1、Designation: D 7279 06An 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 (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 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 covered by this testmethod is from 0.2 to 1000 mm2/s in the temperature rangebetween 20C and 150C; however, the precision has onlybeen determine
4、d for the materials, viscosity range, and tem-peratures as stated in the precision section (viscosity range 25to 150 mm2/s at 40C and 5 to 16 mm2/s at 100C).1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.4 This standard d
5、oes 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 regulatory limitations prior to use. For specificwarning statements, s
6、ee 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 Calibration of Master Viscom-eters and Viscosity Oil StandardsD 4057 Practice for Manual Sampling of Pet
7、roleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD 6299 Practice for Applying Statistical Quality AssuranceTechniques to Evaluate Analytical Measurement SystemPerformanceD 6708 Practice for Statistical Assessment and Improve-ment of Expected Agreem
8、ent Between Two Test Methodsthat Purport to Measure the Same Property of a MaterialD 6792 Practice for Quality System in Petroleum Productsand Lubricants Testing LaboratoriesD 7042 Test Method for Dynamic Viscosity and Density ofLiquids by Stabinger Viscometer (and the Calculation ofKinematic Viscos
9、ity)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 Calibration Laboratories32.3 NIST Standard:NIST Technical Note 1297 Guideline for Evaluating andExpressing the Uncertainty of NIST M
10、easurement 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 injected into the apparatus andthen flows into the viscometer tube which is equipped with twodetection cel
11、ls. 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 edgeof the specimen passes in front of the second detection cell, theinstrume
12、nt stops timing the flow. The time interval thusmeasured allows the calculation of the 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:n5C 3 t (1)where:n =
13、the kinematic viscosity in mm2/s,C = the viscometer tube constant in mm2/s, and1This 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 Oct. 1, 2006. Publis
14、hed October 2006.2For 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.3Available from American National Standards
15、Institute (ANSI), 25 W. 43rd St.,4th Floor, New York, NY 10036.4Available from National Institute of Standards and Technology (NIST), 100Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United Stat
16、es.t = 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. Additionally, t
17、heviscosity 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
18、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. Apparatu
19、s5.1 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 control th
20、e 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. 1). This technique allows the viscosity to be measuredover a wide range of values (see Fig. 2).5.1.4 Cleaning/Vacuum System, consisting of one or
21、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, controllin
22、gthe 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-brated liquid
23、-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 the reading
24、 whentested over the minimum and maximum intervals of expectedflow times.5.1.9 Micropipette, of a volume range from 50 to 250 Lwith an absolute precision of 62.5 L.6. Reagents and Materials6.1 Certified viscosity reference standards shall be certifiedby a laboratory that has been shown to meet the r
25、equirementsof 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 of the certified viscosity referencestandard shall be stated for each certified value (k =295%confi
26、dence). See ISO 5725 or NIST 1297.6.2 Non-chromium-containing, strongly oxidizing acidcleaning solution. (WarningNon-chromium-containing,strongly oxidizing acid cleaning solutions are highly corrosiveFIG. 1 Houillon Tube Schematic DiagramD7279062and potentially hazardous in contact with organic mate
27、rials, butdo not contain chromium which has special disposal prob-lems.)6.3 Solvent(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 na
28、phtha. (WarningFlammable.Health hazard.)6.3.3 Acetone. (WarningExtremely flammable. 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.
29、7. Sampling7.1 Obtain a representative test specimen in accordancewith Practice 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 instru
30、ctions.8.2 If not already mounted, install the detection cells.8.3 After installing 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 instruct
31、ions for the operationof the instrument.8.6 Select a clean, dry, and calibrated 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 ca
32、lculation in 8.6.1 may be used todecide which tube to use.8.6.1 Using Eq 1, the 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 t
33、imes were between 30 and 200 s.8.6.2 If a viscosity estimate is not known, a second 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 a
34、s per9.4.9.2 Use certified viscosity reference standards (see 6.1).9.3 Refer to Section 10 for general operation of 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 the
35、standard. If the value is still out of range, then check all controlsystem settings for the viscometer tube, and recheck 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
36、 particles ofdust lodged in the capillary bore of the viscosity tube (particularly for usedoils) and temperature measurement 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
37、 berequired.5Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR: D021604.NOTEViscosity range of a Houillon tube is based on most practical flow time of 30 to 200 s.FIG. 2 Houillon Viscometer Typical Viscosity Range of Tube Constants
38、D727906310. General Procedure for Kinematic Viscosity10.1 Set and maintain the automated viscometer bath at therequired test temperature.10.1.1 Thermometers, if used, shall be held in an uprightposition under the same conditions of immersion as whencalibrated.10.2 Use a micro-pipette for injecting t
39、he specimen. Thespecimen volume to be used is a function of the viscometertube constant. Follow manufacturers instructions as to thevolume to be used.10.3 Inject the specimen into the viscometer tube. Start themeasurement sequence.10.4 The automated viscometer processing system willmeasure the flow
40、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 new measurement.NOTE 3In some units, the equilibration time required may be muchles
41、s 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 theviscometer tube walls. The solvent is then removed by vacuum.Some units use a seco
42、nd 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 boiling point appropriatefor the bath temperature.11.2.1 The solvent flow must be suffi
43、cient 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 out whilea test is being performed in another tube in the same bath.NOTE 4Some multi
44、ple 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. Hence, this cleaning does not interfere with thevalidity of the tests underway in the
45、 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
46、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 thetube
47、s 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 QC sample.12.2 If a suitable QC oil sample is not available, prepare theQC material by replicate analyses of a batch of oil sample andstatis
48、tically analyze the data to assign a mean value anduncertainty limit to the sample.12.3 When QC/QA protocols are already established in thetesting facility, these may be used when they confirm thereliability of the test result.12.4 When there is no QC/QA protocol established in thetesting facility,
49、Appendix X1 can be used as the QC/QAsystem. Further guidance can be obtained from Guide D 6792.13. Report13.1 Report the test results for the kinematic viscosity tofour significant figures, together with the test temperature andreference to this test method.14. Precision and Bias14.1 PrecisionBased on an interlaboratory study per-formed in 2004 using 10 used and 5 fresh oil samples (viscosityrange 25 to 150 mm2/s at 40C and 6 to 16 mm2/s at 100C)and 15 laboratories, the following precisions were obtained.514.1.1 RepeatabilityThe difference between
