ASTM D6482-99
(Test Method)Standard Test Method for Determination of Cooling Characteristics of Aqueous Polymer Quenchants by Cooling Curve Analysis with Agitation (Tensi Method)
Standard Test Method for Determination of Cooling Characteristics of Aqueous Polymer Quenchants by Cooling Curve Analysis with Agitation (Tensi Method)
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 Tensi agitation apparatus.
1.3 The values in SI units are to be regarded as the standard. The values in parentheses are 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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Designation: D 6482 – 99 An American National Standard
Standard Test Method for
Determination of Cooling Characteristics of Aqueous
Polymer Quenchants by Cooling Curve Analysis with
Agitation (Tensi Method)
This standard is issued under the fixed designation D 6482; 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 (e) indicates an editorial change since the last revision or reapproval.
1. Scope trial Quenching Media
1.1 This test method covers the equipment and the proce-
3. Terminology
dure for evaluation of quenching characteristics of a quenching
3.1 Definitions of Terms Specific to This Standard:
fluid by cooling rate determination.
3.1.1 aqueous polymer quenchant—an aqueous solution
1.2 This test method is designed to evaluate quenching
containing a water soluble polymer; typically including poly-
fluids with agitation, using the Tensi agitation apparatus.
(alkylene glycol), poly(ethyl oxazoline), poly(solium acrylate)
1.3 The values in SI units are to be regarded as the standard.
and poly(vinyl pyrrolidone) (1,2). The quenchant solution also
The values in parentheses are for information only.
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 as shown in Figs. 1-3 respectively.
bility of regulatory limitations prior to use.
3.1.2 cooling curve—a graphical representation of the cool-
2. Referenced Documents ing time (t)-temperature (T) response of the probe (see 7.3). An
example is illustrated in Fig. 4a.
2.1 ASTM Standards:
3.1.3 cooling curve analysis—the process of quantifying the
D 6200 Test Method for Determination of Cooling Charac-
cooling characteristics of a quenchant based on the temperature
teristics of Quench Oils by Cooling Curve Analysis
versus time profile obtained by cooling a preheated metal probe
E 220 Test Method for Calibration of Thermocouples by
assembly (see Fig. 5) under standard conditions (1,3,4).
Comparison Techniques
3.1.4 cooling rate curve—obtained by calculating the first
E 230 Specification and Temperature-Electromotive Force
derivative (dT/dt) of the cooling time-temperature curve. An
(EMF) Tables for Standardized Thermocouples
example is illustrated in Fig. 4b.
2.2 SAE Standard:
3.1.5 quenchant—any medium, liquid or gas that may be
AMS 5665 Nickel Alloy Corrosion and Heat Resistant Bars,
used to mediate heat transfer during the cooling of hot metal.
Forgings and Rings
5 3.1.6 quench severity—the ability of a quenching medium
2.3 Japanese Industrial Standards:
to extract heat from a hot metal (5).
JIS K 2242 Heat Treating Oil
JIS K 6753 Di-2-ethylhexyl Phthalate
4. Summary of Test Method
2.4 Wolfson Engineering Group:
4.1 The nickel alloy probe assembly’s cooling time versus
Laboratory Tests for Assessing the Cooling Curve of Indus-
temperature is determined after placing the assembly in a
furnace and heating to 850°C (1562°F) and then quenching
This test method is under the jurisdiction of ASTM Committee D02 on
into an aqueous polymer quenchant solution. The temperature
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
inside the probe assembly and the cooling times are recorded at
D02.L06 on Nonlubricating Process Fluids.
selected time intervals to establish a cooling temperature
Current edition approved Nov. 10, 1999. Published February 2000.
Annual Book of ASTM Standards, Vol 05.04.
versus time curve. The resulting cooling curve may be used to
Annual Book of ASTM Standards, Vol 14.03.
evaluate quench severity (see Note 1).
Available from Society of Automotive Engineers, 400 Commonwealth Drive,
Warrendale, PA 15096.
NOTE 1—For production testing, the furnace temperature of 815 to
Available from Japanese Standards Association, 1-24, Akasaka 4, Minato-ku,
Tokyo 107 Japan.
Wolfson Engineering Group Specification, available from Wolfson Heat
Treatment Centre, Aston University, Aston Triangle, Birmingham B4 7ET, England, The boldface numbers in parentheses refer to the list of references at the end of
1980. this standard.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 6482
FIG. 1 Illustration of the Effect of Quenchant Concentration on Cooling Curve Performance for Poly(Alkylene Glycol) Quenchant at 30°C
and 0.5 m/s
FIG. 2 Illustration of the Effect of Bath Temperature Variation on Cooling Curve Performance for 15 % Aqueous Solution of Poly
(Alkylene Glycol) Quenchant at 0.5 m/s
857°C (1500 to 1575°F) may be used.
hydraulic fluids, sludge, additive loss, and oil degradation, may
similarly affect the cooling curve behavior of oil quenchants.
5. Significance and Use
7. Apparatus
5.1 This test method provides a cooling time versus tem-
7.1 Furnace—Use a horizontal or vertical electrical resis-
perature pathway that is directly proportional to physical
tance tube-type furnace capable of maintaining a constant
properties such as the hardness obtainable upon quenching of
minimum temperature of 850°C (1562°F) over a heated length
a metal. The results obtained by this test method may be used
of not less than 120 mm (4.72 in.) and a probe positioned in the
as a guide in quenchant selection or comparison of quench
center of the heating chamber. The furnace shall be capable of
severities of different quenchants, new or used.
maintaining the probe’s temperature within 62.5°C (4.5°F)
6. Interferences
over the specimen length. The furnace, that is, the radiant tube
6.1 The presence of contaminants, such as oil, salt, metal- heating media, shall be used with ambient atmosphere.
working fluids, forging lubricants, and polymer degradation, 7.2 Measurement System—The temperature-time measure-
may affect cooling curve results obtained by this test method ment system shall be a computer based data acquisition system
for aqueous polymer quenchants. Contaminants, such as water, capable of providing a permanent record of the cooling
D 6482
FIG. 3 Illustration of the Effect of Agitation Rate Variation on Cooling Curve Performance for 15 % Aqueous Solution of Poly (Alkylene
Glycol) Quenchant at 0.5 m/s
A. Cooling time - temperature curve (cooling curve) B. Cooling rate - temperature curve (cooling rate curve)
FIG. 4 Typical Temperature/Time and Temperature/Cooling Rate Plots for Test Probe Cooled in Quenching Oil
characteristics of each oil sample tested, producing a record of shall be the same material as the probe (see Note 2). See Fig.
variation in the test probe assembly of temperature with respect 4 for recommended manufacturing details.
to time and of cooling rate with respect to temperature.
NOTE 2—Exercise care that the probe specimen is not damaged because
7.3 Probe, shall be cylindrical, having a diameter of 12.5 6
surface irregularities will influence the results of the test.
0.01 mm (0.492 6 0.0004 in.) and a length of 60 6 0.25 mm
7.4 Tensi Agitation Assembly:
(2.362 6 0.01 in.) with a 1.45 to 1.65 mm (0.057 to 0.065 in.)
7.4.1 Construction:
sheathed type K thermocouple in its geometric center. The
probe shall be made of a nickel alloy 600 (UNS N06600) 7.4.1.1 The 125 by 60 by 60-mm Tensi agitation assembly is
purchased to SAE specification (see AMS 5665), that has a illustrated in Fig. 6. The volume of the assembly is approxi-
–3 3
nominal composition of 76.0 % Ni, 15.5 % Cr, 8.0 % Fe, mately 1.5 by 10 m . This assembly may be constructed from
0.08 % C, and 0.25 % maximum Cu. The probe shall be glass or any transparent and temperature-resistent synthetic
attached to a support tube with a minimum length of 200 mm material that is chemically compatible with the quenching
(7.874 in.). The thermocouple sheathing and the support tube fluids to be evaluated. Alternatively, the agitation assembly,
D 6482
FIG. 5 Probe Details and General Probe Assembly
illustrated in Fig. 7, may be purchased assembled. light to and from a reflector fastened on to the impeller shaft.
7.4.1.2 Quenchant agitation is provided by an impeller A typical calibration plot is illustrated in Fig. 8.
mixer. The three-blade impeller is 50 mm in diameter with a
NOTE 4—The impeller velocity will depend to some extent on the
pitch setting 42 mm ’ _ 3 0.85. The impeller is commercially
viscosity of the quenchant solution. However, the variation was found to
available.
be minimal over a wide range of viscosities from water to a polymer
quenchant at 30 % by volume.
NOTE 3—This procedure is recommended for aqueous polymer quen-
chants. Quench oils are not compatible with the poly(methyl methacry-
7.4.3.2 Flow Direction—The correct fluid flow direction is
late) materials used for construction of this apparatus.
illustrated in Fig. 6. However, if the wiring of the electrical
motor is reversed, it is possible that the flow direction will also
7.4.2 Cleaning—The agitation assembly shall be cleaned
be reversed. If this occurs, which is easily detected visually, the
prior to use with a detergent solution. After cleaning, the
polarity of the electrical motor is reversed by reversing the two
assembly shall be rinsed with water at least three times to
wire leads to the motor.
ensure that no quenchant residue or detergent solution remains.
7.4.4 Fluid Volume—The resulting cooling curve will be
7.4.3 Flow Velocity—Correlation of flow velocity through
dependent on the temperature rise during the quench, which is
the quenching chamber and impeller rotational speed for water
dependent on the total fluid volume. Therefore, the cooling
is illustrated in Fig. 8. Flow velocity for other fluids will vary
curve analysis shall be performed with the same volume of
with fluid viscosity.
fluid. The fluid shall be level with the lower distance ring in the
7.4.3.1 Impeller Speed—Fluids shall be controlled by the
support tube, as shown in Fig. 10.
rotational speed of the impeller. Standard impeller speed of
7.5 Temperature Measurement—Any temperature detection
1000 r/min is recommended and is obtained from a plot of
device may be used that is capable of measuring quenching
revolutions per minute versus potentiometer setting as illus-
fluid temperature to within 61°C (1.8°F).
trated in Fig. 9 and described as impeller speed calibration:
7.6 Transfer Mechanism—The heated probe is transferred
Impeller speed shall be determined using an optical tachom-
manually to the Tensi agitation assembly, which shall be
eter. Optional tachometers operate by emitting and receiving
equipped with a fixture to ensure correct placement in the
The Tensi agitation apparatus is available fully assembled from IVF, Swedish
Institute of Production Engineering Research, Argongatan 30, S-431 53, Molndal, One source of these impellers, part No. 1472, is Fa. Robbe, D-36355,
Sweden. Grebenhain, Germany.
D 6482
FIG. 7 Commercially Available Tensi Agitation Assembly
FIG. 6 Schematic Drawing of Tensi Agitation Assembly
center of the quenching chamber, as illustrated in Figs. 6 and 7.
A timer shall be used to ensure a maximum transfer time of 3.0
s.
7.7 Timer, graduated in seconds and minutes, and may be
part of a computer clock.
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. If the maximum cooling rate is greater than
63 %, the probe shall be reconditioned (see 9.3). Cooling
FIG. 8 Correlation of Flow Velocity Through Quenching Chamber
curve results shall be traceable to a primary standard fluid, such
and Impeller Rotational Speed for Water
as that cited in Wolfson Engineering Group Specification or JIS
K 2242 and JIS K 6753. The reference fluids shall be stored in
8.4 Cloth, lintless and absorbent.
a sealed container when not in use and shall be replaced after
200 quenches or two years, whichever is sooner. Distilled or
9. Cleaning and Conditioning
deionized water at 50°C may also be used.
9.1 Cleaning Used Probes—Wipe probe with a lintless
cloth or absorbent paper after removal from the oil and prior to
NOTE 5—If a reference fluid other than distilled water is used, the
agitation device described here shall not be used. Instead, a suitable returning to the furnace. (Warning—The probe shall always
compatible container consistent with the specified requirement being
be considered hot, as temperature below visual hot tempera-
followed shall be used.
tures can still cause injury to the skin.) A cleaning solvent may
8.2 Cleaning Solvent—A hydrocarbon solvent that will be used, but care should be taken that the probe is below 50°C
evaporate at room temperature, leaving no residue. (122°F). (Warning—Do not use cleaning solvent near the
(Warning—Flammable. Harmful if inhaled.) furnace opening, especially with automated transfer mecha-
8.3 Polishing Paper, 600 grit emery. nisms.)
D 6482
11.2 Connect a dry, conditioned, calibrated probe to the
transfer mechanism in accordance with equipment manufac-
turer’s instructions.
11.3 Removal of Air—After filling the apparatus with the
quenchant to be tested, tilt to both sides to release any air that
may be trapped in the shaft packing box. If air is mixed with
the fluid, test results may be influenced.
11.4 The aqueous polymer quenchant shall be heated or
cooled to the desired temperature if production testing is being
performed, or to 40 6 2°C (104 6 3.6°F) if the reference
FIG. 9 Potentiometer Setting
quenching fluid is being tested. Continuously agitate the test
sample when heating.
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 thermo-
couple 30 mm (1.181 in.) from the end of the probe. Heat the
FIG. 10 Fluid Level
probe and calibrated thermocouple to the selected furnace
temperature of 845 to 855°C (1553 to 1571°F), and allow to
9.2 Conditioning New Probes—Condition the probe prior to
equalize. Compare the outputs of both the furnace and probe
its initial use
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