1、Designation: D7279 14Standard Test Method forKinematic Viscosity of Transparent and Opaque Liquids byAutomated Houillon Viscometer1This standard is issued under the fixed designation D7279; the number immediately following the designation indicates the year oforiginal adoption or, in the case of rev
2、ision, 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 of transparent and opaque liqu
3、ids; such as baseoils, formulated oils, diesel oil, biodiesel, biodiesel blends, andused lubricating oils using a Houillon viscometer in automatedmode.1.2 The range of kinematic viscosity capable of beingmeasured by this test method is from 2 mm2/s to 1500 mm2/s(see Fig. 1). The range is dependent o
4、n the tube constantutilized. The temperature range that the apparatus is capable ofachieving is between 20 C and 150 C, inclusive. However,the precision has only been determined for the viscosity range;2mm2/s to 478 mm2/s at 40 C for base oils, formulated oils,diesel oil, biodiesel, and biodiesel bl
5、ends; 3 mm2/s to106 mm2/s at 100 C for base oils and formulated oils;25 mm2/s to 150 mm2/s at 40 C and 5 mm2/s to 16 mm2/s at100 C for used lubricating oils. As indicated for the materialslisted in the precision section.1.3 The values stated in SI units are to be regarded asstandard. No other units
6、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 determine the applica-bility of regulat
7、ory limitations prior to use. For specificwarning statements, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D2162 Practice for Basic Calibration of Master Viscometersand Viscos
8、ity Oil StandardsD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD
9、6708 Practice for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a MaterialD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing LaboratoriesD7042 Test Method for Dynamic Viscosity and Density o
10、fLiquids 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 Competence ofTesting and Calibration Laboratories32.3 NIST Standard:NIST Technical No
11、te 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. The specimen is introduced into the apparatus andt
12、hen 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 automatedinstrument starts the timing sequence. When the leading edg
13、e1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.07 on Flow Properties.Current edition approved May 1, 2014. Published July 2014. Originally approvedin 2006. Last previous edition
14、 approved in 2008 as D7279 08. DOI: 10.1520/D7279-14.2For 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.3Availab
15、le 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.*A Summary of Changes section appear
16、s at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1of the specimen passes in front of the second detection cell, theinstrument stops timing the flow. The time interval thusmeasured allows the calculation of t
17、he kinematic viscosityusing a viscometer tube constant determined earlier by calibra-tion with certified viscosity reference standards.3.2 The kinematic viscosity is calculated using the formula: 5 C 3t (1)where: = the kinematic viscosity in mm2/s,C = the viscometer tube constant in mm2/s, andt = th
18、e 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. Additionally, theviscosi
19、ty 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 industry to assess
20、 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. Apparatus5.1 Auto
21、mated 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 control the bathtem
22、perature to within 0.02 C.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 of one or moresolv
23、ent 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, controllingthe ope
24、ration 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-brated liquid-in-glas
25、s thermometers, of an accuracy after cor-rection of 60.02 C 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 the reading whente
26、sted 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.)NOTE 1Viscosity range of a Houillon tube is based on m
27、ost practical flow time of 30 s to 200 s.FIG. 1 Houillon Viscometer Typical Viscosity Range of Tube ConstantsD7279 1426. Reagents and Materials6.1 Certified viscosity reference standards shall be certifiedby a laboratory that has been shown to meet the requirementsof ISO/EC 17025 by independent asse
28、ssment. The certifiedviscosity reference standards shall be traceable to masterviscometer procedures described in Test Method D2162.6.1.1 The uncertainty of the certified viscosity referencestandard shall be stated for each certified value (k =295%confidence). See ISO 5725 or NIST 1297.6.2 Non-chrom
29、ium-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 Solvent(s) for cl
30、eaning, 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 flammable. Healthhaz
31、ard.)6.3.4 Heptane. (WarningFlammable. Health hazard.)6.4 Technical grade silicone oil or white oil of appropriateviscosity (for example, about 100 mm2/s 25 C or equiva-lent) to maintain the test temperature.7. Sampling7.1 Obtain a representative test specimen in accordancewith Practice D4057 or Pra
32、ctice D4177.8. 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 installing and securi
33、ng 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 viscometer tub
34、ehaving 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 viscometer tub
35、e should be chosen sothat its constant C falls between /200 C /30 to give flowtimes, T, between 30 s and 200 s.NOTE 1In the interlaboratory study5conducted for the developmentof this test method, the flow times were between 30 s and 200 s.5Supporting data have been filed at ASTM International Headqu
36、arters and maybe obtained by requesting Research Report RR:D02-1604.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 measurement:Sample lower meniscus is on C (start
37、 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 DiagramD7279 1438.6.2 If a viscosity estimate is not known, a second analysismay be necessary using a different
38、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).9.3 Refer to Section 10 for general operation of the auto-ma
39、ted 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 recheck each s
40、tepin 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 measurement er
41、rors. 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 therequired tes
42、t 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 to be used
43、 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. Startthe measure
44、ment 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 performing a
45、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 specimen on th
46、eviscometer 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 have a boil
47、ing 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 be carried o
48、ut 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 measurements. He
49、nce, 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 used. 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
