1、Designation: D7279 16Standard 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,residual fuel oils, marine fuels, and used lubricating oils usinga Houillon viscometer in automated mode.1.2 The range of kinematic viscosity capable of beingmeasured by this test method is from 2 mm2/s to 2500 mm2/s(see
4、 Fig. 1). The range is dependent on 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,diese
5、l oil, biodiesel, and biodiesel blends; 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; 25 mm2/s to 2500 mm2/s at50 C and 6 mm2/s to 110 mm2/s at 100 C for residual fuels.As indicated for the mate
6、rials listed in the precision section.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 does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the u
7、ser 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, see Section 6.2. Referenced Documents2.1 ASTM Standards:2D445 Test Method for Kinematic Viscosity of Transparentand Opaq
8、ue Liquids (and Calculation of Dynamic Viscos-ity)D2162 Practice for Basic Calibration of Master Viscometersand Viscosity Oil StandardsD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Apply
9、ing Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6708 Practice for Statistical Assessment and Improvementof Expe
10、cted Agreement Between Two Test Methods thatPurport to Measure the Same Property of a MaterialD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing LaboratoriesE1137 Specification for Industrial Platinum Resistance Ther-mometers2.2 ISO Standards:ISO 5725 Accuracy (Trueness an
11、d Precision) of Measure-ment Methods and Results3ISO/EC 17025 General Requirements for the Competence ofTesting and Calibration 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
12、 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 andthen flows into the viscometer tube which is equipped with twodetection cells. The specimen reaches the test temperature of1T
13、his 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 June 1, 2016. Published July 2016. Originally approvedin 2006. Last previous edition a
14、pproved in 2014 as D7279 14a. DOI: 10.1520/D7279-16.2For 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.3Availabl
15、e 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 appears
16、 at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1the viscometer bath and when the leading edge of the specimenpasses in front of the first detection cell, the automatedinstrument starts the timing sequence.
17、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 with certified viscosity referen
18、ce 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 = the flow time in s measured during the test.4. Significance and Use4.1 Many petroleum products and some non-petroleumproduct
19、s 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, theviscosity of many petroleum fuels is important for the estima-tion of optimum storage, handling, and operational conditions.Thus,
20、 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 the effect of engine wearon the lube oils used, as well as the degradation of the engineparts during operation.4.3 The Ho
21、uillon 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 Automated ViscometerThe system shall consist of thefollowing components:5.1.1 Viscometer Bath:5.1.1.1 Bath, to ensure optimal
22、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 bathtemperature to within 0.02 C.5.1.3 Houillon Viscometer Tubes, made of glass with acalibrated volume which varies depending on
23、 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 moresolvent reservoirs to transport the solvent(s) to the viscometertubes, dry the viscometer tubes after the flushing cycle, tore
24、move the sample, and for drainage of waste products.5.1.5 Automated Viscometer Control SystemSuitable elec-tronic processor capable of operating the apparatus, controllingthe operation of the timers, regulating the bath temperature,cleaning the viscometer tubes, and recording and reporting theresult
25、s.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-glass thermometers, of an accuracy after cor-rection of 60.02 C or better, or other thermometric devicessuch as a digital cont
26、act thermometer as described in 5.1.7.1with equal or better accuracy.5.1.7.1 When using a digital contact thermometer (DCT) thefollowing shall apply: (1) The only acceptable sensors are aresistance temperature device (RTD), such as a platinumresistance thermometer (PRT) or a thermistor. (2) A minimu
27、mdisplay resolution of 0.01 C. (3) A combined (display andprobe) minimum accuracy of 60.02 C. (4) A response time ofless than6sasdefined in Specification E1137.(5) A drift ofless than 10 mK (0.01 C) per year. (6) Linearity of 10 mK overthe range of intended use. (7) The DCT shall have a report oftem
28、perature calibration traceable to a national calibration ormetrology standards body issued by a competent calibrationNOTE 1Viscosity range of a Houillon tube is based on most practical flow time of 30 s to 200 s.FIG. 1 Houillon Viscometer Typical Viscosity Range of Tube ConstantsD7279 162laboratory
29、with demonstrated competency in temperature cali-bration. (8) The calibration report shall include data for theseries of test points which are appropriate for its intended use.(1) For a constant temperature bath employed in manualviscosity measurements, the probe shall be immersed at least100 mm bel
30、ow the liquid level of the bath but no less than threetimes the sensor element length. The end of the probe sheathshall not extend past the bottom of the viscometer.(2) It is preferable for the center of the sensing element tobe located at the same level as the lower half of the workingcapillary as
31、long as the minimum immersion requirements aremet.(3) In the case of constant temperature baths used ininstruments for automatic viscosity determinations, the user isto contact the instrument manufacturer for the correct DCT thathas performance equivalence to that described here.5.1.8 Timing Devices
32、Use 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 whentested over the minimum and maximum intervals of expectedflow times.5.1.9 Volume Delivery Device, such as a micropipette,capable of delivering a suffi
33、cient volume of sample to theHouillon tube being used. (See Fig. 1 for approximate samplevolumes.)6. 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 assessment. The certifie
34、dviscosity 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-chromium-containing, stro
35、ngly 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 cleaning, drying, reag
36、ent 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. Healthhazard.)6.3.4 Heptane.
37、(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. Sampling and Test Specimens7.1 Obtain a representative test specimen in accordancewith Practice D4057 or Prac
38、tice D4177.7.2 Instructions for Residual Fuel Oils(WarningExercise care as vigorous boil-over can occur when opaqueliquids that contain high levels of water are heated to highA and B = sample reservoirC and D = calibrated volumemeasurement zoneE = bulbF = detection cellTube Filling Volume for a Meas
39、urementThe filling volume is OK when:At the beginning of a 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 Diagr
40、amD7279 163temperatures. Wear appropriate personal protective equipmentfor handling hot materials.)7.2.1 Place the first batch of resid samples to be analyzed forthe day in their original containers in a sample pre-heatapparatus that is held between 60 C and 65 C for 1 h. Ensurethe cap on each conta
41、iner is tightly closed.7.2.2 Rigorously stir each sample for approximately 20 swith a glass or steel rod of sufficient length to reach the bottomof the container.7.2.3 Remove the stirring rod and inspect for sludge or waxadhering to the rod. If there is sludge or wax adhering to therod, continue sti
42、rring until the sample is homogeneous.7.2.4 Recap each container tightly and shake vigorously for1 min. Then loosen the cap, retighten to finger tight, then backoff34 turn to a full turn and place back into the sample pre-heatapparatus.7.2.5 Upon completion of 7.2.4 for all samples in the batch,incr
43、ease the sample pre-heat apparatus temperature to between100 C and 105 C and continue heating for 30 min.7.2.6 Remove each container from the sample pre-heatapparatus, close tightly, and shake vigorously for 60 s.7.2.7 Using a volume delivery device such as amicropipette, introduce sufficient volume
44、 of the sample into theselected Houillon tube. The volume to be used is a function ofthe viscometer tube constant. The volume delivery device maybe pre-warmed to facilitate transfer of highly viscous samples.(See Section 10.)7.2.8 Analysis of all samples in the batch must be completedwithin 1 h from
45、 completion of 7.2.6.8. 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 a
46、nd 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 visco
47、meter 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 visco
48、meter tube 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.8.6.2 If a viscosity estimate is not known, a second
49、 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).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 thestandard. If the value
