Preparation and Use of An Ice-Point Bath As A Reference Temperature
Preparation and Use of An Ice-Point Bath As A Reference Temperature
Preparation and Use of An Ice-Point Bath As A Reference Temperature
1. Scope
1.1 This practice covers a method of preparing, maintaining, and using a temperature reference bath of a mixture of shaved ice
and water, saturated with air at a pressure of 101 325 Pa (1 atm).
1.2 An industrial practice for relating values referenced to the ice point and to the water triple point on the ITS-90 is included.
1.3 Methods to promote uniformity of bath temperature by mechanical stirring or agitation are not described in detail.
1.4 Methods of approximating the ice point, as by thermostatically-controlled refrigeration, are not covered by this practice.
1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility
of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory
limitations prior to use.
2. Referenced Documents
2.1 ASTM Standards:2
D 1193Standard Specification for Reagent Water Specification for Reagent Water
E 344 Terminology Relating to Thermometry and Hydrometry
E 1594 Guide for Expression of Temperature
3. Terminology
3.1 Definitions—Definitions given in Terminology E 344, unless otherwise defined herein, apply to terms as used in this
practice.
3.2 Temperature relationships given in Guide E 1594, unless otherwise defined herein, apply to temperature values as used in
this practice.
3.3 Definitions of Terms Specific to This Standard:
3.3.1 ice-point bath, n—physical system containing ice and water assembled to realize the ice point as a reference temperature,
or to establish a constant temperature near 0 °C.
4. Summary of Practice
4.1 The ice-point bath described by this practice consists of an intimate mixture, without voids, of pure shaved ice or ice
particles and distilled air-saturated water in a thermally insulating vessel open to the atmosphere.
4.2 The ice bath realization of the ice point physically approximates, with small uncertainty, a natural fixed-point temperature.
4.2.1An ice-point bath prepared using distilled-water ice and air-saturated, chilled distilled water, typically has a temperature of
0.000 6 0.002°C. Consequently, when the bath is used as a fixed-point temperature reference, the bath temperature is assumed to
be 0°C, with an uncertainty that depends on the care with which the bath was established and maintained.
4.2.2The ice-point bath is open to the atmosphere; the effect of barometric pressure on the ice point is−75 nK/Pa (−7.6 mK/atm).
The solubility of air in the water is directly proportional to the atmospheric pressure.
4.3The ice-bath temperature can also be measured with an accurately calibrated thermometer or compared to a water triple point
1
This practice is under the jurisdiction of ASTM Committee E20 on Temperature Measurement and is the direct responsibility of Subcommittee E20.07 on Fundamentals
in Thermometry.
Current edition approved October 10, 2002. Published May 2003. Originally approved in 1976. Discontinued February 1996 and reinstated in 1997 as E563–97.
Current edition approved Nov. 1, 2008. Published December 2008. Originally approved in 1976. Discontinued February 1996 and reinstated in 1997 as E 563 – 97. Last
previous ediiton approved in 2002 as E 563–02´1.
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 standard’s Document Summary page on the ASTM website.
Copyright. (C) ASTM International. 100 Barr Harbour Dr. P.O. box C-700 West Conshohocken, Pennsylvania 19428-2959, United States
Copyright by ASTM Int'l (all rights reserved); Mon Apr 4 23:55:36 EDT 2011 1
Downloaded/printed by
Universidad Nacional de Colombia pursuant to License Agreement. No further reproductions authorized.
E 563 – 08
cell and the bath temperature is reported as the measured temperature with an uncertainty that is attributed to the measurement,
not to the ice point.
4.2.1 An ice-point bath prepared by rigorous application of this practice, using distilled-water ice and air-saturated, chilled
distilled water, typically has a temperature of 0.000 6 0.002 °C at a barometric pressure of 101,325 Pa (1 standard atmosphere).
See 8, Precision and Bias.
4.2.2 The ice-point bath is open to the atmosphere. The solubility of air in water, which affects phase change, is directly
proportional to the atmospheric pressure. The effect of barometric pressure on the ice point is −75 nK/Pa (−7.6 mK/atm).
Accordingly, the change in ice-point temperature resulting from an increase in elevation above sea level is -0.86 mK per 1000 m
increase in altitude (-0.26 mK per 1000 ft increase in altitude). See Table 1.
4.3 The ice-bath temperature can also be measured with an accurately calibrated thermometer or compared to a water triple
point cell and the bath temperature reported as the measured temperature with an uncertainty that is attributed to the measurement,
not to the ice point.
6. Hazards
6.1 Excess water accumulating in any region, particularly around the reference location, can elevate the temperature in that
vicinity above the ice point. Errors, usually somewhat less than 4 °C, can occur from this cause in poorly maintained baths and
with poorly positioned test objects (3 and 4).
6.2 For a stirred bath, the temperature of the bath will depend on the heat gained by the bath, the amount of water and ice, and
the vigor of stirring. The uniformity of temperature of the bath can be enhanced by slowly stirring or agitating the slush of ice and
water either manually or by a powered stirring means so that all of the ice and water in the bath come into intimate contact.
6.3 Ice making machines operate below 0 °C. Therefore, when excessively large ice particles are used to prepare the ice-point
bath, the initial temperature of the bath can briefly be slightly below the ice point. Also, some of the water may freeze and bridge
3
The boldface numbers in parentheses refer to the list of references at the end of this standard.
Copyright by ASTM Int'l (all rights reserved); Mon Apr 4 23:55:36 EDT 2011 2
Downloaded/printed by
Universidad Nacional de Colombia pursuant to License Agreement. No further reproductions authorized.
E 563 – 08
some of the particles. Use of the bath must be delayed long enough to establish thermal equilibrium, and the particles shall be
sufficiently small so that the bath approaches the required state of ice and air-saturated water in intimate contact.
6.4 Cleanliness is essential as small amounts of dissolved salts, and other contaminants can cause the equilibrium temperature
to be below that of the ice-point temperature.
7. Procedure
7.1 In the practical use of the ice-point bath, two objectives shall be accomplished: (1) the bath shall be established and
maintained so that its temperature is a good approximation to that of the ice point, and (2) the object for which the reference
temperature is to be obtained shall be in thermal equilibrium with the water-ice equilibrium temperature (water-ice interface
temperature).
7.2 Establishing the Ice-Point :
7.2.1 All equipment that comes in contact with the water and ice of an ice-point bath shall be clean. Thoroughly rinse the
equipment with tap water, then rinse with the type of water used for the ice-point bath medium. Use clean plastic gloves to handle
the ice and equipment.
7.2.2 Use water of purity equivalent to or purerbetter than type IV reagent water, Specification D 1193, for the ice-point bath
medium. Chill a quantity of the water to near 0 °C in a flask and shake vigorously to aerate the water. Freeze another portion of
the water to produce ice for the bath.
7.2.3 Prepare finely divided ice by shaving or crushing. Shaved ice resembling snow is preferred, but crushed ice is acceptable
if the particles are small (not exceeding 2 to 3 mm in diameter).
7.2.4 Prepare the bath in a clean thermally insulated vessel, preferably a wide-mouthed Dewar vacuum flask fitted with an
insulating closure such as a stopper. The vessel should be large enough that its size does not affect the water-ice equilibrium
temperature and of such diameter and depth that in thermal equilibrium the test objects will not significantly modify the
temperature of the bath over the region to which the ice point is to be applied. For usual applications, a diameter of at least 70
mm and a depth of at least 300 mm may be adequate.
7.2.5 Alternately add shaved ice and chilled water to the vessel, using enough water to saturate the ice but not enough to float
it. As the vessel fills, compress the ice-water mixture to force out excess water. The objective is to surround each particle of ice
with water, filling all voids, but to keep the ice particles as close together as possible. Continue adding ice and water and
compressing until the vessel is filled to the required level. Decant or siphon off excess water.
7.2.6 Cover the ice-point bath to protect it. Use an opaque and thermally insulating cover or stopper that is suitable for the
application. Allow the bath and vessel to equilibrate for at least 30 minutesmin before using.
7.3 Using the Ice-Point Bath:
7.3.1 Form a well in the ice-point bath that ishas the diameter of the test object and intended immersion depth of the test object.
7.3.2 Cool the test object to equilibrium in water with temperature less than 3 °C before immersing it in the bath. This reduces
the time to reach equilibrium at the ice point. Cooling Pre-cooling the sensor helps to preserve the bath at the ice point for a
prolonged use. Cooling also time and helps to ensure that the water-ice interface will be in contact with the thermometer because
negligible melting will have occurredoccur to increase the water film thickness.
7.3.3 Insert the test object with the sensor portion of the object, such as the sensing element of an SPRT, to a depth of at least
ten object diameters below the surface. For thermoelectric thermo-elements of high thermal conductivity, as much as 200 mm
immersion may be necessary. For total immersion liquid-in-glass thermometers, immerse to the 0 °C (32 °F) mark. For partial
immersion liquid-in-glass thermometers, immerse to the immersion line or stated immersion depth. Keep the sensor portion of the
object several centimeters above the bottom of the flask to avoid the zone at the bottom where denser melt water tends to
accumulate.
7.3.4 Close the top of the vessel around the test object with an opaque insulating stopper or other thermal barrier to reduce heat
transfer through the surface of the bath.
NOTE 1—When liquid-in-glass thermometers are tested in an ice point bath, the bath may be left uncovered. The loss of precision between a covered
and uncovered bath may be below the resolution of liquid-in-glass thermometers. The user must test for this condition.
7.3.5 Allow the bath and test object to come to thermal equilibrium.
7.4 Maintaining the Bath:
7.4.1 As ice particles in the bath melt, excess water begins to accumulate. This melt water has a temperature slightly warmer
than 0 °C. Since the density of water has its is at a maximum at 4 °C, the slightly warm melt water will collect at the bottom of
the bath and, hence, around the test object. Under these conditions, the bath will no longer be at 0 °C and cannot serve as an
ice-point bath. For this reason surplus water should be removed, as it accumulates, from the bottom of the bath by decanting or
siphoning. The presence of excess water can be detected if water overspill occurs when the ice is depressed. Add ice particles, and
chilled water, as necessary so that the ice slush column always extends to at least 30 mm below the lowest point of the test object.
7.4.2 In order to sustain the ice point over prolonged periods, the ice-point bath may be immersed in another bath that is kept
near 0 °C.
8. Precision and Bias
8.1 If a succession of ice-point baths is prepared by following all of the procedures described in this practice, routine
Copyright by ASTM Int'l (all rights reserved); Mon Apr 4 23:55:36 EDT 2011 3
Downloaded/printed by
Universidad Nacional de Colombia pursuant to License Agreement. No further reproductions authorized.
E 563 – 08
determination of the temperature of each of the baths with a stable, well-calibrated standard platinum resistance thermometer will
yield values of temperature that vary over a range of about 4 mK with a sample standard deviation of about 1 mK (5).
8.2 The variability represents the reproducibility of the ice point under the conditions of this practice, and the standard deviation
may be interpreted as a measure of the imprecision of realizing an ice point.
8.3 The mean of values determined under the conditions of 8.1 will be biased from 0 °C by an amount negligible compared to
the variability (5).
8.4 An ice-point bath prepared by rigorous application of this practice may be assigned a temperature of 0 °C with an expanded
total uncertainty (k = 2) of about 2 mK (5).
8.5 Sources of Error and Uncertainty :
8.5.1 The temperature of a poorly made or poorly maintained ice-point bath can differ from 0 °C by as much as several kelvins.
Impurities in the water usually lower the temperature. Excessive water in the bath can cause an increase in temperature as denser
warm water settles to the bottom. Large chunks of very cold ice added to a bath can produce local temperature depression.
8.5.2 Type IV grade of reagent water prepared with different apparatus can produce ice-point baths with slightly different
temperatures that are detectable with very precise thermometry. Temperature differences of 0.4 mK have been observed in ice-point
baths made from water purified in different stills (5).
8.5.3 The temperature of an ice-point bath made with typical potable city tap water may be low by 10 to 20 mK (3,5).
8.5.4 The temperature of the ice-point bath is slightly dependent on pressure. The temperature is lowered by about 6.3 µK for
each centimeter of depth below the liquid surface due to hydrostatic pressure. There is a corresponding effect for changes in
atmospheric pressure. In most cases, pressure effects can be ignored (4) .
8.5.5 In an ice-point bath, the actual temperature of a point in an immersed test object that conducts heat into the bath depends
on time, position in the bath, and the amount of heat conducted into the bath. A water-ice interface in the bath acts as a heat sink.
As ice melts, the interface moves away from the test object, and a temperature difference, which can be as much as several kelvins,
is established between the test object and the heat sink. At steady state conditions, an error results that depends primarily on the
thermophysical properties of the object, its dimensions and its depth of immersion in the ice-point bath results .
8.5.6 In resistance thermometery the applied electric current results in Joule heating, which raises the temperature of the sensor
above that of the water-ice interface. The temperature increase depends on the electric power being dissipated and the thermal
resistance between the sensor and the water-ice interface.
9. Keywords
9.1 fixed-point temperature references; ice bath; ice point; ITS-90; water triple point
REFERENCES
(1) Preston-Thomas, H., “The International Temperature Scale of 1990 (ITS-90),” Metrologia , Vol 27, 1990, pp. 3–10 and 107 (errata).
(2) Manual on the Use of Thermocouples in Temperature Measurement, MNL 12, ASTM, West Conshohocken.
(3) Caldwell, F. R., “Temperatures of Thermocouple Reference Junctions in an Ice Bath,” Journal of Research, NBS Engineering and Instrumentation,
69C, 1965.
(4) Bauerle, J. E., “Analysis of Immersed Thermocouple Junctions,” Review of Scientific Instruments, 32, 1961, pp. 313–316.
(5) Mangum, B. W., “Reproducibility of the Temperature of the Ice Point in Routine Measurements,” NIST Technical Note 1411, U.S. Government
Printing Office, Washington, DC, June 1995.
(6) “A Procedure for the Effective Recalibration of Liquid-in-Glass Thermometers,” NIST Special Publication 819, US Government Printing Office, 1991.
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).
Copyright by ASTM Int'l (all rights reserved); Mon Apr 4 23:55:36 EDT 2011 4
Downloaded/printed by
Universidad Nacional de Colombia pursuant to License Agreement. No further reproductions authorized.