ASTM D6666-01
(Guide)Standard Guide for Evaluation of Aqueous Polymer Quenchants
Standard Guide for Evaluation of Aqueous Polymer Quenchants
SCOPE
1.1 This guide provides information, without specific limits, for selecting standard test methods for testing aqueous polymer quenchants for initial qualification, determining quality, and the effect of aging.
1.2 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 requirements prior to use.
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An American National Standard
Designation: D 6666 – 01
Standard Guide for
Evaluation of Aqueous Polymer Quenchants
This standard is issued under the fixed designation D 6666; 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 D 5296 Test Method for Molecular Weight Averages and
Molecular Weight Distribution of Polystyrene by High-
1.1 This guide provides information, without specific limits,
Performance Size-Exclusion Chromatography
for selecting standard test methods for testing aqueous polymer
D 6482 Test Method for Determination of Cooling Charac-
quenchants for initial qualification, determining quality, and
teristics of Aqueous Polymer Quenchants by Cooling
the effect of aging.
Curve Analysis with Agitation (Tensi Method)
1.2 This standard does not purport to address all of the
D 6549 Test Method for Determination of Cooling Charac-
safety concerns, if any, associated with its use. It is the
teristics of Quenchants by Cooling Curve Analysis with
responsibility of the user of this standard to establish appro-
Agitation (Drayton Unit)
priate safety and health practices and determine the applica-
E 70 Test Method for pH of Aqueous Solutions With the
bility of regulatory requirements prior to use.
Glass Electrode
2. Referenced Documents
E 686 Test Method for Evaluation of Antimicrobial Agents
in Aqueous Metal Working Fluids
2.1 ASTM Standards:
E 979 Test Method for Evaluation of Antimicrobial Agents
D 95 Test Method for Water in Petroleum Products and
as Preservatives for Invert Emulsion and Other Water
Bituminous Materials by Distillation
Containing Hydraulic Fluids
D 445 Test Method for Kinematic Viscosity of Transparent
and Opaque Liquids (and the Calculation of Dynamic
3. Terminology
Viscosity)
3.1 Definitions of Terms Specific to This Standard:
D 892 Test Method for Foaming Characteristics of Lubri-
3.1.1 austenite, n—solid solution of one or more elements
cating Oils
in face-centered cubic iron (gamma iron) and unless otherwise
D 1744 Test Method for Determination of Water in Liquid
designated, the solute is generally assumed to be carbon (1).
Petroleum Products by Karl Fisher Reagent
3.1.2 austenitizing, n—forming austenite by heating a fer-
D 1747 Test Method for Refractive Index of Viscous Mate-
rous alloy into the transformation range (partial austenitizing)
rials
or above the transformation range (complete austenitizing).
D 1796 Test Method for Water and Sediment in Fuel Oils by
When used without qualification, the term implies complete
the Centrifuge Method (Laboratory Procedure)
austenitizing (1).
D 2624 Test Method for Electrical Conductivity of Aviation
3.1.3 aqueous polymer quenchant, n—a solution containing
and Distillate Fuels
water, and one or more water-soluble polymers including
D 3519 Test Method for Foam in Aqueous Media (Blender
poly(alkylene glycol), poly(vinyl pyrrolidone), poly(sodium
Test)
acrylate), and poly(ethyl oxazoline) (2, 3) and additives for
D 3601 Test Method for Foam in Aqueous Media (Bottle
corrosion and foam control, if needed.
Test)
5 3.1.4 biodegradation, n—the process by which a substrate
D 3867 Test Methods for Nitrite-Nitrate in Water
is converted by biological, usually microbiological, agents into
D 3946 Test Method for Evaluating the Bacteria Resistance
4 simple, environmentally acceptable derivatives. (4)
of Water-Dilutable Metalworking Fluids
3.1.5 biodeterioration, n—loss of product quality and per-
D 4327 Test Method for Anions in Water by Chemically
5 formance and could be regarded as the initial stages of
Suppressed Ion Chromatography
biodegradation (see 3.1.4) , but in the wrong place at the wrong
time, that is when the product is stored or in use. (4)
This guide is under the jurisdiction of ASTM Committee D02 on Petroleum
Products and Lubricants and is the direct responsibility of Subcommittee
D02.L0.06on Nonlubricating Process Fluids. Annual Book of ASTM Standards, Vol 08.03.
Current edition approved May 10, 2001. Published October 2001. Annual Book of ASTM Standards, Vol 05.04.
2 8
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 015.05.
3 9
Discontinued; see 1999 Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 11.05.
4 10
Annual Book of ASTM Standards, Vol 05.02. The boldface numbers in parentheses refer to the list of references at the end
Annual Book of ASTM Standards, Vol 11.01. of this standard.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 6666
3.1.6 convective cooling, n—after continued cooling, and peratures that are important in the formation of martensitic
the interfacial temperature between the cooling metal and the microstructure of steel including: A —equilibrium austeniti-
e1
aqueous polymer quenchant is less than the boiling point of the zation phase change temperature; M —temperature at which
S
water in the quenchant solution at which point cooling occurs transformation of austenite to martensite starts during cooling
by a convective cooling process. For convective cooling, fluid and M —temperature at which transformation of austenite to
f
motion is due to density differences and the action of gravity martensite is completed during cooling. (1)
and includes both natural motion and forced circulation (1, 5).
4. Significance and Use
This process is illustrated in Fig. 1.
3.1.7 cooling curve, n—a graphical representation of the 4.1 The significance and use of each test method will
cooling time (t)—temperature (T) response of the probe such as depend on the system in use and the purpose of the test method
that shown in Fig. 1. (5) listed under Section 7. Use the most recent editions of the test
3.1.8 cooling curve analysis, n—the process of quantifying methods.
the cooling characteristics of a quenchant medium based on the
5. Quenching Process
temperature versus time profile obtained by cooling a pre-
heated metal probe assembly (see Fig. 2) under specified 5.1 Aqueous Polymer Quenchant Cooling Mechanisms—
conditions which include: probe alloy and dimensions, probe Upon initial immersion of a heated metal into a solution of an
and bath temperature, agitation rate, and aqueous polymer aqueous polymer quenchant, an insulating polymer film, which
quenchant concentration. controls the heat transfer rate from the hot metal into the cooler
3.1.9 cooling rate curve, n—obtained by calculating the first quenchant solution, forms around the hot metal which is
derivative (dT/dt) of the cooling time-temperature curve as separated by a vapor film (Fig. 3) (7) for the quenching process
illustrated in Fig. 1. (5) in a poly(alkylene glycol) quenchant. The overall heat transfer
3.1.10 dragout, n—solution carried out of a bath on the mediating properties of the film are dependent on both the film
metal being quenched and associated handling equipment. (1) thickness (a function of polymer concentration) and interfacial
3.1.11 full-film boiling, n—upon initial immersion of hot film viscosity (a function of polymer type and bath tempera-
steel into a quenchant solution, a vapor blanket surrounds the ture). The timing of film formation and subsequent film rupture
metal surface resulting in full-film boiling as shown in Fig. 1. and removal is dependent on the film strength of the polymer,
(5) agitation (both direction and mass flow), and turbulence of the
3.1.12 nucleate boiling, n—when the vapor blanket sur- polymer solution surrounding the cooling metal.
rounding the hot metal collapses and a nucleate boiling process 5.1.1 The cooling process that occurs upon initial immer-
occurs as illustrated in Fig. 1. (5) sion of the hot metal into the aqueous polymer quenchant is
3.1.13 quenchant medium, n—any liquid or gas, or mixture, full-film boiling. This is frequently referred to as the vapor
used to control the cooling of a metal to facilitate the formation blanket stage. Cooling is slowest in this region. When the metal
of the desired microstructure and properties. (1) has cooled sufficiently, the polymer film encapsulating the hot
3.1.14 quench severity, n—the ability of a quenchant me- metal ruptures and a nucleate boiling process results. The
dium to extract heat from hot metal. (6) temperature at the transition from full-film boiling to nucleate
3.1.15 transformation temperatures, n—characteristic tem- boiling is called the Leidenfrost temperature. Cooling is fastest
FIG. 1 Cooling Mechanisms of the Quenching Process
D 6666
NOTE 1—From Wolfson Engineering Group Specification, available from Wolfson Heat Treatment Centre, Aston University, Aston Triangle,
Birmingham B4 7ET, England, 1980.
FIG. 2 Schematic Illustration of the Probe Details and Probe Assembly
FIG. 3 Illustration of the Three Phases of Cooling
in this region. When the surface temperature of the cooling from top to bottom and across the tank. This means there may
metal is less than the boiling temperature of water, convective be significant variations of particulate contamination including
cooling results. All three cooling mechanisms are superim- carbon from the heat treating process and metal scale. For
posed on a cooling curve and illustrated in Fig. 3. (7) uniform sampling, a number of sampling recommendations
have been developed.
6. Sampling
6.1.1 Sampling Recommendations:
6.1 Sampling—Flow is never uniform in agitated quench 6.1.1.1 Minimum Sampling Time—The circulation pumps
tanks. There is always variation of flow rate and turbulence shall be in operation for at least 1 h prior to taking a sample
D 6666
from the quench system. cracking problems. Metal scale contamination is often identi-
6.1.1.2 Sampling Position—For each system, the well- fiable by its magnetic properties by placing a magnet on the
mixed sample shall be taken from the same position each time outside of the bottle next to the scale and determining if the
that system is sampled. The position in the tank where the scale exhibits any attraction for the magnet. Carbon, sludge,
sample is taken shall be recorded. and scale may be removed from the quenchant by filtration or
6.1.1.3 Sampling Values—If a sample is taken from a centrifugation. Alternatively, the quenchant mixture may be
sampling valve, then sufficient quenchant should be taken and allowed to settle, the quenchant solution pumped off, and the
discarded to ensure that the sampling valve and associated separated solids then removed by shoveling. The amount of
piping has been flushed before the sample is taken. insoluble suspended solids or tramp oils may be quantified by
6.1.1.4 Effect of Quenchant Addition as Make-Up due to a modification of Test Method D 1796 where the aqueous
Dragout—It is important to determine the quantity and fre- quenchant is centrifuged without further dilution as described
quency of new quenchant additions, as large additions of new in the method. The amount of tramp oil in the quenchant is
quenchant solution will have an effect on the test results, in determined from the insoluble liquid layer at the top of the
particular, the cooling curve. If a sample was taken just after a centrifuge tube and the volume of the insoluble sediment is
large addition of new quenchant, this shall be taken into taken from the bottom of the centrifuge tube.
consideration when interpreting the cooling curve for this
7.1.2 Refractive Index, (Test Method D 1747)—One of the
sample.
most common methods of monitoring the concentration of
6.1.1.5 Sampling Containers—Samples shall be collected in
aqueous polymer quenchants formulated using poly(alkylene
new containers. Under no circumstances shall used beverage or
glycol) coploymers is refractive index. As Fig. 5 (7) shows,
food containers be used because of the potential for fluid
there is a linear relationship between quenchant concentration
contamination and leakage.
and refractive index. The refractive index of the quenchant
solution is determined using an Abbé refractometer (Test
7. Recommended Test Procedures
Method D 1747) equipped with a constant temperature bath.
7.1 Performance-Related Physical and Chemical Proper- Although the refractive index could potentially be used at any
ties: temperature within the control limits of the constant tempera-
7.1.1 Appearance—Contamination of aqueous polymer ture bath, typically either 40ºC or 100ºF is selected.
quenchants by such fluids as hydraulic or quench oils may
7.1.2.1 Although refractive index is a relatively simple and
result in a non-uniform quench with thermal gradients suffi-
a rapid method for determination of polymer quenchant con-
cient to cause cracking or increased distortion, or possible
centration, it is not sensitive to low levels of polymer degra-
staining, of the metal being quenched. The simplest test (and an
dation and it is often significantly affected by solution con-
excellent test) is to examine the appearance of an aqueous
tamination.
polymer quenchant in a clear glass container, such as a bottle.
NOTE 1—Refractive index is typically unsuitable for aqueous polymer
A sample of an oil-contaminated fluid is illustrated in Fig. 4.
quenchants formulated with polymers with molecular weights greater than
(7) However, if the oil readily separates from the aqueous
50 000 to 60 000 because the total concentration is relatively low. Small
polymer quenchant solution (Fig. 4), it may be removed by
changes in polymer concentration may result even from normal use which
skimming. On the other hand, oil may form a milky-white
impart significant process effects but the corresponding variation in
emulsion which is not readily reclaimed by heat treaters.
refractive index may not be detectable.
7.1.1.1 Other problems that are easy to identify visually
NOTE 2—Although it is most desirable to use an Abbé refractometer
include carbon and sludge contamination which often results in because of its sensitivity, this is only practical in a laboratory environment.
(A) New aqueous polymer quenchant solution.
(B) Used quenchant solution with oil contamination (see separated upper layer).
FIG. 4 Sample of Oil Contaminated Aqueous Polymer Quenchant
D 6666
FIG. 5 Illustration of the Linear Relationship Between Refractive Index and Concentration
In the heat treating industry, for tankside monitoring and control, a refractometer is shown in Fig. 8. (7) Hand-held refractometers are
temperature-comp
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