1、Designation: D6482 06 (Reapproved 2011)Standard Test Method forDetermination of Cooling Characteristics of AqueousPolymer Quenchants by Cooling Curve Analysis withAgitation (Tensi Method)1This standard is issued under the fixed designation D6482; the number immediately following the designation indi
2、cates the year oforiginal adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the equipment and
3、the proce-dure for evaluation of quenching characteristics of a quenchingfluid by cooling rate determination.1.2 This test method is designed to evaluate quenchingfluids with agitation, using the Tensi agitation apparatus.1.3 The values stated in SI units are to be regarded asstandard. The values gi
4、ven in parentheses are for informationonly.1.4 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulato
5、ry limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D6200 Test Method for Determination of Cooling Charac-teristics of Quench Oils by Cooling Curve AnalysisE220 Test Method for Calibration of Thermocouples ByComparison TechniquesE230 Specification and Temperature-Electromotive For
6、ce(EMF) Tables for Standardized Thermocouples2.2 SAE Standard:3AMS 5665 NickelAlloy Corrosion and Heat Resistant Bars,Forgings and Rings2.3 Japanese Industrial Standards:4JIS K 2242 Heat Treating OilJIS K 6753 Di-2-ethylhexyl Phthalate2.4 Wolfson Engineering Group:5Wolfson Engineering Group Specific
7、ation Laboratory Testsfor Assessing the Cooling Curve of Industrial QuenchingMedia2.5 ASTM Adjuncts:6ADJD6300 D2PP, Determination of Precision and BiasData for Use in Test Methods for Petroleum Products3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 aqueous polymer quenchantan
8、 aqueous solutioncontaining a water soluble polymer; typically including poly-(alkylene glycol), poly(ethyl oxazoline), poly(solium acrylate)and poly(vinyl pyrrolidone) (1, 2).7The quenchant solutionalso typically contains additives for corrosion and foam con-trol, if needed. Quench severity of aque
9、ous polymer quen-chants is dependent on concentration and molecular weight ofthe specific polymer being evaluated, quenchant temperature,and agitation rate as shown in Figs. 1-3, respectively.3.1.2 cooling curvea graphical representation of the cool-ing time (t)-temperature (T) response of the probe
10、 (see 7.3).Anexample is illustrated in Fig. 4A.3.1.3 cooling curve analysisthe process of quantifying thecooling characteristics of a quenchant based on the temperatureversus time profile obtained by cooling a preheated metal probeassembly (see Fig. 5) under standard conditions (1, 3, 4).3.1.4 cooli
11、ng rate curveobtained by calculating the firstderivative (dT/dt) of the cooling time-temperature curve. Anexample is illustrated in Fig. 4B.3.1.5 quench severitythe ability of a quenching mediumto extract heat from a hot metal (5).3.1.6 quenchantany medium, liquid or gas that may beused to mediate h
12、eat transfer during the cooling of hot metal.4. Summary of Test Method4.1 The nickel alloy probe assemblys cooling time versustemperature is determined after placing the assembly in a1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the dire
13、ct responsibility of SubcommitteeD02.L0.06 on Non-Lubricating Process Fluids.Current edition approved May 1, 2011. Published August 2011. Originallyapproved in 1999. Last previous edition approved in 2006 as D648206. DOI:10.1520/D6482-06R11.2For referenced ASTM standards, visit the ASTM website, www
14、.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Available from SAE International (SAE), 400 Commonwealth Dr., Warrendale,PA 15096-0001, http:/www.sae.org.4Available fr
15、om Japanese Standards Organization (JSA), 4-1-24 AkasakaMinato-Ku, Tokyo, 107-8440, Japan, http:/www.jsa.or.jp.5Wolfson Heat Treatment Centre, Federation House, Vyse St., Birmingham, B186LT, UK, http:/www.sea.org.uk/whtc.6No longer available from ASTM International Headquarters.7The boldface numbers
16、 in parentheses refer to the list of references at the end ofthis standard.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.furnace and heating to 850C (1562F) and then quenchinginto an aqueous polymer quenchant solution. The temperat
17、ureinside the probe assembly and the cooling times are recorded atselected time intervals to establish a cooling temperatureversus time curve. The resulting cooling curve may be used toevaluate quench severity (see Note 1).NOTE 1For production testing, the furnace temperature of 815 to857C (1500 to
18、1575F) may be used.5. Significance and Use5.1 This test method provides a cooling time versus tem-perature pathway that is directly proportional to physicalproperties such as the hardness obtainable upon quenching ofa metal. The results obtained by this test method may be usedas a guide in quenchant
19、 selection or comparison of quenchseverities of different quenchants, new or used.6. Interferences6.1 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 methodfor aqueous polymer qu
20、enchants. Contaminants, such as water,hydraulic fluids, sludge, additive loss, and oil degradation, maysimilarly affect the cooling curve behavior of oil quenchants.7. Apparatus7.1 FurnaceUse a horizontal or vertical electrical resis-tance tube-type furnace capable of maintaining a constantFIG. 1 Il
21、lustration of the Effect of Quenchant Concentration on Cooling Curve Performance for Poly(Alkylene Glycol) Quenchant at 30Cand 0.5 m/sFIG. 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/sD6
22、482 06 (2011)2minimum temperature of 850C (1562F) over a heated lengthof not less than 120 mm (4.72 in.) and a probe positioned in thecenter of the heating chamber. The furnace shall be capable ofmaintaining the probes temperature within 62.5C (4.5F)over the specimen length. The furnace, that is, th
23、e radiant tubeheating media, shall be used with ambient atmosphere.7.2 Measurement SystemThe temperature-time measure-ment system shall be a computer based data acquisition systemcapable of providing a permanent record of the coolingcharacteristics of each oil sample tested, producing a record ofvar
24、iation in the test probe assembly of temperature with respectto time and of cooling rate with respect to temperature.7.3 Probe, shall be cylindrical, having a diameter of 12.5 60.01 mm (0.492 6 0.0004 in.) and a length of 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.)shea
25、thed type K thermocouple in its geometric center. Theprobe shall be made of a nickel alloy 600 (UNS N06600)purchased to SAE specification (see AMS 5665), that has anominal composition of 76.0 % Ni, 15.5 % Cr, 8.0 % Fe,0.08 % C, and 0.25 % maximum Cu. The probe shall beattached to a support tube with
26、 a minimum length of 200 mm(7.874 in.). The thermocouple sheathing and the support tubeshall be the same material as the probe (see Note 2). See Fig.4 for recommended manufacturing details.NOTE 2Exercise care that the probe specimen is not damaged becausesurface irregularities will influence the res
27、ults of the test.7.4 Tensi Agitation Assembly:7.4.1 Construction:7.4.1.1 The 125 by 60 by 60-mm Tensi agitation assembly isillustrated in Fig. 6. The volume of the assembly is approxi-mately 1.5 by 103m3. This assembly may be constructed fromglass or any transparent and temperature-resistant synthet
28、icmaterial that is chemically compatible with the quenchingFIG. 3 Effect of Agitation Rate Variation on Cooling Curve Performance for a 15 % Aqueous Poly(Alkylene Glycol) Quenchant Solutionat 30CA. Cooling time - temperature curve (cooling curve) B. Cooling rate - temperature curve (cooling rate cur
29、ve)FIG. 4 Typical Temperature/Time and Temperature/Cooling Rate Plots for Test Probe Cooled in Quenching OilD6482 06 (2011)3fluids to be evaluated. Alternatively, the agitation assembly,illustrated in Fig. 7, may be purchased assembled.87.4.1.2 Quenchant agitation is provided by an impellermixer. Th
30、e three-blade impeller is 50 mm in diameter with apitch setting 42 mm _ 3 0.85. The impeller is commerciallyavailable.NOTE 3This procedure is recommended for aqueous polymer quen-chants. Quench oils are not compatible with the poly(methyl methacry-late) materials used for construction of this appara
31、tus.7.4.2 CleaningThe agitation assembly shall be cleanedprior to use with a detergent solution. After cleaning, theassembly shall be rinsed with water at least three times toensure that no quenchant residue or detergent solution remains.7.4.3 Flow VelocityCorrelation of flow velocity throughthe que
32、nching chamber and impeller rotational speed for wateris illustrated in Fig. 8. Flow velocity for other fluids will varywith fluid viscosity.7.4.3.1 Impeller SpeedFluids shall be controlled by therotational speed of the impeller. Standard impeller speed of1000 r/min is recommended and is obtained fr
33、om a plot ofrevolutions per minute versus potentiometer setting as illus-trated in Fig. 9 and described as impeller speed calibration:Impeller speed shall be determined using an optical tachom-eter. Optional tachometers operate by emitting and receivinglight to and from a reflector fastened on to th
34、e impeller shaft.A typical calibration plot is illustrated in Fig. 8.NOTE 4The impeller velocity will depend to some extent on theviscosity of the quenchant solution. However, the variation was found tobe minimal over a wide range of viscosities from water to a polymerquenchant at 30 % by volume.7.4
35、.3.2 Flow DirectionThe correct fluid flow direction isillustrated in Fig. 6. However, if the wiring of the electricalmotor is reversed, it is possible that the flow direction will alsobe reversed. If this occurs, which is easily detected visually, thepolarity of the electrical motor is reversed by r
36、eversing the twowire leads to the motor.7.4.4 Fluid VolumeThe resulting cooling curve will bedependent on the temperature rise during the quench, which isdependent on the total fluid volume. Therefore, the coolingcurve analysis shall be performed with the same volume offluid. The fluid shall be leve
37、l with the lower distance ring in thesupport tube, as shown in Fig. 10.7.5 Temperature MeasurementAny temperature detectiondevice may be used that is capable of measuring quenchingfluid temperature to within 61C (1.8F).7.6 Transfer MechanismThe heated probe is transferredmanually to the Tensi agitat
38、ion assembly, which shall beequipped with a fixture to ensure correct placement in the8The sole source of supply of the Tensi agitation apparatus, fully assembled,known to the committee at this time is IVF, The Swedish Institute of ProductionEngineering Research,Argongatan 30, S-431 53 Mlndal, Swede
39、n. If you are awareof alternative suppliers, please provide this information to ASTM InternationalHeadquarters. Your comments will receive careful consideration at a meeting of theresponsible technical committee,1which you may attend.FIG. 5 Probe Details and General Probe AssemblyD6482 06 (2011)4cen
40、ter of the quenching chamber, as illustrated in Figs. 6 and 7.A timer shall be used to ensure a maximum transfer time of3.0 s.7.7 Timer, graduated in seconds and minutes, and may bepart of a computer clock.8. Reagents and Materials8.1 Reference Quenching FluidUse a reference quenchingfluid for initi
41、al and regular probe calibration to determine if theprobe will give results consistent to those obtained duringinitial break-in (see Test Method D6200). If the maximumcooling rate is greater than 63 %, the probe shall be recondi-tioned (see 9.3). Cooling curve results shall be traceable to aprimary
42、standard fluid, such as that cited in Wolfson Engineer-ing Group Specification or JIS K 2242 and JIS K 6753. Thereference fluids shall be stored in a sealed container when notin use and shall be replaced after 200 quenches or two years,whichever is sooner. Distilled or deionized water at 50C mayalso
43、 be used.NOTE 5If a reference fluid other than distilled water is used, theagitation device described here shall not be used. Instead, a suitablecompatible container consistent with the specified requirement beingfollowed shall be used.8.2 Cleaning SolventA hydrocarbon solvent that willevaporate at
44、room temperature, leaving no residue.(WarningFlammable. Harmful if inhaled.)8.3 Polishing Paper, 600 grit emery.8.4 Cloth, lintless and absorbent.9. Cleaning and Conditioning9.1 Cleaning Used ProbesWipe probe with a lintlesscloth or absorbent paper after removal from the oil and prior toreturning to
45、 the furnace. (WarningThe probe shall alwaysbe considered hot, as temperature below visual hot tempera-tures can still cause injury to the skin.) A cleaning solvent maybe used, but care should be taken that the probe is below 50CFIG. 6 Schematic Drawing of Tensi Agitation AssemblyFIG. 7 Commercially
46、 Available Tensi Agitation AssemblyFIG. 8 Correlation of Flow Velocity Through Quenching Chamberand Impeller Rotational Speed for WaterD6482 06 (2011)5(122F). (WarningDo not use cleaning solvent near thefurnace opening, especially with automated transfer mecha-nisms.)9.2 Conditioning New ProbesCondi
47、tion the probe prior toits initial use with any quenchant by carrying out a minimumof six trial quenches, or a greater number if required to achieveconsistency, using a general purpose hydrocarbon oil. Consis-tency shall mean the last two tests shall have maximum coolingrates within 62 % in temperat
48、ure and cooling rate. Clean theprobe assembly between quenches as specified in 9.1. Quenchthe probe in the reference quenching fluid and check accordingto 12.3. If the probe does not meet the requirements of 12.3,recondition according to 9.3 and then recalibrate again accord-ing to 12.3. Do not use
49、probes that do not meet theserequirements.9.3 Probe Reconditioning:9.3.1 The probe shall be reconditioned when the probecalibration according to 12.3 does not meet the calibrationlimits (63 % at the maximum cooling rate) of the referencefluid. Recondition the probe by cleaning with emery paper.Although coarser 320-grit paper may be used for initialcleaning, the final finish shall be provided using 600-grit emerypaper. Following this surface cleaning procedure, the probeshall be quenched until repeatable cooling curve results of
