1、Designation: D6200 01 (Reapproved 2012)Standard Test Method forDetermination of Cooling Characteristics of Quench Oils byCooling Curve Analysis1This standard is issued under the fixed designation D6200; the number immediately following the designation indicates the year oforiginal adoption or, in th
2、e 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 describes the equipment and theprocedure for evaluation of a quenchin
3、g oils quenchingcharacteristics by cooling rate determination.1.2 This test is designed to evaluate quenching oils in anon-agitated system. There is no correlation between these testresults and the results obtained in agitated systems.1.3 The values in SI units are to be regarded as the standard.The
4、 values in parentheses are provided for information only.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-bili
5、ty of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D1744 Test Method for Determination of Water in LiquidPetroleum Products by Karl Fischer Reagent3E220 Test Method for Calibration of Thermocouples ByComparison TechniquesE230 Specification and Temperature-Electromot
6、ive Force(EMF) Tables for Standardized Thermocouples2.2 SAE Standards:4AMS 5665 NickelAlloy Corrosion and Heat Resistant Bars,Forgings and Rings2.3 Japanese Industrial Standards (JIS):5JIS K 2242 - 1980 Heat Treating OilJIS K 6753 - 1977 Di-2-ethylhexyl Phthalate3. Terminology3.1 Definitions of Term
7、s Specific to This Standard:3.1.1 cooling curve, nthe cooling curve is a graphicalrepresentation of the cooling time (t) - temperature (T) re-sponse of the probe (see 7.3). An example is illustrated in PartBofFig. 1.3.1.2 cooling curve analysis, nthe process of quantifyingthe cooling characteristics
8、 of a heat treating oil based on thetemperature versus time profile obtained by cooling a pre-heated metal probe assembly (see Fig. 2) under standardconditions.3.1.3 cooling rate curve, nThe cooling rate curve isobtained by calculating the first derivative (dT/dt)ofthecooling time - temperature curv
9、e. An example is illustrated inPart B of Fig. 1.3.1.4 heat treating oil, na hydrocarbon containing prod-uct, often derived from petroleum base stock, that is used tomediate heat transfer between heated metal, such as austen-itized steel, to control the microstructure that is formed uponcooling and a
10、lso control distortion and minimize crackingwhich may accompany the cooling process.3.1.5 quench severity, nthe ability of a quenching me-dium to extract heat from a hot metal.64. Summary of Test Method4.1 Determine the nickel alloy probe assemblys coolingtime versus temperature after placing the as
11、sembly in a furnaceand heating to 850C (1562F) and then quenching in a heattreating oil. The temperature inside the probe assembly and thecooling times are recorded at selected time intervals to estab-lish a cooling temperature versus time curve. The resultingcooling curve may be used to evaluate qu
12、ench severity (seeNote 1).NOTE 1For production testing, the furnace temperature of 815 to857C (1500 to 1575F) may be used.5. Significance and Use5.1 This test method provides a cooling time versus tem-perature pathway which is directly proportional to physical1This test method is under the jurisdict
13、ion of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.L0.06 on Non-Lubricating Process Fluids.Current edition approved April 15, 2012. Published May 2012. Originallyapproved in 1997. Last previous edition approved in 2007 as D620001(2007).D
14、OI: 10.1520/D6200-01R12.2For referenced ASTM standards, visit the ASTM website, www.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.3Withdrawn. The last approved version
15、 of this historical standard is referencedon www.astm.org.4Available from Society of Automotive Engineers (SAE), 400 CommonwealthDr., Warrendale, PA 15096-0001, http:/www.sae.org.5Available from Japanese Standards Organization (JSA), 4-1-24 AkasakaMinato-Ku, Tokyo, 107-8440, Japan, http:/www.jsa.or.
16、ja.6Boyer, H. E. and Cary, P. R., Quenching and Distortion Control, ASMInternational, Materials Park, OH, 1988, p. 162.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.properties such as the hardness obtainable upon quenching ofa meta
17、l. The results obtained by this test may be used as a guidein heat treating oil selection or comparison of quench severitiesof different heat treating oils, new or used.FIG. 1 Typical Temperature/Time and Temperature/Cooling Rate Plots For Test Probe Cooled in a Quenching OilFIG. 2 Probe Details and
18、 General Probe AssemblyD6200 01 (2012)26. Interferences6.1 The presence of water in a heat treating oil has a majoreffect upon the results obtained with this test method. Watercontent of calibration fluids shall be confirmed by Test MethodD1744. If water is present above 0.01 %, the calibration flui
19、dshall be dried at a minimum temperature of 102C (216F)until Test Method D1744 indicates water content at or below0.01 %.7. Apparatus7.1 FurnaceUse a horizontal or vertical electrical resis-tance tube-type furnace capable of maintaining a constantminimum temperature of 850C (1562F) over a heated len
20、gthof 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, the radiant tubeheating media, shall be used with ambient atmosphere.
21、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 ofvariation in the test probe assembly of temperature with respectto tim
22、e, and cooling rate with respect to temperature.7.3 ProbeThe probe shall be cylindrical, having a diam-eter of 12.5 60.01 mm (0.492 6 0.0004 in.) and a length of 6060.25 mm (2.362 6 0.01 in.) with a 1.45 to 1.65 mm (0.057to 0.065 in.) sheathed Type K thermocouple in its geometriccenter. The probe sh
23、all be made of a nickel alloy 600 (UNSN06600) purchased to SAE SpecificationAMS 5665 which hasa nominal composition of 76.0 % Ni, 15.5 % Cr, 8.0 % Fe,.08 % C, and .25 % max Cu. The probe shall be attached to asupport tube with a minimum length of 200 mm (7.874 in.).The thermocouple sheathing and the
24、 support tube shall be thesame material as the probe (see Note 2). See Fig. 2 forrecommended manufacturing details.NOTE 2Care must be taken that the probe specimen is not damaged assurface irregularities will influence the results of the test.7.4 Transfer MechanismOne of the following shall beused t
25、o transfer the heated probe from the furnace to the testfluid.7.4.1 Automated Transfer MechanismThe transfer fromthe furnace to the oil shall be completed within 3.0 s. Immersethe probe in the center, 0 to 5 mm (0 to 0.197 in.), of the heattreating oil container to a depth where there is 50 6 2mm(1.
26、97 6 0.08 in.) of fluid above and below the probe whenquenched. A mechanical stop shall be used for reproducibilityof probe placement.7.4.2 Manual TransferIf manual transfer is used, thesample container shall be equipped with a fixture to ensurecorrect placement in the center of the heat treating oi
27、l containerand to the depth defined in 7.4.1. A timer shall be used toensure a maximum transfer time of 3.0 s.7.5 Sample ContainerA container, preferably a damage-resistant, tall form vessel having an internal diameter of 115 65 mm (4.528 6 0.197 in.) shall be selected to provide 50 mL(1.97 in.) of
28、fluid above and below the probe when quenched.It is recommended that 2000 6 50 mL of oil be used. Theresulting cooling curve will be dependent on the temperaturerise during the quench and on the total fluid volume. Therefore,the cooling curve analysis shall be performed with the samevolume of fluid.
29、7.6 Oil Temperature MeasurementAny temperature de-tection device may be used that is capable of measuring oiltemperature to within 61C (1.8F) during drying.7.7 TimerGraduated in seconds and minutes, and may bepart of a computer clock.8. Reagents and Materials8.1 Reference Quenching FluidA reference
30、quenchingfluid shall be used for initial and regular system calibration.The primary reference fluid, as described in the WolfsonEngineering Group Specification7, exhibits the following cool-ing characteristics:Time to cool to 600C (1112F) 12 - 14 sTime to cool to 400C (752F) 19 - 21 sTime to cool to
31、 200C (392F) 50 - 55 sCooling rate, max 47 - 53C/s (85-95F/s)Temperature of the maximum cooling rate 490 - 530C (914-986F)Cooling rate at 300C (572F) 6 - 8C/s (10.8-14.4F/s)8.1.1 These characteristics are based on quenching a 2000650 mL volume of the primary reference fluid in the samplecontainer de
32、scribed in 7.5 according to the procedure outlinedin Section 13.8.1.2 A secondary reference fluid, such as JIS StandardsK 2242 and K 6753, may be used, provided that sufficientstatistical cooling curve testing has been conducted so thatresults are traceable to the six cooling characteristics of thep
33、rimary reference fluid.8.1.3 The reference fluids shall be stored in a sealedcontainer when not in use and shall be replaced after 200quenches or two years, whichever is sooner.8.2 Cleaning SolventA hydrocarbon solvent that willevaporate at room temperature, leaving no residue (Warning -Flammable. H
34、armful 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 the furnace. (WarningThe probe shall alwaysbe considere
35、d hot, as temperature below visual hot tempera-tures can still cause injury to the skin (WarningDo not usecleaning solvent near the furnace opening especially withautomated transfer mechanisms.).) A cleaning solvent may beused, but care should be taken that the probe is below 50C(122F).9.2 Condition
36、ing New ProbesCondition 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 with
37、in 62 % in temperature and cooling rate. Clean the7Available from Wolfson Heat Treatment Centre, Aston University, AstonTriangle, Birmingham B4 7ET, England.D6200 01 (2012)3probe assembly between quenches as specified in 9.1. Quenchthe probe in the reference quenching fluid and check accordingto 12.
38、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 probes that do not meet theserequirements.9.3 Probe ReconditioningThe probe shall be recondi-tioned when the probe calibration according to 12.3 does notmeet
39、the calibration limits, of the reference fluid. Reconditionthe probe by cleaning with emery paper. Although coarser320-grit paper may be used for initial cleaning, the final finishshall be provided using 600-grit emery paper. Following thissurface cleaning procedure, the probe shall be quenched unti
40、lrepeatable cooling curve results of a reference oil are obtained.9.3.1 An alternative is to recondition the probe after everyrun. Before testing a set of heat treating oils, the probe isquenched into the reference fluid after surface conditioning. Ifthe results comply with the limits prescribed for
41、 the referencefluid, the probe may be used for further testing. When testing,the probe is cleaned prior to each run. After testing of the setof fluids is completed, the probe is quenched into the referencefluid to ensure that it is still within calibration.10. Sampling10.1 Sampling shall be in accor
42、dance with 7.5. Ensure thesample is representative of the oil being tested.Aclean and drysample container shall be used.11. Preparation of Apparatus11.1 Preheat furnace to 850 6 2C (1562 6 4F), (1500 to1575F).11.2 Connect a dry, conditioned, calibrated probe to thetransfer mechanism according to equ
43、ipment manufacturersinstructions.11.3 Heat fluid to the desired temperature, if productiontesting is being performed or to 40 6 1C (104 6 1.8F) if thereference quenching fluid is being tested. Continuously agitatethe test sample when heating and remove stirring mechanismprior to start of test.12. Ca
44、libration and Standardization12.1 Probe:12.1.1 Check the accuracy of the probe thermocouple byattaching a previously calibrated thermocouple to the outersurface of the probe. Locate the tip of the calibrated thermo-couple 30 mm (1.181 in.) from the end of the probe. Heat theprobe and calibrated ther
45、mocouple to the selected furnacetemperature of 850 6 2C (1562 6 4F) and allow to equalize.Compare the outputs of both the furnace and probe thermo-couples by any calibrated temperature measuring device ca-pable of required accuracy as described in Specifications E220and E230.12.1.2 Frequency of Prob
46、e CalibrationCalibrate theprobe against a reference quenching fluid before each set of testruns.12.2 Equipment CalibrationCalibrate desired recordingmechanism as described in Annex A1.12.3 Total System CalibrationCalibrate the system with areference quenching fluid (see 8.1) following the procedured
47、escribed in Section 13. Calibrate the system prior to using anew probe for testing and before and after each new set of testruns. The limits of the results obtained on the reference fluidwill be established for each reference fluid prior to use asdescribed in 8.1. The limits shall include, as a mini
48、mum, thefollowing values: maximum cooling rate (C/s, F/s), thetemperature at the maximum cooling rate (C, F), cooling rate(C/s, F/s) at 300C (572F), and the time in seconds fromimmersion to three different temperatures such as: (a) 600C(1112F), (b) 400C (752F), and (c) 200C (392F). If theresults dev
49、iate from the limits prescribed for each of the sixcooling characteristics of the reference fluid (8.1), the systemshall not be considered as being in calibration. The probe mayneed to be reconditioned (see 9.3). Alternatively, when resultsdeviate from the prescribed limits, it is also appropriate toexamine the test setup and procedure for compliance to thisstandard and the manufacturers recommended practice.13. Procedure13.1 Place the probe in the preheated furnace. Bring theprobe temperature to the
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