Designation: D 5931 – 96 (Reapproved 2002)

Standard Test Method for

Density and Relative Density of Engine Coolant
Concentrates and Aqueous Engine Coolants by Digital
Density Meter1
This standard is issued under the fixed designation D 5931; 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 (e) indicates an editorial change since the last revision or reapproval.

1. Scope caused by the change in the mass of the tube is used in

1.1 This test method covers the determination of the density conjunction with calibration data to determine the density of
or relative density of engine coolant concentrates and aqueous the sample.
engine coolants. 5. Significance and Use
1.2 This test method should not be applied to samples so
dark in color that the absence of air bubbles in the sample cell 5.1 Density is a fundamental physical property that can be
cannot be established with certainty. used in conjunction with other properties to characterize engine
1.3 The accepted units of measure for density are grams per coolant concentrates and aqueous engine coolants.
milliliter or kilograms per cubic meter. 5.2 Determination of the density or relative density of these
1.4 This standard does not purport to address all of the products is necessary for the conversion of measured volumes
safety concerns, if any, associated with its use. It is the to volumes at the standard temperature of 20°C (68°F).
responsibility of the user of this standard to establish appro- 6. Apparatus
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard 6.1 Digital Density Analyzer, consisting of a U-shaped,
statements, see Note 1. oscillating sample tube and a system for electronic excitation,
frequency counting, and display. The analyzer must accommo-
2. Referenced Documents date the accurate measurement of the sample temperature
2.1 ASTM Standards: during measurement or must control the sample temperature as
D 1193 Specification for Reagent Water2 described in 6.2. The instrument must meet the precision
D 4052 Test Method for Density and Relative Density of requirements described in this test method.
Liquids by Digital Density Meter3 6.2 Circulating Constant—Temperature Bath, (optional) ca-
pable of maintaining the temperature of the circulating liquid
3. Terminology constant to 60.05°C in the desired range. Temperature control
3.1 Definitions: can be maintained as part of the density analyzer instrument
3.1.1 relative density, n—the ratio of the density of a package.
material at a stated temperature to the density of water at the 6.3 Syringes, at least 2 mL in volume with a tip or an
same stated temperature. adapter tip that will fit the opening of the oscillating tube.
6.4 Flow-Through or Pressure Adapter, for use as an
4. Summary of Test Method alternative means of introducing the sample into the density
4.1 A small volume of liquid sample is introduced into an analyzer either by a pump or by vacuum.
oscillating sample tube, and the change in oscillating frequency 6.5 Thermometer, calibrated and graduated to 0.1°C, with a
thermometer holder that can be attached to the instrument for
setting and observing the test temperature. In calibrating the
1
This test method is under the jurisdiction of ASTM Committee D15 on Engine thermometer, the freeze point should be estimated to the
Coolants and is the direct responsibility of Subcommittee D15.03 on Physical nearest 0.05°C.
Properties.
Current edition approved April 10, 1996. Published June 1996.
2
Annual Book of ASTM Standards, Vol 11.01.
3
Annual Book of ASTM Standards, Vol 05.02.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
 D 5931
7. Reagents and Materials suitable syringe. The test portion must be homogeneous and
7.1 Purity of Reagents—Use reagent grade chemicals in all free of even the smallest air or gas bubbles. The sample tube
tests. Unless otherwise indicated, all reagents shall conform to does not have to be completely full as long as the liquid
the specifications of the Committee on Analytical Reagents of meniscus is beyond the suspension point. Allow the display to
the American Chemical Society, where such specifications are reach a steady reading and record the T-value for water.
available.4 Other grades may be used, provided it is first 9.2.4 Record the density of air at the temperature and
ascertained that the reagent is of sufficiently high purity to atmospheric pressure of the test. Calculate the density of air at
permit its use without lessening the accuracy of the determi- the temperature of test using the following equation:
nation. da, g/mL 5 0.001293@273.15/T#@P/760# (1)
7.2 Purity of Water—Unless otherwise indicated, references
to water mean reagent water as defined by Type II of
where:
Specification D 1193.
T = temperature, degrees Kelvin, K, and
7.3 Water, redistilled, freshly boiled and cooled reagent P = barometric pressure, torr.
water for use as a primary calibration standard.
9.2.5 Determine the density of water at the temperature of
7.4 Acetone, for flushing and drying the sample tube.
test by reference to Table 1.
NOTE 1—Warning: Acetone is extremely flammable. 9.2.6 Using the observed T-values and the reference values
7.5 Dry Air, for drying the oscillator tube. for water and air, calculate the values of the constants A and B
using the following equations:
8. Preparation of Apparatus A 5 @Tw2 2 Ta2#/@dw 2 da# (2)
8.1 Set up the density analyzer and constant temperature 2
B 5 Ta 2 ~A 3 da! (3)
bath following the manufacturer’s instructions. Adjust the bath
or internal temperature control so that the desired test tempera- where:
ture is established and maintained in the sample compartment Tw = observed period of oscillation for cell containing
of the analyzer. Calibrate the instrument at the same tempera- water,
ture at which the density of the sample is to be measured. Ta = observed period of oscillation for cell containing air,
dw = density of water at test temperature, °C, and
NOTE 2—Precise setting and control of the test temperature in the
sample tube is extremely important. An error of 1.0°C can result in a
da = density of air at test temperature,° C.
change in density of one in the third decimal place. Alternatively, use the T and d values for the other reference
liquid if one is used.
9. Calibration of Apparatus 9.2.7 If the instrument is equipped to calculate density from
9.1 Calibrate the instrument when first set up and whenever the constants A and B and the observed T-value from the
the test temperature is changed. Thereafter, conduct calibration sample, enter the constants in the instrument memory in
checks at weekly intervals during routine operation. accordance with the manufacturer’s instructions.
9.2 Initial calibration, or calibration after a change in test 9.2.8 Check the calibration and adjust if needed by perform-
temperature, necessitates calculation of the values of the ing the routine calibration check described in 9.3.
constants A and B from the periods of oscillation (T) observed 9.2.9 To calibrate the instrument to display relative density,
when the sample cell contains air and redistilled, freshly boiled that is, the density of the sample at a given temperature relative
and cooled reagent water. to the density of water at the same temperature, follow
9.2.1 While monitoring the oscillator period, (T), flush the 9.2.1-9.2.7, but substitute 1.000 for dw in performing the
sample tube with distilled water followed by an acetone flush calculations described in 9.2.6.
and drying with dry air. Contaminated or humid air can affect 9.3 Weekly calibration adjustments to constants A and B can
the calibration. When these conditions exist in the laboratory, be made if required without repeating the calculation proce-
pass the air used for calibration through a suitable purification dure.
and drying train. In addition, the inlet and outlet ports for the
U-tube must be plugged during measurement of the calibration TABLE 1 Density of WaterA
air to prevent ingress of moist air. Temper- Temper- Temper-
Density, Density, Density,
ature, ature, ature,
9.2.2 Allow the dry air in the U-tube to come to thermal °C
g/mL
°C
g/mL
°C
g/mL
equilibrium with the test temperature and record the T-value
0 0.99987 21 0.99802 40 0.99224
for air. 3 0.99999 22 0.99780 45 0.99025
9.2.3 Introduce a small volume of redistilled, freshly boiled 4 1.00000 23 0.99756 50 0.98807
5 0.99999 24 0.99732 55 0.98573
and cooled reagent water into the sample tube opening using a 10 0.99973 25 0.99707 60 0.98324
15 0.99913 26 0.99681 65 0.98059
15.56 0.99904 27 0.99654 70 0.97781
4
Reagent Chemicals, American Chemical Society Specifications, American 16 0.99897 28 0.99626 75 0.97489
Chemical Society, Washington, DC. For suggestions on the testing of reagents not 17 0.99880 29 0.99597 80 0.97183
listed by the American Chemical Society, see Analar Standards for Laboratory 18 0.99862 30 0.99567 85 0.96865
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia 19 0.99843 35 0.99406 90 0.96534
20 0.99823 37.78 0.99307 100 0.95838
and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
A
MD. From Test Method D 4052.

2
 D 5931
NOTE 3—The need for a change in calibration generally is attributable 10. Procedure
to deposits in the sample tube that are not removed by the routine flushing
procedure. Although this condition can be compensated for by adjusting A
10.1 Mix the sample, if required, to be completely homo-
and B, it is good practice to clean the tube sequentially with water, geneous. If suspended solids are present in the sample, filter
petroleum ether, and acetone. through a 0.5 µm filter. Introduce a small amount (about 0.7
mL) of sample into the clean, dry sample tube of the instrument
9.3.1 Flush and dry the sample tube as described in 9.2.1 using a suitable syringe.
and allow the display to reach a steady reading. If the display 10.2 Turn on the illumination light and examine the sample
does not exhibit the correct density for air at the temperature of tube carefully. Make sure that no bubbles are trapped in the
test, repeat the cleaning procedure or adjust the value of tube and that it is filled to just beyond the suspension point. The
constant B commencing with the last decimal place until the sample must be homogeneous and free of even the smallest
correct density is displayed. bubbles.
9.3.2 If adjustment to constant B was necessary in 9.3.1, NOTE 5—If the sample is too dark in color to determine the absence of
continue the recalibration by introducing redistilled, freshly bubbles with certainty, the density cannot be measured within the stated
boiled and cooled reagent water into the sample tube as precision limits of Section 13.
described in 9.2.3 and allow the display to reach a steady
10.3 Turn the illumination light off immediately after
reading. If the instrument has been calibrated to display the
sample introduction because the heat generated can affect the
density, adjust the reading to the correct value for water at the
measurement temperature.
test temperature (see Table 1) by changing the value of
10.4 After the instrument displays a steady reading to four
constant A, commencing with the last decimal place. If the
significant figures for density and five for T-values, indicating
instrument has been calibrated to display the relative density, that temperature equilibrium has been reached, record the
adjust the reading to the value 1.000. density or T-value.
NOTE 4—In applying this weekly calibration procedure, it can be found
that more than one value for A and B, differing in the fourth decimal place, 11. Calculation
will yield the correct density reading for the density of air and water. The 11.1 Calculating Density Analyzers—The recorded value is
setting chosen then would be dependent upon whether it is approached
the final result, expressed either as density in g/mL, kg/m3 or as
from a higher or lower value. The setting selected by this test method
could have the effect of altering the fourth place of the reading obtained
relative density. Note that kg/m3 = 1000 3 g/mL.
for a sample. 11.2 Noncalculating Density Analyzers—Using the ob-
served T-value for the sample and the T-value for water and
9.4 Some analyzer models are designed to display the appropriate instrument constants determined in 9.4.3, calculate
measured period of oscillation only (T-values) and their the density or relative density using (Eq 6) and (Eq 7). Carry
calibration requires the determination of an instrument constant out all calculations to six significant figures and round the final
K, which must be used to calculate the density or relative results to five.
density from the observed data. For density:
9.4.1 Flush and dry the sample tube as described in 9.2.1 density, g/mL ~kg/dm 3! at t 5 dw 1 K1 ~Ts2 2 Tw2! (6)
and allow the display to reach a steady reading. Record the
T-value for air.
For relative density:
9.4.2 Introduce redistilled, freshly boiled and cooled reagent
water into the sample tube as described in 9.2.3, and allow the relative density, t/t 5 1 1 K2 ~Ts2 2 Tw2! (7)
display to reach a steady reading and record the T-value for
water. where:
9.4.3 Using the observed T-values and the reference values Tw = observed period of oscillation for cell containing
for water and air (9.2.4 and 9.2.5), calculate the instrument water,
constant K using the following equations: Ts = observed period of oscillation for cell containing
For density: sample,
dw = density of water at test temperature,
K1 5 $dw 2 da%/$Tw 2 2 Ta 2% (4) K1 = instrument constant for density,
K2 = instrument constant for relative density, and
For relative density: t = temperature of test,° C.
K2 5 $1.0000 2 da%/$Tw 2 2 Ta 2% (5)
12. Report
12.1 In reporting density, give the test temperature and the
where: units, for example, density at 20°C = 1.0360 g/mL or 1036
Tw = observed period of oscillation for cell containing kg/m3.
water, 12.2 In reporting relative density, give both the test tem-
Ta = observed period of oscillation for cell containing air, perature and the reference temperature but no units, for
dw = density of water at test temperature, °C, and example, relative density at 20/20°C = 1.0361.
da = density of air at test temperature,° C. 12.3 Report the final results to the five significant figures.

3
 D 5931
13. Precision and Bias 5 1.0360–1.1140 g/mL 0.0002 0.0008
13.1 The precision of this test method as obtained by 13.1.2 Reproducibility—The difference between two single
statistical examination of interlaboratory test results at test and independent results, obtained by different operators work-
temperature of 20°C is as follows: ing in different laboratories on identical test materials would, in
13.1.1 Repeatability—The difference between successive the long run, in the normal and correct operation of this test
test results obtained by the same operator with the same method, be expected to be as follows:
apparatus under constant operating conditions on identical test Range Reproducibility Standard Deviation
material would, in the long run, in the normal and correct
operation of this test method, be expected to be as follows: 1.0360–1.1140 g/mL 0.0020 0.0008

Range Repeatability Standard Deviation 13.2 Bias—This test method is an absolute measure of
physical property so no bias is expected.
14. Keywords
5
Supporting data are available from ASTM International Headquarters. Request 14.1 aqueous engine coolants; density; digital density ana-
RR:D15-1011. lyzer; engine coolant concentrates; relative density

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
of infringement of such rights, are entirely their own responsibility.

This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years and
if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standards
and should be addressed to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you should
make your views known to the ASTM Committee on Standards, at the address shown below.

This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,
United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the above
address or at 610-832-9585 (phone), 610-832-9555 (fax), or service@astm.org (e-mail); or through the ASTM website
(www.astm.org).