ASTM D7042 - 21a
ASTM D7042 - 21a
for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
1
D7042 − 21a
2.2 ISO Standards:3 cylinder under the influence of the shear stress of the test
ISO 5725 Accuracy (Trueness and Precision) of Measure- specimen and an eddy current brake in conjunction with
ment Methods and Results adjustment data. The density is determined by the oscillation
ISO 8217 Petroleum products – Fuels (class F) frequency of the U-tube in conjunction with adjustment data.
ISO/IEC 17025 General Requirements for the Competence The kinematic viscosity is calculated by dividing the dynamic
of Testing and Calibration Laboratories viscosity by the density.
2.3 Other Documents:4
NIST Technical Note 1297 Guideline for Evaluating and 5. Significance and Use
Expressing the Uncertainty of NIST Measurement Results 5.1 Many petroleum products, and some non-petroleum
DEF STAN 91-091 Turbine Fuel, Kerosene Type, Jet A-15 materials, are used as lubricants and the correct operation of
the equipment depends upon the appropriate viscosity of the
3. Terminology
liquid being used. In addition, the viscosity of many petroleum
3.1 Definitions: fuels is important for the estimation of optimum storage,
3.1.1 density, n—mass per unit volume. handling, and operational conditions. Thus, the accurate deter-
3.1.2 dynamic viscosity [η], n—the ratio between the ap- mination of viscosity is essential to many product specifica-
plied shear stress and rate of shear of a liquid at a given tions.
temperature. 5.2 Density is a fundamental physical property that can be
3.1.2.1 Discussion—It is sometimes called the coefficient of used in conjunction with other properties to characterize both
dynamic viscosity or, simply, viscosity. Thus, dynamic viscos- the light and heavy fractions of petroleum and petroleum
ity is a measure of the resistance to flow or to deformation of products.
a liquid under external shear forces.
3.1.2.2 Discussion—The term dynamic viscosity can also be 5.3 Determination of the density or relative density of
used in a different context to denote a frequency-dependent petroleum and its products is necessary for the conversion of
quantity in which shear stress and shear rate have a sinusoidal measured volumes to volumes at the standard temperature of
time dependence. 15 °C.
3.1.3 kinematic viscosity, n—the ratio of the dynamic vis- 6. Apparatus
cosity (η) to the density (ρ) of a liquid at a given temperature.
3.1.3.1 Discussion—For gravity flow under a given hydro- 6.1 Stabinger Viscometer6,7
static head, the pressure head of a liquid is proportional to its 6.1.1 Viscosity Measurement—The Stabinger viscometer
density (ρ). Therefore, the kinematic viscosity (ν) is a measure uses a rotational coaxial cylinder measuring system. The outer
of the resistance to flow of a liquid under gravity. cylinder (tube) is driven by a motor at a constant and known
rotational speed. The low-density inner cylinder (rotor) is held
3.1.4 relative density (also called specific gravity (SG)),
in the axis of rotation by the centrifugal forces of the higher
n—the ratio of the density of a material at a stated temperature
density sample and in its longitudinal position by the magnet
to the density of a reference material (usually water) at a stated
and the soft iron ring. Consequently, the system works free of
temperature.
bearing friction as found in rotational viscometers. A perma-
3.2 Definitions of Terms Specific to This Standard: nent magnet in the inner cylinder induces eddy currents in the
3.2.1 T at 12 mm2/s, °C, n—the temperature at which the surrounding copper casing. The rotational speed of the inner
material has a kinematic viscosity of 12 mm2/s. cylinder establishes itself as the result of the equilibrium
3.2.1.1 Discussion—Term mostly is associated with jet fuel between the driving torque of the viscous forces and the
where 12 mm2/s is considered a critical viscosity value. The retarding eddy current torque. This rotational speed is mea-
temperature is determined using Practice D341 interpolation or sured by an electronic system (Hall effect sensor) by counting
extrapolation calculations from two kinematic viscosity data the frequency of the rotating magnetic field (see Fig. 1 and Fig.
points. Other critical viscosity data can similarly be determined 2, No. 2).
for other materials as T at (xx) mm2/s. 6.1.2 Density Measurement—The digital density analyzer
uses a U-shaped oscillating sample tube and a system for
4. Summary of Test Method electronic excitation and frequency counting (see Fig. 2, No.
4.1 The test specimen is introduced into the measuring cells, 3).
which are at a closely controlled and known temperature. The
measuring cells consist of a pair of rotating concentric cylin-
ders and an oscillating U-tube. The dynamic viscosity is 6
The Stabinger viscometer is covered by a patent. Interested parties are invited
determined from the equilibrium rotational speed of the inner to submit information regarding the identification of an alternative to this patented
item to the ASTM International headquarters. Your comments will receive careful
consideration at a meeting of the responsible technical committee, which you may
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St., attend.
7
4th Floor, New York, NY 10036, http://www.ansi.org. The sole source of supply of the apparatus known to the committee at this time
4
Available from National Institute of Standards and Technology (NIST), 100 is Anton Paar GmbH, Anton-Paar-Str. 20, A-8054 Graz, Austria. If you are aware of
Bureau Dr., Stop 1070, Gaithersburg, MD 20899-1070, http://www.nist.gov. alternative suppliers, please provide this information to ASTM International
5
Available from IHS, 15 Inverness Way East, Englewood, CO 80112, http:// headquarters. Your comments will receive careful consideration at a meeting of the
www.global.ihs.com. responsible technical committee, which you may attend.
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D7042 − 21a
suring cells either by pressure or by suction, provided that
sufficient care and control is used to avoid any bubble
formation in the test specimen. All construction materials for
adaptors shall be fully compatible with all sample liquids and
cleaning agents, which contact them.
6.4 Hot Filling Adapter, for use with manual syringe filling
for the purpose of preventing the precipitation of waxy
components dissolved in sample and lowering sample viscosity
for easier sample introduction and cleaning routines.
6.5 Autosampler, for use in automated injection analyses.
The autosampler shall be designed to ensure the integrity of the
FIG. 1 Viscosity Cell
test specimen prior to and during the analysis and be equipped
to transfer a representative portion of test specimen into the
measuring cells. The autosampler shall transfer the test speci-
men from the sample vial to the measuring cells of the
apparatus without interfering with the integrity of the test
specimen. The autosampler shall be able to mimic the proce-
dure for sample handling as set forth in 11.1 and 11.2. The
autosampler may have heating capability as a means to prevent
the precipitation of waxy components dissolved in the sample
and lower the viscosity of the sample for filling the measuring
cells.
6.6 Screen, with an aperture of 75 µm, to remove particles
from the sample.
6.7 Magnet, strong enough to remove ferromagnetic mate-
rials from the sample. Magnetic stirring rods are suitable.
6.8 Ultrasonic Bath, Unheated (optional), with an operating
FIG. 2 Cell Block frequency between 25 kHz to 60 kHz and a typical power
output of ≤100 W, of suitable dimensions to hold container(s)
6.1.3 Temperature Control—The copper block surrounds placed inside of bath, for use in effectively dissipating and
both the viscosity and the density measuring cell in a way that removing air or gas bubbles that can be entrained in viscous
both cells are held at the same temperature. A thermoelectric sample types prior to analysis. It is permissible to use ultra-
heating and cooling system (see Fig. 2, No. 1) ensures the sonic baths with operating frequencies and power outputs
temperature stability of the copper block within 60.005 °C outside this range, however it is the responsibility of the
from the set temperature at the position of the viscosity cell laboratory to conduct a data comparison study to confirm that
over the whole temperature range. The uncertainty (k = 2; 95 % results determined with and without the use of such ultrasonic
confidence level) of the temperature calibration shall be no baths does not materially impact results.
more than 60.03 °C over the range from 15 °C to 100 °C.
Outside this range the calibration uncertainty shall be no more 7. Reagents and Materials
than 60.05 °C.
7.1 Sample Solvent, completely miscible with the sample.
6.1.4 The thermal equilibration time depends on the heat
7.1.1 For most samples, a volatile petroleum spirit or
capacity and conductivity of the liquid and on the difference
naphtha is suitable. If the solvent dries up without residues in
between injection temperature and test temperature. Adequate
an applicable time frame, the use of a separate drying solvent
temperature equilibration of the test specimen is automatically
is not required.
determined when successive viscosity values are constant
within 60.07 % over 1 min and successive density values are 7.1.2 For residual fuels, a prewash with an aromatic solvent
constant within 60.00003 g/cm3 over 60 s. such as toluene or xylene may be necessary to remove asphaltic
material.
NOTE 1—The Stabinger Viscometer, manufactured by Anton Paar
GmbH, fulfills the stated requirements when operated in the most precise 7.2 Drying Solvent, a volatile solvent miscible with the
mode of operation. sample solvent (see 7.1).
6.2 Syringes, commercially available, at least 5 mL in 7.2.1 Highly concentrated ethanol (96 % or higher),
volume, with a Luer tip. All construction materials for syringes n-hexane or n-heptane is suitable.
shall be fully compatible with all sample liquids and cleaning 7.3 Dry Air or Nitrogen, for blowing the measuring cells.
agents, which contact them. 7.3.1 If the measuring cell temperature is below or near the
6.3 Flow-Through or Pressure Adapter, for use as an alter- dew point temperature of the ambient air, the use of an
native means of introducing the test specimen into the mea- appropriate desiccator is required.
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8. Sampling, Test Specimens, and Test Units 8.2.4 Remove the stirring rod and inspect for sludge or wax
8.1 General Considerations and Guidelines: adhering to the rod. If there is sludge or wax adhering to the
8.1.1 Sampling is defined as all the steps required to obtain rod, continue stirring until the sample is homogeneous.
an aliquot of the contents of any pipe, tank, or other system, 8.2.5 Recap each container tightly and shake vigorously for
and to place the sample into the laboratory test container. The 1 min. Then loosen the cap, retighten to finger tight, then back
laboratory test container and sample volume shall be of off 3⁄4 to a full turn and place back into the sample preheat
sufficient capacity to mix the sample and obtain a homoge- apparatus.
neous sample for analysis. 8.2.6 Upon completion of 8.2.5 for all samples in the batch,
8.1.2 For some sample types, such as viscous lube oils that increase the sample pre-heat apparatus temperature to between
are prone to having entrained air or gas bubbles present in the 100 °C and 105 °C and heat for 30 min.
sample, the use of an ultrasonic bath (see 6.8) without the 8.2.7 Remove each container from the sample pre-heat
heater turned on (if so equipped), has been found effective in apparatus, close tightly, and shake vigorously for 60 s.
dissipating bubbles typically within 1 min. 8.2.8 If a heated auto sampler is used, follow instructions in
8.1.3 Particles—For samples that are likely to contain 8.2.8.1 below. If a sample handler is used, follow instructions
particles (for example, used oils or crude oils) pass the sample in 8.2.8.2 below.
through a 75 µm screen to remove the particles. For the 8.2.8.1 Ensure the sample vial magazine is held at a
removal of ferromagnetic materials the use of a magnet is temperature between 60 °C and 80 °C. Load each sample into
appropriate. Waxy samples must be heated to dissolve the wax its own preheated sample vial from 8.2.1, insert the vials into
crystals prior to filtration and a preheated filter shall be used. the sample vial magazine, and wait for 10 min to 15 min before
8.1.4 Test Specimen—A portion or volume of sample ob- commencing measurement.
tained from the laboratory sample and delivered to the mea- 8.2.8.2 Load a preheated sample vial from 8.2.1 with the
suring cells. The test specimen is obtained as follows: first sample to be tested in the batch and place the sample vial
8.1.4.1 Mix the sample, if required, to homogenize. Mixing into the sampler handler that is held between 60 °C and 80 °C.
at room temperature in an open container can result in the loss Loosen the cap of the other containers, retighten to finger tight,
of volatile material; mixing in closed, pressurized containers, then back off 3⁄4 to full turn and place the containers back into
or at sub-ambient temperatures is recommended. the sample preheat apparatus that is reset to hold temperature
8.1.4.2 Draw the test specimen from a properly mixed between 60 °C and 80 °C.
laboratory sample using an appropriate syringe. Alternatively, 8.2.9 Complete the measurements according to 11.1 or 11.3.
if the proper attachments and connecting tubes are used, the Analysis of all samples in the batch must be completed within
test specimen may be delivered directly to the measuring cells 1 h from completion of 8.2.7.
using a flow through or pressure adapter (see 6.3) or autosam- 9. Calibration and Verification
pler (see 6.5) from the mixing container. For waxy or other
samples with a high pour point, before drawing the test 9.1 Use only a calibrated apparatus as described in 6.1. The
specimen, heat the laboratory sample to the desired test calibration shall be checked periodically using certified refer-
temperature, which has to be high enough to dissolve the wax ence standards as described in 9.2 and 9.3. The recommended
crystals. interval for viscosity and density calibration is once a month,
for temperature control once a year. For the calibration
8.2 Instructions for Residual Fuel Oils: procedure follow the instructions of the manufacturer of the
8.2.1 (Warning—Exercise care as vigorous boil-over can apparatus.
occur when opaque liquids which contain high levels of water
are heated to high temperatures. Wear appropriate personal 9.2 Certified Viscosity and Density Reference Standards—
protective equipment for handling hot materials.) Place the These are for use as confirmatory checks on the procedure in
required number of disposable syringes or samples vials to be the laboratory. Certified viscosity and density reference stan-
used for the batch analysis into a sample preheat apparatus dards shall be certified by a laboratory, which has shown to
(such as an oven, bath, or heating block) held between 60 °C meet the requirements of ISO/IEC 17025 or a corresponding
and 65 °C. If using manual syringe filling, a hot filling adapter national standard by independent assessment. Viscosity stan-
must be installed on the apparatus and the injection adapters dards shall be traceable to master viscometer procedures
must also be pre-warmed along with the syringes. described in Test Method D2162. Density standards shall have
8.2.2 Place the first batch of residual fuel samples to be a certified uncertainty of the density values of 0.0001 g/cm3.
analyzed for the day in their original containers in a sample The uncertainty of the reference standards shall be stated for
preheat apparatus that is between 60 °C and 65 °C for 1 h. each certified value (k = 2; 95 % confidence level). See ISO
Ensure the cap on each container is tightly closed. For samples 5725 or NIST Technical Note 1297.
of a very waxy nature or oils of high kinematic viscosity, it 9.3 Thermometer—For calibration and adjustment of the
may be necessary to increase the heating temperature above temperature control, a digital thermometer with a probe diam-
60 °C to achieve proper mixing. The sample should be suffi- eter of 6.25 mm and a maximal length of 80 mm shall be used.
ciently fluid for ease of stirring and shaking. For smaller probes the use of an adapter is suitable. The
8.2.3 Vigorously stir each sample for approximately 20 s uncertainty (k = 2; 95 % confidence level) of this thermometer
with a glass or steel rod of sufficient length to reach the bottom must be no more than 60.01 °C and has to be certified by a
of the container. laboratory which has shown to meet the requirements of
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D7042 − 21a
ISO/IEC 17025 or a corresponding national standard by structions. Wait for the instrument to indicate that the determi-
independent assessment. A suitable thermometer is available nation is valid and record the values.
from the manufacturer of the apparatus. 11.1.5 Inject a further 1 mL without taking off the syringe
9.4 Acceptable Tolerance—If the determined values of a and repeat the measurement.
calibration check measurement do not agree within the accept- 11.1.6 If the deviation between two consecutive determina-
able tolerance band of the certified values, as calculated from tions exceeds the determinability limits as stated in Table 1 for
Annex A1, recheck each step in the procedure, including the this product, repeat step 11.1.5 until the deviation is within
special cleaning procedure from 12.2, to locate the source of these limits. Discard all previously determined values and
error. report the values of the last determination as the result.
11.1.6.1 For products not listed in the precision section, it is
NOTE 2—Values exceeding the acceptable tolerance are generally
attributable to deposits in the measuring cells that are not removed by the
the responsibility of the user of this standard to establish
routine flushing procedure. reasonable determinability limits by a series of tests.
11.1.6.2 If the syringe is empty before obtaining a valid
10. Adjustment determination, rinse and dry the measuring cells as described in
10.1 An adjustment has to be carried out when repeated 12.1 and repeat step 11.1.4. If it is not possible to obtain a valid
calibration check measurements do not agree with the Accept- result within an applicable number of repetitions, report the
able Tolerance Band as stated in 9.4 and the error cannot be robust mean value and the standard deviation (k = 2; 95 %
located elsewhere. For the adjustment procedure follow the confidence level) together with a remark indicating that the
instructions of the manufacturer of the apparatus. determinability exceeded the limits stated in 15.2.1 for this
10.2 For an adjustment, use only certified viscosity and product.
density reference standards that fulfill the requirements as 11.1.7 Remove the test specimen immediately, rinse and dry
stated in 9.2. The reference standards have to be within the the measuring cells as described in 12.1.
viscosity, density, and temperature range specified by the 11.2 Alternative Procedure (Sample Displacement)—For a
manufacturer of the apparatus. series of samples that are mutually soluble (for example,
10.3 After an adjustment procedure a calibration check various diesel fuels). It is the responsibility of the user of this
measurement shall be performed. standard to determine the applicability of this procedure to
each class of samples.
11. Procedure 11.2.1 Set the internal temperature control to the desired
11.1 Standard procedure (rinsing and drying) measuring temperature.
11.1.1 Set the internal temperature control to the desired 11.2.2 Set the determinability limits and temperature stabil-
measuring temperature. ity criteria to the values stated in Table 1 for the specific
11.1.2 Set the determinability limits and temperature stabil- product.
ity criteria to the values stated in Table 1 for the specific 11.2.3 Make sure that the measuring cells are clean and dry
product. as described in 12.1.
11.1.3 Make sure that the measuring cells are clean and dry 11.2.4 Load a minimum of 5 mL of the test specimen to the
as described in 12.1. syringe; if enough sample is available it is recommended to use
11.1.4 Load a minimum of 5 mL of the test specimen to the a 10 mL or larger syringe and to fill the entire syringe. Pour
syringe; if enough sample is available it is recommended to fill slowly at least 3 mL of the test specimen into the measuring
the entire syringe. Pour at least 2 mL of the test specimen into cells. A slow flow ensures that the new test specimen displaces
the measuring cells. Leave the syringe in the inlet opening and the old one rather than merging with it. Leave the syringe in the
start the motor and wait for about 10 s, then stop the motor inlet opening, start the motor and wait for about 10 s, then stop
again. Inject an additional 1 mL, leave the syringe in the inlet the motor. Inject an additional 1 mL, leave the syringe in the
opening, and start the measurement. Alternatively, the instru- inlet opening, and start the measurement. Alternatively, the
ment may be configured to perform pre-wetting automatically instrument may be configured to perform pre-wetting automati-
prior to starting the measurement. Follow manufacture’s in- cally prior to starting the measurement. Follow manufacture’s
Residual Fuel Oils at 50 °C and 100 °C 0.35 % 0.0003 g/cm3 ±0.010 °C ±0.10 % 0.00005 g/cm3 40 s 3 30 s
0.0035 X
Jet fuel at –20 °C and –40 °C, Scanning 0.0011889 X 0.000113 g/cm3 ±0.005 °C ±0.07 % 0.0001 g/cm3 60 s 0 0s
procedure
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D7042 − 21a
instructions. Wait for the instrument to indicate that the The apparatus reports measured density and dynamic viscosity
determination is valid and record the values. values as well as calculated kinematic viscosity and the
11.2.5 Inject slowly a further 2 mL without taking off the temperature for a pre-defined kinematic viscosity in accor-
syringe and repeat the measurement. dance with Practice D341, Standard Viscosity-Temperature
11.2.6 If the deviation between two consecutive determina- Charts for Liquid Petroleum Products. This procedure can be
tions exceeds the determinability limits as stated in Table 1 for applied with either sample filling procedure.
this product, repeat step 11.2.5 until the deviation is within 11.4.2 The temperature range of interest shall be defined as
these limits. Discard all previously determined values and well as the temperature points at which data shall be reported.
report the values of the last determination as the result. Ensure that the study material’s boiling and freezing points are
11.2.6.1 For products not listed in the precision section it is not exceeded by the defined temperature range. The tempera-
the responsibility of the user of this standard to establish ture range and data reporting temperatures shall be entered into
reasonable determinability limits by a series of tests. the apparatus in either table format or defined as start, stop and
11.2.6.2 If the syringe is empty before obtaining a valid interval temperature.
determination repeat step 11.2.4. If it is not possible to obtain 11.4.3 When performing measurements at sub-zero tem-
a valid result within an applicable number of repetitions, report peratures it is essential that the risk of ice formation during
the robust mean value and the standard deviation (k = 2; 95 % drying routines and sample filling in the measuring cells is
confidence level) together with a remark indicating that the eliminated. This can be achieved by using dry air after cell
determinability exceeded the limits stated in 15.1.1 for this cleaning and selecting a sample filling temperature which is
product. well above 0 °C.
11.2.7 For the next sample of this series repeat the steps 11.4.4 When testing jet fuel in conformance with this test
11.2.4 – 11.2.6. method, the apparatus shall be equipped with an appropriate
11.2.8 After the last sample of a series perform a cleaning counter cooling system. The filling temperature shall be 15 °C
procedure as described in 12.1. or above, test temperatures shall be –20 °C, –40 °C with
11.3 Procedure for Use with Autosampler: duplicate determinations at –20 °C and –40 °C so that deter-
11.3.1 Set the determinability and temperature stability minability can be verified.
criteria to values in Table 1 for the corresponding testing 11.4.5 For conformance with stated precision on jet fuel
parameter(s) and temperature(s) of interest. Ensure that auto- (see Tables 1-3) set the test stability criteria in accordance with
matic prewetting has been configured. See manufacture’s Table 1.
instructions for details. Temperature control/stability require- 12. Cleaning of the Measuring Cells
ments at the test temperatures of interest are provided in 6.1.3.
For all other sample types, see 11.3.2 for guidance. 12.1 Fill the measuring cells with at least 3 mL of the
11.3.2 For products not listed in the precision section, it is sample solvent (see 7.1). Check if the density cell is filled
the responsibility of the user of this test method to establish completely by examining the displayed density value. Start the
reasonable determinability and temperature stability criteria by motor for at least 10 s. For poorly soluble samples, extend this
a series of tests. time and repeat the procedure. Then rinse the measuring cells
11.3.3 Configure the cleaning and drying routines for the with the drying solvent (see 7.2) and pass through a stream of
autosampler for sufficient cleaning efficiency of the product dry air or nitrogen until the last trace of solvent is removed.
being tested. Make sure that the measuring cells are clean and dry by
checking if the air density value is lower than 0.0020 g/cm3. If
NOTE 3—For specific information on proper configuration, follow the the value exceeds this limit repeat the procedure or parts of it.
manufacturer’s instructions.
12.2 Special Cleaning Procedure—If necessary, clean the
11.3.4 Configure the autosampler for a minimum of two
viscosity measuring cell by manually wiping and brushing the
consecutive determinations per sample.8
measuring rotors using a suitable sample solvent. If necessary
11.3.5 Transfer a portion of the sample into the appropriate
clean the density oscillator using suitable cleaning agents. This
sample vial. Cap or cover the vials as necessary.
procedure must be carried out when repeated calibration check
11.3.5.1 Load sample(s) vial onto vial tray or holder and
measurements do not agree with the acceptable tolerance as
analyze the test specimens.
stated in 9.4. Follow the instructions of the manufacturer of the
11.3.5.2 Evaluate the data. Rerun samples which exceed the
apparatus.
determinability criteria established for the sample type being
analyzed. (See 11.3.1 and 11.3.2.) 13. Calculation of Results
11.4 Procedure for Temperature Scanning: 13.1 The recorded values are the final results, expressed
11.4.1 The Temperature Scan Procedure is used to study the either as dynamic viscosity in millipascal-seconds or as kine-
test material’s temperature dependence over a pre-defined matic viscosity in square millimetre per second and as density
temperature range and with pre-defined temperature intervals. in grams per cubic centimetre or kilograms per cubic metre.
13.2 Viscosity Index—If results are available from the same
8
sample at 40 °C and at 100 °C the Viscosity Index (VI) can be
The Stabinger Viscometer, manufactured by Anton Paar GmbH, uses the terms,
“Repeat Deviation Viscosity, RDV” and “Repeat Deviation Density, RDD” in lieu calculated according to Test Method D2270 from the kinematic
of “Determinability” in apparatus firmware and documentation. viscosity results at the above temperatures.
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D7042 − 21a
TABLE 2 Repeatability (95 %)
NOTE 1—X is the average of results being compared.
NOTE 2—See Table X3.1 for worked examples for cases where Table 2 contains complex formulas.
Material Temperature, °C Density, g/cm3 Dynamic Viscosity, mPa·s Kinematic Viscosity, mm2/s
Base oils 15 0.00046 N/A N/A
Base oils 40 0.0003 0.00101X or (0.10 %) 0.00094X or (0.09 %)
Base oils 100 0.00033 0.0003516 (X+5) 0.0003473 (X+5)
Formulated oils 40 0.0003 0.006279X or (0.63 %) 0.006 (X+10.6)
Formulated oils 100 0.0002 0.01209X0.5 0.002068(X+7.77)
Diesel fuels 40 0.0014 (1.03–X) 0.006705X or (0.67 %) 0.00782X0.778
Jet fuels –20 0.001 0.06477 0.0856
Jet fuels, Scanning procedureA –20 0.00197X 0.005978X 0.007074X
Jet fuels, scanning procedure –40 0.00197X 0.00434X 0.005261X
Biodiesel and biodiesel blends 40 0.0002 0.004 0.004647
Residual fuel oils 50 0.00098 0.09469X or (9.47 %) 0.09093X or (9.09 %)
Residual fuel oils 100 0.00249 0.0517X or (5.17 %) 0.05349X or (5.35 %)
A
This repeatability is currently not referenced in Specification D1655 – 19. Use the precision statement for jet fuel at –20 °C without scanning.
13.3 Density Extrapolation—If results are available from 15. Precision and Bias9
the same sample at 40 °C and at 100 °C density values at other 15.1 Comparison of Results:
temperatures can be calculated by linear extrapolation from the 15.1.1 Determinability, (d)—Quantitative measure of the
density results at the above temperatures. The limit for this variability associated with the same operator in a given
extrapolation temperature is given by the point where changes laboratory, obtaining successive determined values using the
of state (for example, cloud point or gassing) of the involved same apparatus for a series of operations leading to a single
sample occur. It is the responsibility of the user of this standard result. It is defined as that difference between two such single
to determine the applicability of this calculation to each class determined values as would be exceeded in the long run, in
of samples. only one case in 20, in the normal and correct operation of the
test method.8 (See Table 1.)
14. Report
15.2 Comparison of Results:
14.1 Report the following information: 15.2.1 Repeatability (r)—The difference between successive
14.1.1 The type and identification of the product tested. results obtained by the same operator in the same laboratory
14.1.2 The reference to this test method. with the same apparatus under constant operating conditions on
14.1.3 Any deviation, by agreement or otherwise, from the identical test material would, in the long run, in the normal and
procedure specified. correct operation of this test method, exceed the values
14.1.4 The test results for the dynamic or kinematic indicated only in one case in twenty. (See Table 2.)
viscosity, or both, to four significant figures, optionally also for 15.2.2 Reproducibility (R)—The difference between two
the density to three decimal places in g/cm3 or integer in kg/m3 single and independent results obtained by different operators
(example: 0.877 g/cm3 or 877 kg/m3), together with the test
temperature. 9
Supporting data have been filed at ASTM International Headquarters and may
14.1.5 Date and time of the test. be obtained by requesting Research Report RR:D02-1773. Contact ASTM Customer
14.1.6 Name and address of the test laboratory. Service at [email protected].
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D7042 − 21a
working in different laboratories on nominally identical test where:
material would, in the long run, in the normal and correct X = result obtained by Test Method D7042,
operation of this test method, exceed the values indicated only and
in one case in twenty. (See Table 3.) bias-corrected X = predicted Y result that would have been
obtained by Test Method D445 on the
15.3 Bias—No information can be presented on the bias of
same sample.
the procedure in this test method, because no material having
an accepted reference value has been tested. Differences between bias-corrected results from Test Method
D7042 and Test Method D445, for the sample types and
15.4 Relative Bias—No bias to Test Methods D445 and property ranges studied, are expected to exceed the following
D4052 was found to exist for base oils (see Appendix X1 and between methods reproducibility (RXY), as defined in Practice
Appendix X2). D6708, about 5 % of the time. The RXY at 40 mm2/s was
15.4.1 Degree of Agreement between Results by Test Method found to be 0.52156 mm2/s at 40 °C and RXY at 10 mm2/s was
D7042 and Test Method D445—Results on the same materials found to be 0.08819 mm2/s at 100 °C.
produced by Test Method D7042 and Test Method D445 have Additional data was requested to ensure that polymer type
been assessed in accordance with procedures outlined in did not cause differences to the bias between methods. In this
Practice D6708. The findings are: pilot study, it was confirmed that application of the previously
determined bias correction was acceptable regardless of the
15.4.2 For formulated oils, RR:D02-174110 suggests a bias
polymer type.11
correction of:
15.4.3 For diesel fuels, RR:D02-174212 suggests a bias
Y-Estimate 5 0.996 X at 40 °C (1) correction of:
Y-Estimate 5 X 2 2.3538e 2 02 at 100 °C Y-Estimate 5 0.9872 X 2 0.00015 at 40 °C (4)
where: where:
Y-Estimate = estimated D445 result using D7042 result. Y-Estimate = estimated D445 result using D7042 result.
Bias-corrected kinematic viscosity results from Test Method Bias-corrected kinematic viscosity results from Test Method
D7042, as per the bias correction equation that follows, may be D7042, as per the bias correction equation that follows, may be
considered as practically equivalent to results from Test considered as practically equivalent to results from Test
Method D445, for sample types and property ranges studied. Method D445, for sample types and property ranges studied.
No sample-specific bias, as defined in Practice D6708, was No sample-specific bias, as defined in Practice D6708, was
observed after the bias-correction for the materials studied. observed after the bias-correction, for the materials studied.
bias-corrected X ~predicted Y! 5 m X1b; (2) bias-corrected X ~predicted Y! 5 m X1b; (5)
m 5 0.9872;
m 5 0.996;
b 5 20.00015
b 5 0 at 40 °C
and where:
bias-corrected X ~predicted Y! 5 m X1b; (3) X = result obtained by Test Method D7042,
m 5 1; and
b 5 22.3538e 2 02 at 100 °C
11
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1931. Contact ASTM Customer
Service at [email protected].
12
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1742. Contact ASTM Customer
10
Service at [email protected].
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1741. Contact ASTM Customer
Service at [email protected].
8
D7042 − 21a
9
D7042 − 21a
15.5.1 Precision values for base oils were first published in 15.5.5 Precision values for Biodiesel and Biodiesel blend
2003.16 fuels at 40 °C were obtained by statistical examination of
interlaboratory results obtained by:
NOTE 4—Base oil precision values were determined on instruments
using manual sample introduction only. 13 laboratories from 12 biodiesel and biodiesel blend fuels
and one synthetic viscosity standard (B100, B6, B10 and B20
15.5.2 Precision values for formulated oils (commercially from varying feedstock and meeting the specifications of
available formulated oils like motor oils, hydraulic oils, and D6751 and D7467) representing a dynamic viscosity range
synthetic gear oils) were obtained by statistical examination of from 1.9818 mPa·S to 4.4196 mPa·S and a kinematic viscosity
interlaboratory results as follows: range from 2.404 mm2/S to 5.0767 mm2/S.
15.5.2.1 The dynamic viscosity range from 34 mPa·s to 17 laboratories from 12 biodiesel and biodiesel blend fuels
411 mPa·s at 40 °C from 10 formulated oils by 19 laboratories and one synthetic viscosity standard (B100, B6, B10 and B20
and from 5.24 mPa·s to 39.2 mPa·s at 100 °C from 10 from varying feedstock and meeting the specifications of
formulated oils by 18 laboratories. D6751 and D7467) representing a density range from
15.5.2.2 The kinematic viscosity range from 40.164 mm2/s 0.8237 g ⁄cm3 to 0.8704 g/cm3.
to 150.71 mm2/s at 40 °C from 9 formulated oils by 19
NOTE 5—The degrees of freedom associated with the reproducibility
laboratories and from 6.4682 mm2/s to 48.292 mm2/s at 100 °C estimate for density is 19. Since the minimum requirement of 30 (in
from 10 formulated oils by 18 laboratories. accordance with Practice D6300) is not met, users are cautioned that the
15.5.2.3 The density range from 0.82989 g ⁄cm3 to actual reproducibility may be significantly different than these estimates.
0.87300 g ⁄cm3 at 40 °C from 10 formulated oils by 20 labo- 15.5.5.1 Precision values for biodiesel and biodiesel blend
ratories and from 0.79192 g ⁄cm3 to 0.83512 g/cm³ at 100 °C fuels at 40 °C were first published in 2014.
from 10 formulated oils by 19 laboratories. 15.5.6 Precision values for residual fuel oils at 50 °C and
15.5.2.4 Precision values for formulated oils were first 100 °C were obtained by statistical examination of interlabo-
published in 2012. ratory results obtained by 10 laboratories from 10 residual fuel
15.5.3 Precision values for diesel fuels were obtained by samples conforming to D396 Grades No. 5 or 6 and/or ISO
statistical examination of interlaboratory results obtained by 18 8217 RMG and RMK representing a dynamic viscosity range
laboratories from eight diesel fuel grades (#1, #2, and #4 diesel from 25.31 mPa·s to 2212 mPa·s at 50 °C and 5.493 mPa·s to
fuels according to Specification D975) in the dynamic viscosity 109.1 mPa·s at 100 °C.
range from 1 mPa·s to 6 mPa·s at 40 °C (kinematic viscosity 15.5.6.1 The kinematic viscosity range spanned 27.6 mm2/s
range from 1.6477 mm2/s to 7.2315 mm2/s at 40 °C) and ten to 2230 mm2/s at 50 °C and 6.202 mm2/s to 108.1 mm2/s at
diesel fuel grades (#1, #2, and #4 diesel fuels according to 100 °C.
Specification D975) in the density range from 0.76920 g ⁄cm3 15.5.6.2 The density range spanned 0.09173 g ⁄cm3 to
to 0.89174 g/cm3 at 40 °C. 0.9937 g ⁄cm3 at °C and 0.8831 g ⁄cm3 to 0.9611 g ⁄cm3 at
15.5.3.1 Precision values for diesel fuels were first pub- 100 °C.
lished in 2012. 15.5.7 Precision values for jet fuel at –20 °C, –40 °C using
15.5.4 Precision values for jet fuel at –20 °C were obtained the temperature scanning procedure were obtained by statisti-
by statistical examination of interlaboratory results obtained cal examination of interlaboratory results obtained by 10
by: laboratories from 15 jet fuel samples conforming to D1655,
13 laboratories from 12 jet fuel grades (Jet-A, Jet-A1, JP8, D7566, or DEF STAN 91-091. The samples represented a
SPK, SPK blend, and N2B viscosity standard) in the dynamic density range from 0.78313 g ⁄cm3 to 0.85331 g ⁄cm3, a dy-
viscosity range from 3.1705 mPa·s to 6.7489 mPa·s at –20 °C. namic viscosity range from 2.75465 mPa·s to 5.79955 mPa·s
and a kinematic viscosity range from 3.3837 mm2/s to
13 laboratories from 12 jet fuel grades (Jet-A, Jet-A1, JP8,
6.7841 mm2/s at –20 °C.
SPK, SPK blend and N2B viscosity standard) in the kinematic
The samples represented a density range from
viscosity range from 3.8087 mm2/s to 7.9824 mm2/s at –20 °C.
0.79744 g ⁄cm3 to 0.86796 g ⁄cm3, a dynamic viscosity range
13 laboratories from 12 jet fuel grades (Jet-A, Jet-A1, JP8, from 5.2594 mPa·s to 14.002 mPa·s and a kinematic viscosity
SPK, SPK blend and N2B viscosity standard) in the density range from 6.35075 mm2/s to 16.1705 mm2/s at –40 °C.
range from 0.78672 g/cm3 to 0. 85998 g/cm3 at –20 °C. The 15.5.7.1 The interlaboratory studies were performed accord-
degrees of freedom associated with the reproducibility estimate ing to the Practices D6300 and D7915.
from this round robin study are 18. Since the minimum 15.5.7.2 Precision values for jet fuel at –20 °C and –40 °C
requirement of 30 (in accordance with Practice D6300) is not using the temperature scanning method were first published in
met, users are cautioned that the actual reproducibility may be 2019.17
significantly different than these estimates. 15.5.8 The interlaboratory studies were performed accord-
15.5.4.1 Precision values for jet fuel at –20 °C were first ing to Practices D6300 and D6708. For the determination of
published in 2012.13 the relative bias the samples were also tested by kinematic
16 17
Supporting data have been filed at ASTM International Headquarters and may Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1555. Contact ASTM Customer be obtained by requesting Research Report RR:D02-1920. Contact ASTM Customer
Service at [email protected]. Service at [email protected].
10
D7042 − 21a
viscometers according to Test Method D445 and for base oils
by digital density meters according to Test Method D4052 in
the same laboratories.
16. Keywords
16.1 critical viscosity; density; dynamic viscosity; kine-
matic viscosity; Stabinger viscometer; temperature scanning;
viscosity; viscosity index
ANNEX
(Mandatory Information)
A1. CALCULATION OF ACCEPTABLE TOLERANCE ZONE18 (BAND) TO DETERMINE CONFORMANCE WITH A CERTI-
FIED REFERENCE MATERIAL
A1.1 Determine the standard deviation for site A1.3.1 If the coverage factor, k, is not known, use the value
uncertainty,19 σsite, from a laboratory quality control program. 2.
A1.1.1 If the standard deviation for site uncertainty, σsite, is A1.4 Construct the acceptable tolerance zone:
not known, use the value 0.30 % for viscosity and
0.0005 g ⁄cm3 for density. TZ 5 61.44=σ 2 site1SE2 ARV (A1.1)
A1.4.1 Worked out example for viscosity tolerance band:
A1.2 Determine the combined extended uncertainty, CEU,
of the accepted reference value (ARV) of the certified reference σ site 5 0.30 % (A1.2)
material (CRM) from the supplier’s label or included docu-
CEUARV 5 0.35 %
mentation. If the density uncertainty is not known use the value
0.0005 g ⁄cm3 for the CEU.
TZ 5 61.44=0.302 10.1752 5 61.44=0.0910.03 5 60.50 %
A1.3 Calculate the standard error of the accepted reference A1.4.2 Worked out example for density tolerance band:
value, SEARV, by dividing the CEU by the coverage factor, k, σ site 5 0.0005 g/cm3 (A1.3)
listed on the supplier’s label or included documentation.
CEUARV 5 0.0005 g/cm3
APPENDIXES
(Nonmandatory Information)
X1.1 The bias calculation in accordance with Test Method the measured value. A comparison to the precision data from
D6708 applied to the results of the interlaboratory study on this test method and from the reference test method shows that
base oils (see 15.5) suggested a bias correction of (Y = the suggested bias correction is less than even the repeatability
0.998 X) at 100 °C. This corresponds to a deviation of 0.2 % of of both test methods over the whole viscosity range tested in
TABLE X1.1 Kinematic Viscosity Precision versus Bias (Base Oils at 100 °C)
NOTE 1—X is the average of results being compared.
Test Method D445 Test Method D445 at this study Test Method D7042
Reproducibility, R (95 %) 0.0065 X (0.65 %) 0.008916 X (0.89 %) 0.002889 (X+5)
Repeatability, r (95 %) 0.0011 X (0.11 %) 0.002299 X (0.23 %) 0.000347 (X+5)
Bias against Test Method D445 0.998 X (0.2 %)
Reference standard oil uncertainty 0.30 % to 0.32 % for the viscosity range of this study
11
D7042 − 21a
this interlaboratory study and also less than the uncertainty of X1.2 The kinematic viscosity bias at 40 °C was found to be
certified viscosity reference standards (see Table X1.1). There- 1.000 X, corresponding to 0.0 %.
fore the bias can be considered insignificant.
X2.1 The bias calculation in accordance with Practice of this test method over the whole density range tested in this
D6708 applied to the results of the interlaboratory study (see interlaboratory study and also less than the uncertainty of
15.5) suggested a bias correction of (Y = 1.0053 X – certified viscosity reference standards (see Table X2.1). There-
0.0046 g ⁄cm3) at 40 °C. This corresponds to a maximum fore the bias can be considered insignificant.
deviation of 0.0003 g ⁄cm3 over the density range tested in this
interlaboratory study. A comparison to the precision data from X2.2 The density bias at 15 °C was found to be
this test method and from the reference test method shows that 0.0000 g ⁄cm3.
the suggested bias correction is less than even the repeatability
12
D7042 − 21a
TABLE X3.1 Worked Examples for Repeatability Values at Levels of Viscosity in Cases where Table 2 on Repeatability Contains
Complex Formulas
Viscosity Level 5 10 25 50 100 2000
Base oils, dynamic viscosity at 100 °C 0.07 % 0.05 % 0.04 % 0.04 % 0.04 % 0.04 %
Base oils, kinematic viscosity at 100 °C 0.07 % 0.05 % 0.04 % 0.04 % 0.04 % 0.03 %
Formulated oils, dynamic viscosity at 100 °C 0.54 % 0.38 % 0.24 % 0.17 % 0.12 % 0.03 %
Formulated oils, kinematic viscosity at 40 °C 1.87 % 1.24 % 0.85 % 0.73 % 0.66 % 0.60 %
Formulated oils, kinematic viscosity at 100 °C 0.53 % 0.37 % 0.27 % 0.24 % 0.22 % 0.21 %
Viscosity level 1 2 3 4 – –
Diesel fuel, kinematic viscosity at 40 °C 0.78 % 0.67 % 0.61 % 0.57 % ... ...
TABLE X3.2 Worked Examples for Reproducibility Values at Levels of Viscosity in Cases where Table 3 on Reproducibility Contains
Complex Formulas
Viscosity Level 5 10 25 50 100 2000
Base oils, dynamic viscosity at 100 °C 0.51 % 0.38 % 0.31 % 0.28 % 0.27 % 0.26 %
Base oils, kinematic viscosity at 100 °C 0.58 % 0.43 % 0.35 % 0.32 % 0.30 % 0.29 %
Formulated oils, dynamic viscosity at 40 °C 0.70 % 0.80 % 0.97 % 1.11 % 1.28 % 2.32 %
Formulated oils, dynamic viscosity at 100 °C 0.71 % 0.70 % 0.70 % 0.69 % 0.69 % 0.69 %
Formulated oils, kinematic viscosity at 40 °C 3.39 % 2.24 % 1.55 % 1.32 % 1.20 % 1.09 %
Formulated oils, kinematic viscosity at 100 °C 1.62 % 1.13 % 0.83 % 0.73 % 0.68 % 0.64 %
Viscosity level 1 2 3 4 – –
Diesel fuel, kinematic viscosity at 40 °C 3.37 % 2.89 % 2.64 % 2.48 % ... ...
SUMMARY OF CHANGES
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D7042 – 21) that may impact the use of this standard. (Approved Nov. 1, 2021.)
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D7042 – 20) that may impact the use of this standard. (Approved Jan. 1, 2021.)
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D7042 – 19ɛ1) that may impact the use of this standard. (Approved June 1, 2020.)
(1) Revised definitions for density, dynamic viscosity, and (2) Revised subsection 15.4.2 to add footnote 11 and RR:D02-
kinematic viscosity in Section 3. 1931.
13
D7042 − 21a
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