Astm D445-12
Astm D445-12
Astm D445-12
Designation: 71/1/97
1. Scope*
1.1 This test method specifies a procedure for the determination of the kinematic viscosity, n, 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, h,
can be obtained by multiplying the kinematic viscosity, n, by
the density, r, 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.
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.07 on Flow Properties.
Current edition approved April 15, 2012. Published May 2012. Originally
approved in 1937. Last previous edition approved in 2011 as D44511a. DOI:
10.1520/D0445-12.
In the IP, this test method is under the jurisdiction of the Standardization
Committee.
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 12
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
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
E1137/E1137M Specification for Industrial Platinum Resistance 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 819 Guide for the Use of the
International System of Units (SI) 7
3. Terminology
3.1 See also International Vocabulary of Metrology.8
3.2 Definitions:
3.2.1 digital contact thermometer (DCT), nan electronic
device consisting of a digital display and associated temperature sensing probe.
3.3 Definitions of Terms Specific to This Standard:
3
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D445 12
5. Significance and Use
5.1 Many petroleum products, and some non-petroleum
materials, are used as lubricants, and the correct operation of
the equipment depends upon the appropriate viscosity of the
liquid being used. In addition, the viscosity of many petroleum
fuels is important for the estimation of optimum storage,
handling, and operational conditions. Thus, the accurate determination of viscosity is essential to many product specifications.
6. Apparatus
6.1 ViscometersUse only calibrated viscometers of the
glass capillary type, capable of being used to determine
kinematic viscosity within the limits of the precision given in
the precision section.
6.1.1 Viscometers listed in Table A1.1, whose specifications
meet those given in Specifications D446 and in ISO 3105 meet
these requirements. It is not intended to restrict this test method
to the use of only those viscometers listed in Table A1.1.
Annex A1 gives further guidance.
6.1.2 Automated ViscometersAutomated apparatus may
be used as long as they mimic the physical conditions,
operations or processes of the manual apparatus. Any
viscometer, temperature measuring device, temperature
control, temperature controlled bath or timing device incorporated in the automated apparatus shall conform to the specification for these components as stated in Section 6 of this test
method. Flow times of less than 200 s are permitted, however,
a kinetic energy correction shall be applied in accordance with
Section 7 on Kinematic Viscosity Calculation of Specifications
D446. The kinetic energy correction shall not exceed 3.0 % of
the measured viscosity. The automated apparatus shall be
capable of determining kinematic viscosity of a certified
viscosity reference standard within the limits stated in 9.2.1
and Section 17. The precision shall be of statistical equivalence
to, or better (has less variability) than the manual apparatus.
NOTE 3Precision and bias of kinematic viscosity measurements for
flow times of less than 200 s has not been determined. The precision stated
in Section 17 is not know to be valid for kinematic viscosity measurements with flow times less than 200 s.
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D445 12
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D445 12
When used to actuate electrical timing devices, such control
can cause large errors in kinematic viscosity flow time measurements.
7. Reagents and Materials
7.1 Chromic Acid Cleaning Solution, or a nonchromiumcontaining, strongly oxidizing acid cleaning solution.
(WarningChromic acid is a health hazard. It is toxic, a
recognized carcinogen, highly corrosive, and potentially hazardous in contact with organic materials. If used, wear a full
face-shield and full-length protective clothing including suitable gloves. Avoid breathing vapor. Dispose of used chromic
acid carefully as it remains hazardous. Nonchromiumcontaining, strongly oxidizing acid cleaning solutions are also
highly corrosive and potentially hazardous in contact with
organic materials, but do not contain chromium which has
special disposal problems.)
7.2 Sample Solvent, completely miscible with the sample.
Filter before use.
7.2.1 For most samples a volatile petroleum spirit or naphtha is suitable. For residual fuels, a prewash with an aromatic
solvent such as toluene or xylene may be necessary to remove
asphaltenic material.
7.3 Drying Solvent, a volatile solvent miscible with the
sample solvent (see 7.2) and water (see 7.4). Filter before use.
7.3.1 Acetone is suitable. (WarningExtremely flammable.)
7.4 Water, deionized or distilled and conforming to Specification D1193 or Grade 3 of ISO 3696. Filter before use.
8. Certified Viscosity Reference Standards
8.1 Certified viscosity reference standards shall be certified
by a laboratory that has been shown to meet the requirements
of ISO 17025 by independent assessment. Viscosity standards
shall be traceable to master viscometer procedures described in
Test Method D2162.
8.2 The uncertainty of the certified viscosity reference
standard shall be stated for each certified value (k = 2, 95%
confidence). See ISO 5725 or NIST 1297.
9. Calibration and Verification
9.1 ViscometersUse only calibrated viscometers,
thermometers, and timers as described in Section 6.
9.2 Certified Viscosity Reference Standards (Table A1.2)
These are for use as confirmatory checks on the procedure in
the laboratory.
9.2.1 If the determined kinematic viscosity does not agree
within the acceptable tolerance band, as calculated from Annex
A4, of the certified value, recheck each step in the procedure,
including thermometer and viscometer calibration, to locate the
source of error. Annex A1 gives details of standards available.
NOTE 4In previous issues of Test Method D445, limits of 60.35% of
the certified value have been used. The data to support the limit of
60.35% cannot be verified. Annex A4 provides instructions on how to
determine the tolerance band. The tolerance band combines both the
uncertainty of the certified viscosity reference standard as well as the
uncertainty of the laboratory using the certified viscosity reference
standard.
(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 12
10.2.2 When the test temperature is below the dew point, fill
the viscometer in the normal manner as required in 11.1. 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 the bath.
After insertion, allow the viscometer to reach bath temperature,
and the remove the stoppers. When performing manual viscosity determinations, do not use those viscometers which cannot
be removed from the constant temperature bath for charging
the sample portion.
10.2.2.1 The use of loosely packed drying tubes affixed to
the open ends of the viscometer is permitted, but not required.
If used, the drying tubes shall fit the design of the viscometer
and not restrict the flow of the sample by pressures created in
the instrument.
10.2.3 Viscometers used for silicone fluids, fluorocarbons,
and other liquids which are difficult to remove by the use of a
cleaning agent, shall be reserved for the exclusive use of those
fluids except during their calibration. Subject such viscometers
to calibration checks at frequent intervals. The solvent washings from these viscometers shall not be used for the cleaning
of other viscometers.
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D445 12
time and calculation of kinematic viscosity. Charge two viscometers in the manner dictated by the design of the instrument. For example, for the cross-arm or the BS U-tube
viscometers for opaque liquids, filter the sample through a
75-m filter into two viscometers previously placed in the bath.
For samples subjected to heat treatment, use a preheated filter
to prevent the sample coagulating during the filtration.
12.3.1 Viscometers which are charged before being inserted
into the bath may need to be preheated in an oven prior to
charging the sample. This is to ensure that the sample will not
be cooled below test temperature.
12.3.2 After 10 min, adjust the volume of the sample (where
the design of the viscometer requires) to coincide with the
filling marks as in the viscometer specifications (see Specifications D446).
12.3.3 Allow the charged viscometers enough time to reach
the test temperature (see 12.3.1). Where one bath is used to
accommodate several viscometers, never add or withdraw, or
clean a viscometer while any other viscometer is in use for
measuring flow time.
12.4 With the sample flowing freely, measure in seconds to
within 0.1 s, the time required for the advancing ring of contact
to pass from the first timing mark to the second. Record the
measurement.
12.4.1 In the case of samples requiring heat treatment
described in 12.1 through 12.2.1, complete the measurements
of flow time within 1 h of completing 12.2.2. Record the
measured flow times.
12.5 Calculate kinematic viscosity, n, in mm2/s, from each
measured flow time. Regard these as two determined values of
kinematic viscosity.
12.5.1 For residual fuel oils, if the two determined values of
kinematic viscosity agree within the stated determinability
figure (see 17.1.1), use the average of these determined values
to calculate the kinematic viscosity result to be reported.
Record the result. If the calculated kinematic viscosities do not
agree, repeat the measurements of flow times after thorough
cleaning and drying of the viscometers and filtering of the
sample. If the material or temperature, or both, is not listed in
17.1.1, for temperatures between 15 and 100C use as an
estimate of the determinability 1.0 %, and 1.5 % for temperatures outside this range; it must be realized that these materials
can be non-Newtonian, and can contain solids which can come
out of solution as the flow time is being measured.
13. Cleaning of Viscometer
13.1 Between successive determinations of kinematic
viscosity, clean the viscometer thoroughly by several rinsings
with the sample solvent, followed by the drying solvent (see
7.3). Dry the tube by passing a slow stream of filtered dry air
through the viscometer for 2 min or until the last trace of
solvent is removed.
13.2 Periodically clean the viscometer with the cleaning
solution (Warningsee 7.1), for several hours to remove
residual traces of organic deposits, rinse thoroughly with water
(7.4) and drying solvent (see 7.3), and dry with filtered dry air
or a vacuum line. Remove any inorganic deposits by hydro-
chloric acid treatment before the use of cleaning acid, particularly if the presence of barium salts is suspected. (Warning
It is essential that alkaline cleaning solutions are not used as
changes in the viscometer calibration can occur.)
14. Calculation
14.1 Calculate each of the determined kinematic viscosity
values, n1 and n2, from the measured flow times, t1 and t2, and
the viscometer constant, C, by means of the following equation:
n 1,2 5 Ct 1,2
(2)
where:
n1,2 = determined kinematic viscosity values for n1 and n2,
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, n, as an average of
n1 and n2 (see 11.2.3 and 12.5.1).
14.2 Calculate the dynamic viscosity, h, from the calculated
kinematic viscosity, n, and the density, r, by means of the
following equation:
h 5 n 3 r 3 1023
(3)
where:
h
= dynamic viscosity, mPas,
r
= density, kg/m3, at the same temperature used for the
determination of the kinematic viscosity, and
n
= kinematic viscosity, mm2/s.
14.2.1 The density of the sample can be determined at the
test temperature of the kinematic viscosity determination by an
appropriate method such as Test Methods D1217, D1480, or
D1481.
15. Expression of Results
15.1 Report the test results for the kinematic or dynamic
viscosity, or both, to four significant figures, together with the
test temperature.
16. Report
16.1 Report the following information:
16.1.1 Type and identification of the product tested,
16.1.2 Reference to this test method or a corresponding
international standard,
16.1.3 Result of the test (see Section 15),
16.1.4 Any deviation, by agreement or otherwise, from the
procedure specified,
16.1.5 Date of the test, and
16.1.6 Name and address of the test laboratory.
17. Precision and Bias
17.1 Comparison of Determined Values:
17.1.1 Determinability (d)The difference between successive determined values obtained by the same operator in the
same laboratory using the same apparatus for a series of
operations leading to a single result, would in the long run, in
the normal and correct operation of this test method, exceed the
values indicated only in one case in twenty:
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D445 12
Base oils at 40 and 100C9
Formulated oils at 40 and 100C10
Formulated oils at 150C11
Petroleum wax at 100C12
Residual fuel oils at 80 and 100C13
Residual fuel oils at 50C13
Additives at 100C14
Gas oils at 40C15
Jet fuels at 20C16
0.0020 y
0.0013 y
0.015 y
0.0080 y
0.011 (y + 8)
0.017 y
0.00106 y1.1
0.0013 (y+1)
0.0018 y
(0.20 %)
(0.13 %)
(1.5 %)
(0.80 %)
(1.7 %)
(0.18 %)
identical test material would, in the long run, in the normal and
correct operation of this test method, exceed the values
indicated only in one case in twenty:
Base oils at 40 and 100C9
Formulated oils at 40 and 100C10
Formulated oils at 150C11
Petroleum wax at 100C12
Residual fuel oils at 80 and 100C13
Residual oils at 50C13
Additives at 100C14
Gas oils at 40C15
Jet fuels at 20C16
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
(0.11 %)
(0.26 %)
(0.56 %)
(1.5 %)
(0.7 %)
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
(0.65 %)
(0.76 %)
(1.8 %)
(7.4 %)
(1.9 %)
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D445 12
ANNEXES
(Mandatory Information)
A1. VISCOMETER TYPES AND CERTIFIED VISCOSITY REFERENCE STANDARDS
TABLE A1.1 Viscometer Types
Viscometer Identification
25C
40C
50C
80 C
100C
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
...
...
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 12
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
mm
mm
mm
mm
mm
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
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
Test
Temperature
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 If liquid-in-glass thermometers are used, they shall
have an accuracy after correction of 0.02C or better, calibrated
by a laboratory meeting the requirements of ISO 9000 or ISO
17025, and carrying certificates confirming that the calibration
is traceable to a national standard. As an alternative, thermometric devices such as platinum resistance thermometers, as
defined in 6.4.2, may be used.
A2.2.2 The scale correction of liquid-in-glass thermometers
can change during storage and use, and therefore regular
re-calibration is required. This is most conveniently achieved
in a working laboratory by means of a re-calibration of the ice
point, and all of the main scale corrections altered for the
change seen in the ice point.
A2.2.2.1 For liquid-in-glass thermometers, the interval for
ice-point recalibration shall be no longer than six months (see
NIST GMP 11). For new thermometers, monthly checking for
the first six months is recommended. A change of one or more
scale divisions in the ice point means that the thermometer may
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D445 12
A3. TIMER ACCURACY
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
NOTE A4.1These calculations are based on Practice D6617.
CEUARV
(A4.1)
k
NOTE A4.3Standard Error (SEARV) is equivalent to Combined Standard Uncertainty (UC). See NIST Technical Note 1297.
SEARV 5
(A4.3)
(A4.2)
0.22
5 0.11
2
2.
SUMMARY OF CHANGES
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D44511a) that may impact the use of this standard. (Approved April 15, 2012.)
(1) Revised Annex A2 to clarify the calibration requirements
and recalibration intervals for digital contact thermometers.
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D44511) that may impact the use of this standard. (Approved May 1, 2011.)
(1) Revised 6.4 to define requirements for electronic temperature measurement.
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D445 12
Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D44510) that may impact the use of this standard. (Approved Jan. 1, 2011.)
(1) Revised 3.3.3 and 3.3.4 to update definitions.
(2) Added discussions under 3.3.4 to provide continuity between the old and the new definitions.
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