ASTM D6482-06(2011)
(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)
SIGNIFICANCE AND USE
This test method provides a cooling time versus temperature pathway that is directly proportional 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 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 Tensi agitation apparatus.
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.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: D6482 − 06(Reapproved 2011)
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 D6482; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 2242Heat Treating Oil
1.1 This test method covers the equipment and the proce-
JIS K 6753Di-2-ethylhexyl Phthalate
dureforevaluationofquenchingcharacteristicsofaquenching
2.4 Wolfson Engineering Group:
fluid by cooling rate determination.
Wolfson Engineering Group Specification Laboratory Tests
1.2 This test method is designed to evaluate quenching
for Assessing the Cooling Curve of Industrial Quenching
fluids with agitation, using the Tensi agitation apparatus.
Media
2.5 ASTM Adjuncts:
1.3 The values stated in SI units are to be regarded as
ADJD6300 D2PP, Determination of Precision and Bias
standard. The values given in parentheses are for information
Data for Use in Test Methods for Petroleum Products
only.
1.4 This standard does not purport to address all of the
3. Terminology
safety concerns, if any, associated with its use. It is the
3.1 Definitions of Terms Specific to This Standard:
responsibility of the user of this standard to establish appro-
3.1.1 aqueous polymer quenchant—an aqueous solution
priate safety and health practices and determine the applica-
containing a water soluble polymer; typically including poly-
bility of regulatory limitations prior to use.
(alkylene glycol), poly(ethyl oxazoline), poly(solium acrylate)
and poly(vinyl pyrrolidone) (1, 2) . The quenchant solution
2. Referenced Documents
also typically contains additives for corrosion and foam
control, if needed. Quench severity of aqueous polymer quen-
2.1 ASTM Standards:
chants is dependent on concentration and molecular weight of
D6200Test Method for Determination of Cooling Charac-
the specific polymer being evaluated, quenchant temperature,
teristics of Quench Oils by Cooling Curve Analysis
and agitation rate as shown in Figs. 1-3, respectively.
E220Test Method for Calibration of Thermocouples By
Comparison Techniques 3.1.2 cooling curve—a graphical representation of the cool-
E230Specification and Temperature-Electromotive Force
ingtime(t)-temperature(T)responseoftheprobe(see7.3).An
(EMF) Tables for Standardized Thermocouples example is illustrated in Fig. 4A.
3.1.3 cooling curve analysis—theprocessofquantifyingthe
2.2 SAE Standard:
coolingcharacteristicsofaquenchantbasedonthetemperature
AMS 5665NickelAlloy Corrosion and Heat Resistant Bars,
versustimeprofileobtainedbycoolingapreheatedmetalprobe
Forgings and Rings
assembly (see Fig. 5) under standard conditions (1, 3, 4).
3.1.4 cooling rate curve—obtained by calculating the first
derivative (dT/dt) of the cooling time-temperature curve. An
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of example is illustrated in Fig. 4B.
Subcommittee D02.L0.06 on Non-Lubricating Process Fluids.
Current edition approved May 1, 2011. Published August 2011. Originally
approved in 1999. Last previous edition approved in 2006 as D6482–06. DOI:
10.1520/D6482-06R11. Available from Japanese Standards Organization (JSA), 4-1-24 Akasaka
For referenced ASTM standards, visit the ASTM website, www.astm.org, or Minato-Ku, Tokyo, 107-8440, Japan, http://www.jsa.or.jp.
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM WolfsonHeatTreatmentCentre,FederationHouse,VyseSt.,Birmingham,B18
Standards volume information, refer to the standard’s Document Summary page on 6LT, UK, http://www.sea.org.uk/whtc.
the ASTM website. No longer available from ASTM International Headquarters.
3 7
AvailablefromSAEInternational(SAE),400CommonwealthDr.,Warrendale, Theboldfacenumbersinparenthesesrefertothelistofreferencesattheendof
PA 15096-0001, http://www.sae.org. this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6482 − 06 (2011)
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 (Alky-
lene Glycol) Quenchant at 0.5 m/s
NOTE 1—For production testing, the furnace temperature of 815 to
3.1.5 quenchseverity—theabilityofaquenchingmediumto
857°C (1500 to 1575°F) may be used.
extract heat from a hot metal (5).
3.1.6 quenchant—any medium, liquid or gas that may be
5. Significance and Use
used to mediate heat transfer during the cooling of hot metal.
5.1 This test method provides a cooling time versus tem-
4. Summary of Test Method perature pathway that is directly proportional to physical
properties such as the hardness obtainable upon quenching of
4.1 The nickel alloy probe assembly’s cooling time versus
a metal. The results obtained by this test method may be used
temperature is determined after placing the assembly in a
as a guide in quenchant selection or comparison of quench
furnace and heating to 850°C (1562°F) and then quenching
severities of different quenchants, new or used.
into an aqueous polymer quenchant solution. The temperature
insidetheprobeassemblyandthecoolingtimesarerecordedat
6. Interferences
selected time intervals to establish a cooling temperature
versus time curve. The resulting cooling curve may be used to 6.1 The presence of contaminants, such as oil, salt, metal-
evaluate quench severity (see Note 1). working fluids, forging lubricants, and polymer degradation,
D6482 − 06 (2011)
FIG. 3 Effect of Agitation Rate Variation on Cooling Curve Performance for a 15 % Aqueous Poly(Alkylene Glycol) Quenchant Solution
at 30°C
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
may affect cooling curve results obtained by this test method capable of providing a permanent record of the cooling
foraqueouspolymerquenchants.Contaminants,suchaswater, characteristics of each oil sample tested, producing a record of
hydraulicfluids,sludge,additiveloss,andoildegradation,may variationinthetestprobeassemblyoftemperaturewithrespect
similarly affect the cooling curve behavior of oil quenchants. to time and of cooling rate with respect to temperature.
7.3 Probe, shall be cylindrical, having a diameter of 12.5 6
7. Apparatus
0.01 mm (0.492 6 0.0004 in.) and a length of 60 6 0.25 mm
7.1 Furnace—Use a horizontal or vertical electrical resis-
(2.362 6 0.01 in.) with a 1.45 to 1.65 mm (0.057 to 0.065 in.)
tance tube-type furnace capable of maintaining a constant
sheathed type K thermocouple in its geometric center. The
minimum temperature of 850°C (1562°F) over a heated length
probe shall be made of a nickel alloy 600 (UNS N06600)
ofnotlessthan120mm(4.72in.)andaprobepositionedinthe
purchased to SAE specification (see AMS 5665), that has a
center of the heating chamber. The furnace shall be capable of
nominal composition of 76.0% Ni, 15.5% Cr, 8.0% Fe,
maintaining the probe’s temperature within 62.5°C (4.5°F)
0.08% C, and 0.25% maximum Cu. The probe shall be
over the specimen length.The furnace, that is, the radiant tube
attached to a support tube with a minimum length of 200 mm
heating media, shall be used with ambient atmosphere.
(7.874 in.). The thermocouple sheathing and the support tube
7.2 Measurement System—The temperature-time measure- shall be the same material as the probe (see Note 2). See Fig.
mentsystemshallbeacomputerbaseddataacquisitionsystem 4 for recommended manufacturing details.
D6482 − 06 (2011)
FIG. 5 Probe Details and General Probe Assembly
NOTE2—Exercisecarethattheprobespecimenisnotdamagedbecause
assembly shall be rinsed with water at least three times to
surface irregularities will influence the results of the test.
ensurethatnoquenchantresidueordetergentsolutionremains.
7.4 Tensi Agitation Assembly: 7.4.3 Flow Velocity—Correlation of flow velocity through
7.4.1 Construction: the quenching chamber and impeller rotational speed for water
7.4.1.1 The125by60by60-mmTensiagitationassemblyis is illustrated in Fig. 8. Flow velocity for other fluids will vary
illustrated in Fig. 6. The volume of the assembly is approxi- with fluid viscosity.
–3 3
mately1.5by10 m .Thisassemblymaybeconstructedfrom 7.4.3.1 Impeller Speed—Fluids shall be controlled by the
glass or any transparent and temperature-resistant synthetic rotational speed of the impeller. Standard impeller speed of
material that is chemically compatible with the quenching 1000 r/min is recommended and is obtained from a plot of
fluids to be evaluated. Alternatively, the agitation assembly, revolutions per minute versus potentiometer setting as illus-
illustrated in Fig. 7, may be purchased assembled. trated in Fig. 9 and described as impeller speed calibration:
7.4.1.2 Quenchant agitation is provided by an impeller Impeller speed shall be determined using an optical tachom-
mixer. The three-blade impeller is 50 mm in diameter with a eter. Optional tachometers operate by emitting and receiving
pitch setting 42 mm ≈ _ × 0.85. The impeller is commercially light to and from a reflector fastened on to the impeller shaft.
available. A typical calibration plot is illustrated in Fig. 8.
NOTE 4—The impeller velocity will depend to some extent on the
NOTE 3—This procedure is recommended for aqueous polymer quen-
viscosity of the quenchant solution. However, the variation was found to
chants. Quench oils are not compatible with the poly(methyl methacry-
be minimal over a wide range of viscosities from water to a polymer
late) materials used for construction of this apparatus.
quenchant at 30% by volume.
7.4.2 Cleaning—The agitation assembly shall be cleaned
7.4.3.2 Flow Direction—The correct fluid flow direction is
prior to use with a detergent solution. After cleaning, the
illustrated in Fig. 6. However, if the wiring of the electrical
motorisreversed,itispossiblethattheflowdirectionwillalso
bereversed.Ifthisoccurs,whichiseasilydetectedvisually,the
The sole source of supply of the Tensi agitation apparatus, fully assembled,
known to the committee at this time is IVF, The Swedish Institute of Production
polarityoftheelectricalmotorisreversedbyreversingthetwo
EngineeringResearch,Argongatan30,S-43153Mölndal,Sweden.Ifyouareaware
wire leads to the motor.
of alternative suppliers, please provide this information to ASTM International
7.4.4 Fluid Volume—The resulting cooling curve will be
Headquarters.Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. dependent on the temperature rise during the quench, which is
D6482 − 06 (2011)
FIG. 7 Commercially Available Tensi Agitation Assembly
FIG. 6 Schematic Drawing of Tensi Agitation Assembly
dependent on the total fluid volume. Therefore, the cooling
curve analysis shall be performed with the same volume of
fluid.Thefluidshallbelevelwiththelowerdistanceringinthe
support tube, as shown in Fig. 10.
7.5 Temperature Measurement—Any temperature detection
device may be used that is capable of measuring quenching
fluid temperature to within 61°C (1.8°F).
7.6 Transfer Mechanism—The heated probe is transferred
manually to the Tensi agitation assembly, which shall be
equipped with a fixture to ensure correct placement in the
centerofthequenchingchamber,asillustratedinFigs.6and7.
FIG. 8 Correlation of Flow Velocity Through Quenching Chamber
A timer shall be used to ensure a maximum transfer time of
and Impeller Rotational Speed for Water
3.0s.
7.7 Timer, graduated in seconds and minutes, and may be
reference fluids shall be stored in a sealed container when not
part of a computer clock.
in use and shall be replaced after 200 quenches or two years,
8. Reagents and Materials
whichever is sooner. Distilled or deionized water at 50°C may
also be used.
8.1 Reference Quenching Fluid—Useareferencequenching
fluidforinitialandregularprobecalibrationtodetermineifthe
NOTE 5—If a reference fluid other than distilled water is used, the
probe will give results consistent to those obtained during
agitation device described here shall not be used. Instead, a suitable
compatible container consistent with the specified requirement being
initial break-in (see Test Method D6200). If the maximum
followed shall be used.
cooling rate is greater than 63%, the probe shall be recondi-
tioned (see 9.3). Cooling curve results shall be traceable to a 8.2 Cleaning Solvent—A hydrocarbon solvent that will
primary standard fluid, such as that cited inWolfson Engineer- evaporate at room temperature, leaving no residue.
ing Group Specification or JIS K 2242 and JIS K 6753. The (Warning—Flammable. Harmful if inhaled.)
D6482 − 06 (2011)
9.3.2 An alternative is to recondition the probe after every
run. Before testing a set of aqueous polymer quenchant
solutions, the probe is quenched into the reference fluid after
surface conditioning. If the maximum cooling rate of the
reference fluid is within 63% of the calibration limit, the
probe may be used for further testing. When testing, the probe
is cleaned prior to each run. After testing the set of fluids is
completed, the probe is quenched into the reference fluid to
ensure that it is still within calibration.
FIG. 9 Potentiometer Setting
10. Sampling
10.1 Sampling shall be in accordance with 7.5.Take care to
ensure the sample is representative of the oil being tested. Use
a clean and dry sample container.
11. Preparation of Apparatus
11.1 Preheat furnace to 815 to 857°C, (1500 to 1575°F).
11.2 Connect a dry, conditioned, calibrated probe to the
FIG. 10 Fluid Level
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
8.3 Polishing Paper, 600 grit emery.
may be trapped in the shaft packing box. If air is mixed with
8.4 Cloth, lintless and absorbent.
the fluid, test results may be influenced.
9. Cleaning and C
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