ASTM D6660-01

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Designation:D6660–01
Standard Test Method for
Freezing Point of Aqueous Ethylene Glycol Base Engine
Coolants by Automatic Phase Transition Method
This standard is issued under the fixed designation D 6660; 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 3. Terminology
1.1 This test method covers the determination of the freez- 3.1 Definitions:
ing point of an aqueous engine coolant solution. 3.1.1 automatic phase transition method, n—in this stan-
1.2 This test method is designed to cover ethylene glycol dard, the procedures of automatically cooling an engine
base coolants up to a maximum concentration of 60 % (v/v) in coolant sample until solid crystals appear, followed by con-
water; however, theASTM interlaboratory study mentioned in trolled warming and recording the temperature at which the
12.2 has only demonstrated the test method with samples crystals redissolve into the liquid phase.
having a concentration range of 40 to 60 % (v/v) water. 3.1.2 freezing point, n—the temperature at which crystalli-
zation begins in the absence of supercooling, or the maximum
NOTE 1—Where solutions of specific concentrations are to be tested,
temperature reached immediately after initial crystal formation
they shall be prepared from representative samples as directed in Test
in the case of supercooling, or the temperature at which solid
Method D 1176. Secondary phases separating on dilution need not be
crystals, formed on cooling, disappear when the temperature of
separated.
NOTE 2—The products may also be marketed in a ready-to-use form
the specimen is allowed to rise.
(prediluted).
3.1.3 peltier device, n—a solid state thermoelectric device
constructed with dissimilar semiconductor materials, config-
1.3 The values stated in SI units are to be regarded as the
ured in such a way that it will transfer heat to and away from
standard. The values given in parenthesis are for information
a test specimen dependent on the direction of electric current
only.
applied to the device.
1.4 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the
4. Summary of Test Method
responsibility of the user of this standard to establish appro-
4.1 Aspecimen is cooled by a Peltier device while continu-
priate safety and health practices and determine the applica-
ously being illuminated by a light source. The specimen is
bility of regulatory limitations prior to use.
continuously monitored by an array of optical detectors for the
2. Referenced Documents
first formation of crystals. Once the crystals are formed, the
specimen is then warmed at controlled rates until all the
2.1 ASTM Standards:
crystals return to the liquid phase. The detectors are sufficient
D 1176 Test Method for Sampling and Preparing Aqueous
in number to ensure that any crystals are detected. The
Solutions of Engine Coolants or Antirusts for Testing
specimen temperature at which the crystals return to the liquid
Purposes
phase is recorded by the temperature sensor as the freezing
D 1177 Test Method for Freezing Point of Aqueous Engine
point.
Coolants
D 3306 Specification for Glycol Base Engine Coolant for
2 5. Significance and Use
Automobile and Light Duty Service
5.1 The freezing point of an engine coolant indicates the
D 6210 Specification for Fully Formulated Ethylene Glycol
coolant freeze protection.
Base Engine Coolant for Heavy Duty Engines
5.2 The freezing point of an engine coolant may be used to
determine the approximate glycol content, provided the glycol
This test method is under the jurisdiction ofASTM Committee D15 on Engine
type is known.
Coolants and is the direct responsibility of Subcommittee D15.03 on Physical
5.3 Freezing point as measured by Test Method D 1177 or
Properties.
approved alternative method is a requirement in Specifications
Current edition approved April 10, 2001. Published June 2001.
Annual Book of ASTM Standards, Vol 15.05. D 3306 and D 6210.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6660
5.4 This test method provides results that are equivalent to 9. Calibration and Standardization
Test Method D 1177 and expresses results to the nearest 0.1°C
9.1 Ensure that all of the manufacturer’s instructions for
with improved reproducibility over Test Method D 1177.
calibrating, checking and operating the apparatus are followed.
5.5 This test method determines the freezing point in a
9.2 A sample with a mutually agreed upon freezing point
shorter period of time than Test Method D 1177.
can be used to verify performance of the apparatus.
5.6 This test method removes most of the operator time and
judgement required by Test Method D 1177. 10. Procedure
10.1 Open the test chamber lid and clean the specimen cup
6. Apparatus
inside the test chamber with a cotton swab.
6.1 Automatic Apparatus —The apparatus described in this 10.2 Use the pipette to deliver 0.15 ml 6 0.01 ml of
specimen into the specimen cup. Clean the specimen out of the
method consists of a test chamber controlled by a micropro-
cup by using a cotton swab. The cup should be cleaned to the
cessor that is capable of cooling and heating the test specimen,
point where no visible droplets of specimen remain in the cup.
optically observing the appearance and disappearance of solid
10.3 Repeat step 10.2.
crystals and recording the temperature of the specimen.
6.2 The apparatus shall be equipped with a specimen cup, 10.4 Carefully measure 0.15 ml 6 0.01 ml of specimen into
the specimen cup.
optical detector array, light source, digital display, Peltier
device and a specimen temperature measuring device. 10.5 Close and lock the test chamber lid.
10.6 Push the “RUN” button located on the front panel of
6.3 The temperature measuring device in the specimen cup
shall be capable of measuring the temperature of the test the apparatus. The specimen is cooled by the Peltier device
while the appearance of solid crystals is continuously moni-
specimen from -80°C to +50°C at a resolution of 0.1°C.
6.4 The apparatus shall be equipped with fittings to permit tored by the optical detectors.The temperature of the specimen
is continuously monitored and displayed on the front panel of
the circulation of liquid cooling media to remove heat gener-
ated by the Peltier device and other electronic components of the apparatus. Once the crystals are detected, the specimen is
then warmed until all the crystals re-dissolve into the liquid
the apparatus.
phase. The measurement is automatically terminated once the
freezing point is detected.
7. Reagents and Materials
10.7 When the measurement is complete the freezing point
7.1 Cooling Media—Liquidheatexchangemediatoremove
value per D 6660 will be displayed on the front panel of the
the heat generated by the Peltier device and other electronic
apparatus.
components from the apparatus.
10.8 Unlock and open the test chamber lid and clean the
NOTE 3—Some apparatus are designed to use tap water as cooling
specimen out of the specimen cup with a cotton swab.
media to bring specimen temperature to -60°C. To achieve cooling of
specimento-80°C,providecirculationofliquidcoolingmediaat-30°Cor
11. Report
lower to the apparatus. Refer to manufacturer’s operating instructions on
11.1 Report the temperature recorded in 10.7 as the freezing
the relationship between cooling media temperature and the minimum
point, Test Method D 6660.
specimen temperature.
7.2 Adjustable Volume Pipette , capable of dispensing 0.15
12. Precision and Bias
6 0.01 ml of sample.
12.1 Precision—The precision of this test method as deter-
7.3 Cotton Swabs —Plastic or paper shaft cotton swabs to
mined by the statistical examination of the interlaboratory test
clean the specimen cup.
results is as follows:
NOTE 4—Caution: The use of swabs with wooden shafts may damage
12.1.1 Repeatability—The difference between two test re-
the mirrored surface of the specimen cup.
sults obtained by the sam
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