ASTM D7646-10(2019)
(Test Method)Standard Test Method for Determination of Cooling Characteristics of Aqueous Polymer Quenchants for Aluminum Alloys by Cooling Curve Analysis
Standard Test Method for Determination of Cooling Characteristics of Aqueous Polymer Quenchants for Aluminum Alloys by Cooling Curve Analysis
SIGNIFICANCE AND USE
5.1 This test method provides a cooling time versus temperature pathway. The results obtained by this test method may be used as a guide in quenchant selection or comparison of quench severities of different quenchants, new or used.
SCOPE
1.1 This test method covers the description of the equipment and the procedure for evaluating quenching characteristics of aqueous polymer quenchants by cooling rate determination.
1.2 This test method is designed to evaluate aqueous polymer quenchants for aluminum alloys in a non-agitated system. There is no correlation between these test results and the results obtained in agitated systems.
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.
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.
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Designation: D7646 − 10 (Reapproved 2019)
Standard Test Method for
Determination of Cooling Characteristics of Aqueous
Polymer Quenchants for Aluminum Alloys by Cooling Curve
Analysis
This standard is issued under the fixed designation D7646; 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 (emf) Tables for Standardized Thermocouples
1.1 This test method covers the description of the equipment 2.2 ISO Standards:
and the procedure for evaluating quenching characteristics of ISO 3819 Laboratory Glassware—Beakers
aqueous polymer quenchants by cooling rate determination. 4
2.3 Japanese Industrial Standards:
1.2 This test method is designed to evaluate aqueous poly- JIS K 2242 Heat Treating Oil
mer quenchants for aluminum alloys in a non-agitated system. 5
2.4 Wolfson Engineering Group Specification:
There is no correlation between these test results and the results
Laboratory Tests for Assessing the Cooling Curve of Indus-
obtained in agitated systems.
trial Quenching Media
1.3 The values stated in SI units are to be regarded as
standard. No other units of measurement are included in this 3. Terminology
standard.
3.1 Definitions of Terms Specific to This Standard:
1.4 This standard does not purport to address all of the
3.1.1 aqueous polymer quenchant, n—aqueous solution
safety concerns, if any, associated with its use. It is the
containing a water soluble polymer; typically including poly-
responsibility of the user of this standard to establish appro-
(alkylene glycol), poly(ethyl oxazoline), poly(sodium acrylate)
priate safety, health, and environmental practices and deter-
and poly(vinyl pyrrolidone). The quenchant solution also
mine the applicability of regulatory limitations prior to use.
typically contains additives for corrosion and foam control, if
1.5 This international standard was developed in accor-
needed. Quench severity of aqueous polymer quenchants is
dance with internationally recognized principles on standard-
dependent on concentration and molecular weight of the
ization established in the Decision on Principles for the
specific polymer being evaluated, quenchant temperature, and
Development of International Standards, Guides and Recom-
agitation rate.
mendations issued by the World Trade Organization Technical
3.1.2 characteristic temperature, n—transition temperature
Barriers to Trade (TBT) Committee.
from vapor blanket phase (film boiling phase) to rapid cooling
phase (nucleate boiling phase) on cooling curve.
2. Referenced Documents
3.1.3 cooling curve, n—cooling curve is a graphical repre-
2.1 ASTM Standards:
sentation of the cooling time (t)–temperature (T) response of
D6200 Test Method for Determination of Cooling Charac-
the probe (see 7.3). An example is illustrated in Part B of Fig.
teristics of Quench Oils by Cooling Curve Analysis
1.
E220 Test Method for Calibration of Thermocouples By
3.1.4 cooling curve analysis, n—the process of quantifying
Comparison Techniques
the cooling characteristics of a heat treating oil based on the
E230 Specification for Temperature-Electromotive Force
temperature versus time profile obtained by cooling a pre-
heated metal probe assembly (see Fig. 2) under standard
1 conditions.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.L0.06 on Non-Lubricating Process Fluids.
Current edition approved May 1, 2019. Published July 2019. Originally approved
in 2010. Last previous edition approved in 2014 as D7646 – 10 (2014). Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale,
DOI:10.1520/D7646-10R19. PA 15096, http://www.sae.org.
2 4
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Available from Japanese Standards Association (JSA), Mita MT Bldg., 3-13-12
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM Mita, Minato-ku, Tokyo 108-0073, Japan, http://www.jsa.or.jp.
Standards volume information, refer to the standard’s Document Summary page on Available from Wolfson Heat Treatment Centre, Aston University, Aston
the ASTM website. Triangle, Birmingham B4 7ET, England, http://www.sea.org.uk/whtc/.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7646 − 10 (2019)
FIG. 1 Typical Temperature/Time and Temperature/Cooling Rate Plots for Test Probe Cooled in an Aqueous Polymer Quenchant
3.1.5 cooling rate curve, n—The cooling rate curve is length. The furnace, that is, the radiant tube heating media,
obtained by calculating the first derivative (dT/dt) of the shall be used with ambient atmosphere.
cooling time–temperature curve. An example is illustrated in
NOTE 1—Although the probe temperature is significantly lower 500 °C
Part B of Fig. 1.
than the recommended furnace temperature capability 850 °C, this higher
temperature capability is recommended since the same apparatus may be
3.1.6 quench severity, n—the ability of a quenching medium
used for cooling curve analysis for steel alloys which is performed at
to extract heat from a hot metal.
805 °C to 815 °C.
3.1.7 quenchant, n—any medium, liquid, or gas that may be
7.2 Measurement System—The temperature–time measure-
used to mediate heat transfer during the cooling of hot metal.
ment system shall be a computer based data acquisition system
capable of providing a permanent record of the cooling
4. Summary of Test Method
characteristics of each oil sample tested, producing a record of
4.1 Determine the silver rod probe assembly’s cooling time
variation in the test probe assembly of temperature with respect
versus temperature after placing the assembly in a furnace and
to time, and cooling rate with respect to temperature.
heating to 500 °C and then quenching in an aqueous polymer
7.3 Probe—Shall be cylindrical, having a diameter of
quenchant solution. The temperature inside the probe assembly
and the cooling times are recorded at selected time intervals to 10 mm 6 0.1 mm and a length of 30 mm 6 0.1 mm with a
establish a cooling temperature versus time curve. The result- 1.0 mm sheathed Type K thermocouple in its geometric center.
The probe shall be made of a silver of purity 99.99 % or more.
ing cooling curve may be used to evaluate quench severity.
The probe shall be attached to a support tube. See Fig. 2 for
5. Significance and Use recommended manufacturing details. Preparation method for
silver rod shall be as follows:
5.1 This test method provides a cooling time versus tem-
7.3.1 Screw the connecting rod of heat-resistant steel in the
perature pathway. The results obtained by this test method may
silver rod body.
be used as a guide in quenchant selection or comparison of
quench severities of different quenchants, new or used. 7.3.2 Insert the sheath type thermocouple through the sup-
porting rod and supporting part.
6. Interferences
7.3.3 Screw the connecting rod of heat resistant steel in the
supporting part as inserting the sheath type thermocouple in the
6.1 The presence of contaminants, such as oil, salt, metal-
central part of silver rod body.
working fluids, forging lubricants, and polymer degradation,
7.3.4 Screw the supporting part in the supporting rod to
may affect cooling curve results obtained by this test method
for aqueous polymer quenchants. connect.
7.3.5 Fix the thermocouple connecting part to the support-
7. Apparatus
ing rod by using a set screw while pushing the sheath type
thermocouple in the direction of silver rod body. In such a case,
7.1 Furnace—Use a horizontal or vertical electrical resis-
take care so that the tip of thermocouple is completely pressed
tance tube-type furnace capable of maintaining a constant
to the central part of silver rod body.
minimum temperature of 850 °C over a heated length of not
less than 120 mm and a probe positioned in the center of the 7.3.6 Heat the temperature of the silver rod body and
heating chamber. The furnace shall be capable of maintaining supporting part at 700 °C to 800 °C, and coat the connecting
the probe’s temperature within 62.5 °C over the specimen part with the crystal of silver nitrate and joint them.
D7646 − 10 (2019)
FIG. 2 Probe Details and General Probe Assembly
D7646 − 10 (2019)
7.3.7 After cooling, finish the surface smoothly by using Safety Data Sheet supplied with this material prior to use and
emery papers. Although coarser 320 grit paper may be used for appropriate safety precautions shall be implemented during
initial cleaning, the final finish shall be provided using 500 grit use.)
emery paper. 8.1.2 A secondary reference fluid may be used provided that
sufficient statistical cooling curve testing has been conducted
7.4 Fluid Volume—The resulting cooling curve will be
so that results are traceable to the primary reference fluid such
dependent on the temperature rise during the quench, which is
as that cited in JIS K 2242.
dependent on the total fluid volume. Therefore, the cooling
8.1.2.1 The 10 mass% of brine solution which is prepared
curve analysis shall be performed with the same volume of
by dissolving sodium chloride in distilled water has also been
fluid.
used as reference quenching fluid for initial calibration and for
7.5 Sample Container—300 mL beaker specified in ISO periodic calibration of the probe and the total system.
3819.
8.2 Cleaning Solvent—A hydrocarbon solvent that will
evaporate at room temperature, leaving no residue.
7.6 Temperature Measurement—Any temperature detection
(Warning—Flammable. Harmful if inhaled.)
device may be used that is capable of measuring quenching
fluid temperature to within 61 °C.
8.3 Polishing Paper—500 grit emery.
7.7 Transfer Mechanism—One of the following shall be 8.4 Cloth—Lint-free and absorbent.
used to transfer the heated probe from the furnace to the test
9. Cleaning and Polishing
fluid:
7.7.1 Automated Transfer Mechanism—The transfer from 9.1 Cleaning Used Probes—Wipe probe with a lint-free
the furnace to the oil shall be completed within 3.0 s. Immerse cloth or absorbent paper after removal from the quenchant and
the probe in the center, 0 mm to 5 mm, of the fluid container to prior to returning to the furnace. (Warning—The probe shall
a depth where there is 50 mm 6 2 mm of fluid above and always be considered hot, as temperature below visual hot
below the probe when quenched. A mechanical stop sha
...
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.
Designation: D7646 − 10 (Reapproved 2014) D7646 − 10 (Reapproved 2019)
Standard Test Method for
Determination of Cooling Characteristics of Aqueous
Polymer Quenchants for Aluminum Alloys by Cooling Curve
Analysis
This standard is issued under the fixed designation D7646; 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
1.1 This test method covers the description of the equipment and the procedure for evaluating quenching characteristics of
aqueous polymer quenchants by cooling rate determination.
1.2 This test method is designed to evaluate aqueous polymer quenchants for aluminum alloys in a non-agitated system. There
is no correlation between these test results and the results obtained in agitated systems.
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.
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:
D6200 Test Method for Determination of Cooling Characteristics of Quench Oils by Cooling Curve Analysis
E220 Test Method for Calibration of Thermocouples By Comparison Techniques
E230 Specification for Temperature-Electromotive Force (emf) Tables for Standardized Thermocouples
2.2 ISO Standards:
ISO 3819 Laboratory Glassware—Beakers
2.3 Japanese Industrial Standards:
JIS K 2242 Heat Treating Oil
2.4 Wolfson Engineering Group Specification:
Laboratory Tests for Assessing the Cooling Curve of Industrial Quenching Media
3. Terminology
3.1 Definitions of Terms Specific to This Standard:
3.1.1 aqueous polymer quenchant, n—aqueous solution containing a water soluble polymer; typically including poly(alkylene
glycol), poly(ethyl oxazoline), poly(sodium acrylate) and poly(vinyl pyrrolidone). The quenchant solution also typically contains
additives for corrosion and foam control, if needed. Quench severity of aqueous polymer quenchants is dependent on concentration
and molecular weight of the specific polymer being evaluated, quenchant temperature, and agitation rate.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommittee
D02.L0.06 on Non-Lubricating Process Fluids.
Current edition approved Dec. 1, 2014May 1, 2019. Published February 2015July 2019. Originally approved in 2010. Last previous edition approved in 20102014 as
D7646 – 10.D7646 – 10 (2014). DOI:10.1520/D7646-10R14.DOI:10.1520/D7646-10R19.
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.
Available from Society of Automotive Engineers, International, SAE International (SAE), 400 Commonwealth Dr., Warrendale, PA 15096-0001.15096, http://
www.sae.org.
Available from Japanese Standards Association, 4-1-24, Akasaka Minato-ku, Tokyo 107–8440, Japan.Association (JSA), Mita MT Bldg., 3-13-12 Mita, Minato-ku, Tokyo
108-0073, Japan, http://www.jsa.or.jp.
Available from Wolfson Heat Treatment Centre, Aston University, Aston Triangle, Birmingham B4 7ET, England.England, http://www.sea.org.uk/whtc/.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7646 − 10 (2019)
3.1.2 characteristic temperature, n—transition temperature from vapor blanket phase (film boiling phase) to rapid cooling phase
(nucleate boiling phase) on cooling curve.
3.1.3 cooling curve, n—cooling curve is a graphical representation of the cooling time (t)–temperature (T) response of the probe
(see 7.3). An example is illustrated in Part B of Fig. 1.
3.1.4 cooling curve analysis, n—the process of quantifying the cooling characteristics of a heat treating oil based on the
temperature versus time profile obtained by cooling a pre-heated metal probe assembly (see Fig. 2) under standard conditions.
3.1.5 cooling rate curve, n—The cooling rate curve is obtained by calculating the first derivative (dT/dt) of the cooling
time–temperature curve. An example is illustrated in Part B of Fig. 1.
3.1.6 quench severity, n—the ability of a quenching medium to extract heat from a hot metal.
3.1.7 quenchant, n—any medium, liquid, or gas that may be used to mediate heat transfer during the cooling of hot metal.
4. Summary of Test Method
4.1 Determine the silver rod probe assembly’s cooling time versus temperature after placing the assembly in a furnace and
heating to 500°C500 °C and then quenching in an aqueous polymer quenchant solution. The temperature inside the probe assembly
and the cooling times are recorded at selected time intervals to establish a cooling temperature versus time curve. The resulting
cooling curve may be used to evaluate quench severity.
5. Significance and Use
5.1 This test method provides a cooling time versus temperature pathway. The results obtained by this test method may be used
as a guide in quenchant selection or comparison of quench severities of different quenchants, new or used.
6. Interferences
6.1 The presence of contaminants, such as oil, salt, metal-working fluids, forging lubricants, and polymer degradation, may
affect cooling curve results obtained by this test method for aqueous polymer quenchants.
7. Apparatus
7.1 Furnace—Use a horizontal or vertical electrical resistance tube-type furnace capable of maintaining a constant minimum
temperature of 850°C850 °C over a heated length of not less than 120 mm 120 mm and a probe positioned in the center of the
heating chamber. The furnace shall be capable of maintaining the probe’s temperature within 62.5°C62.5 °C over the specimen
length. The furnace, that is, the radiant tube heating media, shall be used with ambient atmosphere.
NOTE 1—Although the probe temperature is significantly lower 500°C500 °C than the recommended furnace temperature capability 850°C,850 °C, this
higher temperature capability is recommended since the same apparatus may be used for cooling curve analysis for steel alloys which is performed at
805805 °C to 815°C.815 °C.
7.2 Measurement System—The temperature–time measurement system shall be a computer based data acquisition system
capable of providing a permanent record of the cooling characteristics of each oil sample tested, producing a record of variation
in the test probe assembly of temperature with respect to time, and cooling rate with respect to temperature.
FIG. 1 Typical Temperature/Time and Temperature/Cooling Rate Plots for Test Probe Cooled in an Aqueous Polymer Quenchant
D7646 − 10 (2019)
FIG. 2 Probe Details and General Probe Assembly
7.3 Probe—Shall be cylindrical, having a diameter of 1010 mm 6 0.1 mm 0.1 mm and a length of 3030 mm 6 0.1 mm 0.1 mm
with a 1.0 mm 1.0 mm sheathed Type K thermocouple in its geometric center. The probe shall be made of a silver of purity
D7646 − 10 (2019)
99.99%99.99 % or more. The probe shall be attached to a support tube. See Fig. 2 for recommended manufacturing details.
Preparation method for silver rod shall be as follows:
7.3.1 Screw the connecting rod of heat–resistantheat-resistant steel in the silver rod body.
7.3.2 Insert the sheath type thermocouple through the supporting rod and supporting part.
7.3.3 Screw the connecting rod of heat resistant steel in the supporting part as inserting the sheath type thermocouple in the
central part of silver rod body.
7.3.4 Screw the supporting part in the supporting rod to connect.
7.3.5 Fix the thermocouple connecting part to the supporting rod by using a set screw while pushing the sheath type
thermocouple in the direction of silver rod body. In such a case, take care so that the tip of thermocouple is completely pressed
to the central part of silver rod body.
7.3.6 Heat the temperature of the silver rod body and supporting part at 700700 °C to 800°C,800 °C, and coat the connecting
part with the crystal of silver nitrate and joint them.
7.3.7 After cooling, finish the surface smoothly by using emery papers. Although coarser 320-grit320 grit paper may be used
for initial cleaning, the final finish shall be provided using 500-grit500 grit emery paper.
7.4 Fluid Volume—The resulting cooling curve will be dependent on the temperature rise during the quench, which is dependent
on the total fluid volume. Therefore, the cooling curve analysis shall be performed with the same volume of fluid.
7.5 Sample Container—300 mL 300 mL beaker specified in ISO 3819.
7.6 Temperature Measurement—Any temperature detection device may be used that is capable of measuring quenching fluid
temperature to within 61°C.61 °C.
7.7 Transfer Mechanism—One of the following shall be used to transfer the heated probe from the furnace to the test fluid:
7.7.1 Automated Transfer Mechanism—The transfer from the furnace to the oil shall be completed within 3.0 s. 3.0 s. Immerse
the probe in the center, 00 mm to 5 mm, 5 mm, of the fluid container to a depth where there is 5050 mm 6 2 mm 2 mm of fluid
above and below the probe when quenched. A mechanical stop shall be used for reproducibility of probe placement.
7.7.2 Manual Transfer—If manual transfer is used, the sample container shall be equipped with a fixture to ensure correct
placement in the center of the fluid container and to the depth defined in 7.4. A timer shall be used to ensure a maximum transfer
time of 3.0 s.3.0 s.
7.8 Timer—Graduated in seconds and minutes; may be part of a computer clock.
7.9 Fluid Volume—The resulting cooling curve will be dependent on the temperature rise during the quench, which is dependent
on the total fluid volume. Therefore, the cooling curve analysis shall be performed with the same volume of fluid.
7.10 Temperature Measurement—Any temperature detection device may be used that is capable of measuring quenching fluid
temperature to within 61°C.61 °C.
8. Reagents and Materials
8.1 Reference Quenching Fluid—Use a reference quenching fluid for initial and regular probe calibration to determine if the
probe will give results consistent to those obtained during initial break-in.
8.1.1 Dioctylphthalate DOP (Di-2-ethylthexyl Phthalate)—Used as primary reference quenching fluid for initial calibration and
for periodic calibration of the probe. Properties of DOP used as reference fluid are as follows:
3 3
Density (20°C): 0.986(20 °C): 0.986 g ⁄m 6 0.003 0.003 g g/m⁄m
Refractive index (25°C):(25 °C): 1.485 6 0.003
Water content: Not greater than 0.1 mass%0.1 mass%
Purity (GC method): Not lower than 97.0 mass%97.0 mass%
(Warning—Potential acute and chronic health effects have been reported for D.O.P. and the user shall consult the Material
Safety Data Sheet supplied with this material prior to use and appropriate safety precautions shall be implemented during
use.Potential acute and chronic health effects have been reported for D.O.P. and the user shall consult the Material Safety Data
Sheet supplied with this material prior to use and appropriate safety precautions shall be implemented during use.))
8.1.2 A secondary reference fluid may be used provided that sufficient statistical cooling curve testing has been conducted so
that results are traceable to the primary reference fluid such as that cited in JIS K 2242.
8.1.2.1 The 10 mass% 10 mass% of brine solution which is prepared by dissolving sodium chloride in distilled water has also
been used as reference quenching fluid for initial calibration and for periodic calibration of the probe and the total system.
8.2 Cleaning Solvent—A hydrocarbon solvent that will evaporate at room temperature, leaving no residue. (Warning—
Flammable. Harmful if inhaled.)
8.3 Polishing Paper—500 grit 500 grit emery.
8.4 Cloth—Lint-free and absorbent.
D7646 − 10 (2019)
9. Cleaning and Polishing
9.1 Cleaning Used Probes—Wipe probe with a lint-free cloth or absorbent paper after removal from the quenchant and prior
to returning to the furnace. (Warning—The probe shall always be considered hot, as temperature below visual hot temperatures
can still cause injury to the skin.) A cleaning solvent may be used, but care should be taken that the probe is below 50°C.50 °C.
(Warning—Do not use cleaning solvent near the furnace opening, especially with automated transfer mechanisms.). Water may
be also be used as a cleaning solvent which may by followed by polishing (see 9.2).
9.2 Polishing Used Probes Using Emery Paper—Polish probe surface lightly at every trial using 500-grit500 grit emery paper
until its metallic luster is recovered.
10. Sampling
10.1 Sampling shall be in accordance with 7.5. Take care to ensure the sample is representative of the quenchant being tested.
Use a clean and dry sample container.
11. Preparation of Apparatus
11.1 Preheat furnace to 520520 °C to 550°C.550 °C.
11.2 Connect a dry, cleaned, calibrated probe to the transfer mechanism in accordance with equipment manufacturer’s
instructions.
11.3 The aqueous polymer quenchant shall be heated or cooled to the desired temperature if production testing is being
performed, or to 80°C80 °C if the reference fluid dioctylphthalate (DOP) is being tested.
12. Calibration and Standardization
12.1 Probe:
12.1.1 Check the accuracy of the probe thermocouple by attaching a previously calibrated thermocouple to the outer surface of
the probe. Locate the tip of the calibrated thermocouple 15 mm 15 mm from the end of the probe. Heat the probe and calibrated
thermocouple to the selected furnace temperature of 510510 °C 6 5°C,5 °C, an
...
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