 Place sufficient sample in a 1-quart paint can Using the smallest container recommended by the manufacturer, placesufficient sample to cover the immersion mark on the viscometer spindle. Equilibrate the sample in the 25C constant-temperaturebath. Cover the container and immer
35、se it to the sample level in a constant temperature bath. Stir occasionally without trapping airbubbles. Check the temperature at several different locations in the container to make sure uniformity has been achieved.10.2 Attach the No. 1 spindle to the viscometer following the directions supplied w
36、ith the instrument. Set the speed using theguidelines in Table 1 (see Note 3). If the viscosity range of the sample is unknown, selection is accomplished by trial and error.NOTE 3The No. 1 spindle is suitable for the majority of crude or modified isocyanates. If it is necessary to use a different sp
37、indle and speedcombination, conversion factors for spindle number versus spindle speed are given in Table 2.Adial reading as close to the center of the scale as possibleis recommended. When there is a choice between two combinations with the same conversion factor, choose the combination with the lo
38、wer speed.14.2 Immerse the viscometer spindle and guard into theAfter the desired temperature has been observed throughout the samplefor 10 min, immerse the viscometer spindle (and the guard when recommended by the manufacturer) into a sample to theimmersion line marked on the spindle. Avoid forming
39、 Exercise caution to avoid air bubbles gathering under the spindle duringimmersion. If bubbles are observed, detach the spindle, keeping it in the sample, and stir until the bubbles are released, thenreattach the spindle. Center the spindle in the test material.released. Reattach the spindle.14.3 Pr
40、ess down the viscometer clutch lever and start the motor. Release the clutch lever after the spindle has made 8 to 10revolutions. Depress the clutch lever, stop the motor, and read the scale. If the pointer is not in view or if it is below 10 % torquewhen the dial comes to rest, rapidly throw the mo
41、tor switch on and off (with the clutch lever still depressed) until the pointer isin view and is above 10 % torque.Follow the manufacturers instructions to measure the viscosity for the sample using a 15 secondrotation time.14.4 Repeat the procedure until the readings (after each 8 to 10 revolutions
42、) agree to within one scale division. (After theanalysis, spindles are cleaned with a solvent appropriate for the isocyanate and equipment used, for example, dichloromethane oracetone.WarningAlways release the clutch lever when the spindle is still immersed in the liquid so that pointer will float b
43、ackrather than snap back to zero.)15. Calculation15.1 Viscosity, mPa s (Multiply the reading bycP the) = factorA provided byF. the manufacture for the speed/spindlecombination used to convert the instrument reading to the viscosity in mPa.s (cP). Most instruments automatically perform thiscalculatio
44、n.11.1.1 A = dial reading on the 100 scale.11.1.2 F = conversion factor (see Table 2).16. Report16.1 Report the following information:16.1.1 Temperature of test,16.1.2 Model of viscometer,16.1.3 Speed of rotation,16.1.4 Spindle number, and16.1.5 Viscosity in millipascal seconds (centipoises) mPas(cP
45、).D4889 15317. Precision and Bias17.1 PrecisionAttempts to develop a precision and bias statement for this test method have not been successful; however, theprecision is expected to be equivalent to that reported by the instrument manufacturer. For this reason, data on precision and biascannot be gi
46、ven. Because this test method does not contain a numerical precision and bias statement, it shall not be used as a refereetest method in case of dispute. Anyone wishing to participate in the development of precision and bias data should contact theChairman, Subcommittee D 20.22 (Section D 20.22.01),
47、 ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428.17.2 BiasThe bias of this test method has not yet been determined.TEST METHOD BCANNON-FENSKEBKINEMATIC VISCOSITY18. General:18.1 A general test method for Cannon-Fenskekinematic viscosity which applies to isocyanates as well as other material
48、s ispublished in Test Method D445.19. Keywords19.1 Brookfield; dynamic viscosity; Cannon-Fenske; isocyanates; isocyanates;kinematic viscosity; polyurethane raw materials;rotational viscosity; viscositySUMMARY OF CHANGESCommittee D20 has identified the location of selected changes to this standard si
49、nce the last issue(D488904(2011) that may impact the use of this standard. (May 1, 2015)(1) Subsection 1.1: ScopeChanged naming of methylene di(phenylisocyanate) to be consistent with the other polyurethane rawmaterial methods.(2) Section 1, NOTE 1: ScopeNumerous changes throughout to remove specific instrument manufacturer names and make themethod more applicable to all instruments.(3) Section 1, NOTE 2: ScopeUpdated ISO equivalency.(4) Subsection 2.2: ISO StandardsAdded equivalent ISO standards.(5) Subsection 5.1: SamplingThe previ
