ASTM D445 - 24 PDF - Standard Test Method for Kinematic Viscosity

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to...

This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee. Designation: D445 − 24 Standard Test Method for Kinematic Viscosity of Transparent and Opaque Liquids (and Calculation of Dynamic Viscosity)1 This standard is issued under the fixed designation D445; the number immediately following the designation indicates the year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A superscript epsilon (´) indicates an editorial change since the last revision or reapproval. This standard has been approved for use by agencies of the U.S. Department of Defense. 1. Scope* serious medical issues. Mercury, or its vapor, has been dem- 1.1 This test method specifies a procedure for the determi- onstrated to be hazardous to health and corrosive to materials. nation of the kinematic viscosity, ν, of liquid petroleum Use Caution when handling mercury and mercury-containing products, both transparent and opaque, by measuring the time products. See the applicable product Safety Data Sheet (SDS) for a volume of liquid to flow under gravity through a for additional information. The potential exists that selling calibrated glass capillary viscometer. The dynamic viscosity, η, mercury or mercury-containing products, or both, is prohibited can be obtained by multiplying the kinematic viscosity, ν, by by local or national law. Users must determine legality of sales the density, ρ, of the liquid. in their location. 1.6 This standard does not purport to address all of the NOTE 1—For the measurement of the kinematic viscosity and viscosity of bitumens, see also Test Methods D2170 and D2171. safety concerns, if any, associated with its use. It is the NOTE 2—ISO 3104 corresponds to Test Method D445 – 03. responsibility of the user of this standard to establish appro- priate safety, health, and environmental practices and deter- 1.2 The result obtained from this test method is dependent mine the applicability of regulatory limitations prior to use. upon the behavior of the sample and is intended for application 1.7 This international standard was developed in accor- to liquids for which primarily the shear stress and shear rates dance with internationally recognized principles on standard- are proportional (Newtonian flow behavior). If, however, the ization established in the Decision on Principles for the viscosity varies significantly with the rate of shear, different Development of International Standards, Guides and Recom- results may be obtained from viscometers of different capillary mendations issued by the World Trade Organization Technical diameters. The procedure and precision values for residual fuel Barriers to Trade (TBT) Committee. oils, which under some conditions exhibit non-Newtonian behavior, have been included. 2. Referenced Documents 1.3 The range of kinematic viscosities covered by this test 2.1 ASTM Standards:2 method is from 0.2 mm2/s to 300 000 mm2/s (see Table A1.1) D396 Specification for Fuel Oils at all temperatures (see 6.3 and 6.4). The precision has only D446 Specifications and Operating Instructions for Glass been determined for those materials, kinematic viscosity Capillary Kinematic Viscometers ranges and temperatures as shown in the footnotes to the D1193 Specification for Reagent Water precision section. D1217 Test Method for Density and Relative Density (Spe- 1.4 The values stated in SI units are to be regarded as cific Gravity) of Liquids by Bingham Pycnometer standard. The SI unit used in this test method for kinematic D1480 Test Method for Density and Relative Density (Spe- viscosity is mm2/s, and the SI unit used in this test method for cific Gravity) of Viscous Materials by Bingham Pycnom- dynamic viscosity is mPa·s. For user reference, 1 mm2/s = eter 10-6 m2/s = 1 cSt and 1 mPa·s = 1 cP = 0.001 Pa·s. D1481 Test Method for Density and Relative Density (Spe- 1.5 WARNING—Mercury has been designated by many cific Gravity) of Viscous Materials by Lipkin Bicapillary regulatory agencies as a hazardous substance that can cause Pycnometer (Withdrawn 2023)3 1 2 This test method is under the jurisdiction of Committee D02 on Petroleum For referenced ASTM standards, visit the ASTM website, www.astm.org, or Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcom- contact ASTM Customer Service at [email protected]. For Annual Book of ASTM mittee D02.07 on Flow Properties. Standards volume information, refer to the standard’s Document Summary page on Current edition approved April 1, 2024. Published April 2024. Originally the ASTM website. 3 approved in 1937. Last previous edition approved in 2023 as D445 – 23. DOI: The last approved version of this historical standard is referenced on 10.1520/D0445-24. www.astm.org. *A Summary of Changes section appears at the end of this standard Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States 1 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 D2162 Practice for Basic Calibration of Master Viscometers NIST GMP 11 Good Measurement Practice for Assignment and Viscosity Oil Standards and Adjustment of Calibration Intervals for Laboratory D2170 Test Method for Kinematic Viscosity of Asphalts Standards7 D2171 Test Method for Viscosity of Asphalts by Vacuum NIST Special Publication 811 Guide for the Use of the Capillary Viscometer International System of Units (SI)8 D6071 Test Method for Low Level Sodium in High Purity NIST Special Publication 1088 Maintenance and Validation Water by Graphite Furnace Atomic Absorption Spectros- of Liquid-in-Glass Thermometers9 copy 3. Terminology D6074 Guide for Characterizing Hydrocarbon Lubricant Base Oils 3.1 See also International Vocabulary of Metrology.10 D6299 Practice for Applying Statistical Quality Assurance 3.2 Definitions: and Control Charting Techniques to Evaluate Analytical 3.2.1 digital contact thermometer (DCT), n—an electronic Measurement System Performance device consisting of a digital display and associated tempera- D6300 Practice for Determination of Precision and Bias ture sensing probe. Data for Use in Test Methods for Petroleum Products, 3.2.1.1 Discussion—This device consists of a temperature Liquid Fuels, and Lubricants sensor connected to a measuring instrument; this instrument D6617 Practice for Laboratory Bias Detection Using Single measures the temperature-dependent quantity of the sensor, Test Result from Standard Material computes the temperature from the measured quantity, and D6708 Practice for Statistical Assessment and Improvement provides a digital output. This digital output goes to a digital of Expected Agreement Between Two Test Methods that display and/or recording device that may be internal or external Purport to Measure the Same Property of a Material to the device. D8278 Specification for Digital Contact Thermometers for 3.2.1.2 Discussion—The devices are often referred to as a Test Methods Measuring Flow Properties of Fuels and “digital thermometers,” however the term includes devices that Lubricants sense temperature by means other than being in physical E1 Specification for ASTM Liquid-in-Glass Thermometers contact with the media. E77 Test Method for Inspection and Verification of Ther- 3.2.1.3 Discussion—PET is an acronym for portable elec- mometers tronic thermometers, a subset of digital contact thermometers (DCT). E563 Practice for Preparation and Use of an Ice-Point Bath as a Reference Temperature 3.3 Definitions of Terms Specific to This Standard: E1750 Guide for Use of Water Triple Point Cells 3.3.1 automated viscometer, n—apparatus which, in part or E2593 Guide for Accuracy Verification of Industrial Plati- in whole, has mechanized one or more of the procedural steps num Resistance Thermometers indicated in Section 11 or 12 without changing the principle or technique of the basic manual apparatus. The essential ele- 2.2 ISO Standards:4 ments of the apparatus in respect to dimensions, design, and ISO 3104 Petroleum products—Transparent and opaque operational characteristics are the same as those of the manual liquids—Determination of kinematic viscosity and calcu- method. lation of dynamic viscosity 3.3.1.1 Discussion—Automated viscometers have the capa- ISO 3105 Glass capillary kinematic viscometers— bility to mimic some operation of the test method while Specification and operating instructions reducing or removing the need for manual intervention or ISO 3696 Water for analytical laboratory use—Specification interpretation. Apparatus which determine kinematic viscosity and test methods by physical techniques that are different than those used in this ISO 5725 Accuracy (trueness and precision) of measurement test method are not considered to be Automated Viscometers. methods and results 3.3.2 density, n—the mass per unit volume of a substance at ISO 9000 Quality management and quality assurance a given temperature. standards—Guidelines for selection and use 3.3.3 dynamic viscosity, η, n—the ratio between the applied ISO 17025 General requirements for the competence of shear stress and rate of shear of a material. testing and calibration laboratories 3.3.3.1 Discussion—It is sometimes called the coefficient of 2.3 NIST Standards:5 dynamic viscosity or absolute viscosity. Dynamic viscosity is a NIST Technical Note 1297 Guideline for Evaluating and measure of resistance to flow or deformation which constitutes Expressing the Uncertainty of NIST Measurement Re- a material’s ability to transfer momentum in response to steady sults6 or time-dependent external shear forces. Dynamic viscosity has 7 http://ts.nist.gov/WeightsAndMeasures/upload/GMP_11_Mar_2003.pdf 4 8 Available from American National Standards Institute (ANSI), 25 W. 43rd St., http://www.nist.gov/pml/pubs/sp811/index.cfm 9 4th Floor, New York, NY 10036, http://www.ansi.org. http://www.nist.gov/pml/pubs/sp1088/index.cfm 5 10 Available from National Institute of Standards and Technology (NIST), 100 International Vocabulary of Metrology — Basic and General Concepts and Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460. Associated Terms (VIM), 3rd ed., 2008, http://www.bipm.org/en/publications/ 6 http://physics.nist.gov/cuu/Uncertainty/bibliography.html guides/vim.html. 2 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 the dimension of mass divided by length and time and its SI 6.1.2 Automated Viscometers—Automated apparatus may unit is pascal times second (Pa·s). Among the transport be used as long as they mimic the physical conditions, properties for heat, mass, and momentum transfer, dynamic operations, or processes of the manual apparatus. Any viscosity is the momentum conductivity. viscometer, temperature measuring device, temperature 3.3.4 kinematic viscosity, ν, n—the ratio of the dynamic control, temperature-controlled bath, or timing device incorpo- viscosity (η) to the density (ρ) of a material at the same rated in the automated apparatus shall conform to the specifi- temperature and pressure. cation for these components as stated in Section 6 of this test 3.3.4.1 Discussion—Kinematic viscosity is the ratio be- method. Flow times of less than 200 s are permitted, however, tween momentum transport and momentum storage. Such a kinetic energy correction shall be applied in accordance with ratios are called diffusivities with dimensions of length squared Section 7 on Kinematic Viscosity Calculation of Specifications divided by time and the SI unit is metre squared divided by D446. The kinetic energy correction shall not exceed 3.0 % of second (m2/s). Among the transport properties for heat, mass, the measured viscosity. The automated apparatus shall be and momentum transfer, kinematic viscosity is the momentum capable of determining kinematic viscosity of a certified diffusivity. viscosity reference standard within the limits stated in 9.2.1 3.3.4.2 Discussion—Formerly, kinematic viscosity was de- and Section 17. The precision has been determined for auto- fined specifically for viscometers covered by this test method mated viscometers tested on the sample types listed in 17.3.1 as the resistance to flow under gravity. More generally, it is the and is no worse than the manual apparatus (that is, exhibits the ratio between momentum transport and momentum storage. same or less variability). 3.3.4.3 Discussion—For gravity-driven flow under a given NOTE 3—Precision and bias of kinematic viscosity measurements for hydrostatic head, the pressure head of a liquid is proportional flow times as low as 10 s have been determined for automated instruments to its density, ρ, if the density of air is negligible compared to tested with the sample types listed in 17.3.1. that of the liquid. For any particular viscometer covered by this 6.2 Viscometer Holders—Use viscometer holders to enable test method, the time of flow of a fixed volume of liquid is all viscometers which have the upper meniscus directly above directly proportional to its kinematic viscosity, ν, where the lower meniscus to be suspended vertically within 1° in all ν = η ⁄ρ, and η is the dynamic viscosity. directions. Those viscometers whose upper meniscus is offset from directly above the lower meniscus shall be suspended 4. Summary of Test Method vertically within 0.3° in all directions (see Specifications D446 4.1 The time is measured for a fixed volume of liquid to and ISO 3105). flow under gravity through the capillary of a calibrated 6.2.1 Viscometers shall be mounted in the constant tempera- viscometer under a reproducible driving head and at a closely ture bath in the same manner as when calibrated and stated on controlled and known temperature. The kinematic viscosity the certificate of calibration. See Specifications D446, see (determined value) is the product of the measured flow time Operating Instructions in Annexes A1–A3. For those viscom- and the calibration constant of the viscometer. Two such eters which have Tube L (see Specifications D446) held determinations are needed from which to calculate a kinematic vertical, vertical alignment shall be confirmed by using (1) a viscosity result that is the average of two acceptable deter- holder ensured to hold Tube L vertical, or (2) a bubble level mined values. mounted on a rod designed to fit into Tube L, or (3) a plumb line suspended from the center of Tube L, or (4) other internal 5. Significance and Use means of support provided in the constant temperature bath. 5.1 Many petroleum products, and some non-petroleum 6.3 Temperature-Controlled Bath—Use a transparent liquid materials, are used as lubricants, and the correct operation of bath of sufficient depth such, that at no time during the the equipment depends upon the appropriate viscosity of the measurement of flow time, any portion of the sample in the liquid being used. In addition, the viscosity of many petroleum viscometer is less than 20 mm below the surface of the bath fuels is important for the estimation of optimum storage, liquid or less than 20 mm above the bottom of the bath. handling, and operational conditions. Thus, the accurate deter- mination of viscosity is essential to many product specifica- 6.3.1 Temperature Control—For each series of flow time tions. measurements, the temperature control of the bath liquid shall be such that within the range from 15 °C to 100 °C, the 6. Apparatus temperature of the bath medium does not vary by more than 60.02 °C of the selected temperature over the length of the 6.1 Viscometers—Use only calibrated viscometers of the viscometer, or between the position of each viscometer, or at glass capillary type, capable of being used to determine the location of the thermometer. For temperatures outside this kinematic viscosity within the limits of the precision given in range, the deviation from the desired temperature must not the precision section. exceed 60.05 °C. 6.1.1 Viscometers listed in Table A1.1, whose specifications meet those given in Specifications D446 and in ISO 3105 meet 6.4 Temperature Measuring Devices: these requirements. It is not intended to restrict this test method 6.4.1 Liquid-in-glass Thermometers—Use calibrated ther- to the use of only those viscometers listed in Table A1.1. mometers noted in Annex A2. Devices with a nominal tem- Annex A1 gives further guidance. perature range from 0 °C to 100 °C will have an accuracy after 3 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 correction of 60.02 °C or better. When the nominal tempera- accomplished with the use of a water triple point cell, an ice ture range is outside the 0 °C to 100 °C range, they will have bath, or other suitable constant temperature device which has a an accuracy after correction of 60.05 °C or better. known temperature value of suitable precision. See Practice 6.4.1.1 If calibrated liquid-in-glass thermometers are used, E563 and Guides E1750 and E2593 for more information the use of two thermometers is recommended. When the regarding checking calibrations. temperature range is from 0 °C to 100 °C, the two 6.4.2.2 In the case of constant temperature baths used in thermometers, with corrections applied, shall agree within instruments for automatic viscosity determinations, the user is 0.04 °C. When the temperature range is outside 0 °C to 100 °C, to contact the instrument manufacturer for the correct DCT that the two thermometers, with corrections applied, shall agree to has performance equivalence to that described here. within 0.1 °C. 6.4.2 Digital Contact Thermometer—Use the indicated 6.4.3 Outside the range from 0 °C to 100 °C, use either DCT for the following nominal temperature ranges: calibrated liquid-in-glass thermometers of an accuracy after correction of 60.05 °C or better, or any other thermometric Nominal Temperature Range Specification D8278 DCT Id –80 °C to 0 °C D02-DCT04 device of equal or better accuracy. When two temperature 0 °C to 100 °C D02-DCT05 measuring devices are used in the same bath, they shall agree 100 °C to 175 °C D02-DCT06 within 60.1 °C. 6.4.2.1 Verify the calibration at least annually. The probe 6.4.4 Temperature Device Placement: shall be recalibrated when the check value differs by more than 0.02 °C from the last probe calibration. Verification can be FIG. 1 Temperature Probe Immersion in Constant Temperature Bath 4 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 6.4.4.1 Liquid-in-glass Thermometer, shall be suspended 7. Reagents and Materials vertically and positioned so that the top of the liquid column is 7.1 Chromic Acid Cleaning Solution, or a nonchromium- just below the surface of the bath fluid. See Fig. 1. containing, strongly oxidizing acid cleaning solution. 6.4.4.2 DCT Probe, shall be immersed by more than its (Warning—Chromic acid is a health hazard. It is toxic, a minimum immersion depth in a constant temperature bath so recognized carcinogen, highly corrosive, and potentially haz- that the center of the probe’s sensing region is at the same level ardous in contact with organic materials. If used, wear a full as the lower half of the working capillary provided the probe’s face-shield and full-length protective clothing including suit- minimum immersion depth is met and is no less than indicated able gloves. Avoid breathing vapor. Dispose of used chromic on calibration certificate. See Fig. 1. The end of the probe acid carefully as it remains hazardous. Nonchromium- sheath shall not extend past the bottom of the viscometer. It is containing, strongly oxidizing acid cleaning solutions are also preferable for the center of the sensing element to be located at highly corrosive and potentially hazardous in contact with the same level as the lower half of the working capillary as organic materials, but do not contain chromium which has long as the minimum immersion requirements are met. special disposal problems.) 6.4.5 When using liquid-in-glass thermometers, such as those in Table A2.1, use a magnifying device to read the 7.2 Sample Solvent, completely miscible with the sample. thermometer to the nearest 1⁄5 division (for example, 0.01 °C or Filter before use. 0.02 °F) to ensure that the required test temperature and 7.2.1 For most samples, a volatile petroleum spirit or temperature control capabilities are met (see 10.1). It is naphtha is suitable. For residual fuels, a prewash with an recommended that thermometer readings (and any corrections aromatic solvent such as toluene or xylene may be necessary to supplied on the certificates of calibrations for the thermom- remove asphaltenic material. eters) be recorded on a periodic basis to demonstrate compli- 7.3 Drying Solvent, a volatile solvent miscible with the ance with the test method requirements. This information can sample solvent (see 7.2) and water (see 7.4). Filter before use. be quite useful, especially when investigating issues or causes 7.3.1 Acetone is suitable. (Warning—Extremely flam- relating to testing accuracy and precision. mable.) 6.5 Timing Device for Manual Viscometers—Use any timing 7.4 Water, deionized or distilled and conforming to Speci- device, mechanical (spring-wound or motor driven) or digital, fication D1193 or Grade 3 of ISO 3696. Filter before use. that is capable of taking readings with a discrimination of 0.1 s or better and has an accuracy within 60.07 % (see Annex A3) 8. Certified Viscosity Reference Standards of the reading when tested over the minimum and maximum 8.1 Certified viscosity reference standards shall be certified intervals of expected flow times. by a laboratory that has been shown to meet the requirements 6.5.1 Timing devices powered by alternating electric current of ISO 17025 by independent assessment. Viscosity standards motors may be used if the current frequency is controlled to an shall be traceable to master viscometer procedures described in accuracy of 0.05 % or better. Alternating currents, as provided Practice D2162. by some public power systems, are intermittently rather than continuously controlled. When used to actuate electrical timing 8.2 The uncertainty of the certified viscosity reference devices, such control can cause large errors in kinematic standard shall be stated for each certified value (k = 2, 95 % viscosity flow time measurements. confidence). See ISO 5725 or NIST 1297. 6.5.2 Timing devices employed in automated viscometers are an integral part of the apparatus and typically are digital 9. Calibration and Verification (using a precision crystal oscillator) with discriminations of 9.1 Viscometers—Use only calibrated viscometers, 0.01 s or better. As such, the timing devices are included within thermometers, and timers as described in Section 6. the overall system calibration of automated viscometers. Fol- low the manufacturer’s instructions for ensuring the automated 9.2 Certified Viscosity Reference Standards (Table A1.2)— viscometer is properly calibrated using CRM’s such that it is These are for use as confirmatory checks on the procedure in capable of determining kinematic viscosity of a certified the laboratory. viscosity reference standard within the limits stated in 9.2.1 9.2.1 If the determined kinematic viscosity does not agree and Section 17 (see 6.1.2). within the acceptable tolerance band, as calculated from Annex A4, of the certified value, recheck each step in the procedure, 6.6 Ultrasonic Bath, Unheated—(optional), with an operat- including thermometer and viscometer calibration, to locate the ing frequency between 25 kHz to 60 kHz and a typical power source of error. Annex A1 gives details of standards available. output of ≤100 W, of suitable dimensions to hold container(s) placed inside of bath, for use in effectively dissipating and NOTE 4—In previous issues of Test Method D445, limits of 60.35 % of the certified value have been used. The data to support the limit of removing air or gas bubbles that can be entrained in viscous 60.35 % cannot be verified. Annex A4 provides instructions on how to sample types prior to analysis. It is permissible to use ultra- determine the tolerance band. The tolerance band combines both the sonic baths with operating frequencies and power outputs uncertainty of the certified viscosity reference standard as well as the outside this range, however it is the responsibility of the uncertainty of the laboratory using the certified viscosity reference laboratory to conduct a data comparison study to confirm that standard. results determined with and without the use of such ultrasonic 9.2.1.1 As an alternative to the calculation in Annex A4, the baths does not materially impact results. approximate tolerance bands in Table 1 may be used. 5 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 TABLE 1 Approximate Tolerance Bands open ends of the viscometer is permitted but not mandatory. NOTE 1—The tolerance bands were determined using Practice D6617. These are designed to prevent water condensation. It is The calculation is documented in Research Report RR:D02-1498.A essential that they do not set up a pressure differential and Viscosity of Reference Material, affect the rate of flow. Before the first use of drying tubes, it is Tolerance Band mm2/s recommended that a certified viscosity reference standard is < 10 ±0.30 % used to verify the correct use of the viscometer with and 10 to 100 ±0.32 % 100 to 1000 ±0.36 % without drying tubes in order to ensure that there is no 1000 to 10 000 ±0.42 % restriction in the flow. When the test temperature is below the 10 000 to 100 000 ±0.54 % dew point, fill the viscometer in the normal manner as required > 100 000 ±0.73 % A in 11.1. It is recommended to charge the viscometer outside the Supporting data have been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1498. bath. To ensure that moisture does not condense or freeze on the walls of the capillary, draw the test portion into the working capillary and timing bulb, place rubber stoppers into the tubes to hold the test portion in place, and insert the viscometer into 9.2.2 The most common sources of error are caused by the bath. After insertion, allow the viscometer to reach bath particles of dust lodged in the capillary bore and temperature temperature, and then remove the stoppers. When performing measurement errors. It must be appreciated that a correct result manual viscosity determinations, do not use those viscometers obtained on a standard oil does not preclude the possibility of which cannot be removed from the constant temperature bath a counterbalancing combination of the possible sources of for charging the sample portion. error. 10.2.3 Viscometers used for silicone fluids, fluorocarbons, and other liquids which are difficult to remove by the use of a 9.3 The calibration constant, C, is dependent upon the cleaning agent, shall be reserved for the exclusive use of those gravitational acceleration at the place of calibration and this fluids except during their calibration. Subject such viscometers must, therefore, be supplied by the standardization laboratory to calibration checks at frequent intervals. The solvent wash- together with the instrument constant. Where the acceleration ings from these viscometers shall not be used for the cleaning of gravity, g, differs by more than 0.1 %, correct the calibration of other viscometers. constant as follows: C 2 5 ~ g 2 /g 1 ! × C 1 (1) 11. Procedure for Transparent Liquids where the subscripts 1 and 2 indicate, respectively, the 11.1 Although not mandatory, for some transparent liquid standardization laboratory and the testing laboratory. sample types such as viscous oils that are prone to having entrained air or gas bubbles present in the sample, the use of an 10. General Procedure for Kinematic Viscosity ultrasonic bath (see 6.6) without the heater turned on (if so 10.1 Adjust and maintain the viscometer bath at the required equipped) has been found effective in homogenizing and test temperature within the limits given in 6.3.1, taking account dissipating bubbles typically within 5 min prior to taking a test of the conditions given in Annex A2 and of the corrections specimen for analysis, with no material impact on results. supplied on the certificates of calibration for the thermometers. Charge the viscometer in the manner dictated by the design of 10.1.1 Thermometers shall be held in an upright position the instrument, this operation being in conformity with that under the same conditions of immersion as when calibrated. employed when the instrument was calibrated. If the sample is 10.1.2 In order to obtain the most reliable temperature thought or known to contain fibers or solid particles, filter measurement, it is recommended that two thermometers with through a 75 µm screen, either prior to or during charging (see valid calibration certificates be used (see 6.4). Specifications D446). 10.1.3 They should be viewed with a lens assembly giving NOTE 5—To minimize the potential of particles passing through the approximately five times magnification and be arranged to filter from aggregating, it is recommended that the time lapse between eliminate parallax errors. filtering and charging be kept to a minimum. 10.2 Select a clean, dry, calibrated viscometer having a 11.1.1 In general, the viscometers used for transparent range covering the estimated kinematic viscosity (that is, a liquids are of the type listed in Table A1.1; however, for the wide capillary for a very viscous liquid and a narrower manual measurement of kinematic viscosity of jet fuels at capillary for a more fluid liquid). The flow time for manual –20 °C only suspended-level type viscometers as noted in viscometers shall not be less than 200 s or the longer time Table A1.1 shall be used. The suspended level type viscometer noted in Specifications D446. Flow times of less than 200 s are types used for jet fuel do not require a correction to the permitted for automated viscometers, provided they meet the calibration constant for the test temperature being used. requirements of 6.1.2. 11.1.2 With certain products which exhibit gel-like 10.2.1 The specific details of operation vary for the different behavior, exercise care that flow time measurements are made types of viscometers listed in Table A1.1. The operating at sufficiently high temperatures for such materials to flow instructions for the different types of viscometers are given in freely, so that similar kinematic viscosity results are obtained Specifications D446. in viscometers of different capillary diameters. 10.2.2 When the test temperature is below the ambient dew 11.1.3 Allow the charged viscometer to remain in the bath point, the use of loosely-packed drying tubes affixed to the long enough to reach the test temperature. Where one bath is 6 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 used to accommodate several viscometers, never add or 12. Procedure for Residual Fuel Oils and Opaque withdraw, or clean a viscometer while any other viscometer is Liquids in use for measuring a flow time. 12.1 For steam-refined cylinder oils and black lubricating 11.1.4 Because this time will vary for different instruments, oils, proceed to 12.2 ensuring a thoroughly representative for different temperatures, and for different kinematic sample is used. The kinematic viscosity of residual fuel oils viscosities, establish a safe equilibrium time by trial. and similar waxy products can be affected by the previous 11.1.4.1 Thirty minutes should be sufficient except for the thermal history and the following procedure described in highest kinematic viscosities, however a minimum of 30 min is 12.1.1 to 12.1.8 shall be followed to minimize this. specifically required for manual analysis of jet fuels at −20 °C. 12.1.1 In general, the viscometers used for opaque liquids 11.1.5 Where the design of the viscometer requires it, adjust are of the reverse-flow type listed in Table A1.1, C. the volume of the sample to the mark after the sample has 12.1.2 Heat the sample in the original container at a reached temperature equilibrium. temperature between 60 °C and 65 °C for 1 h. 11.2 Use suction (if the sample contains no volatile con- 12.1.3 Place the BS/IP/RF U-tube reverse-flow, or Zeitfuchs stituents) or pressure to adjust the head level of the test sample Cross-arm, or Lantz-Zeitfuchs type reverse-flow viscometer to a position in the capillary arm of the instrument about 7 mm for the samples to be tested in the viscometer bath(s) at the above the first timing mark, unless any other value is stated in required test temperature. If the viscometers are to be charged the operating instructions for the viscometer. With the sample prior to insertion in the viscometer bath, for example, Cannon flowing freely, measure, in seconds to within 0.1 s, the time Fenske Opaque, see 12.2.1. required for the meniscus to pass from the first to the second 12.1.4 Upon completion of step 12.1.2, vigorously stir each timing mark. If this flow time is less than the specified sample for approximately 20 s with a glass or steel rod of minimum (see 10.2), select a viscometer with a capillary of sufficient length to reach the bottom of the container. For smaller diameter and repeat the operation. samples of a very waxy nature or oils of high kinematic 11.2.1 Repeat the procedure described in 11.2 to make a viscosity, it may be necessary to increase the heating tempera- second measurement of flow time. Record both measurements. ture above 65 °C to achieve proper mixing. The sample should 11.2.2 From the two measurements of flow time, calculate be sufficiently fluid for ease of stirring and shaking. two determined values of kinematic viscosity. 12.1.5 Remove the stirring rod and inspect for sludge or 11.2.3 If the two determined values of kinematic viscosity wax adhering to the rod. Continue stirring until there is no calculated from the flow time measurements agree within the sludge or wax adhering to the rod. stated determinability figure (see 17.1.1) for the product, use 12.1.6 Recap the container tightly and shake vigorously for the average of these determined values to calculate the kine- 1 min to complete the mixing. To protect the integrity of the matic viscosity result to be reported. Record the result. If not, sample should a repeat analysis be required, pour sufficient repeat the measurements of flow times (11.2 to 11.2.2) after a sample to fill two flasks and loosely stopper. (Each flask should thorough cleaning and drying of the viscometers and filtering hold sufficient sample to fill two viscometers in order to obtain (where required, see 11.1) of the sample until the calculated two determinations. The second flask is required to carry out a kinematic viscosity determinations agree with the stated deter- repeat analysis.) If a repeat analysis is not a consideration the minability. next steps can be performed using the original container, loosely capped. NOTE 6—Poor determinability can be the result of several factors including: air bubbles trapped in the sample within the viscometer, poor 12.1.7 Heat the first sample flask or sample container temperature stability of the constant temperature bath, particulate con- between 100 °C and 105 °C for 30 min. tamination in the viscometer, or specimen heterogeneity. Additional 12.1.8 Remove the first sample flask or sample container sample-specific issues may be conformational changes related to time and from the heat, close tightly, and shake vigorously for 60 s. thermal history (incomplete reaction of blended chemistries, re-alignment of polymeric chains, or outgassing of un-reacted components) or the 12.2 Two determinations of the kinematic viscosity of the sample is a binary mixture of mixed phases (i.e., there may be precipitated test material are required. For those viscometers that require a solids such as waxes in the liquid portion of the sample). complete cleaning after each flow time measurement, two 11.2.4 If the material or temperature, or both, is not listed in viscometers must be used. These two determinations are used 17.1.1, use 1.5 % as an estimate of the determinability. to calculate one result. Charge two viscometers in the manner 11.2.5 In automated apparatuses, it is permissible to con- dictated by the design of the instrument. For example, for the tinue running successive determinations after the initial two Lantz-Zeitfuchs Cross-arm or the BS/IP/RF U-tube reverse- determinations up to a maximum of four, without the need to flow viscometers for opaque liquids, filter the sample through clean and dry the viscometer tube in between determinations. a 75 µm filter into two viscometers previously placed in the Choose from any two successive determinations (i.e., 1-2, 2-3, bath. For samples subjected to heat treatment, use a preheated 3-4) which meet the corresponding determinability precision filter to prevent the sample coagulating during the filtration. statement for the material type being measured. If two succes- 12.2.1 Viscometers which are charged before being inserted sive determinations that meet the determinability precision into the bath may need to be preheated in an oven prior to cannot be found for a sample, suspend execution of this test charging the sample. This is to ensure that the sample will not method for that sample. See Note 6 for further guidance. be cooled below test temperature. 7 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 12.2.2 After 10 min, adjust the volume of the sample (where 13. Cleaning of Viscometer the design of the viscometer requires) to coincide with the 13.1 Between successive determinations of kinematic filling marks as in the viscometer specifications (see Specifi- viscosity, clean the viscometer thoroughly by several rinsings cations D446). with the sample solvent, followed by the drying solvent (see 12.2.3 Allow the charged viscometers enough time to reach 7.3). Dry the tube by passing a slow stream of filtered dry air the test temperature (see 12.2.1). Where one bath is used to through the viscometer for 2 min or until the last trace of accommodate several viscometers, never add or withdraw, or solvent is removed. clean a viscometer while any other viscometer is in use for measuring flow time. 13.2 If periodic verification of the viscometer calibration using certified viscosity reference standards (see 9.2) is outside 12.3 With the sample flowing freely, measure in seconds to of the acceptable tolerance band, the viscometer may need to within 0.1 s, the time required for the advancing ring of contact be cleaned. Clean the viscometer with the cleaning solution to pass from the first timing mark to the second. Record the (Warning—see 7.1), for several hours to remove residual measurement. traces of organic deposits, rinse thoroughly with water (7.4) 12.3.1 In the case of samples requiring heat treatment and drying solvent (see 7.3), and dry with filtered dry air or a described in 12.1 through 12.1.8, complete the measurements vacuum line. Remove any inorganic deposits by hydrochloric of flow time within 1 h of completing 12.1.8. Record the acid treatment before the use of cleaning acid, particularly if measured flow times. the presence of barium salts is suspected. (Warning—It is essential that alkaline cleaning solutions are not used as 12.4 Calculate kinematic viscosity, ν, in millimetres squared changes in the viscometer calibration can occur.) per second, from each measured flow time. Regard these as two determined values of kinematic viscosity. 14. Calculation 12.4.1 For residual fuel oils, if the two determined values of 14.1 Calculate each of the determined kinematic viscosity kinematic viscosity agree within the stated determinability values, ν1 and ν2, from the measured flow times, t1 and t2, and figure (see 17.1.1), use the average of these determined values the viscometer constant, C, by means of the following equa- to calculate the kinematic viscosity result to be reported. This tion: constitutes one analysis. Record the result. If a second value (repeat) is required, then repeat the analysis after thorough ν 1,2 5 C·t 1,2 (2) cleaning and drying of the viscometers starting from sample where: preparation steps 12.1.6 using the second flask. If the original ν1,2 = determined kinematic viscosity values for ν1 and ν2, container has been conditioned using steps 12.1.2 to 12.1.8, respectively, mm2/s, then this is not suitable for a repeat analysis. If the calculated C = calibration constant of the viscometer, mm2/s2, and kinematic viscosities do not agree, repeat the measurements of t1,2 = measured flow times for t1 and t2, respectively, s. flow times after thorough cleaning and drying of the viscom- eters and filtering of the sample. If the material or temperature, Calculate the kinematic viscosity result, ν, as an average of or both, is not listed in 17.1.1, for temperatures between 15 °C ν1 and ν2 (see 11.2.3 and 12.4.1). and 100 °C use as an estimate of the determinability 1.0 %, and 14.2 Calculate the dynamic viscosity, η, from the calculated 1.5 % for temperatures outside this range; it must be realized kinematic viscosity, ν, and the density, ρ, by means of the that these materials can be non-Newtonian, and can contain following equation: solids which can come out of solution as the flow time is being η 5 ν × ρ × 1023 (3) measured. where: NOTE 7—Poor determinability can be the result of several factors including: air bubbles trapped in the sample within the viscometer, poor η = dynamic viscosity, mPa·s, temperature stability of the constant temperature bath, particulate con- ρ = density, kg/m3, at the same temperature used for the tamination in the viscometer, or specimen heterogeneity. Additional determination of the kinematic viscosity, and sample-specific issues may be conformational changes related to time and ν = kinematic viscosity, mm2/s. thermal history (incomplete reaction of blended chemistries, re-alignment of polymeric chains, or outgassing of un-reacted components) or the 14.2.1 The density of the sample can be determined at the sample is a binary mixture of mixed phases (i.e., there may be precipitated test temperature of the kinematic viscosity determination by an solids such as waxes in the liquid portion of the sample). appropriate method such as Test Method D1217, D1480, or 12.4.2 In automated apparatuses, it is permissible to con- D1481. tinue running successive determinations after the initial two 15. Expression of Results determinations up to a maximum of four, without the need to clean and dry the viscometer tube in between determinations. 15.1 Report the test results for the kinematic or dynamic Choose from any two successive determinations (i.e., 1-2, 2-3, viscosity, or both, to four significant figures, together with the 3-4) which meet the corresponding determinability precision test temperature. statement for the material type being measured. If two succes- sive determinations that meet the determinability precision 16. Report cannot be found for a sample, suspend execution of this test 16.1 Report the following information: method for that sample. See Note 7 for further guidance. 16.1.1 Type and identification of the product tested, 8 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 16.1.2 Reference to this test method or a corresponding Gas oils at 40 °C16 0.0013 (y+1) international standard, Jet fuels at –20 °C17 0.007608 Kerosine, diesel fuels, 0.0037 y (0.37 %) 16.1.3 Result of the test (see Section 15), biodiesel fuels, and biodiesel 16.1.4 Any deviation, by agreement or otherwise, from the fuel blends at 40 °C18 procedure specified, where: y is the average of determined values being com- 16.1.5 Date of the test, and pared. 16.1.6 Name and address of the test laboratory. 17.1.2 The determinability for used (in-service) formulated oils has not been determined, however use a limit of 1.0 % (see 17. Precision and Bias 12.4.1) for temperatures between 15 °C and 100 °C.19 17.1 Comparison of Determined Values: 17.2 Comparison of Results: 17.2.1 Repeatability (r)—The difference between successive 17.1.1 Determinability (d)—The difference between succes- results obtained by the same operator in the same laboratory sive determined values obtained by the same operator in the with the same apparatus under constant operating conditions on same laboratory using the same apparatus for a series of identical test material would, in the long run, in the normal and operations leading to a single result, would in the long run, in correct operation of this test method, exceed the values the normal and correct operation of this test method, exceed the indicated only in one case in twenty: values indicated only in one case in twenty: Base oils at 40 °C11 0.0101 x (1.01 %) Base oils at 40 °C11 0.0037 y (0.37 %) Base oils at 100 °C11 0.0085 x (0.85 %) Base oils at 100 °C11 0.0036 y (0.36 %) Formulated oils at 40 °C11 0.0074 x (0.74 %) Formulated oils at 40 °C11 0.0037 y (0.37 %) Formulated oils at 100 °C11 0.0084 x (0.84 %) Formulated oils at 100 °C11 0.0036 y (0.36 %) Formulated oils at 150 °C12 0.0056 x (0.56 %) Formulated oils at 150 °C12 0.015 y (1.5 %) Petroleum wax at 100 °C13 0.0141 x1.2 Petroleum wax at 100 °C13 0.0080 y (0.80 %) Residual fuel oils at 50 °C14 0.07885 x (7.88 %) Residual fuel oils at 50 °C14 0.0244 y (2.44 %) Residual fuel oils at 100 °C14 0.08088 x (8.08 %) Residual fuel oils at 100 °C14 0.03 y (3 %) Additives at 100 °C15 0.00192 x1.1 Additives at 100 °C15 0.00106 y1.1 Gas oils at 40 °C16 0.0043 (x+1) Jet fuels at –20 °C17 0.001368 x1.4 Kerosine, diesel fuels, biodiesel 0.0056 x (0.56 %) fuels, and biodiesel fuel blends at 11 40 °C18 Supporting data has been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1788. These precision values were obtained by statistical examination of interlaboratory results for the following samples: Base Oils with viscosities between (12.0 and 476.0) mm2/s at 40 °C tested 16 in seven laboratories; Formulated Oils with viscosities between (28.0 and Supporting data have been filed at ASTM International Headquarters and may 472.0) mm2/s at 40 °C tested in seven laboratories; Base Oils with viscosities be obtained by requesting Research Report RR:D02-1422. These precision values between (2.90 and 32.0) mm2/s at 100 °C tested in eight laboratories; Formulated were obtained by statistical examination of interlaboratory results from eight gas Oils with viscosities between (6.50 and 107.0) mm2/s at 100 °C tested in eight oils in the range from 1 mm2/s to 13 mm2/s at 40 °C and were first available in 1997. laboratories. Formulated Oils include automatic transmission fluids, hydraulic Kerosine and diesel fuel samples, which can be considered as gas oils, were fluids, motor oils, gear oils, polymers in base oil and additives in base oil. The included in a dataset to determine the precision for kerosine, diesel fuels, biodiesel determinability, repeatability, and reproducibility results are for tests performed with fuels, and biodiesel fuel blends at 40 °C (RR:D02-1780). The precision stated in manual viscometers. Determinability, repeatability, and reproducibility for RR:D02-1780 was developed in a more recent interlaboratory study than the automated/automatic instruments are no worse than that for the manual instruments. precision stated in RR:D02-1422. Therefore, the gas oil precision statements do not For the precision of specific automated/automatic instruments see Research Report apply to kerosine and diesel fuels and a user should refer to the precision statements RR:D02-1820. for kerosine, diesel fuels, biodiesel fuels, and biodiesel fuel blends at 40 °C. 12 17 Supporting data have been filed at ASTM International Headquarters and may Supporting data may be obtained by requesting ILS2017_71_3 from the be obtained by requesting Research Report RR:D02-1333. These precision values Energy Institute, http://www.energyinst.org. This data was obtained using manual were obtained by statistical examination of interlaboratory results for eight fully analysis. formulated engine oils in the range from 7 mm2/s to 19 mm2/s at 150 °C, and first 18 Supporting data have been filed at ASTM International Headquarters and may published in 1991. See Guide D6074. be obtained by requesting Research Report RR:D02-1780. These precision values 13 Supporting data have been filed at ASTM International Headquarters and may were obtained by statistical examination of interlaboratory results from seven be obtained by requesting Research Report RR:D02-1334. These precision values samples including kerosine, diesel fuels, biodiesel fuels, and biodiesel fuel blends were obtained by statistical examination of interlaboratory results from five (RR:D02-1780) in the range from 2.06 mm2/s to 4.50 mm2/s at 40 °C. The petroleum waxes in the range from 3 mm2/s to 16 mm2/s at 100 °C, and were first determinability, repeatability, and reproducibility results are for tests performed with published in 1988. manual viscometers. Determinability, repeatability, and reproducibility for 14 Supporting data have been filed at ASTM International Headquarters and may automated/automatic instruments are no worse than that for the manual instruments. be obtained by requesting Research Report RR:D02-1837. These precision values For the precision of specific automated/automatic instruments see Research Report were obtained by statistical examination of interlaboratory results from eleven RR:D02-1820. 19 laboratories on residual fuel oil samples conforming to D396 Grades 5 or 6 and/or Supporting data have been filed at ASTM International Headquarters and may ISO8217 RMG and RMK at 50 °C and 10 at 100 °C in the range from 27.34 mm2/s be obtained by requesting Research Report RR:D02-1852. The precision values to 2395 mm2/s at 50 °C and 6.36 mm2/s to 120.8 mm2/s at 100 °C. These precision were obtained by statistical examination of interlaboratory results from ten used statements only refer to measurement of viscosity using manual viscometers. (in-service) formulated oil samples. These consisted of steam turbine, gas turbine, 15 Supporting data have been filed at ASTM International Headquarters and may diesel engine, hydraulic, and gasoline engine oil samples which were analyzed by be obtained by requesting Research Report RR:D02-1421. These precision values ten laboratories using both manual and automated apparatuses. The kinematic were obtained by statistical examination of interlaboratory results from eight viscosities of these samples ranged from 25 mm2/s to 125 mm2/s at 40 °C, and from additives in the range from 145 mm2/s to 1500 mm2/s at 100 °C and were first 6 mm2/s to 16 mm2/s at 100 °C. The statistical output is based on ten laboratories available in 1997. and eight samples at 40 °C and ten laboratories and ten samples at 100 °C. 9 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 Used (in-service) formulated oils at 0.000233 x1.722 17.3.1 The determinability, repeatability, and reproducibil- 40 °C19 ity have been determined for automated/automatic viscometers Used (in-service) formulated oils at 0.001005 x1.4633 100 °C19 for the following sample types and temperatures: where: x is the average of results being compared. Distillates, fatty acid methyl esters, and distillates contain- 17.2.1.1 The degrees of freedom associated with the repeat- ing fatty acid methyl esters at 40 °C ability estimate for the kerosine, diesel fuels, biodiesel fuels, Base oils at 40 °C and 100 °C and biodiesel fuel blends at 40 °C round robin study are 16. Formulated oils at 40 °C and 100 °C Since the minimum requirement of 30 (in accordance with For these sample types, determinability, repeatability, and Practice D6300) is not met, users are cautioned that the actual reproducibility for automated/automatic instruments are no repeatability may be significantly different than these esti- worse than that for the manual instruments. For the precision of mates. specific automated/automatic instruments see Research Report 17.2.2 Reproducibility (R)—The difference between two RR:D02-1820. single and independent results obtained by different operators The precision has been determined for automated viscom- working in different laboratories on nominally identical test eters and the range of r and R values for automated instruments material would, in the long run, in the normal and correct is shown in RR:D02-1820. For the samples listed in RR:D02- operation of this test method, exceed the values indicated 1820, precision for automated instruments is no worse than that below only in one case in twenty. for the manual instruments.22 Base oils at 40 °C11 0.0136 x (1.36 %) 17.3.1.1 Degree of Agreement Between Results by Manual Base oils at 100 °C11 0.0190 x (1.90 %) and Automated Instruments in Test Method D445—Results for Formulated oils at 40 °C11 0.0122 x (1.22 %) Formulated oils at 100 °C11 0.0138 x (1.38 %) the sample types listed in RR:D02-1820 produced by manual Formulated oils at 150 °C12 0.018 x (1.8 %) and automated instruments in this test method have been Petroleum wax at 100 °C13 0.0366 x1.2 assessed in accordance with procedures outlined in Practice Residual fuel oils at 50 °C14 0.08461 x (8.46 %) Residual fuel oils at 100 °C14 0.1206 x (12.06 %) D6708. Additives at 100 °C15 0.00862 x1.1 17.3.1.2 The findings are: Results from manual and auto- Gas oils at 40 °C16 0.0082 (x+1) mated instruments in Test Method D445 may be considered to Jet fuels at –20 °C17 0.002899 x1.4 Kerosine, diesel fuels, biodiesel fuels, 0.0224 x (2.24 %) be practically equivalent, for sample types listed in RR:D02- and biodiesel fuel blends at 40 °C18 1820. No sample-specific bias, as defined in Practice D6708, 1.722 Used (in-service) formulated oils at 0.000594 x was observed for the materials studied. Differences between 40 °C19 Used (in-service) formulated oils at 0.003361 x1.4633 results from manual and automated instruments in Test Method 100 °C19 D445, for the samples listed in RR:D02-1820, are expected to where: x is the average of results being compared. exceed the following between methods reproducibility: 1.91 % 17.2.2.1 The degrees of freedom associated with the repro- for distillates, fatty acid methyl esters, and distillates contain- ducibility estimate for the kerosine, diesel fuels, biodiesel ing fatty acid methyl esters at 40 °C; 1.27 % for base oils at fuels, and biodiesel fuel blends at 40 °C round robin study are 40 °C; 1.23 % for formulated oils at 40 °C; 1.70 % for base oils 19. Since the minimum requirement of 30 (in accordance with at 100 °C; 1.21 % for formulated oils at 100 °C, as defined in Practice D6300) is not met, users are cautioned that the actual Practice D6708, about 5 % of the time. These percent differ- reproducibility may be significantly different than these esti- ences are based upon the highest calculated combined method mates. reproducibilities (Rxy in Practice D6708).23 17.3 The precision for specific automated and automatic viscometers has been determined for sample types and tem- 18. Keywords peratures listed in 17.3.1. An analysis has been made of a large 18.1 dynamic viscosity; kinematic viscosity; viscometer; dataset including both automated/automatic and manual vis- viscosity cometers over the temperature range of 40 °C to 100 °C for the sample types listed in 17.3.1. The determinability, repeatability, and reproducibility of automated/automatic viscometer data are 22 Supporting data have been filed at ASTM International Headquarters and may no worse than the determinability, repeatability, and reproduc- be obtained by requesting Research Report RR:D02-1787. These precision values ibility for the manual instruments. It is also shown in the were obtained by statistical examination of interlaboratory results from seven research reports that no statistically significant bias was ob- samples including distillates, fatty acid methyl esters, and distillates containing fatty acid methyl esters (RR:D02-1790) in the range from (2.06 to 4.50) mm2/s at 40 °C. served between the automated/automatic data in comparison to These seven samples were tested in 21 different Cannon and Herzog instruments to the manual data.20 For the precision of specific automated/ obtain the precision values shown. automatic instruments, see RR:D02-1820.21 23 Supporting data has been filed at ASTM International Headquarters and may be obtained by requesting Research Report RR:D02-1787. These precision values were obtained by statistical examination of interlaboratory results for the following samples: Base Oils with viscosities between (12.0 and 476.0) mm2/s at 40 °C tested 20 Supporting data have been filed at ASTM International Headquarters and may in 22 laboratories; Formulated Oils with viscosities between (28.0 and 472.0) mm2/s be obtained by requesting Research Report RR:D02-1498. Contact ASTM Customer at 40 °C tested in 22 laboratories; Base Oils with viscosities between (2.90 and 32.0) Service at [email protected]. mm2/s at 100 °C tested in 21 laboratories; Formulated Oils with viscosities between 21 Supporting data have been filed at ASTM International Headquarters and may (6.50 and 107.0) mm2/s at 100 °C tested in 21 laboratories. Formulated Oils include be obtained by requesting Research Report RR:D02-1820. Contact ASTM Customer automatic transmission fluids, hydraulic fluids, motor oils, gear oils, polymers in Service at [email protected]. base oil, and additives in base oil. 10 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 ANNEXES (Mandatory Information) A1. VISCOMETER TYPES AND CERTIFIED VISCOSITY REFERENCE STANDARDS A1.1 Viscometer Types TABLE A1.1 Viscometer Types Viscometer Identification Kinematic Viscosity Range,A mm2/s A1.1.1 Table A1.1 lists capillary viscometers commonly in A. Ostwald Types for Transparent Liquids use for viscosity determinations on petroleum products. For Cannon-Fenske routineB 0.5 to 20 000 specifications, operating instructions, and calibration, refer to Zeitfuchs 0.6 to 3 000 B BS/U-tube 0.9 to 10 000 specifications in Specifications D446. BS/U/M miniature 0.2 to 100 B SIL 0.6 to 10 000 A1.1.2 Table A1.2 lists certified viscosity reference stan- Cannon-Manning semi-micro 0.4 to 20 000 dards. PinkevitchB 0.6 to 17 000 B. Suspended-level Types for Transparent Liquids BS/IP/SLB 3.5 to 100 000 B BS/IP/SL(S) 1.05 to 10 000 BS/IP/MSL 0.6 to 3 000 B Ubbelohde 0.3 to 100 000 FitzSimons 0.6 to 1 200 AtlanticB 0.75 to 5 000 Cannon-Ubbelohde(A), Cannon 0.5 to 100 000 Ubbelohde dilutionB (B) Cannon-Ubbelohde semi-micro 0.4 to 20 000 C. Reverse-flow Types for Transparent and Opaque Liquids Cannon-Fenske opaque 0.4 to 20 000 Zeitfuchs cross-arm 0.6 to 100 000 BS/IP/RF U-tube reverse-flow 0.6 to 300 000 Lantz-Zeitfuchs type reverse-flow 60 to 100 000 A Each range quoted requires a series of viscometers. To avoid the necessity of making a kinetic energy correction, these viscometers are designed for a flow time in excess of 200 s except where noted in Specifications D446. B In each of these series, the minimum flow time for the viscometers with lowest constants exceeds 200 s. TABLE A1.2 Certified Viscosity Reference Standards Approximate Kinematic Viscosity, mm2/s Designation 20 °C 25 °C 40 °C 50 °C 80 °C 100 °C S3 4.6 4.0 2.9...... 1.2 S6 11 8.9 5.7...... 1.8 S20 44 34 18...... 3.9 S60 170 120 54...... 7.2 S200 640 450 180...... 17 S600 2400 1600 520 280 67 32 S2000 8700 5600 1700...... 75 S8000 37 000 23 000 6700......... S30 000... 81 000 23 000 11 000...... A2. KINEMATIC VISCOSITY TEST THERMOMETERS A2.1 Short-Range Specialized Liquid-in-Glass Thermom- A2.1. As an alternative, use a digital contact thermometer eter (DCT) as defined in 6.4.2. A2.1.1 Use a short-range specialized liquid-in-glass ther- A2.1.2 The difference in the designs of the liquid-in-glass mometer conforming to the generic specification given in Table thermometers rests mainly in the position of the ice-point scale. A2.1 and Table A2.2 and to one of the designs shown in Fig. In Design A, the ice point is within the scale range, in Design 11 'RZQORDGHG3ULQWHG$FFHVVHGE\XVHUNKDOHGDOL_'DWH0RQ-XQ  D445 − 24 TABLE A2.1 General Specification for Thermometers NOTE 1—Table A2.2 gives a range of ASTM, IP, and ASTM/IP thermometers that comply with the specification in Table A2.1, together with their designated test temperatures. See Specification E1 and Test Method E77. Immersion Total Scale marks: Subdivisions °C 0.05 Long lines at each °C 0.1 and 0.5 Numbers at each °C 1 Maximum line width mm 0.10 Scale error at test temperature, max °C 0.1 Expansion chamber: Permit heating to °C 105 up to 90, 120 between 90 and 95 130 between 95 and 105, 170 above 105 Total length mm 300 to 310 Stem outside diameter mm 6.0 to 8.0 Bulb length mm 45 to 55 Bulb outside diameter mm no greater than stem Length of scale range mm 40 to 90 TABLE A2.2 Complying Thermometers