ASTM D6660-01(2019)

Standard Test Method for Freezing Point of Aqueous Ethylene Glycol Base Engine Coolants by Automatic Phase Transition Method

SIGNIFICANCE AND USE
5.1 The freezing point of an engine coolant indicates the coolant freeze protection.  
5.2 The freezing point of an engine coolant may be used to determine the approximate glycol content, provided the glycol type is known.  
5.3 Freezing point as measured by Test Method D1177 or approved alternative method is a requirement in Specifications D3306 and D6210.  
5.4 This test method provides results that are equivalent to Test Method D1177 and expresses results to the nearest 0.1 °C with improved reproducibility over Test Method D1177.  
5.5 This test method determines the freezing point in a shorter period of time than Test Method D1177.  
5.6 This test method removes most of the operator time and judgement required by Test Method D1177.
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 Practice D1176. 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 standard. No other units of measurement are included in this standard.  
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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. Some specific hazards statements are given in 7.3.  
1.5 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

General Information

• Status: Historical
• Publication Date: 31-Mar-2019
• ICS: 19.040 - Environmental testing
• ICS: 71.100.45 - Refrigerants and antifreezes
• Technical Committee: D15 - Engine Coolants and Related Fluids
• Drafting Committee: D15.03 - Physical Properties

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 2019)
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 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 tions of Engine Coolants or Antirusts for Testing Purposes
D1177 Test Method for Freezing Point of Aqueous Engine
1.1 This test method covers the determination of the freez-
Coolants
ing point of an aqueous engine coolant solution.
D3306 Specification for Glycol Base Engine Coolant for
1.2 This test method is designed to cover ethylene glycol
Automobile and Light-Duty Service
base coolants up to a maximum concentration of 60 % (v ⁄v) in
D6210 Specification for Fully-Formulated Glycol Base En-
water; however, the ASTM interlaboratory study mentioned in
gine Coolant for Heavy-Duty Engines
12.2 has only demonstrated the test method with samples
having a concentration range of 40 to 60 % (v/v) water.
3. Terminology
NOTE 1—Where solutions of specific concentrations are to be tested, 3.1 Definitions of Terms Specific to This Standard:
they shall be prepared from representative samples as directed in Practice
3.1.1 automatic phase transition method, n—in this
D1176. Secondary phases separating on dilution need not be separated.
standard, the procedures of automatically cooling an engine
NOTE 2—The products may also be marketed in a ready-to-use form
coolant sample until solid crystals appear, followed by con-
(prediluted).
trolled warming and recording the temperature at which the
1.3 The values stated in SI units are to be regarded as
crystals redissolve into the liquid phase.
standard. No other units of measurement are included in this
3.1.2 freezing point, n—the temperature at which crystalli-
standard.
zation begins in the absence of supercooling, or the maximum
1.4 This standard does not purport to address all of the
temperature reached immediately after initial crystal formation
safety concerns, if any, associated with its use. It is the
in the case of supercooling, or the temperature at which solid
responsibility of the user of this standard to establish appro-
crystals, formed on cooling, disappear when the temperature of
priate safety, health, and environmental practices and deter-
the specimen is allowed to rise.
mine the applicability of regulatory limitations prior to use.
3.1.3 peltier device, n—a solid state thermoelectric device
Some specific hazards statements are given in 7.3.
constructed with dissimilar semiconductor materials, config-
1.5 This international standard was developed in accor-
ured in such a way that it will transfer heat to and away from
dance with internationally recognized principles on standard-
a test specimen dependent on the direction of electric current
ization established in the Decision on Principles for the
applied to the device.
Development of International Standards, Guides and Recom-
mendations issued by the World Trade Organization Technical
4. Summary of Test Method
Barriers to Trade (TBT) Committee.
4.1 A specimen is cooled by a Peltier device while continu-
2. Referenced Documents ously being illuminated by a light source. The specimen is
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
crystals return to the liquid phase. The detectors are sufficient
in number to ensure that any crystals are detected. The
This test method is under the jurisdiction of ASTM Committee D15 on Engine
Coolants and Related Fluids and is the direct responsibility of Subcommittee
specimen temperature at which the crystals return to the liquid
D15.03 on Physical Properties.
phase is recorded by the temperature sensor as the freezing
Current edition approved April 1, 2019. Published April 2019. Originally
e1 point.
approved in 2001. Last previous edition approved in 2014 as D6660–01(2014) .
DOI: 10.1520/D6660-01R19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or 5. Significance and Use
contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM
5.1 The freezing point of an engine coolant indicates the
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website. coolant freeze protection.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6660 − 01 (2019)
5.2 The freezing point of an engine coolant may be used to 8. Preparation of Apparatus
determine the approximate glycol content, provided the glycol
8.1 Install the analyzer for operation in accordance with
type is known.
manufacturer’s instructions.
5.3 Freezing point as measured by Test Method D1177 or
8.2 Make liquid cooling media connections and ensure that
approved alternative method is a requirement in Specifications
they do not leak.
D3306 and D6210.
8.3 Turn on the liquid cooling media.
5.4 This test method provides results that are equivalent to
8.4 Turn on the main power switch of the analyzer. After the
Test Method D1177 and expresses results to the nearest 0.1 °C
automatic self diagnostics start-up sequence is completed, the
with improved reproducibility over Test Method D1177.
instrument will display a “READY” message.
5.5 This test method determines the freezing point in a
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.
9.2 A sample with a mutually agreed upon freezing point
6. Apparatus
can be used to verify performance of the apparatus.
6.1 Automatic Apparatus —The apparatus described in this
method consists of a test chamber controlled by a micropro-
10. Procedure
cessor that is capable of cooling and heating the test specimen,
10.1 Open the test chamber lid and clean the specimen cup
optically observing the appearance and disappearance of solid
inside the test chamber with a cotton swab.
crystals and recording the temperature of the specimen.
10.2 Use the pipette to deliver 0.15 ml 6 0.01 ml of
6.2 The apparatus shall be equipped with a specimen cup,
specimen into the specimen cup. Clean the specimen out of the
optical detector array, light source, digital display, Peltier
cup by using a cotton swab. The cup should be cleaned to the
device and a specimen temperature measuring device.
point where no visible droplets of specimen remain in the cup.
6.3 The temperature measuring device in the specimen cup
10.3 Repeat step 10.2.
shall be capable of measuring the temperature of the test
10.4 Carefully measure 0.15 ml 6 0.01 ml of specimen into
specimen from –80 °C to +50 °C at a resolution of 0.1 °C.
the specimen cup.
6.4 The apparatus shall be equipped with fittings to permit
10.5 Close and lock the test chamber lid.
the circulation of liquid cooling media to remove heat gener-
ated by the Peltier device and other electronic components of
10.6 Push the “RUN” button located on the front panel of
the apparatus.
the apparatus. The specimen is cooled by the Peltier device
while the appearance of solid crystals is continuously moni-
7. Reagents and Materials
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
phase. The measurement is automatically terminated once the
NOTE 3—Some apparatus are designed to use tap water as cooling
freezing point is detected.
media to bring specimen temperature to –60 °C. To achieve cooling of
specimen to –80 °C, provide circulation of liquid cooling media at –30 °C
10.7 When the measurement is complete the freezing point
or lower to the apparatus. Refer to manufacturer’s operating instructions
value per Test Method D6660 will be displayed on the front
on the relationship between cooling media temperature and the minimum
panel of the apparatus.
specimen temperature.
10.8 Unlock and open the test chamber lid and clean the
7.2 Adjustable Volume Pipette, capable of dispensing 0.15
specimen out of the specimen cup with a cotton swab.
6 0.01 ml of sample.
7.3 Cotton Swabs —Plastic or paper shaft cotton swabs
...

This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Because
it may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current version
of the standard as published by ASTM is to be considered the official document.
´1
Designation: D6660 − 01 (Reapproved 2014) D6660 − 01 (Reapproved 2019)
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 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.
ε NOTE—Units information was corrected and Note 4 was changed to a warning statement and included in Section 7.3
editorially in July 2014.
1. 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
Practice D1176. 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 standard. No other units of measurement are included in this standard.
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 safety, health, and healthenvironmental practices and determine the
applicability of regulatory limitations prior to use. Some specific hazards statements are given in 7.3.
1.5 This international standard was developed in accordance with internationally recognized principles on standardization
established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued
by the World Trade Organization Technical Barriers to Trade (TBT) Committee.
2. Referenced Documents
2.1 ASTM Standards:
D1176 Practice for Sampling and Preparing Aqueous Solutions of Engine Coolants or Antirusts for Testing Purposes
D1177 Test Method for Freezing Point of Aqueous Engine Coolants
D3306 Specification for Glycol Base Engine Coolant for Automobile and Light-Duty Service
D6210 Specification for Fully-Formulated Glycol Base Engine Coolant for Heavy-Duty Engines
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 automatic phase transition method, n—in this standard, the procedures of automatically cooling an engine coolant sample
until solid crystals appear, followed by controlled warming and recording the temperature at which the crystals redissolve into the
liquid phase.
3.1.2 freezing point, n—the temperature at which crystallization begins in the absence of supercooling, or the maximum
temperature reached immediately after initial crystal formation in the case of supercooling, or the temperature at which solid
crystals, formed on cooling, disappear when the temperature of the specimen is allowed to rise.
3.1.3 peltier device, n—a solid state thermoelectric device constructed with dissimilar semiconductor materials, configured in
such a way that it will transfer heat to and away from a test specimen dependent on the direction of electric current applied to the
device.
This test method is under the jurisdiction of ASTM Committee D15 on Engine Coolants and Related Fluids and is the direct responsibility of Subcommittee D15.03 on
Physical Properties.
Current edition approved July 1, 2014April 1, 2019. Published July 2014April 2019. Originally approved in 2001. Last previous edition approved in 20072014 as
e1
D6660D6660–01(2014) – 01(2007). . DOI: 10.1520/D6660-01R14E01.10.1520/D6660-01R19.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or contact ASTM Customer Service at [e-mail]. For Annual Book of ASTM Standards
volume information, refer to the standard’s Document Summary page on the ASTM website.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6660 − 01 (2019)
4. Summary of Test Method
4.1 A specimen is cooled by a Peltier device while continuously being illuminated by a light source. The specimen is
continuously monitored by an array of optical detectors for the first formation of crystals. Once the crystals are formed, the
specimen is then warmed at controlled rates until all the crystals return to the liquid phase. The detectors are sufficient in number
to ensure that any crystals are detected. The specimen temperature at which the crystals return to the liquid phase is recorded by
the temperature sensor as the freezing point.
5. Significance and Use
5.1 The freezing point of an engine coolant indicates the coolant freeze protection.
5.2 The freezing point of an engine coolant may be used to determine the approximate glycol content, provided the glycol type
is known.
5.3 Freezing point as measured by Test Method D1177 or approved alternative method is a requirement in Specifications D3306
and D6210.
5.4 This test method provides results that are equivalent to Test Method D1177 and expresses results to the nearest 0.1°C0.1 °C
with improved reproducibility over Test Method D1177.
5.5 This test method determines the freezing point in a shorter period of time than Test Method D1177.
5.6 This test method removes most of the operator time and judgement required by Test Method D1177.
6. Apparatus
6.1 Automatic Apparatus —The apparatus described in this method consists of a test chamber controlled by a microprocessor
that is capable of cooling and heating the test specimen, optically observing the appearance and disappearance of solid crystals and
recording the temperature of the specimen.
6.2 The apparatus shall be equipped with a specimen cup, optical detector array, light source, digital display, Peltier device and
a specimen temperature measuring device.
6.3 The temperature measuring device in the specimen cup shall be capable of measuring the temperature of the test specimen
from -80°C–80 °C to +50°C+50 °C at a resolution of 0.1°C.0.1 °C.
6.4 The apparatus shall be equipped with fittings to permit the circulation of liquid cooling media to remove heat generated by
the Peltier device and other electronic components of the apparatus.
7. Reagents and Materials
7.1 Cooling Media—Liquid heat exchange media to remove the heat generated by the Peltier device and other electronic
components from the apparatus.
NOTE 3—Some apparatus are designed to use tap water as cooling media to bring specimen temperature to -60°C.–60 °C. To achieve cooling of
specimen to -80°C,–80 °C, provide circulation of liquid cooling media at -30°C–30 °C or lower to the apparatus. Refer to manufacturer’smanufacturer’s
operating instructions on the relationship between cooling media temperature and the minimum specimen temperature.
7.2 Adjustable Volume Pipette, capable capable of dispensing 0.15 6 0.01 ml of sample.
7.3 Cotton Swabs —Plastic or paper shaft cotton swabs to clean the specimen cup. (Warning—The use of swabs with wooden
shafts may damage the mirrored surface of the specimen cup.)
8. Preparation of Apparatus
8.1 Install the analyzer for operation in accordance with manufacturer’s instructions.
8.2 Make liquid cooling media connections and ensure that they do not leak.
8.3 Turn on the liquid cooling media.
8.4 Turn on the main power switch of the analyzer. After the automatic self diagnostics start-up sequence is completed, the
instrument will display a “READY” message.
The following instrument has been found suitable for use in this test method: Phase Technology Freezing Point Analyzer model series 70 and 70V. The sole source of
supply of the apparatus known to the committee at this time is Phase Technology, i 1168 Hammersmith Gate, Richmond, B.C. Canada, V7A 5H8. If you are aware of
alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at a meeting of the responsible
technical committee, which you may attend.
A suitable pipette is an Eppendorf pipette.
Suitable cotton swabs are Q-tips or equivalent with paper or plastic shafts.
D6660 − 01 (2019)
9. Calibration and Standardization
9.1 Ensure that all of the manufacturer’s instructions for calibrating, checking and operating the apparatus are followed.
9.2 A sample with a mutually agreed upon freezing point can be used to verify performance of the apparatus.
10. Procedure
10.1 Open the test chamber lid and clean the specimen cup inside the test chamber with a cotton swab.
10.2 Use the pipette to deliver 0.15 ml 6 0.
...