ASTM D7646-10(2014)
(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 and health practices and determine the applicability of regulatory limitations prior to use.
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Designation: D7646 − 10 (Reapproved 2014)
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 2.3 Japanese Industrial Standards:
JIS K 2242 Heat Treating Oil
1.1 Thistestmethodcoversthedescriptionoftheequipment
2.4 Wolfson Engineering Group Specification:
and the procedure for evaluating quenching characteristics of
Laboratory Tests forAssessing the Cooling Curve of Indus-
aqueous polymer quenchants by cooling rate determination.
trial Quenching Media
1.2 This test method is designed to evaluate aqueous poly-
mer quenchants for aluminum alloys in a non-agitated system. 3. Terminology
Thereisnocorrelationbetweenthesetestresultsandtheresults
3.1 Definitions of Terms Specific to This Standard:
obtained in agitated systems.
3.1.1 aqueous polymer quenchant, n—aqueous solution
containing a water soluble polymer; typically including poly-
1.3 The values stated in SI units are to be regarded as
(alkylene glycol), poly(ethyl oxazoline), poly(sodium acrylate)
standard. No other units of measurement are included in this
and poly(vinyl pyrrolidone). The quenchant solution also
standard.
typically contains additives for corrosion and foam control, if
1.4 This standard does not purport to address all of the
needed. Quench severity of aqueous polymer quenchants is
safety concerns, if any, associated with its use. It is the
dependent on concentration and molecular weight of the
responsibility of the user of this standard to establish appro-
specific polymer being evaluated, quenchant temperature, and
priate safety and health practices and determine the applica-
agitation rate.
bility of regulatory limitations prior to use.
3.1.2 characteristic temperature, n—transition temperature
from vapor blanket phase (film boiling phase) to rapid cooling
2. Referenced Documents
phase (nucleate boiling phase) on cooling curve.
2.1 ASTM Standards:
3.1.3 cooling curve, n—cooling curve is a graphical repre-
D6200 Test Method for Determination of Cooling Charac-
sentation of the cooling time (t)–temperature (T) response of
teristics of Quench Oils by Cooling Curve Analysis
the probe (see 7.3). An example is illustrated in Part B of Fig.
E220 Test Method for Calibration of Thermocouples By
1.
Comparison Techniques
3.1.4 cooling curve analysis, n—the process of quantifying
E230 Specification and Temperature-Electromotive Force
the cooling characteristics of a heat treating oil based on the
(EMF) Tables for Standardized Thermocouples
temperature versus time profile obtained by cooling a pre-
2.2 ISO Standards:
heated metal probe assembly (see Fig. 2) under standard
ISO 3819 Laboratory Glassware—Beakers
conditions.
3.1.5 cooling rate curve, n—The cooling rate curve is
obtained by calculating the first derivative (dT/dt)ofthe
This test method is under the jurisdiction of ASTM Committee D02 on
cooling time–temperature curve. An example is illustrated in
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Part B of Fig. 1.
Subcommittee D02.L0.06 on Non-Lubricating Process Fluids.
Current edition approved Dec. 1, 2014. Published February 2015. Originally
3.1.6 quench severity, n—the ability of a quenching medium
approved in 2010. Last previous edition approved in 2010 as D7646 – 10.
to extract heat from a hot metal.
DOI:10.1520/D7646-10R14.
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 Available from Japanese Standards Association, 4-1-24, Akasaka Minato-ku,
the ASTM website. Tokyo 107–8440, Japan.
3 5
Available from Society ofAutomotive Engineers, International, 400 Common- Available from Wolfson Heat Treatment Centre, Aston University, Aston
wealth Dr., Warrendale, PA 15096-0001. Triangle, Birmingham B4 7ET, England.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7646 − 10 (2014)
FIG. 1 Typical Temperature/Time and Temperature/Cooling Rate Plots for Test Probe Cooled in an Aqueous Polymer Quenchant
used for cooling curve analysis for steel alloys which is performed at 805
3.1.7 quenchant, n—any medium, liquid, or gas that may be
to 815°C.
used to mediate heat transfer during the cooling of hot metal.
7.2 Measurement System—The temperature–time measure-
4. Summary of Test Method
ment system shall be a computer based data acquisition system
capable of providing a permanent record of the cooling
4.1 Determine the silver rod probe assembly’s cooling time
versus temperature after placing the assembly in a furnace and characteristics of each oil sample tested, producing a record of
variationinthetestprobeassemblyoftemperaturewithrespect
heating to 500°C and then quenching in an aqueous polymer
quenchant solution.The temperature inside the probe assembly to time, and cooling rate with respect to temperature.
and the cooling times are recorded at selected time intervals to
7.3 Probe—Shall be cylindrical, having a diameter of 10 6
establish a cooling temperature versus time curve. The result-
0.1 mm and a length of 30 6 0.1 mm with a 1.0 mm sheathed
ing cooling curve may be used to evaluate quench severity.
Type K thermocouple in its geometric center. The probe shall
be made of a silver of purity 99.99% or more. The probe shall
5. Significance and Use
be attached to a support tube. See Fig. 2 for recommended
5.1 This test method provides a cooling time versus tem-
manufacturing details. Preparation method for silver rod shall
perature pathway.The results obtained by this test method may
be as follows:
be used as a guide in quenchant selection or comparison of
7.3.1 Screw the connecting rod of heat–resistant steel in the
quench severities of different quenchants, new or used.
silver rod body.
7.3.2 Insert the sheath type thermocouple through the sup-
6. Interferences
porting rod and supporting part.
6.1 The presence of contaminants, such as oil, salt, metal-
7.3.3 Screw the connecting rod of heat resistant steel in the
working fluids, forging lubricants, and polymer degradation,
supportingpartasinsertingthesheathtypethermocoupleinthe
may affect cooling curve results obtained by this test method
central part of silver rod body.
for aqueous polymer quenchants.
7.3.4 Screw the supporting part in the supporting rod to
connect.
7. Apparatus
7.3.5 Fix the thermocouple connecting part to the support-
7.1 Furnace—Use a horizontal or vertical electrical resis-
ing rod by using a set screw while pushing the sheath type
tance tube-type furnace capable of maintaining a constant
thermocoupleinthedirectionofsilverrodbody.Insuchacase,
minimum temperature of 850°C over a heated length of not
take care so that the tip of thermocouple is completely pressed
less than 120 mm and a probe positioned in the center of the
to the central part of silver rod body.
heating chamber. The furnace shall be capable of maintaining
7.3.6 Heat the temperature of the silver rod body and
the probe’s temperature within 62.5°C over the specimen
supporting part at 700 to 800°C, and coat the connecting part
length. The furnace, that is, the radiant tube heating media,
with the crystal of silver nitrate and joint them.
shall be used with ambient atmosphere.
7.3.7 After cooling, finish the surface smoothly by using
emerypapers.Althoughcoarser320-gritpapermaybeusedfor
NOTE 1—Although the probe temperature is significantly lower 500°C
initial cleaning, the final finish shall be provided using 500-grit
than the recommended furnace temperature capability 850°C, this higher
temperature capability is recommended since the same apparatus may be emery paper.
D7646 − 10 (2014)
FIG. 2 Probe Details and General Probe Assembly
D7646 − 10 (2014)
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
periodic calibration of the probe and the total system.
7.5 Sample Container—300 mL beaker specified in ISO
8.2 Cleaning Solvent—A hydrocarbon solvent that will
3819.
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
8.3 Polishing Paper—500 grit emery.
fluid temperature to within 61°C.
8.4 Cloth—Lint-free and absorbent.
7.7 Transfer Mechanism—One of the following shall be
used to transfer the heated probe from the furnace to the test
9. Cleaning and Polishing
fluid:
9.1 Cleaning Used Probes—Wipe probe with a lint-free
7.7.1 Automated Transfer Mechanism—The transfer from
cloth or absorbent paper after removal from the quenchant and
the furnace to the oil shall be completed within 3.0 s. Immerse
prior to returning to the furnace. (Warning—The probe shall
the probe in the center, 0 to 5 mm, of the fluid container to a
always be considered hot, as temperature below visual hot
depth where there is 50 6 2 mm of fluid above and below the
temperatures can still cause injury to the skin.) A cleaning
probe when quenched. A mechanical stop shall be used for
solvent may be used, but care should be taken that the probe is
reproducibility of probe placement.
below 50°C. (Warning—Do not use cleaning solvent near the
7.7.2 Manual Transfer—If manual transfer is used, the
furnace opening, especially with automated transfer mecha-
sample container shall be equipped with a fixture to ensure
nisms.).Water m
...
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 D7646 − 10 (Reapproved 2014)
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 and health practices and determine the applicability of regulatory
limitations prior to use.
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 and Temperature-Electromotive Force (EMF) Tables for Standardized Thermocouples
2.2 ISO Standards:
ISO 3819 Laboratory glassware — BeakersGlassware—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.
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.
This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.L0.06 on Non-Lubricating Process Fluids.
Current edition approved July 1, 2010Dec. 1, 2014. Published August 2010February 2015. DOI:10.1520/D7646-10.Originally approved in 2010. Last previous edition
approved in 2010 as D7646 – 10. DOI:10.1520/D7646-10R14.
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, 400 Commonwealth Dr., Warrendale, PA 15096-0001.
Available from Japanese Standards Association, 4-1-24, Akasaka Minato-ku, Tokyo 107–8440, Japan.
Available from Wolfson Heat Treatment Centre, Aston University, Aston Triangle, Birmingham B4 7ET, England.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D7646 − 10 (2014)
FIG. 1 Typical Temperature/Time and Temperature/Cooling Rate Plots for Test Probe Cooled in an Aqueous Polymer Quenchant
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°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°C over a heated length of not less than 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°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°C than the recommended furnace temperature capability 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 805 to
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.
7.3 Probe—Shall be cylindrical, having a diameter of 10 6 0.1 mm and a length of 30 6 0.1 mm with a 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. 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–resistant steel in the silver rod body.
7.3.2 Insert the sheath type thermocouple through the supporting rod and supporting part.
D7646 − 10 (2014)
FIG. 2 Probe Details and General Probe Assembly
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.
D7646 − 10 (2014)
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 700 to 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-grit paper may be used for initial
cleaning, the final finish shall be provided using 500-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 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.
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. Immerse the
probe in the center, 0 to 5 mm, of the fluid container to a depth where there is 50 6 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.
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.
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 prim
...
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