ASTM D6200-01(2012)
(Test Method)Standard Test Method for Determination of Cooling Characteristics of Quench Oils by Cooling Curve Analysis
Standard Test Method for Determination of Cooling Characteristics of Quench Oils by Cooling Curve Analysis
SIGNIFICANCE AND USE
This test method provides a cooling time versus temperature pathway which is directly proportional to physical properties such as the hardness obtainable upon quenching of a metal. The results obtained by this test may be used as a guide in heat treating oil selection or comparison of quench severities of different heat treating oils, new or used.
SCOPE
1.1 This test method describes the equipment and the procedure for evaluation of a quenching oil's quenching characteristics by cooling rate determination.
1.2 This test is designed to evaluate quenching oils in a non-agitated system. There is no correlation between these test results and the results obtained in agitated systems.
1.3 The values in SI units are to be regarded as the standard. The values in parentheses are provided for information only.
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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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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D6200 − 01 (Reapproved 2012)
Standard Test Method for
Determination of Cooling Characteristics of Quench Oils by
Cooling Curve Analysis
This standard is issued under the fixed designation D6200; 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 3. Terminology
1.1 This test method describes the equipment and the 3.1 Definitions of Terms Specific to This Standard:
procedure for evaluation of a quenching oil’s quenching
3.1.1 cooling curve, n—the cooling curve is a graphical
characteristics by cooling rate determination.
representation of the cooling time (t) - temperature (T) re-
sponse of the probe (see 7.3).An example is illustrated in Part
1.2 This test is designed to evaluate quenching oils in a
Bof Fig. 1.
non-agitated system. There is no correlation between these test
results and the results obtained in agitated systems.
3.1.2 cooling curve analysis, n—the process of quantifying
the cooling characteristics of a heat treating oil based on the
1.3 The values in SI units are to be regarded as the standard.
temperature versus time profile obtained by cooling a pre-
The values in parentheses are provided for information only.
heated metal probe assembly (see Fig. 2) under standard
1.4 This standard does not purport to address all of the
conditions.
safety concerns, if any, associated with its use. It is the
responsibility of the user of this standard to establish appro-
3.1.3 cooling rate curve, n—The cooling rate curve is
priate safety and health practices and determine the applica- obtained by calculating the first derivative (dT/dt)ofthe
bility of regulatory limitations prior to use.
cooling time - temperature curve. An example is illustrated in
Part B of Fig. 1.
2. Referenced Documents
3.1.4 heat treating oil, n—a hydrocarbon containing
2.1 ASTM Standards:
product, often derived from petroleum base stock, that is used
D1744 Test Method for Determination of Water in Liquid
to mediate heat transfer between heated metal, such as austen-
Petroleum Products by Karl Fischer Reagent
itized steel, to control the microstructure that is formed upon
E220 Test Method for Calibration of Thermocouples By
cooling and also control distortion and minimize cracking
Comparison Techniques
which may accompany the cooling process.
E230 Specification and Temperature-Electromotive Force
(EMF) Tables for Standardized Thermocouples 3.1.5 quench severity, n—the ability of a quenching medium
3 5
2.2 SAE Standards:
to extract heat from a hot metal.
AMS 5665 NickelAlloy Corrosion and Heat Resistant Bars,
Forgings and Rings
4. Summary of Test Method
2.3 Japanese Industrial Standards (JIS):
4.1 Determine the nickel alloy probe assembly’s cooling
JIS K 2242 - 1980 Heat Treating Oil
time versus temperature after placing the assembly in a furnace
JIS K 6753 - 1977 Di-2-ethylhexyl Phthalate
and heating to 850°C (1562°F) and then quenching in a heat
treating oil.The temperature inside the probe assembly and the
This test method is under the jurisdiction of ASTM Committee D02 on
cooling times are recorded at selected time intervals to estab-
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.L0.06 on Non-Lubricating Process Fluids. lish a cooling temperature versus time curve. The resulting
Current edition approved April 15, 2012. Published May 2012. Originally
cooling curve may be used to evaluate quench severity (see
approved in 1997. Last previous edition approved in 2007 as D6200–01(2007).
Note 1).
DOI: 10.1520/D6200-01R12.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
NOTE 1—For production testing, the furnace temperature of 815 to
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
857°C (1500 to 1575°F) may be used.
Standards volume information, refer to the standard’s Document Summary page on
the ASTM website.
Available from Society of Automotive Engineers (SAE), 400 Commonwealth
Dr., Warrendale, PA 15096-0001, http://www.sae.org.
4 5
Available from Japanese Standards Organization (JSA), 4-1-24 Akasaka Boyer, H. E. and Cary, P. R., Quenching and Distortion Control, ASM
Minato-Ku, Tokyo, 107-8440, Japan, http://www.jsa.or.ja. International, Materials Park, OH, 1988, p. 162.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6200 − 01 (2012)
FIG. 1 Typical Temperature/Time and Temperature/Cooling Rate Plots For Test Probe Cooled in a Quenching Oil
FIG. 2 Probe Details and General Probe Assembly
5. Significance and Use properties such as the hardness obtainable upon quenching of
ametal.Theresultsobtainedbythistestmaybeusedasaguide
5.1 This test method provides a cooling time versus tem-
perature pathway which is directly proportional to physical
D6200 − 01 (2012)
inheattreatingoilselectionorcomparisonofquenchseverities 7.5 Sample Container—A container, preferably a damage-
of different heat treating oils, new or used. resistant, tall form vessel having an internal diameter of 115 6
5 mm (4.528 6 0.197 in.) shall be selected to provide 50 mL
6. Interferences (1.97 in.) of fluid above and below the probe when quenched.
It is recommended that 2000 6 50 mL of oil be used. The
6.1 The presence of water in a heat treating oil has a major
resulting cooling curve will be dependent on the temperature
effect upon the results obtained with this test method. Water
riseduringthequenchandonthetotalfluidvolume.Therefore,
content of calibration fluids shall be confirmed byTest Method
the cooling curve analysis shall be performed with the same
D1744. If water is present above 0.01 %, the calibration fluid
volume of fluid.
shall be dried at a minimum temperature of 102°C (216°F)
7.6 Oil Temperature Measurement —Any temperature de-
until Test Method D1744 indicates water content at or below
tection device may be used that is capable of measuring oil
0.01 %.
temperature to within 61°C (1.8°F) during drying.
7. Apparatus
7.7 Timer—Graduated in seconds and minutes, and may be
part of a computer clock.
7.1 Furnace—Use a horizontal or vertical electrical resis-
tance tube-type furnace capable of maintaining a constant
8. Reagents and Materials
minimum temperature of 850°C (1562°F) over a heated length
8.1 Reference Quenching Fluid—A reference quenching
ofnotlessthan120mm(4.72in.)andaprobepositionedinthe
fluid shall be used for initial and regular system calibration.
center of the heating chamber. The furnace shall be capable of
The primary reference fluid, as described in the Wolfson
maintaining the probe’s temperature within 62.5°C (4.5°F)
Engineering Group Specification , exhibits the following cool-
over the specimen length. The furnace, that is, the radiant tube
ing characteristics:
heating media, shall be used with ambient atmosphere.
Time to cool to 600°C (1112°F) 12 - 14 s
7.2 Measurement System—The temperature-time measure-
Time to cool to 400°C (752°F) 19 - 21 s
Time to cool to 200°C (392°F) 50 - 55 s
ment system shall be a computer based data acquisition system
Cooling rate, max 47 - 53°C/s (85-95°F/s)
capable of providing a permanent record of the cooling
Temperature of the maximum cooling rate 490 - 530°C (914-986°F)
characteristics of each oil sample tested, producing a record of
Cooling rate at 300°C (572°F) 6 - 8°C/s (10.8-14.4°F/s)
variationinthetestprobeassemblyoftemperaturewithrespect
8.1.1 These characteristics are based on quenching a 2000
to time, and cooling rate with respect to temperature.
650 mL volume of the primary reference fluid in the sample
container described in 7.5 according to the procedure outlined
7.3 Probe—The probe shall be cylindrical, having a diam-
in Section 13.
eter of 12.5 60.01 mm (0.492 6 0.0004 in.) and a length of 60
8.1.2 A secondary reference fluid, such as JIS Standards
60.25 mm (2.362 6 0.01 in.) with a 1.45 to 1.65 mm (0.057
K 2242 and K 6753, may be used, provided that sufficient
to 0.065 in.) sheathed Type K thermocouple in its geometric
statistical cooling curve testing has been conducted so that
center. The probe shall be made of a nickel alloy 600 (UNS
results are traceable to the six cooling characteristics of the
N06600)purchasedtoSAESpecificationAMS5665whichhas
primary reference fluid.
a nominal composition of 76.0 % Ni, 15.5 % Cr, 8.0 % Fe,
8.1.3 The reference fluids shall be stored in a sealed
.08 % C, and .25 % max Cu. The probe shall be attached to a
container when not in use and shall be replaced after 200
support tube with a minimum length of 200 mm (7.874 in.).
quenches or two years, whichever is sooner.
The thermocouple sheathing and the support tube shall be the
same material as the probe (see Note 2). See Fig. 2 for
8.2 Cleaning Solvent—A hydrocarbon solvent that will
recommended manufacturing details.
evaporate at room temperature, leaving no residue (Warning -
Flammable. Harmful if inhaled.).
NOTE 2—Care must be taken that the probe specimen is not damaged as
surface irregularities will influence the results of the test.
8.3 Polishing Paper, 600 grit Emery.
7.4 Transfer Mechanism—One of the following shall be
8.4 Cloth, lintless and absorbent.
used to transfer the heated probe from the furnace to the test
9. Cleaning and Conditioning
fluid.
7.4.1 Automated Transfer Mechanism—The transfer from
9.1 Cleaning Used Probes—Wipeprobewithalintlesscloth
the furnace to the oil shall be completed within 3.0 s. Immerse
or absorbent paper after removal from the oil and prior to
the probe in the center, 0 to 5 mm (0 to 0.197 in.), of the heat
returning to the furnace. (Warning —The probe shall always
treating oil container to a depth where there is 50 62mm
be considered hot, as temperature below visual hot tempera-
(1.97 6 0.08 in.) of fluid above and below the probe when
tures can still cause injury to the skin (Warning—Do not use
quenched. A mechanical stop shall be used for reproducibility
cleaning solvent near the furnace opening especially with
of probe placement.
automated transfer mechanisms.).) A cleaning solvent may be
7.4.2 Manual Transfer—If manual transfer is used, the used, but care should be taken that the probe is below 50°C
(122°F).
sample container shall be equipped with a fixture to ensure
correctplacementinthecenteroftheheattreatingoilcontainer
and to the depth defined in 7.4.1. A timer shall be used to
Available from Wolfson Heat Treatment Centre, Aston University, Aston
ensure a maximum transfer time of 3.0 s. Triangle, Birmingham B4 7ET, England.
D6200 − 01 (2012)
9.2 Conditioning New Probes—Condition the probe prior to 12.1.2 Frequency of Probe Calibration—Calibratetheprobe
its initial use with any quenchant by carrying out a minimum against a reference quenching fluid before each set of test runs.
of six trial quenches, or a greater number if required to achieve
12.2 Equipment Calibration—Calibrate desired recording
consistency, using a general purpose hydrocarbon oil. Consis-
mechanism as described in Annex A1.
tencyshallmeanthelasttwotestsshallhavemaximumcooling
12.3 Total System Calibration—Calibrate the system with a
rates within 62 % in temperature and cooling rate. Clean the
reference quenching fluid (see 8.1) following the procedure
probe assembly between quenches as specified in 9.1. Quench
described in Section 13. Calibrate the system prior to using a
the probe in the reference quenching fluid and check according
new probe for testing and before and after each new set of test
to 12.3. If the probe does not meet the requirements of 12.3,
runs. The limits of the results obtained on the reference fluid
recondition according to 9.3 and then recalibrate again accord-
will be established for each reference fluid prior to use as
ing to 12.3. Do not use probes that do not meet these
described in 8.1. The limits shall include, as a minimum, the
requirements.
following values: maximum cooling rate (°C/s, °F/s), the
9.3 Probe Reconditioning—The probe shall be recondi-
temperature at the maximum cooling rate (°C, °F), cooling rate
tioned when the probe calibration according to 12.3 does not
(°C/s, °F/s) at 300°C (572°F), and the time in seconds from
meet the calibration limits, of the reference fluid. Recondition
immersion to three different temperatures such as: (a) 600°C
the probe by cleaning with emery paper. Although coarser
(1112°F), (b) 400°C (752°F), and (c) 200°C (392°F). If the
320-grit paper may be used for initial cleaning, the final finish
results deviate from the limits prescribed for each of the six
shall be provided using 600-grit emery paper. Following this
cooling characteristics of the reference fluid (8.1), the system
surface cleaning procedure, the probe shall be quenched until
shall not be considered as being in calibration. The probe may
repeatable cooling curve results of a reference oil are obtained.
need to be reconditioned (see 9.3). Alternatively, when results
9.3.1 An alternative is to recondition the probe after every
deviate from the prescribed limits, it is also appropriate to
run. Before testing a set of heat treating oils, the probe is
examine the test setup and procedure for compliance to this
quenched into the reference fluid after surface conditioning. If
standard and the manufacturer’s recommended practice.
the results comply with the limits prescribed for the reference
fluid, the probe may be used for further testing. When testing,
13. Procedure
the probe is cleaned prior to each run. After testing of the set
13.1 Place the probe in the preheated furnace. Bring the
of fluids is completed, the probe is quenched into the reference
probe temperature to the required temperature of 850 6 2°C,
fluid to ensure that it is still within calibration.
(1562 6 4°F) and soak at this temperature for at least 2 min.
10. Sampling
13.2 Transfer the probe to the center of the quench oil
10.1 Sampling shall be in accordance with 7.5. Ensure the
sample activating the data collection equipment at the same
sample is representative of the oil being tested.Aclean and dry
time. (Warning—Electric resistance type furnaces may have
sample container shall be used.
to be turned off prior to the transfer from the furnaces to the
sample when interference with the data collection device is
11. Preparation of Apparatus
noted.).
11.1 Preheat furnace to 850 6 2°C (1562 6 4°F), (1500 to
13.3 Hold the probe assembly without movement, with the
1575°F).
mechanical transfer device or a holding fixture.
11.2 Connect a dry, conditioned, calibrated
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