ASTM D6549-06(2011)
(Test Method)Standard Test Method for Determination of Cooling Characteristics of Quenchants by Cooling Curve Analysis with Agitation (Drayton Unit)
Standard Test Method for Determination of Cooling Characteristics of Quenchants by Cooling Curve Analysis with Agitation (Drayton Unit)
SIGNIFICANCE AND USE
This test method provides a cooling time versus temperature curve (profile) that can be related to physical properties, such as the hardness obtainable upon quenching of a metal. The results obtained by this test method may be used as a guide in quenchant selection or as a comparison of quench severities of different quenchants, new or used.
SCOPE
1.1 This test method covers the equipment and the procedure for evaluation of quenching characteristics of a quenching fluid by cooling rate determination.
1.2 This test method is designed to evaluate quenching fluids with agitation, using the Drayton Agitation Unit.
1.3 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.
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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Standards Content (Sample)
NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D6549 − 06(Reapproved 2011)
Standard Test Method for
Determination of Cooling Characteristics of Quenchants by
Cooling Curve Analysis with Agitation (Drayton Unit)
This standard is issued under the fixed designation D6549; 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 2.4 ASTM Adjuncts:
ADJD6300 D2PP, Determination of Precision and Bias
1.1 This test method covers the equipment and the proce-
Data for Use in Test Methods for Petroleum Products and
dure for evaluation of quenching characteristics of a quenching
Lubricants
fluid by cooling rate determination.
1.2 This test method is designed to evaluate quenching 3. Terminology
fluids with agitation, using the Drayton Agitation Unit.
3.1 Definitions of Terms Specific to This Standard:
1.3 The values stated in SI units are to be regarded as 3.1.1 aqueous polymer quenchant—an aqueous polymer
standard. The values given in parentheses are for information quenchant is an aqueous solution containing a water soluble
only. polymer, typically including poly(alkylene glycol), poly(ethyl
oxazoline), poly(sodium acrylate), and poly(vinyl pyrrolidone)
1.4 This standard does not purport to address all of the
(1, 2, 3). The quenchant solution also typically contains
safety concerns, if any, associated with its use. It is the
additives for corrosion and foam control, if needed. Quench
responsibility of the user of this standard to establish appro-
severity of aqueous polymer quenchants is dependent on
priate safety and health practices and determine the applica-
concentration and molecular weight of the specific polymer
bility of regulatory limitations prior to use.
being evaluated, quenchant temperature, and agitation rate as
shown in Fig. 1, Fig. 2, and Fig. 3, respectively.
2. Referenced Documents
3.1.2 cooling curve—the cooling curve is a graphical repre-
2.1 ASTM Standards:
sentation of the cooling time (t) versus temperature (T)
E220 Test Method for Calibration of Thermocouples By
response of the probe (see 7.3). An example is illustrated in
Comparison Techniques
Fig. 4.
E230 Specification and Temperature-Electromotive Force
(EMF) Tables for Standardized Thermocouples 3.1.3 cooling curve analysis—the process of quantifying the
coolingcharacteristicsofaquenchantbasedonthetemperature
2.2 SAE Standards:
versustimeprofileobtainedbycoolingapreheatedmetalprobe
AMS 5665 NickelAlloy Corrosion and Heat Resistant Bars,
assembly (see Fig. 4) under standard conditions (1-7).
Forgings and Rings
3.1.4 cooling rate curve—the cooling rate curve is a graphi-
2.3 Other Standards:
Wolfson Engineering Group Specification Laboratory Tests cal representation of first derivative of the cooling curve, the
rate of temperature change (dT/dt) versus temperature. An
forAssessing the Cooling Curve Characteristics of Indus-
trial Quenching Media example is illustrated in Fig. 4.
3.1.5 quenchant—a quenching medium may be either a
liquid or a gas. Gasses that are used as quenchants include air,
This test method is under the jurisdiction of ASTM Committee D02 on
nitrogen, argon, and hydrogen and, with the exception of air,
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
whichisusedatatmosphericpressure,areusedunderpressure.
Subcommittee D02.L0.06 on Non-Lubricating Process Fluids.
Current edition approved May 1, 2011. Published August 2011. Originally Liquid quenchants include water, brine (most commonly dilute
approved in 2000. Last previous edition approved in 2006 as D6549–06. DOI:
aqueous solutions of sodium chloride or sodium hydroxide),
10.1520/D6549-06R11.
oil, molten salt, molten metal, and aqueous solutions of water
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
soluble polymers. Water, brine, oil, and aqueous polymer
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
quenchants are generally used with agitation.
the ASTM website.
Available from SAE International (SAE), 400 Commonwealth Dr.,Warrendale,
PA 15096-0001, http://www.sae.org. No longer available from ASTM International Headquarters.
Available from Wolfson Heat Treatment Centre, Federation House, Vyse St., The boldface numbers in parentheses refer to the list of references at the end of
Birmingham, B18 6LT, UK. http://www.sea.org.uk/whtc. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6549 − 06 (2011)
FIG. 1 Effect of Quenchant Concentration on Cooling Curve Performance for a Poly(Alkylene Glycol) Quenchant at 30°C and 0.5 m/s
FIG. 2 Effect of Bath Temperature Variation on Cooling Curve Performance for 15 % Aqueous Solution of Poly(Alkylene Glycol) Quen-
chant at 0.5 m/s
FIG. 3 Effect of Agitation Rate Variation on Cooling Curve Performance for a 15 % Aqueous Poly(Alkylene Glycol) Quenchant Solution
at 30°C
3.1.6 quench severity—theabilityofaquenchingmediumto
extract heat from a hot metal (8).
D6549 − 06 (2011)
NOTE 1—a) Cooling Curve; b) Cooling Rate Curve
FIG. 4 Typical Temperature/Time and Temperature/Cooling Rate Plots for Test Probe Cooled in a Quenching Oil
4. Summary of Test Method 7.2 Measurement System—The temperature-time measure-
ment system shall be a computer based data acquisition system
4.1 This test method determines the cooling time versus
capable of providing a permanent record of the cooling
temperature of a standard nickel alloy probe assembly after it
characteristics of each sample tested, producing a record of
has been heated in a furnace to 850°C (1562°F) and then
variationinthetestprobeassemblyoftemperaturewithrespect
quenched in an aqueous polymer quenchant solution. The
to time and cooling rate with respect to temperature.
temperature inside the probe assembly and the cooling times
are recorded at selected time intervals to establish a cooling
7.3 Probe—The probe shall be cylindrical, having a diam-
temperature versus time curve. The resulting cooling curve
eter of 12.5 6 0.01 mm (0.492 6 0.0004 in.) and a length of
(profile) may be used to evaluate quench severity (see Note 1).
60 6 0.25 mm (2.362 6 0.01 in.) with a 1.45 to 1.65-mm
(0.057 to 0.065-in.) sheathed Type K thermocouple in its
NOTE 1—Where appropriate for production testing, a furnace tempera-
geometric center. The probe shall be made of a nickel Alloy
ture from 815 to 857°C (1500 to 1575°F) may be used.
600 (UNS N06600), purchased in accordance withAMS 5665,
which has a nominal composition of 76.0 % Ni, 15.5 % Cr,
5. Significance and Use
8.0 % Fe, 0.08 % C, and 0.25 % maximum Cu.The probe shall
5.1 This test method provides a cooling time versus tem-
be attached to a support tube with a minimum length of 200
perature curve (profile) that can be related to physical
mm (7.874 in.). The thermocouple sheathing and the support
properties, such as the hardness obtainable upon quenching of
tube shall be the same material as the probe (see Note 2). See
a metal. The results obtained by this test method may be used
Fig. 5 for other manufacturing requirements.
as a guide in quenchant selection or as a comparison of quench
severities of different quenchants, new or used.
NOTE 2—Care shall be taken that the probe specimen is not damaged as
surface irregularities will influence results of the test.
6. Interferences
7.4 Drayton Agitation Unit:
6.1 The presence of contaminants, such as oil, salt, metal-
7.4.1 Construction—The sample container, a 2000-mL
working fluids, forging lubricants, and polymer degradation,
stainless steel beaker that is the same as the standard container
may affect cooling curve results obtained by this test method
used in nonagitated cooling curve test, is modified to provide
for aqueous polymer quenchants.
upwardoraxialflowofthequenchantpasttheprobe.Thisflow
occurs through a vertical flow tube located in the geometric
7. Apparatus
center of the container.As shown in Fig. 6, the unit includes a
variable speed dc drive centrifugal pump and large diameter
7.1 Furnace—Use a horizontal or vertical electrical resis-
flowmeter for direct measurement of flow velocity. It is noted
tance tube-type furnace capable of maintaining a constant
that the flow tube is removable, which will provide a more
minimum temperature of 850°C (1562°F) over a heated length
turbulent flow pattern.
ofnotlessthan120mm(4.72in.)andaprobepositionedinthe
center of the heating chamber. The furnace shall be capable of 7.4.2 Cleaning—The agitation assembly shall be cleaned
maintaining the probe’s temperature within 62.5°C (4.5°F) prior to use with a detergent solution. After cleaning, the
over the specimen length. The furnace, that is, the radiant tube assembly shall be rinsed with water at least three times to
heating media, shall be used with ambient atmosphere. ensurethatnoquenchantresidueordetergentsolutionremains.
D6549 − 06 (2011)
NOTE 1—Dimensions above are nominal.
FIG. 5 Probe Details and General Probe Assembly
FIG. 6 Drayton Agitation Unit
D6549 − 06 (2011)
7.4.3 Flow Velocity—The variable speed pump and flow 8.1.1 If results do not comply with the specified ranges, the
meter allow reproducible setting of quenchant flow through the probe shall be replaced or reconditioned (see 9.3) or system
tube. The flowmeter is calibrated for water at 25°C. Flow adjustments made. Compliance to the specified limits of the
velocity for other fluids will vary with fluid viscosity and primaryreferencefluidiscriticalforestablishingthevalidityof
temperature. subsequent test results. It has been shown that the test method
7.4.4 Fluid Volume—The resulting cooling curve is influ- has an excellent level of repeatability and reproducibility when
enced by the temperature rise during the quench, which is the probe and system are shown to be in calibration (9, 10).
dependent on the total fluid volume. Therefore, the cooling 8.1.2 A secondary reference fluid may be used, provided
curve test shall be performed with a fixed volume of fluid. that sufficient statistical cooling curve testing has been con-
ducted so that the results are (1) traceable to the primary
7.5 Temperature Measurement—Any temperature detection
referencefluidand(2)comparedonthebasisofthesixprimary
device may be used that is capable of measuring quenching
cooling characteristics.
fluid temperature to within 61°C (1.8°F).
8.1.3 Reference fluids shall be stored in a sealed container
7.6 Transfer Mechanism—One of the following shall be
when not in use and shall be replaced after 200 quenches or
used to transfer the heated probe from the furnace to the test
two years, whichever is sooner.
fluid.
8.2 Polishing Paper, 600 grit emery.
7.6.1 Mechanical Transfer—The agitation unit is positioned
with the center of the test chamber coincident with the probe 8.3 Cotton Cloth or Paper, lintless and absorbent.
centerline.Thetransfermechanismissettodelivertheprobeto
9. Cleaning and Conditioning
the vertical center of the sample.
9.1 Cleaning Used Probes—Wipe the probe with a clean,
7.6.2 Manual Transfer—The probe is transferred to the
wet, lintless cotton cloth or absorbent paper after removal from
agitation unit through a probe guide, which is set (1) to the test
thequenchantandpriortoreturningtothefurnace.Unmounted
chamber centerline and (2) with a preset stop that causes the
probes may be cleaned in the same manner or, alternatively,
probe to rest in the vertical center of the sample. The unit is
washedunderastreamofwater,andthenwipeddry.(Warning
illustrated further in the sketch and photograph of Fig. 6 and
—The probe shall always be considered hot as a temperature
Fig.7,respectively.Atimershallbeusedtoensureamaximum
below visual hot temperatures can still cause injury to the skin
transfer time of 3.0 s.
or ignition of the cloth or paper used in cleaning.)
7.7 Timer, graduated in seconds and minutes, and may be
9.2 Conditioning New Probes—Condition the probe prior to
part of a computer clock.
its initial use by carrying out a minimum of six trial quenches,
or a grater number if required to achieve consistency, using a
8. Reagents and Materials
clean, neutral, general purpose hydrocarbon oil. Clean the
8.1 Reference Quenching Fluid, used for initial calibration
probe assembly between quenches, as specified in 9.1. Quench
and for periodic calibration verification. Data collected from
the probe in the reference quenching fluid and check in
quench tests with the reference fluid shall be evaluated for
accordance with 12.3. If the probe does not meet the require-
compliance to the specified values for the six primary charac-
ments of 12.3, recondition in accordance with 9.3 and then
teristics.Thesecharacteristics,asdefinedinWolfsonEngineer-
recalibrate again in accordance with 12.3. Do not use probes
ing Group Specification, are as follows:
that do not meet these requirements.
Time to cool to 600°C (1112°F) 12-14 s
9.3 Probe Reconditioning—The probe shall be recondi-
Time to cool to 400°C (752°F) 19-21 s
Time to cool to 200°C (392°F) 50-55 s
tioned when the probe calibration, as described in 12.3, does
Maximum cooling rate 47-53°C/s (85-95°F/s)
not meet the calibration limits of the six cooling characteristics
Temperature of the maximum cooling rate 490-530°C (914-986°F)
Cooling rate at 300°C (572°F) 6-8°C/s (10.8-14.4°F/s) specified for the reference fluid. Recondition the probe by
polishing with emery paper. Although coarser 320-grit paper
may be used for initial polishing, the final finish shall be
provided by use of 600-grit emery paper. Following this
procedure, the probe shall be quenched until satisfactory
cooling curve results are obtained from the reference fluid.
10. Sampling
10.1 Take care that the gross media, from which the sample
istakentofilltheagitationunit,iswellmixedtoensurethatthe
sample is representative of the media being tested. Any
containers used to secure the quenchant sample must be clean
and dry.
11. Preparation of Apparatus
11.1 Preheat furnace to 850 6 2°C (1562 6 4°F), or
alternatively, to 815 to 857°C (1500 to 1575°F) for production
FIG. 7 Commercially Available Drayton Agitation Unit testing.
D6549 − 06 (2011)
11.2 Connect a dry, conditioned, calibrated probe in accor- 13.4 When the test is complete (generally within 60 s) and
dance with the equipment manufacturer’s in
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