1、Designation: D 7279 08An American National StandardStandard Test Method forKinematic Viscosity of Transparent and Opaque Liquids byAutomated Houillon Viscometer1This standard is issued under the fixed designation D 7279; the number immediately following the designation indicates the year oforiginal
2、adoption 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*1.1 This test method covers the measurement of the kine-matic viscosity
3、 of transparent and opaque liquids such as freshand used lubricating oils using a Houillon viscometer inautomated mode.1.2 The range of kinematic viscosity capable of beingmeasured by this test method is from 2 to 1500 mm2/s (see Fig.1). The range is dependent on the tube constant utilized. Thetempe
4、rature range that the apparatus is capable of achieving isbetween 20C and 150C, inclusive; however, the precision hasonly been determined for the viscosity range 25 to 150 mm2/sat 40C and 5 to 16 mm2/s at 100C for the materials listed inthe precision section.1.3 The values stated in SI units are to
5、be regarded asstandard. No other units of measurement are included in thisstandard.1.4 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
6、determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D 2162 Practice for Basic Ca
7、libration of Master Viscom-eters and Viscosity Oil StandardsD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Eval
8、uate AnalyticalMeasurement System PerformanceD 6708 Practice for Statistical Assessment and Improve-ment of Expected Agreement Between Two Test Methodsthat Purport to Measure the Same Property of a MaterialD 6792 Practice for Quality System in Petroleum Productsand Lubricants Testing LaboratoriesD 7
9、042 Test Method for Dynamic Viscosity and Density ofLiquids by Stabinger Viscometer (and the Calculation ofKinematic Viscosity)2.2 ISO Standards:ISO 5725 Accuracy (Trueness and Precision) of Measure-ment Methods and Results3ISO/EC 17025 General Requirements for the Competenceof Testing and Calibrati
10、on Laboratories32.3 NIST Standard:NIST Technical Note 1297 Guideline for Evaluating andExpressing the Uncertainty of NIST Measurement Re-sults43. Summary of Test Method3.1 The kinematic viscosity is determined by measuring thetime taken for a sample to fill a calibrated volume at a giventemperature.
11、 The specimen is introduced into the apparatus andthen flows into the viscometer tube which is equipped with twodetection cells. The specimen reaches the test temperature ofthe viscometer bath and when the leading edge of the specimenpasses in front of the first detection cell, the automatedinstrume
12、nt starts the timing sequence. When the leading edgeof the specimen passes in front of the second detection cell, theinstrument stops timing the flow. The time interval thusmeasured allows the calculation of the kinematic viscosityusing a viscometer tube constant determined earlier by calibra-tion w
13、ith certified viscosity reference standards.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.07 on Flow Properties.Current edition approved July 1, 2008. Published August 2008. Originallyapproved
14、 in 2006. Last previous edition approved in 2006 as D 727906.2For referenced ASTM standards, visit the ASTM website, www.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.
15、3Available from American National Standards Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036, http:/www.ansi.org.4Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http:/www.nist.gov.1*A Summary of Changes secti
16、on appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.2 The kinematic viscosity is calculated using the formula:n5C 3 t (1)where:n = the kinematic viscosity in mm2/s,C = the viscometer tube constant
17、in mm2/s, andt = the flow time in s measured during the test.4. Significance and Use4.1 Many petroleum products and some non-petroleumproducts are used as lubricants in the equipment, and thecorrect operation of the equipment depends upon the appropri-ate viscosity of the lubricant being used. Addit
18、ionally, theviscosity of many petroleum fuels is important for the estima-tion of optimum storage, handling, and operational conditions.Thus, the accurate determination of viscosity is essential tomany product specifications.4.2 The viscosity of used oils is a commonly determinedparameter in the oil
19、 industry to assess the effect of engine wearon the lube oils used, as well as the degradation of the engineparts during operation.4.3 The Houillon viscometer tube method offers automateddetermination of kinematic viscosity. Typically a sample vol-ume of less than 1 mL is required for the analysis.5
20、. Apparatus5.1 Automated ViscometerThe system shall consist of thefollowing components:5.1.1 Viscometer Bath:5.1.1.1 Bath, to ensure optimal thermal equilibration of thesystem, the bath is filled with mineral or silicone oil andequipped with a stirring device.5.1.2 Temperature Regulation System, to
21、control the bathtemperature to within 0.02C.5.1.3 Houillon Viscometer Tubes, made of glass with acalibrated volume which varies depending on the tube size (seeFig. 2). This technique allows the viscosity to be measuredover a wide range of values (see Fig. 1).5.1.4 Cleaning/Vacuum System, consisting
22、of one or moresolvent reservoirs to transport the solvent(s) to the viscometertubes, dry the viscometer tubes after the flushing cycle, toremove the sample, and for drainage of waste products.5.1.5 Automated Viscometer Control SystemSuitable elec-tronic processor capable of operating the apparatus,
23、controllingthe operation of the timers, regulating the bath temperature,cleaning the viscometer tubes, and recording and reporting theresults.5.1.6 PC-compatible Computer System, may be used fordata acquisition, as per manufacturers instructions.5.1.7 Temperature Measuring DevicesUse either cali-bra
24、ted liquid-in-glass thermometers, of an accuracy after cor-rection of 60.02C or better, or other thermometric devices ofequal or better accuracy.5.1.8 Timing DevicesUse any timing device that is ca-pable of taking readings with a discrimination of 0.01 s orbetter with an accuracy within 60.07 % of t
25、he reading whentested over the minimum and maximum intervals of expectedflow times.5.1.9 Volume Delivery Device, such as a micropipette,capable of delivering a sufficient volume of sample to theHouillon tube being used. (See Fig. 1 for approximate samplevolumes.)6. Reagents and Materials6.1 Certifie
26、d viscosity reference standards shall be certifiedby a laboratory that has been shown to meet the requirementsof ISO/EC 17025 by independent assessment. The certifiedviscosity reference standards shall be traceable to masterviscometer procedures described in Test Method D 2162.6.1.1 The uncertainty
27、of the certified viscosity referencestandard shall be stated for each certified value (k =295%confidence). See ISO 5725 or NIST 1297.NOTEViscosity range of a Houillon tube is based on most practical flow time of 30 to 200 s.FIG. 1 Houillon Viscometer Typical Viscosity Range of Tube ConstantsD7279082
28、6.2 Non-chromium-containing, strongly oxidizing acidcleaning solution. (WarningNon-chromium-containing,strongly oxidizing acid cleaning solutions are highly corrosiveand potentially hazardous in contact with organic materials, butdo not contain chromium which has special disposal prob-lems.)6.3 Solv
29、ent(s) for cleaning, drying, reagent grade. Refer tomanufacturers recommendations. Filter before use if neces-sary. Typical solvent(s) include:6.3.1 Toluene. (WarningFlammable. Vapor harmful.)6.3.2 Petroleum spirit or naphtha. (WarningFlammable.Health hazard.)6.3.3 Acetone. (WarningExtremely flammab
30、le. Healthhazard.)6.3.4 Heptane. (WarningFlammable. Health hazard.)6.4 Technical grade silicone oil or white oil of appropriateviscosity (for example, about 100 mm2/s 25C or equiva-lent) to maintain the test temperature.7. Sampling7.1 Obtain a representative test specimen in accordancewith Practice
31、D 4057 or Practice D 4177.8. Preparation of Apparatus8.1 Place the automated viscometer on a stable and levelhorizontal surface. Make appropriate piping, drainage, andvacuum connections. Refer to the manufacturers instructions.8.2 If not already mounted, install the detection cells.8.3 After install
32、ing and securing all viscometer tubes in thebath, fill the bath with appropriate amount of bath fluid (see6.4).8.4 Add the appropriate amount of solvent(s) to the solventreservoir(s).8.5 Follow the manufacturers instructions for the operationof the instrument.8.6 Select a clean, dry, and calibrated
33、viscometer tubehaving a range covering the estimated kinematic viscosity ofthe specimen to be tested, if known. The appropriate viscom-eter tube to use depends on the estimated viscosity of thesample to be tested. The calculation in 8.6.1 may be used todecide which tube to use.8.6.1 Using Eq 1, the
34、viscometer tube should be chosen sothat its constant C falls between n/200 C n/30 to give flowtimes, T, between 30 and 200 s.NOTE 1In the interlaboratory study5conducted for the developmentof this test method, the flow times were between 30 and 200 s.8.6.2 If a viscosity estimate is not known, a sec
35、ond analysismay be necessary using a different viscometer tube after a firsttrial analysis.9. Calibration9.1 Calibrate according to the manufacturers instructions.Calibrated tubes may be purchased but shall be verified as per9.4.9.2 Use certified viscosity reference standards (see 6.1).5Supporting d
36、ata have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D021604.A and B = sample reservoirC and D = calibrated volumemeasurement zoneE = bulbF = detection cellTube Filling Volume for a MeasurementThe filling volume is OK when:At the beginning of a
37、measurement:Sample lower meniscus is on C (start timing)Sample upper meniscus should be below AAt the end of a measurement:Sample lower meniscus is on D (stop timing)Sample upper meniscus should be above BFIG. 2 Houillon Tube Schematic DiagramD72790839.3 Refer to Section 10 for general operation of
38、the auto-mated viscometer and to the manufacturers instructions.9.4 The determined kinematic viscosity should match thecertified value within 60.5 %. If it does not, then reanalyze thestandard. If the value is still out of range, then check all controlsystem settings for the viscometer tube, and rec
39、heck each stepin the procedure, including the temperature measuring device,and viscometer calibration to locate the source of error.NOTE 2The most common sources of error are caused by particles ofdust lodged in the capillary bore of the viscosity tube (particularly for usedoils) and temperature mea
40、surement errors. Modification of the cleaningconstants by increasing the number of cycles and increasing the aspirationtime before and after passage of the solvent (see Section 11) may berequired.10. General Procedure for Kinematic Viscosity10.1 Set and maintain the automated viscometer bath at ther
41、equired test temperature.10.1.1 Thermometers, if used, shall be held in an uprightposition under the same conditions of immersion as whencalibrated.10.2 Introduce a sufficient volume of sample to the Houillontube, using a volume delivery device (see 5.1.9) such as amicro-pipette. The specimen volume
42、 to be used is a function ofthe viscometer tube constant (see Fig. 1). Fig. 2 shows thecorrect specimen levels during a measurement.NOTE 3Use a volume delivery device that is capable of introducingthe entire specimen volume in one operation.10.3 Introduce the specimen into the viscometer tube. Start
43、the measurement sequence.10.4 The automated viscometer processing system willmeasure the flow times, calculate the viscosity according to Eq1, and record the result.10.5 Start the cleaning sequence (see Section 11).10.6 Allow the viscometer tube to reach the bath tempera-ture (about 5 min) before pe
44、rforming a new measurement.NOTE 4In some units, the equilibration time required may be muchless than 5 min.11. Cleaning of Viscosity Tubes11.1 The viscometer tubes are cleaned by vacuuming thespecimen residue left in the viscometer tube followed by theuse of a solvent to remove any traces of the spe
45、cimen on theviscometer tube walls. The solvent is then removed by vacuum.Some units use a second solvent for drying the tube. Thisoperation is repeated several times until the viscometer tube isclean. Periodically, the viscometer tube calibration constantshould be checked.11.2 The solvent(s) should
46、have a boiling point appropriatefor the bath temperature.11.2.1 The solvent flow must be sufficient to clean the entireinternal section of the viscometer tube. This can be achieved byadjusting the solvent flow(s) and the flow rate using appropri-ate controls.11.3 The cleaning of one tube shall not b
47、e carried out whilea test is being performed in another tube in the same bath.NOTE 5Some multiple tube systems, although not included in theinterlaboratory study5conducted to obtain the precision and bias of thistest method, are designed to clean tubes while other tubes are performingviscosity measu
48、rements. Hence, this cleaning does not interfere with thevalidity of the tests underway in the instrument.11.4 To ensure good operation, regularly check the viscom-eter tubes for damage and cleanliness. The latter can be doneby checking with the reference oils suitable for the particulartube being u
49、sed. Use these check oils like regular samples. Ifthe results obtained are different from the certified values ofthese oils, it is necessary to carry out a more vigorous cleaningof the tubes in question. Non-chromium containing cleaningsolution (see 6.2) may have to be used.11.5 The frequency at which the tubes should be checkedusing reference oils depends on the frequency with which thetubes are used for measurements.12. Quality Control/Quality Assurance (QC/QA)12.1 Confirm proper performance of the instrument and thetest procedure by analyzing a Q
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