Quenching Control and Distortion, September 9–13, 2012, Chicago, Illinois, USA Copyright © 2012 ASM International®

Proceedings from the 6th International Quencing and Control of Distortion Conference All rights reserved
Including the 4th International Distortion Engineering Conference www.asminternational.org
D. Scott MacKenzie, editor

Effect of Contamination on the Cooling Rate of Quench Oils

D. Scott MacKenzie, Gloria Graham, J. Jankowski
Houghton International, Inc., Valley Forge, PA USA

Keywords: Quenching, Oil, Heat Transfer, Cooling Curve

Abstract

Modern quench oils offer a wide range of capability and performance. However,
contamination of quench oils can markedly affect their performance. This effect can result in
fire, spotty work, cracking, distortion and potentially injury or property damage. This paper
examines the effect of several common contaminants on the quenching performance of
premium medium speed oil. Contaminants examined include water, hydraulic fluid, soot, and
heat treating salts, as well as the effects of temperature and aging. The effect of each of these
contaminants on the cooling curve of medium speed oil is illustrated.

Introduction

A high performance quench oil must be oxidation-resistant (low sludge formation),

non-staining, have an elevated flash point and acceptable heat transfer characteristics [1].
Most modern quench oils are based on refined petroleum base stocks. The use of higher
fractions of napthenic compounds will result in lower flash points and greater sludge
formation [2]. The presence of sludge reduces the oil’s heat transfer efficiency, which can
produce inadequately hardened parts. Sludge is the result of oxidation and polymerization of
quench oils while in use [3]. In general, the higher the sludge content, the older the quench
oil is.
Quench oil should not stain parts. Paraffinic oils impart a light gray color to quenched
parts. If the oils contain sulfur, unacceptable black stains can appear. While sulfur is usually
removed in the refining process, it is possible that sulfur-containing compounds (such as
lubricants) can contaminate the oil and create problems with staining.
Quench oils should not catch fire during use. The flash point of oil is a measure of the
tendency of the oil to catch fire. An elevated flash point minimizes the tendency of the oil to
catch fire during use. As indicated earlier, the use of larger fractions of napthenic compounds
(greater amounts of napthenic compounds?) results in lower flash points, which increases the
tendency of quench oils to catch fire during use.
Quench oils should be selected on the basis of their heat transfer characteristics.
Typically, quench oils are classified into three groups [1] [4] [5] [6] [7] [8]: fast, accelerated
oils, medium speed or conventional oils, and mar-quenching or hot oils. Fast, accelerated oils
usually are formulated from mineral oils, and contain additives to increase the quenching

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speed. Medium speed or conventional oils usually are mineral oils, also. These quench oils
contain anti-oxidation agents to reduce the rate of sludge formation and thermal degradation.
Mar-tempering oils are used at elevated temperatures, from 90° to 200°C. Typically they
are formulated from solvent-refined mineral oils. These oils have a large paraffinic fraction to
substantially reduce oxidation and sludge formation. Additional anti-oxidation agents also are
added to enhance stability. Different speeds of mar-tempering oils are available. Typical
properties of quenching oils are shown in .

Table 1 - Typical characteristics of quenching oils

Quench Oil Typical Quench Flash Point (°C) Typical Viscosity GM Hot-Wire
Type Tank at 40°C, SUS Quenchometer Test, A
Temperature Test (Nickel
Ball), time,
seconds
Accelerated < 120 180 94 10 39
Conventional < 65 170 105 16 30
Mar-quenching < 200 300 700 30 30

Contamination of quench oils is a problem for most heat treating shops. An analysis of
data from The Houghton International database of customer cooling curves showed that the most
common contaminants are water, soot, salt, sludge (oxidation) and hydraulic oils. Water
contamination is the most common contaminant. Its presence can contribute to spotty hardness,
distortion, cracking, staining and potentially personnel injury if the concentration is too high
(generally greater than 0.1%) [9]. Sources of water include water-cooled bearings, fans, water-
oil heat exchangers, and condensation in humid environments. Soot is generally from the
furnace atmosphere, especially if high carbon potentials are used, or if the atmosphere is not in
control. This is a very fine particulate which is difficult to filter, except using very small filter
meshes (2-3 µm) [10].Accumulation of fine particulate is reported [11] initially to increase =
quenching speed, but eventually the accumulation reduces the speed of quenching oil [12]. This
is theorized to occur because increasing amounts of soot change the heat transfer characteristics
and cause more rapid oxidation of the oil. Salt contamination is generally from drag-out from
salt bath furnaces. Sludge or oxidation is due to extended operation at elevated temperatures or
breakdown of the oil during quenching operations. Hydraulic oils are also common
contaminants, typically from leaking doors or other hydraulic operations. Because any or all of
these contaminants can be present in a quenching operation, it was decided to evaluate their
effects on the cooling curve of medium speed oil, specifically Houghton Houghto-Quench® G.

Experimental Procedure

A test matrix was developed to examine the individual and combined effects of these
contaminants on the maximum cooling rate and the temperature of maximum cooling.
Temperature, though not technically a contaminant, was also included in the matrix to represent
the range of typical operating practices common in the heat treating industry. This test matrix is
shown in Table 2. The specific contaminants used in this study and their levels, are shown in
Table 3.

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 Two-liter oil mixtures were made according to the test matrix. These mixtures were split
into one-liter portions? and heated to 28°C and 82°C. Cooling curves were generated using the
IVF SmartQuench [13]. Results and comments are shown in Table 4.

Table 2 - Test matrix used to examine the individual and combined effects of contaminants.
Trial Temperature Organic Water (%) Oxidation Salt (%) Solids
°C Contaminati (days at Contaminati
on 126°C) on (soot, %)
(Hydraulic
Oils, %)
1 27 2.5 0.1 7 0 0.05
2 27 2.5 0.1 0 0 0
3 27 2.5 0 7 5 0
4 27 2.5 0 0 5 0.05
5 27 0 0.1 0 5 0.05
6 27 0 0.1 7 5 0
7 27 0 0 0 0 0
8 27 0 0 7 0 0.05
9 82 2.5 0.1 7 0 0.05
10 82 2.5 0.1 0 0 0
11 82 2.5 0 7 5 0
12 82 2.5 0 0 5 0.05
13 82 0 0.1 0 5 0.05
14 82 0 0.1 7 5 0
15 82 0 0 0 0 0
16 82 0 0 7 0 0.05

Table 3 - Contaminants and levels of contaminants used to evaluate cooling rate effects
Contaminate Low High
Organic Contamination None 2.5% Houghton Cosmolubric HF-122
Oxidation New 7 days at 90-95°C (~190-202°F)
Water < 0.02% 0.1% Water
Solids Contamination (soot) None 0.05% graphite
Salt None 5% Draw Temp 430SN
Temperature 28°C 90°C

Results

A statistical analysis of the effects of each contaminant was performed (Table 4Error!
Reference source not found. and Figure 1, Figure 2, and Figure 3). Typically, whenever the hot
probe was immersed in the test oil, there was a small flash on the surface of the oil and then the
fire went out. In test sequences #3, 4, 11 and 12, a fire occurred that did not go out on its own.
This phenomenon was not observed in any other test sequence. This would suggest that the
interaction of salt and hydraulic oil substantially reduces the flash point of the oil. Further work
will be done to verify this effect.
Examining the effects of the main variables (Figure 1) on the maximum cooling rate
during nucleate boiling, it was found that oil temperature had the most significant effect in
raising the maximum cooling rate. By increasing the temperature, the maximum cooling rate

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increased. This appears to be counter-intuitive. However, it can be explained by the change in
viscosity of the quench oil. At room temperature, 28°C, the oil is rather viscous. The oil does
not wet the surface of the part well. The oil, being viscous, does not carry the heat away from
the part. When the temperature of the oil is raised, the viscosity of the oil also decreases. This
causes increased wetting of the part, and better heat transfer. Increasing the temperature also
increased the temperature at which the maximum cooling occurred. This also is thought to be
associated with the decreased viscosity of the oil, improving wettability.
Soot has the second largest impact on the maximum cooling rate. As the amount of soot
increased in the quench oil, the maximum cooling rate also increased. This is probably because
very fine soot particles acted as nucleation sites for bubble formation during nucleate boiling.
However, additions of soot also caused the temperature at maximum cooling to decrease. If soot
acted as a nucleation site for bubble formation, it is likely that the temperature of maximum
cooling would also increase. The reason for this apparent contradiction is not yet fully
understood.
Salt additions had similar effects to those of soot, and it is likely that the mechanism is
similar. Salt crystals will not dissolve in oil, because of the polar nature of salt. Therefore,
crystals could act as a discrete nucleation sites for bubble formation during nucleate boiling.

Table 4 - Results of the test matrix in Table 2

Trial Maximum Temp. at Theta 1 Theta 2 Temp. C Maximum Comments
Cooling Max. C C at Max. Heat
Rate C/s Cooling HTC Transfer
Rate C Coefficient
1 117 560 698 297 418 4652 No sharp 2-3 transition
2 114 576 704 310 424 4413 No sharp 2-3 transition
3 94 620 781 413 497 2752 Sharp 1-2 & 2-3 transition
4 115 651 801 427 414 2722 Indistinct vapor phase and
2-3 transition
5 114 573 707 312 399 4211 Sharp 1-2 and indistinct 2-
3 transition
6 107 612 727 393 571 3638 Very sharp 1-2 & 2-3
transition
7 107 611 734 390 479 3737 Very sharp 1-2 & 2-3
transition
8 107 612 729 394 466 3665 Very sharp 1-2 & 2-3
transition
9 134 516 652 300 4913 4913 Sharp 1-2 transition, and
very indistinct 2-3
transition present
10 112 587 719 361 434 4070 Sharp 1-2 transition,
somewhat sharp 2-3
transition present
11 118 657 793 425 544 3237 1-2 & 2-3 transition visible
12 125 718 849 475 728 5397 No vapor phase present
13 122 577 713 327 388 5366 Distinct 1-2, indistinct 2-3
transition
14 122 579 724 341 373 5070 Distinct 1-2, indistinct 2-3
transition
15 115 604 729 395 400 3960 Very sharp 1-2 & 2-3
transition
16 112 613 730 396 403 3685 Very sharp 1-2 & 2-3

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 transition
Water increased the maximum cooling rate, and substantially decreased the temperature
of maximum cooling. This increases the distortion of a part by increasing the thermal gradients
within a part. It can also create spotty work by the insulating effect of water bubble formation.
Contamination by hydraulic fluid increased the maximum cooling rate and the
temperature at which maximum cooling occurred. Since organic hydraulic fluids are miscible in
mineral oil, the properties of the quench oil change. The boiling point of the oil and hydraulic
fluid would likely increase, causing an increase in the maximum cooling rate, and the
temperature where the maximum cooling occurs.
Oxidation caused the maximum cooling rate and the temperature of maximum cooling to
decrease. It is suspected that this decrease is caused by an increase in the viscosity of the
quenching oil. This increase would cause decreases in the wettability of the quench oil. Since
the oil is more viscous, bubble formation is more difficult, and the maximum cooling rate and the
temperature of maximum cooling are reduced.

Figure 1- Main Effects (Data Means) of Contamination on the maximum cooling rate, and
the Temperature of Maximum Cooling Rate.

A cooling curve of a fluid is generally characterized by the maximum cooling rate, the
temperature at which the maximum cooling rate occurs, the temperature for the vapor to boiling
transition, and the transition temperature from boiling to convection. These two transition
temperatures, θ1 and θ2 respectively, are determined according to French Standard NFT 60178.
The effects of contaminants on the cooling curve behavior were generally similar for both
θ1 and θ2 (Figure 2). Temperature had a small effect on the vapor/boil transition and the
boiling/convection transition. Water had the largest effect in changing the cooling curve, with
the effect of depressing the boiling/convection transition and stabilizing the vapor phase by
depressing the vapor/boiling transition temperature. Salt tended to destabilize the vapor phase
and increase, θ1 and θ2. Organic contamination with a hydraulic fluid tended to destabilize θ1
(increase the transition temperature) in a similar fashion as salt. The effects of contamination on
θ1 and θ2 are shown in Figure 2.

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Figure 2 - Main Effects (Data Means) of the effect of contamination on Theta 1 & Theta 2.

Figure 3 - Main Effects (Data Means of the effect of contaminates on the heat transfer
coefficient and the temperature of maximum heat transfer coefficient.

When examining the effect of contaminants on the maximum heat transfer coefficient
Figure 3, it was determined that temperature, water and solids contamination (soot) increased the
maximum heat transfer coefficient. Organic contamination and salt tended to slightly depress the
maximum heat transfer coefficient. Interestingly, it was observed that oxidation tended to
slightly depress the maximum heat transfer coefficient. This is counter to conventional wisdom
and data. Further investigation is needed to understand this phenomenon.
Temperature, organic contamination, water, oxidation and solids contamination
increased the temperature where the maximum heat transfer coefficient occurs. Salted tended to
depress the temperature where the maximum heat transfer coefficient occurs.

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 Conclusions

Based on this investigation, it is concluded that:

• The presence of hydraulic fluid, soot, salts or water increases the maximum cooling rate of
conventional quench oils.
• Oxidation decreases the maximum cooling rate and the temperature of maximum cooling, by
increasing the viscosity of the quench oil.
• Temperature increases the maximum cooling rate of the oil, and the temperature of maximum
cooling rate, within the temperatures studied, because of decreases in viscosity and improved
heat transfer.
• The presence of salt, or hydraulic fluids increases the temperature of maximum cooling by
different mechanisms. Salt provides additional sites for bubble formation, causing the
temperature of maximum cooling to increase. The presence of hydraulic fluid reduces the
viscosity of the quench oil, and enhances bubble formation because of the different boiling
points of oil and hydraulic fluid.
• Water decreases the temperature of maximum cooling, which in turn can cause increased
distortion.

The effects of contamination of quench oil can cause significant changes in the maximum cooling
rate and temperature of maximum cooling. This can result in increased part distortion, cracking, and non-
uniformity of properties. A control program to monitor and track quench oil performance is necessary to
insure quality parts and customer satisfaction.

Acknowledgments

The authors would like to thank our management for allowing us to attend this event and
present our results. We would also like to thank Joe Jankowski for performing the cooling curve
measurements presented here.

References

[1] R.J. Windgassen, Paper presented at Metalworking Fluids Today, Society of Tribologist and
Lubrication Engineers, Feb. 1989.
[2] G.D. Hobson, W. Pohl, Modern Petroleum Technology, (John Wiley and Sons, New York) 1973,
Chapter 6.
[3] J.A. Hasson, "Preventative Maintenance for Quenching Oils", Industrial Heating, Sept., 1981
[4] G. R. Furman, Lubrication, 57 (1971) 13.
[5] S.W. Han, R. Yul Chev, Kong Hak Hoe Jie, 2 (1989) 59.
[6] T. W. Dicken, Heat Treat. Met., 1 (1986) 6.
[7] "Houghton on Quenching", Houghton International, Valley Forge PA.
[8] S. B. Lasday, Industrial Heating, Oct. (1976) 8.
[9] Anon., "Quenching Oils: Maintenance Procedures to Optimize Life", The Houghton Line, Winter
(1990).
[10] J.A. Hasson, Industial Heating, Nov. (1995) 63.
[11] V. Srimongkolkul, Heat Treating, Dec. (1990).
[12] V. Srimongkolkul, Industrial Heating, Sept. (1998) 81.
[13] B. Brennan, Industrial Heating, Jan. (1991).

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