ASTM D6660-01(2007)
(Test Method)Standard Test Method for Freezing Point of Aqueous Ethylene Glycol Base Engine Coolants by Automatic Phase Transition Method
Standard Test Method for Freezing Point of Aqueous Ethylene Glycol Base Engine Coolants by Automatic Phase Transition Method
SIGNIFICANCE AND USE
The freezing point of an engine coolant indicates the coolant freeze protection.
The freezing point of an engine coolant may be used to determine the approximate glycol content, provided the glycol type is known.
Freezing point as measured by Test Method D 1177 or approved alternative method is a requirement in Specifications D 3306 and D 6210.
This test method provides results that are equivalent to Test Method D 1177 and expresses results to the nearest 0.1°C with improved reproducibility over Test Method D 1177.
This test method determines the freezing point in a shorter period of time than Test Method D 1177.
This test method removes most of the operator time and judgement required by Test Method D 1177.
SCOPE
1.1 This test method covers the determination of the freezing point of an aqueous engine coolant solution.
1.2 This test method is designed to cover ethylene glycol base coolants up to a maximum concentration of 60 % (v/v) in water; however, the ASTM interlaboratory study mentioned in 12.2 has only demonstrated the test method with samples having a concentration range of 40 to 60 % (v/v) water.
Note 1—Where solutions of specific concentrations are to be tested, they shall be prepared from representative samples as directed in Test Method D 1176. Secondary phases separating on dilution need not be separated.
Note 2—The products may also be marketed in a ready-to-use form (prediluted).
1.3 The values stated in SI units are to be regarded as the standard. The values given in parenthesis are for information only.
1.4 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.
General Information
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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
Designation: D6660 − 01 (Reapproved 2007)
StandardTest Method for
Freezing Point of Aqueous Ethylene Glycol Base Engine
Coolants by Automatic Phase Transition Method
This standard is issued under the fixed designation D6660; 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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope gine Coolant for Heavy-Duty Engines
1.1 This test method covers the determination of the freez-
3. Terminology
ing point of an aqueous engine coolant solution.
3.1 Definitions of Terms Specific to This Standard:
1.2 This test method is designed to cover ethylene glycol
3.1.1 automatic phase transition method, n—in this
base coolants up to a maximum concentration of 60 % (v/v) in
standard, the procedures of automatically cooling an engine
water; however, theASTM interlaboratory study mentioned in
coolant sample until solid crystals appear, followed by con-
12.2 has only demonstrated the test method with samples
trolled warming and recording the temperature at which the
having a concentration range of 40 to 60 % (v/v) water.
crystals redissolve into the liquid phase.
NOTE 1—Where solutions of specific concentrations are to be tested, 3.1.2 freezing point, n—the temperature at which crystalli-
they shall be prepared from representative samples as directed in Test
zation begins in the absence of supercooling, or the maximum
Method D1176. Secondary phases separating on dilution need not be
temperature reached immediately after initial crystal formation
separated.
in the case of supercooling, or the temperature at which solid
NOTE 2—The products may also be marketed in a ready-to-use form
crystals, formed on cooling, disappear when the temperature of
(prediluted).
the specimen is allowed to rise.
1.3 The values stated in SI units are to be regarded as the
3.1.3 peltier device, n—a solid state thermoelectric device
standard. The values given in parenthesis are for information
constructed with dissimilar semiconductor materials, config-
only.
ured in such a way that it will transfer heat to and away from
1.4 This standard does not purport to address all of the
a test specimen dependent on the direction of electric current
safety concerns, if any, associated with its use. It is the
applied to the device.
responsibility of the user of this standard to establish appro-
priate safety and health practices and determine the applica-
4. Summary of Test Method
bility of regulatory limitations prior to use.
4.1 Aspecimen is cooled by a Peltier device while continu-
ously being illuminated by a light source. The specimen is
2. Referenced Documents
continuously monitored by an array of optical detectors for the
2.1 ASTM Standards:
first formation of crystals. Once the crystals are formed, the
D1176 Practice for Sampling and Preparing Aqueous Solu-
specimen is then warmed at controlled rates until all the
tions of Engine Coolants orAntirusts forTesting Purposes
crystals return to the liquid phase. The detectors are sufficient
D1177 Test Method for Freezing Point of Aqueous Engine
in number to ensure that any crystals are detected. The
Coolants
specimen temperature at which the crystals return to the liquid
D3306 Specification for Glycol Base Engine Coolant for
phase is recorded by the temperature sensor as the freezing
Automobile and Light-Duty Service
point.
D6210 Specification for Fully-Formulated Glycol Base En-
5. Significance and Use
5.1 The freezing point of an engine coolant indicates the
This test method is under the jurisdiction ofASTM Committee D15 on Engine
coolant freeze protection.
Coolants and is the direct responsibility of Subcommittee D15.03 on Physical
Properties.
5.2 The freezing point of an engine coolant may be used to
Current edition approved April 1, 2007. Published May 2007. Originally
determine the approximate glycol content, provided the glycol
´1
approved in 2001. Last previous edition approved in 2001 as D6660 - 01 . DOI:
type is known.
10.1520/D6660-01R07.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
5.3 Freezing point as measured by Test Method D1177 or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved alternative method is a requirement in Specifications
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. D3306 and D6210.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6660 − 01 (Reapproved 2007)
5.4 This test method provides results that are equivalent to 8.3 Turn on the liquid cooling media.
Test Method D1177 and expresses results to the nearest 0.1°C
8.4 Turnonthemainpowerswitchoftheanalyzer.Afterthe
with improved reproducibility over Test Method D1177.
automatic self diagnostics start-up sequence is completed, the
5.5 This test method determines the freezing point in a instrument will display a “READY” message.
shorter period of time than Test Method D1177.
9. Calibration and Standardization
5.6 This test method removes most of the operator time and
9.1 Ensure that all of the manufacturer’s instructions for
judgement required by Test Method D1177.
calibrating, checking and operating the apparatus are followed.
6. Apparatus
9.2 A sample with a mutually agreed upon freezing point
6.1 Automatic Apparatus —The apparatus described in this
can be used to verify performance of the apparatus.
method consists of a test chamber controlled by a micropro-
cessor that is capable of cooling and heating the test specimen, 10. Procedure
optically observing the appearance and disappearance of solid
10.1 Open the test chamber lid and clean the specimen cup
crystals and recording the temperature of the specimen.
inside the test chamber with a cotton swab.
6.2 The apparatus shall be equipped with a specimen cup,
10.2 Use the pipette to deliver 0.15 ml 6 0.01 ml of
optical detector array, light source, digital display, Peltier
specimen into the specimen cup. Clean the specimen out of the
device and a specimen temperature measuring device.
cup by using a cotton swab. The cup should be cleaned to the
6.3 The temperature measuring device in the specimen cup point where no visible droplets of specimen remain in the cup.
shall be capable of measuring the temperature of the test
10.3 Repeat step 10.2.
specimen from -80°C to +50°C at a resolution of 0.1°C.
10.4 Carefully measure 0.15 ml 6 0.01 ml of specimen into
6.4 The apparatus shall be equipped with fittings to permit
the specimen cup.
the circulation of liquid cooling media to remove heat gener-
10.5 Close and lock the test chamber lid.
ated by the Peltier device and other electronic components of
the apparatus. 10.6 Push the “RUN” button located on the front panel of
the apparatus. The specimen is cooled by the Peltier device
7. Reagents and Materials
while the appearance of solid crystals is continuously moni-
tored by the optical detectors.The temperature of the specimen
7.1 Cooling Media—Liquid heat exchange media to remove
is continuously monitored and displayed on the front panel of
the heat generated by the Peltier device and other electronic
the apparatus. Once the crystals are detected, the specimen is
components from the apparatus.
then warmed until all the crystals re-dissolve into the liquid
NOTE 3—Some apparatus are designed to use tap water as cooling
phase. The measurement is automatically terminated once the
media to bring specimen temperature to -60°C. To achieve cooling of
freezing point is detected.
specimento-80°C,providecirculationofliquidcoolingmediaat-30°Cor
lower to the apparatus. Refer to manufacturer’s operating instructions on
10.7 When the measurement is complete the freezing point
the relationship between cooling media temperature and the minimum
value per D6660 will be displayed on the front panel of the
specimen temperature.
apparatus.
7.2 Adjustable Volume Pipette , capable of dispensing 0.15
10.8 Unlock and open the test chamber lid and clean the
6 0.01 ml of sample.
specimen out of the specimen cup with a cotton swab.
7.3 Cotton Swabs —Plastic or paper shaft cotton swabs to
clean the specimen cup.
11. Report
NOTE 4—Caution: The use of swabs with wooden shafts may damage
11.1 Report the temperature recorded in 10.7 as the freezing
the mirrored surface of the specimen cup.
point, Test Method D6660.
8. Preparation of Apparatus
12. Precision and Bias
8.1 Install the analyzer for operation in accordance with
12.1 Precis
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