ASTM D 445 - Unprotected
ASTM D 445 - Unprotected
ASTM D 445 - Unprotected
1. Scope*
1.1 This test method specifies a procedure for the determination of the kinematic viscosity, , of liquid petroleum
products, both transparent and opaque, by measuring the time
for a volume of liquid to flow under gravity through a
calibrated glass capillary viscometer. The dynamic viscosity, ,
can be obtained by multiplying the kinematic viscosity, , by
the density, , of the liquid.
NOTE 1For the measurement of the kinematic viscosity and viscosity
of bitumens, see also Test Methods D2170 and D2171.
NOTE 2ISO 3104 corresponds to Test Method D445 03.
2. Referenced Documents
2.1 ASTM Standards:2
D446 Specifications and Operating Instructions for Glass
Capillary Kinematic Viscometers
D1193 Specification for Reagent Water
D1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham Pycnometer
D1480 Test Method for Density and Relative Density (Specific Gravity) of Viscous Materials by Bingham Pycnometer
D1481 Test Method for Density and Relative Density (Specific Gravity) of Viscous Materials by Lipkin Bicapillary
Pycnometer
D2162 Practice for Basic Calibration of Master Viscometers
and Viscosity Oil Standards
D2170 Test Method for Kinematic Viscosity of Asphalts
(Bitumens)
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
the ASTM website.
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D445 14a
D2171 Test Method for Viscosity of Asphalts by Vacuum
Capillary Viscometer
D6071 Test Method for Low Level Sodium in High Purity
Water by Graphite Furnace Atomic Absorption Spectroscopy
D6074 Guide for Characterizing Hydrocarbon Lubricant
Base Oils
D6299 Practice for Applying Statistical Quality Assurance
and Control Charting Techniques to Evaluate Analytical
Measurement System Performance
D6300 Practice for Determination of Precision and Bias
Data for Use in Test Methods for Petroleum Products and
Lubricants
D6617 Practice for Laboratory Bias Detection Using Single
Test Result from Standard Material
E1 Specification for ASTM Liquid-in-Glass Thermometers
E77 Test Method for Inspection and Verification of Thermometers
E563 Practice for Preparation and Use of an Ice-Point Bath
as a Reference Temperature
E644 Test Methods for Testing Industrial Resistance Thermometers
E1137/E1137M Specification for Industrial Platinum Resistance Thermometers
E1750 Guide for Use of Water Triple Point Cells
E2593 Guide for Accuracy Verification of Industrial Platinum Resistance Thermometers
E2877 Guide for Digital Contact Thermometers
2.2 ISO Standards:3
ISO 3104 Petroleum ProductsTransparent and Opaque
LiquidsDetermination of Kinematic Viscosity and Calculation of Dynamic Viscosity
ISO 3105 Glass Capillary Kinematic Viscometers
Specification and Operating Instructions
ISO 3696 Water for Analytical Laboratory Use
Specification and Test Methods
ISO 5725 Accuracy (trueness and precision) of measurement
methods and results.
ISO 9000 Quality Management and Quality Assurance
StandardsGuidelines for Selection and Use
ISO 17025 General Requirements for the Competence of
Testing and Calibration Laboratories
2.3 NIST Standards:4
NIST Technical Note 1297 Guideline for Evaluating and
Expressing the Uncertainty of NIST Measurement Results5
NIST GMP 11 Good Measurement Practice for Assignment
and Adjustment of Calibration Intervals for Laboratory
Standards6
NIST Special Publication 811 Guide for the Use of the
International System of Units (SI) 7
3
Available from American National Standards Institute (ANSI), 25 W. 43rd St.,
4th Floor, New York, NY 10036, http://www.ansi.org.
4
Available from National Institute of Standards and Technology (NIST), 100
Bureau Dr., Stop 3460, Gaithersburg, MD 20899-3460.
5
http://physics.nist.gov/cuu/Uncertainty/bibliography.html
6
http://ts.nist.gov/WeightsAndMeasures/upload/GMP_11_Mar_2003.pdf
7
http://www.nist.gov/pml/pubs/sp811/index.cfm
http://www.nist.gov/pml/pubs/sp1088/index.cfm
International Vocabulary of Metrology Basic and General Concepts and
Associated Terms (VIM), 3rd ed., 2008, http://www.bipm.org/en/publications/
guides/vim.html.
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D445 14a
ratios are called diffusivities with dimensions of length squared
divided by time and the SI unit is metre squared divided by
second (m2/s). Among the transport properties for heat, mass,
and momentum transfer, kinematic viscosity is the momentum
diffusivity.
3.3.4.2 DiscussionFormerly, kinematic viscosity was defined specifically for viscometers covered by this test method
as the resistance to flow under gravity. More generally, it is the
ratio between momentum transport and momentum storage.
3.3.4.3 DiscussionFor gravity-driven flow under a given
hydrostatic head, the pressure head of a liquid is proportional
to its density, , if the density of air is negligible compared to
that of the liquid. For any particular viscometer covered by this
test method, the time of flow of a fixed volume of liquid is
directly proportional to its kinematic viscosity, , where
= , and is the dynamic viscosity.
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D445 14a
device of equal or better accuracy. When two temperature
measuring devices are used in the same bath, they shall agree
within 60.1 C.
6.4.4 When using liquid-in-glass thermometers, such as
those in Table A2.1, use a magnifying device to read the
thermometer to the nearest 15 division (for example, 0.01 C or
0.02 F) to ensure that the required test temperature and
temperature control capabilities are met (see 10.1). It is
recommended that thermometer readings (and any corrections
supplied on the certificates of calibrations for the thermometers) be recorded on a periodic basis to demonstrate compliance with the test method requirements. This information can
be quite useful, especially when investigating issues or causes
relating to testing accuracy and precision.
Minimum Requirements
DCT
Display resolution
Display accuracy
E2877 Class A
0.01 C, recommended 0.001 C
20 mK (0.02 C) for combined probe and sensor
RTD, such as a PRT or thermistor
less than 10 mK (0.01 C) per year
less than or equal to 6 s as defined in Specification E1137/E1137M
10 mK over range of intended use
The DCT shall have a report of temperature calibration traceable to a national calibration or metrology standards body issued by a competent
calibration laboratory with demonstrated competency in temperature calibration. An ISO 17025
accredited laboratory with temperature calibration
in its accreditation scope would meet this requirement.
The calibration report shall include at least 3 calibration temperatures at least 5 C apart which
are appropriate for its intended use.
Sensor type
Drift
Response time
Linearity
Calibration Report
Calibration Data
6.6 Ultrasonic Bath, Unheated(optional), with an operating frequency between 25 kHz to 60 kHz and a typical power
output of 100 W, of suitable dimensions to hold container(s)
placed inside of bath, for use in effectively dissipating and
removing air or gas bubbles that can be entrained in viscous
sample types prior to analysis. It is permissible to use ultrasonic baths with operating frequencies and power outputs
outside this range, however it is the responsibility of the
laboratory to conduct a data comparison study to confirm that
results determined with and without the use of such ultrasonic
baths does not materially impact results.
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D445 14a
7.4 Water, deionized or distilled and conforming to Specification D1193 or Grade 3 of ISO 3696. Filter before use.
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(1)
Tolerance Band
< 10
10 to 100
100 to 1000
1000 to 10 000
10 000 to 100 000
> 100 000
0.30 %
0.32 %
0.36 %
0.42 %
0.54 %
0.73 %
A
Supporting data have been filed at ASTM International Headquarters and may be
obtained by requesting Research Report RR:D02-1498.
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D445 14a
12.1.4 Recap the container tightly and shake vigorously for
1 min to complete the mixing.
12.1.4.1 With samples of a very waxy nature or oils of high
kinematic viscosity, it may be necessary to increase the heating
temperature above 60 C to achieve proper mixing. The sample
should be sufficiently fluid for ease of stirring and shaking.
11.2 Use suction (if the sample contains no volatile constituents) or pressure to adjust the head level of the test sample
to a position in the capillary arm of the instrument about 7 mm
above the first timing mark, unless any other value is stated in
the operating instructions for the viscometer. With the sample
flowing freely, measure, in seconds to within 0.1 s, the time
required for the meniscus to pass from the first to the second
timing mark. If this flow time is less than the specified
minimum (see 10.2), select a viscometer with a capillary of
smaller diameter and repeat the operation.
11.2.1 Repeat the procedure described in 11.2 to make a
second measurement of flow time. Record both measurements.
11.2.2 From the two measurements of flow time, calculate
two determined values of kinematic viscosity.
11.2.3 If the two determined values of kinematic viscosity
calculated from the flow time measurements agree within the
stated determinability figure (see 17.1.1) for the product, use
the average of these determined values to calculate the kinematic viscosity result to be reported. Record the result. If not,
repeat the measurements of flow times after a thorough
cleaning and drying of the viscometers and filtering (where
required, see 11.1) of the sample until the calculated kinematic
viscosity determinations agree with the stated determinability.
11.2.4 If the material or temperature, or both, is not listed in
17.1.1, use 1.5 % as an estimate of the determinability.
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15. Expression of Results
14. Calculation
14.1 Calculate each of the determined kinematic viscosity
values, 1 and 2, from the measured flow times, t1 and t2, and
the viscometer constant, C, by means of the following equation:
1,2 5 Ct 1,2
0.015 y
0.0080 y
0.011 (y + 8)
(1.5 %)
(0.80 %)
0.017 y
(1.7 %)
23
10
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Reports RR:D02-1331 and RR:D02-1132.
These precision values were obtained by statistical examination of interlaboratory
results from six mineral oils (base oils without additive package) in the range from
8 mm2/s to 1005 mm2/s at 40 C and from 2 mm2/s to 43 mm2/s at 100 C, and were
first published in 1989. See Guide D6074.
11
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1332. These precision values
were obtained by statistical examination of interlaboratory results from seven fully
formulated engine oils in the range from 36 mm2/s to 340 mm2/s at 40 C and from
6 mm2/s to 25 mm2/s at 100 C, and were first published in 1991. See Guide D6071.
12
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1333. These precision values
were obtained by statistical examination of interlaboratory results for eight fully
formulated engine oils in the range from 7 mm2/s to 19 mm2/s at 150 C, and first
published in 1991. See Guide D6074.
13
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1334. These precision values
were obtained by statistical examination of interlaboratory results from five
petroleum waxes in the range from 3 mm2/s to 16 mm2/s at 100 C, and were first
published in 1988.
14
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1198. These precision values
were obtained by statistical examination of interlaboratory results from fourteen
residual fuel oils in the range from 30 mm2/s to 1300 mm2/s at 50 C and from
5 mm2/s to 170 mm2/s at 80 C and 100 C, and were first published in 1984.
(3)
where:
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(0.20 %)
(0.13 %)
(2)
where:
1,2 = determined kinematic viscosity values for 1 and 2,
respectively, mm2/s,
C
= calibration constant of the viscometer, mm2/s2, and
t1,2 = measured flow times for t1 and t2, respectively, s.
Calculate the kinematic viscosity result, , as an average of
1 and 2 (see 11.2.3 and 12.5.1).
14.2 Calculate the dynamic viscosity, , from the calculated
kinematic viscosity, , and the density, , by means of the
following equation:
5 3 3 10
0.0020 y
0.0013 y
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D445 14a
Additives at 100 C15
Gas oils at 40 C16
Jet fuels at 20 C17
Kerosine, diesel fuels, biodiesel
fuels, and biodiesel fuel blends at
40 C18
0.00106 y1.1
0.0013 (y+1)
0.0018 y
0.0037 y
(0.18 %)
(0.37 %)
0.0011 x
0.0026 x
0.0056 x
0.0141 x1.2
0.013 (x + 8)
0.015 x
0.00192 x1.1
0.0043 (x+1)
0.007 x
0.0056 x
(0.11 %)
(0.26 %)
(0.56 %)
(1.5 %)
(0.65 %)
(0.76 %)
(1.8 %)
(7.4 %)
(1.9 %)
(2.24 %)
(0.7 %)
(0.56 %)
17.3 The precision for used oils has not been determined but
is expected to be poorer than that for formulated oils. Because
of the extreme variability of such used oils, it is not anticipated
that the precision of used oils will be determined.
17.4 The precision for specific automated viscometers has
not been determined. However, an analysis has been made of a
large data set including both automated and manual viscometers over the temperature range of 40 C to 100 C. The
reproducibility of automated viscometer data is not statistically
significantly different than the reproducibility of manual viscometer data. It is also shown that there is no bias of the
automated data in comparison to the manual data.19
18. Keywords
18.1 dynamic viscosity; kinematic viscosity; viscometer;
viscosity
19
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1498.
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0.0065 x
0.0076 x
0.018 x
0.0366 x1.2
0.04 (x + 8)
0.074 x
0.00862 x1.1
0.0082 (x+1)
0.019 x
0.0224 x
D445 14a
ANNEXES
(Mandatory Information)
A1. VISCOMETER TYPES AND CERTIFIED VISCOSITY REFERENCE STANDARDS
TABLE A1.1 Viscometer Types
Viscometer Identification
25 C
40 C
50 C
80 C
100 C
4.6
11
44
170
640
2400
8700
37 000
...
4.0
8.9
34
120
450
1600
5600
23 000
81 000
2.9
5.7
18
54
180
520
1700
6700
23 000
...
...
...
...
...
280
...
...
11 000
...
...
...
...
...
67
...
...
...
1.2
1.8
3.9
7.2
17
32
75
...
...
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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.
A2.1.1 Use a short-range specialized Liquid-in-Glass thermometer conforming to the generic specification given in Table
A2.1 and Table A2.2 and to one of the designs shown in Fig.
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D445 14a
TABLE A2.1 General Specification for Thermometers
Total
Scale marks:
Subdivisions
C
Long lines at each
C
Numbers at each
C
Maximum line width
mm
Scale error at test temperature, max C
Expansion chamber:
Permit heating to
C
Total length
Stem outside diameter
Bulb length
Bulb outside diameter
Length of scale range
0.05
0.1 and 0.5
1
0.10
0.1
105 up to 90, 120 between 90 and 95
130 between 95 and 105, 170 above
105
300 to 310
6.0 to 8.0
45 to 55
no greater than stem
40 to 90
mm
mm
mm
mm
mm
Test
Temperature
C
150
135
98.9,
100
93.3
82.2
80
60
54.4
50
40
37.8
30
25
20
Thermometer No.
F
275
210,
212
200
180
C
ASTM
ASTM
ASTM
ASTM
ASTM
ASTM
0
32
17.8 0
20
4
26.1 20
40 40
53.9 65
140
130
122
100
86
77
68
B, the ice point is below the scale range, and in Design C, the
ice point is above the scale range.
A2.2 Calibration
A2.2.1 When using a liquid-in-glass thermometer, it shall
have a report of temperature calibration traceable to a national
calibration or metrology standards body issued by a competent
calibration laboratory with demonstrated competency in temperature calibration. An ISO 17025 accredited laboratory with
temperature calibration in its accreditation scope would meet
this requirement. The calibration report shall include data for a
series of temperatures which are appropriate for its intended
use.
A2.2.2 The scale correction of liquid-in-glass thermometers
can change during storage and use. Therefore, regular in-house
ice point verifications are required, and can be achieved within
the working laboratory, using an ice melting bath. However,
these checks may not be an adequate means of recalibration as
the use of a single-point recalibration at the ice point adds an
additional uncertainty to the updated thermometer calibration
result at every temperature but the ice point. The user must
determine if the thermometer requires complete re-calibration
Test
Temperature
D445 14a
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D445 14a
mercury column with the remainder of the stem and the
expansion volume at the uppermost end exposed to room
temperature and pressure. In practice, this means that the top of
the mercury column shall be within a length equivalent to four
scale divisions of the surface of the medium whose temperature
is being measured.
WWV
WWVH
CHU
Fort Collins, CO
Kauai, HI
Ottawa, Canada
A4. CALCULATION OF ACCEPTABLE TOLERANCE ZONE (BAND) TO DETERMINE CONFORMANCE WITH A CERTIFIED REFERENCE MATERIAL
2
2
TZ 5 61.44 = site
1SEARV
(A4.3)
0.22
5 0.11
2
CEUARV
(A4.1)
k
NOTE A4.3Standard Error (SEARV) is equivalent to Combined Standard Uncertainty (UC). See NIST Technical Note 1297.
SEARV 5
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(A4.2)
D445 14a
SUMMARY OF CHANGES
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D445 142) that may impact the use of this standard. (Approved Dec. 15, 2014.)
(3) Reformatted and revised DCT requirements in 6.4.
(4) Revised wording in 6.5 regarding timing devices.
(5) Revised A2.2 regarding liquid-in-glass thermometer calibration.
(1) Revised Referenced Documents, adding additional Committee E20 and NIST references.
(2) Revised definition of DCT and renumbered subsequent
notes.
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D445 12) that may impact the use of this standard. (Approved July 1, 2014.)
(3) Updated Section 17.
ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
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of infringement of such rights, are entirely their own responsibility.
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make your views known to the ASTM Committee on Standards, at the address shown below.
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