1、Designation: D 6666 04 (Reapproved 2009)Standard Guide forEvaluation of Aqueous Polymer Quenchants1This standard is issued under the fixed designation D 6666; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last revisio
2、n. 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 guide provides information, without specific limits,for selecting standard test methods for testing aqueous polymerquenchants
3、 for initial qualification, determining quality, andthe effect of aging.1.2 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 t
4、he applica-bility of regulatory requirements prior to use.2. Referenced Documents2.1 ASTM Standards:2D95 Test Method for Water in Petroleum Products andBituminous Materials by DistillationD 445 Test Method for Kinematic Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-it
5、y)D 892 Test Method for Foaming Characteristics of Lubri-cating OilsD 1744 Standard Test Method for Determination of Water inLiquid Petroleum Products by Karl Fischer Reagent3D 1747 Test Method for Refractive Index of Viscous Mate-rialsD 1796 Test Method for Water and Sediment in Fuel Oils bythe Cen
6、trifuge Method (Laboratory Procedure)D 2624 Test Methods for Electrical Conductivity of Avia-tion and Distillate FuelsD 3519 Test Method for Foam in Aqueous Media (BlenderTest)D 3601 Test Method for Foam In Aqueous Media (BottleTest)D 3867 Test Methods for Nitrite-Nitrate in WaterD 4327 Test Method
7、for Anions in Water by ChemicallySuppressed Ion ChromatographyD 5296 Test Method for Molecular Weight Averages andMolecular Weight Distribution of Polystyrene by HighPerformance Size-Exclusion ChromatographyD 6482 Test Method for Determination of Cooling Charac-teristics of Aqueous Polymer Quenchant
8、s by CoolingCurve Analysis with Agitation (Tensi Method)D 6549 Test Method for Determination of Cooling Charac-teristics of Quenchants by Cooling Curve Analysis withAgitation (Drayton Unit)E70 Test Method for pH of Aqueous Solutions With theGlass ElectrodeE 979 Practice for Evaluation of Antimicrobi
9、al Agents asPreservatives for Invert Emulsion and Other Water Con-taining Hydraulic FluidsE 2275 Practice for Evaluating Water-Miscible Metalwork-ing Fluid Bioresistance and Antimicrobial Pesticide Per-formance3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 austenite, nsolid s
10、olution of one or more elementsin face-centered cubic iron (gamma iron) and unless otherwisedesignated, the solute is generally assumed to be carbon (1).43.1.2 austenitizing, nforming austenite by heating a fer-rous alloy into the transformation range (partial austenitizing)or above the transformati
11、on range (complete austenitizing).When used without qualification, the term implies completeaustenitizing (1).3.1.3 aqueous polymer quenchant, na solution containingwater, and one or more water-soluble polymers includingpoly(alkylene glycol), poly(vinyl pyrrolidone), poly(sodiumacrylate), and poly(e
12、thyl oxazoline) (2, 3) and additives forcorrosion and foam control, if needed.3.1.4 biodegradation, nthe process by which a substrateis converted by biological, usually microbiological, agents intosimple, environmentally acceptable derivatives. (4)3.1.5 biodeterioration, nloss of product quality and
13、 per-formance and could be regarded as the initial stages ofbiodegradation (see 3.1.4) , but in the wrong place at the wrongtime, that is when the product is stored or in use. (4)3.1.6 convective cooling, nafter continued cooling, andthe interfacial temperature between the cooling metal and the1This
14、 guide is under the jurisdiction of ASTM Committee D02 on PetroleumProducts and Lubricants and is the direct responsibility of Subcommittee D02.L0.06on Non-Lubricating Process Fluids.Current edition approved April 15, 2009. Published July 2009. Originallyapproved in 2001. Last previous edition appro
15、ved in 2004 as D 6666 04.2For 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.4The boldface numbers in
16、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.aqueous polymer quenchant is less than the boiling point of thewater in the quenchant solution at which point cool
17、ing occursby a convective cooling process. For convective cooling, fluidmotion is due to density differences and the action of gravityand includes both natural motion and forced circulation (1, 5).This process is illustrated in Fig. 1.3.1.7 cooling curve, na graphical representation of thecooling ti
18、me (t)temperature (T) response of the probe such asthat shown in Fig. 1. (5)3.1.8 cooling curve analysis, nthe process of quantifyingthe cooling characteristics of a quenchant medium based on thetemperature versus time profile obtained by cooling a pre-heated metal probe assembly (see Fig. 2) under
19、specifiedconditions which include: probe alloy and dimensions, probeand bath temperature, agitation rate, and aqueous polymerquenchant concentration.3.1.9 cooling rate curve, nobtained by calculating the firstderivative (dT/dt) of the cooling time-temperature curve asillustrated in Fig. 1. (5)3.1.10
20、 dragout, nsolution carried out of a bath on themetal being quenched and associated handling equipment. (1)3.1.11 full-film boiling, nupon initial immersion of hotsteel into a quenchant solution, a vapor blanket surrounds themetal surface resulting in full-film boiling as shown in Fig. 1.(5)3.1.12 n
21、ucleate boiling, nwhen the vapor blanket sur-rounding the hot metal collapses and a nucleate boiling processoccurs as illustrated in Fig. 1. (5)3.1.13 quenchant medium, nany liquid or gas, or mixture,used to control the cooling of a metal to facilitate the formationof the desired microstructure and
22、properties. (1)3.1.14 quench severity, nthe ability of a quenchant me-dium to extract heat from hot metal. (6)3.1.15 transformation temperatures, ncharacteristic tem-peratures that are important in the formation of martensiticmicrostructure of steel including: Ae1equilibrium austeniti-zation phase c
23、hange temperature; MStemperature at whichtransformation of austenite to martensite starts during coolingand Mftemperature at which transformation of austenite tomartensite is completed during cooling. (1)4. Significance and Use4.1 The significance and use of each test method willdepend on the system
24、 in use and the purpose of the test methodlisted under Section 7. Use the most recent editions of the testmethods.5. Quenching Process5.1 Aqueous Polymer Quenchant Cooling MechanismsUpon initial immersion of a heated metal into a solution of anaqueous polymer quenchant, an insulating polymer film, w
25、hichcontrols the heat transfer rate from the hot metal into the coolerquenchant solution, forms around the hot metal which isseparated by a vapor film (Fig. 3) (7) for the quenching processin a poly(alkylene glycol) quenchant. The overall heat transfermediating properties of the film are dependent o
26、n both the filmthickness (a function of polymer concentration) and interfacialfilm viscosity (a function of polymer type and bath tempera-ture). The timing of film formation and subsequent film ruptureand removal is dependent on the film strength of the polymer,agitation (both direction and mass flo
27、w), and turbulence of thepolymer solution surrounding the cooling metal.5.1.1 The cooling process that occurs upon initial immer-sion of the hot metal into the aqueous polymer quenchant isfull-film boiling. This is frequently referred to as the vaporblanket stage. Cooling is slowest in this region.
28、When the metalhas cooled sufficiently, the polymer film encapsulating the hotmetal ruptures and a nucleate boiling process results. Thetemperature at the transition from full-film boiling to nucleateboiling is called the Leidenfrost temperature. Cooling is fastestin this region. When the surface tem
29、perature of the coolingmetal is less than the boiling temperature of water, convectiveFIG. 1 Cooling Mechanisms of the Quenching ProcessD 6666 04 (2009)2cooling results. All three cooling mechanisms are superim-posed on a cooling curve and illustrated in Fig. 3. (7)6. Sampling6.1 SamplingFlow is nev
30、er uniform in agitated quenchtanks. There is always variation of flow rate and turbulencefrom top to bottom and across the tank. This means there maybe significant variations of particulate contamination includingcarbon from the heat treating process and metal scale. Foruniform sampling, a number of
31、 sampling recommendationshave been developed.NOTEFrom Wolfson Engineering Group Specification, available from Wolfson Heat Treatment Centre,Aston University,Aston Triangle, BirminghamB4 7ET, England, 1980.FIG. 2 Schematic Illustration of the Probe Details and Probe AssemblyFIG. 3 Illustration of the
32、 Three Phases of CoolingD 6666 04 (2009)36.1.1 Sampling Recommendations:6.1.1.1 Minimum Sampling TimeThe circulation pumpsshall be in operation for at least 1 h prior to taking a samplefrom the quench system.6.1.1.2 Sampling PositionFor each system, the well-mixed sample shall be taken from the same
33、 position each timethat system is sampled. The position in the tank where thesample is taken shall be recorded.6.1.1.3 Sampling ValuesIf a sample is taken from asampling valve, then sufficient quenchant should be taken anddiscarded to ensure that the sampling valve and associatedpiping has been flus
34、hed before the sample is taken.6.1.1.4 Effect of Quenchant Addition as Make-Up due toDragoutIt is important to determine the quantity and fre-quency of new quenchant additions, as large additions of newquenchant solution will have an effect on the test results, inparticular, the cooling curve. If a
35、sample was taken just after alarge addition of new quenchant, this shall be taken intoconsideration when interpreting the cooling curve for thissample.6.1.1.5 Sampling ContainersSamples shall be collected innew containers. Under no circumstances shall used beverage orfood containers be used because
36、of the potential for fluidcontamination and leakage.7. Recommended Test Procedures7.1 Performance-Related Physical and Chemical Proper-ties:7.1.1 AppearanceContamination of aqueous polymerquenchants by such fluids as hydraulic or quench oils mayresult in a non-uniform quench with thermal gradients s
37、uffi-cient to cause cracking or increased distortion, or possiblestaining, of the metal being quenched. The simplest test (and anexcellent test) is to examine the appearance of an aqueouspolymer quenchant in a clear glass container, such as a bottle.A sample of an oil-contaminated fluid is illustrat
38、ed in Fig. 4.(7) However, if the oil readily separates from the aqueouspolymer quenchant solution (Fig. 4), it may be removed byskimming. On the other hand, oil may form a milky-whiteemulsion which is not readily reclaimed by heat treaters.7.1.1.1 Other problems that are easy to identify visuallyinc
39、lude carbon and sludge contamination which often results incracking problems. Metal scale contamination is often identi-fiable by its magnetic properties by placing a magnet on theoutside of the bottle next to the scale and determining if thescale exhibits any attraction for the magnet. Carbon, slud
40、ge,and scale may be removed from the quenchant by filtration orcentrifugation. Alternatively, the quenchant mixture may beallowed to settle, the quenchant solution pumped off, and theseparated solids then removed by shoveling. The amount ofinsoluble suspended solids or tramp oils may be quantified b
41、ya modification of Test Method D 1796 where the aqueousquenchant is centrifuged without further dilution as describedin the method. The amount of tramp oil in the quenchant isdetermined from the insoluble liquid layer at the top of thecentrifuge tube and the volume of the insoluble sediment istaken
42、from the bottom of the centrifuge tube.7.1.2 Refractive Index, (Test Method D 1747)One of themost common methods of monitoring the concentration ofaqueous polymer quenchants formulated using poly(alkyleneglycol) coploymers is refractive index. As Fig. 5 (7) shows,there is a linear relationship betwe
43、en quenchant concentrationand refractive index. The refractive index of the quenchantsolution is determined using an Abb refractometer (TestMethod D 1747) equipped with a constant temperature bath.Although the refractive index could potentially be used at anytemperature within the control limits of
44、the constant tempera-ture bath, typically either 40C or 100F is selected.7.1.2.1 Although refractive index is a relatively simple anda rapid method for determination of polymer quenchant con-centration, it is not sensitive to low levels of polymer degra-dation and it is often significantly affected
45、by solution con-tamination.NOTE 1Refractive index is typically unsuitable for aqueous polymerquenchants formulated with polymers with molecular weights greater than50 000 to 60 000 because the total concentration is relatively low. Smallchanges in polymer concentration may result even from normal us
46、e whichimpart significant process effects but the corresponding variation inrefractive index may not be detectable.NOTE 2Although it is most desirable to use an Abb refractometer(A) New aqueous polymer quenchant solution.(B) Used quenchant solution with oil contamination (see separated upper layer).
47、FIG. 4 Sample of Oil Contaminated Aqueous Polymer QuenchantD 6666 04 (2009)4because of its sensitivity, this is only practical in a laboratory environment.In the heat treating industry, for tankside monitoring and control, atemperature-compensated handheld refractometer (similar to the oneillustrate
48、d in Fig. 6) is used. The hand-held refractometer is self-compensated for temperatures between 60 and 100F. Although there arevarious models available, the most common models provide arbitraryrefractive index readings in Brix units overa0to30range. Typically, thesmallest scale that can be read direc
49、tly is in divisions of 0.2 as shown inFig. 7. A concentration-refractive index curve obtained by a hand-heldrefractometer is shown in Fig. 8. (7) Hand-held refractometers areavailable whose scale readings correlate directly to the concentration ofthe polymer quenchant being used. This is particularly convenient forindustrial tank-side use. However, since refractive index varies withcontamination (such as dissolved salts) that may accumulate fromevaporation of hard water, the actual quenchant concentration shall beverified periodically by oth
