Fuel Processing Technology 142 (2016) 8691

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Fuel Processing Technology

journal homepage: www.elsevier.com/locate/fuproc

Research article

Effect of dissolved oxygen concentration on coke deposition of kerosene

Xin-yan Pei, Ling-yun Hou
School of Aerospace Engineering, Tsinghua University, Beijing 100084, China

a r t i c l e i n f o a b s t r a c t

Article history: Coke deposition is an obstacle to the application of fuel cooling. The effect of dissolved oxygen concentration at
Received 3 April 2015 the supercritical pressure on the thermal oxidative coking deposition of Chinese RP-3 kerosene was investigated
Received in revised form 28 September 2015 using thermal uid experiments. Tests were conducted in a small-diameter, indirectly electrically heated, single-
Accepted 28 September 2015
pass straight tube covering the temperature range of the thermal oxidation reaction. The amount of coke depo-
Available online 8 October 2015
sition was measured by weighting. The results of the experiments for high-dissolved-oxygen, air-saturated, and
Keywords:
deoxygenated fuels were compared at the supercritical pressure of 3 MPa and a fuel outlet temperature of 410 C.
Dissolved oxygen In comparison with the air-saturated fuel, the high-dissolved-oxygen fuel experienced a sharp rise in deposits,
Coke deposition while the deoxygenated fuel had the lowest deposition quantity. The consumption fraction of the dissolved ox-
Supercritical condition ygen increased notably above 200 C and tted a pseudo-rst-order reaction. The entrance effect, inducing high
Entrance effect depositions, was interpreted by the temperature gradient and the boundary layer. Finally the relationship be-
tween thermal oxidative deposition and heat transfer was examined.
2015 Elsevier B.V. All rights reserved.

1. Introduction experiments, a near-isothermal ow test rig was applied to investigate

Recent advances in jet aircraft technology have induced an ever-in-
creasing heat load on aircraft air cooling systems. Cooled cooling air
with hydrocarbon aviation fuels is a potential technique for the thermal
management systems of next-generation aircraft [1]. As the jet fuel ex-
posed to air, oxygen in the air is dissolved in the fuel. Accordingly, au-
toxidation reactions occur in the fuel temperature range of 150400 C
[2]. The jet fuel reacts with dissolved oxygen to produce oxidized prod-
ucts, and deposits form on the inner-wall surface. These deposits would
block fuel lines, valves, nozzles, and various other aircraft components,
potentially resulting in engine function failure [3].
Various experiments have been performed on the thermal oxidation
stability. Many physical and chemical factors [4,5] inuence the thermal
oxidation stability, listed as temperature [6], system pressure [7,8], ow
mass rates or velocity, test duration [9,10], fuel compositions [2,11], ad-
ditives [12,13], catalysis and surface effect [14,15], especially, the dis-
solved oxygen concentration [16,17] which is one of the most
important factors for oxidation deposition. It is well cognized that the
reaction of dissolved oxygen with hydrocarbons forms hydroperoxides,
which are intimately involved in deposit formation [18]. The effect of
dissolved oxygen has been studied using many different devices, classi-
ed as static [19] and dynamic ones [20]. In static experiments, the jet
fuel thermal oxidative stability in quartzcrystal microbalances has
been examined using crystal electrodes with various metal materials,
namely gold, platinum, aluminum, and silver [19,21,22]. In dynamic
the role of dissolved oxygen by reducing the oxygen concentration in
various fuels subjected to a thermal environment, with the carbon
burn-off analysis of surface deposits [2,16,23]. It has been indicated
that control of dissolved oxygen at sub parts-per-million (ppm) levels
greatly improved the thermal stability and decreased heat exchanger
fouling. In addition to the oxygen concentration, uid dynamics and
heat transfer also affected fuel oxidation deposition [24,25]. The remov-
al of oxygen has been proposed as a promising method for improving
the thermal stability of fuel [16,17]. Most studies have focused on the
mechanisms and reactions of thermal oxidation and decomposition
coking for various fuels [2628], and few studies have considered the ef-
fect of oxygen consumption on deposition and heat transfer.
The above researches prove that it is important to understand the
main factors affecting the deposit formation for a given jet fuel. The ob-
jective of this work is to examine the effect of dissolved oxygen concen-
tration on coke deposition of jet fuel at supercritical pressure and
temperatures. In the experiments, the oxygen in the fuel was partly con-
sumed, and was monitored at the inlet and exit of the reactor during the
tests. The inuence on deposition of the entrance effect, which is char-
acterized by the boundary layer and the temperature gradient, was
interpreted. The relationship between heat transfer and the oxidation
stability of RP-3 was investigated based on the Nusselt number (Nu)
and deposition rate.
2. Experimental

Corresponding author. Chinese No.3 (RP-3) kerosene was chosen as the fuel. The physical
E-mail address: lyhou@tsinghua.edu.cn (L. Hou). properties of RP-3 aviation kerosene are listed in Table 1 [29]. The

http://dx.doi.org/10.1016/j.fuproc.2015.09.029
0378-3820/ 2015 Elsevier B.V. All rights reserved.
 X. Pei, L. Hou / Fuel Processing Technology 142 (2016) 8691
Table 1
Characteristics of RP-3 aviation kerosene.
Critical pressure (MPa) Critical temperature (C) Density (g/cm3) (20 C)
2.39 372.5 0.7913
thermal physical properties of the aviation kerosene are temperature-
dependent. The bulk temperature of fuel along the reactor tube could
be predicted in the simulation results. The thermal physical properties
were determined by using a three-component surrogate model [30].
An indirectly electrically heated tube was employed to simulate a
heat-exchanger in which heat transfer and thermal oxidation deposi-
tion of fuel occur. As shown in Fig. 1, the experimental apparatus
consisted of four subsystems, i.e., feeding, heating and reactor, data ac-
quisition/controlling system, and sampling/online analysis systems. A
vacuum pump (6, N86 KT.18, KNF Inc.) and a magnetic stirrer (3)
were applied to deoxidize the fuel. The oxygen concentration was mon-
itored via two observation windows xed on the opposite walls of the
fuel tank (4) and an oxygen sensor (5, InPro 6850i, Mettler Toledo
Inc.) dipped in the fuel. The oxygen sensor was designed for continuous
measurement of dissolved oxygen over a 0100% full range, i.e., up to
70 ppm. The transmitter, which was coupled to the sensor, was a
Mettler Toledo dissolved oxygen microprocessor transmitter (Model
3000). A mass ow controller (2; CS2000, Seven-star Inc.) was used to
control the amount of oxygen bubbled into the deoxidized fuel to the
desired dissolved oxygen concentration. The fuel with a specic dis-
solved oxygen concentration was introduced into the reactor through
a lter (7) to remove any impurities. The inlet mass ow rate was set
at 1 g/s, and was monitored using a plunger metering pump (8) and
coriolis mass ow meter (11; DMF-1-1-ADMF-DX, Sincerity Inc.). The
fuel pressure stability was maintained using a pressure damper. Nitro-
gen was used to blow down the residual fuel in all pipes before heating.
The reactor straight tube was made of the 316 stainless steel with a
length of 450 mm, an inner diameter of 2 mm and a wall thickness of
0.5 mm. The test section was xed horizontally and the heating ux
was simulated by an electrical heating stove. After heating, the fuel
was cooled using a counter-ow water-fuel exchanger (18). The fuel
pressure was adjusted to 3 MPa using a back-pressure regulator (19;
SS-9833F-1P-B, Xiongchuan Value Inc.) installed after the heat-ex-
changer to guarantee the jet fuel in a supercritical phase. The oxygen
Fig. 1. Experimental setup for the coke deposition. 1: Oxygen cylinder; 2:Gas mass ow controller; 3: Magnetic stirrer; 4: Fuel tank; 5: Online oxygen sensor; 6: Vacuum pump; 7: Filter; 8:
Plunger metering pump; 9: Pressure damper; 10: Nitrogen cylinder; 11: Mass ow meter; 12: Relief valve; 13: Preheater; 14: Pressure gauge; 15: Thermocouple; 16: Electrical heating
stove; 17: Reactor tube; 18: Water-cooled exchanger; 19: Backpressure regulator; 20: Collection container; 21: Sampling and online analysis system; 22: Pressure difference transducer;
23: Data acquisition/controlling system.
87
Flash point (C) Distillation range (C) Relative molecular weight Averaged molecular
(g/mol) formula
50 163212 148.33 C10.5H22
concentrations after the thermal experiments were measured continu-
ously, but the oxygen sensor could not be placed immediately down-
stream of the heated test section exit because of the high exit
temperature and pressure. A sampling and online analysis system (21)
was therefore installed behind the cooling exchanger for consistent
measurements. To ensure a constant oxygen concentration along the
whole tube, the seal design was tested at pressure of 3 MPa by checking
the inlet and exit oxygen concentrations to verify the absence of oxygen
leakage from, or addition to, the system. The residuals were collected in
a container (20). A pressure difference transducer (22; 300S1AAD1M5,
Rosemount Inc.) was used to monitor the pressure drop between the
inlet and outlet of the reactor during heating. The outer-wall tempera-
ture of the reactor tube was measured using 18 K-type thermocouples
spot-welded at 2.5 cm intervals along the tube. The fuel inlet and outlet
temperatures were measured using K-type thermocouples inserted into
the center of the tube. The amount of oxidized deposition was strongly
affected by the test time, therefore heating was performed for 105 min
to guarantee the formation of sufcient deposit for analysis.
As the amount of deposit formed by oxidation is smaller than that
formed by thermal cracking, a segmentation method was used to
weigh the mass of oxidized deposition [31]. The formation of oxidation
deposits depends on a two-step mechanism: rstly, the chemical for-
mation of deposit precursors by fuel reacting with the dissolved oxygen;
and secondly, the mass transport of deposit precursors to the wall. As
the fuel heated in the reactor, the coke was gradually deposited on the
inner surface of the tube with increase in the temperature and the
heating duration. After each experiment, the tube was divided into 11
sections with each length of 4 cm. Each segment surface was polished
out and cleaned with ethanol. This operation was to eliminate errors in-
troduced by the insoluble impurities on the surface. And then the seg-
ments were dried above 100 C for at least 1 h to remove residual
water and ethanol. A high-precision balance (ESJ1824, Long-Teng
Inc.) was used to weigh each segment. The segments were then washed
for at least 2 h in an ultrasonic vibrator lled with potassium
88 X. Pei, L. Hou / Fuel Processing Technology 142 (2016) 8691
permanganate (125 mg/L) to remove the deposits. The segments were
washed with water and ethanol, dried, and weighed again. The differ-
ence between the two weights was the mass of coke deposition.
The experimental heat transfer coefcient can be calculated as fol-
lows: h = q/(Tw Tb), where q is the heat ux and it depends on the
heating power and excludes the heat loss. The system heat loss to the
environment can be minimized through insulation and can be obtained
through calibration without a fuel ow. The inner-wall temperature Tw
was calculated from the measured outer-wall temperature. The bulk
temperature Tb of the fuel along the reactor tube, was predicted using
a commercial software, i.e., Ansys Fluent [32]. Nu is dened as
(h d) / , where h is the convective heat transfer coefcient, d is the
inner diameter of the tube, and is the thermal conductivity of the fuel.
3. Results and discussion
The dissolved oxygen concentration plays a major role in coke depo-
sition. The autoxidation of hydrocarbons consists of a complex set of
free radical reactions and the dissolved oxygen is involved in fuel initi-
ates reactions. In fuel-cooling system design, it is essential to investigate
the effect of dissolved oxygen concentration on the fuel thermal stabil-
ity. The solubility of oxygen in the fuel increases with increasing fuel
temperature. The three dissolved oxygen concentrations at the inlet
were xed at 32 ppm (high-level), 10 ppm (normal-level, air-saturated
fuel), and 01 ppm (deoxidized-level, below the precision of the oxygen
sensor). As listed in Table 2, the heating power and time were kept uni-
form for the three cases, ensuring a constant heat ux. The pressure in
the tube and mass ow rates were controlled at 3 MPa and 1 g/s,
respectively.
As presented in Table 3, the total mass of coke deposition increases
with increasing concentration of the dissolved oxygen. In comparison
with the deposition in the normal case, the mass deposition by the
deoxidized fuel is 31% lower. The mass deposition and oxygen con-
sumption in the high-level case are nearly three times as much as
those at the normal level. Thus, the total oxygen consumption is related
to mass deposition. In a ow system, oxygen consumption is controlled
by both the oxidation kinetics and species transport. In the autoxidation
chain mechanism, the cycle begins with the initiation of thermal de-
composition of the hydrocarbon, producing hydrocarbon radicals R,
which react rapidly with dissolved oxygen, forming peroxy radicals
ROO. The peroxy radicals then form hydroperoxides, which act as initi-
ators, increasing the free-radical pool and the resulting in rapid oxida-
tion [33]. Oxygen is therefore important in oxidation deposition
reactions.
As illustrated in Fig. 2, more than 50% of the oxygen is consumed at
the outlet. The oxygen consumption proles of these two cases follow
the same trend, and consumption increases with increasing outlet fuel
temperature. The oxygen concentration was plotted as the oxygen con-
sumption fraction ([O2c/O2in]) versus the outlet fuel temperature (Tout),
to make the results independent of the initial oxygen concentration. The
oxygen consumption fraction ([O2c/O2in]) is dened as the ratio of the
concentration of the consumed oxygen in the fuel to the concentration
of dissolved oxygen at the inlet of the test section during the experi-
ment. In a ow system, the oxygen consumption reaction follows pseu-
do-rst-order kinetics [34]. Pseudo-rst-order kinetics means that
compared with that of oxygen, the concentrations of all other reactants
are sufcient for them to be treated as constants. Eq. (1) was used to t
Table 2
Experimental parameters.
Heat ux (kW/m2) Heating time (min) Inlet mass ow rated (g/s)
384.6 105 1 3
Table 3
Coke deposition and oxygen consumption at different oxygen concentrations.
Case Inlet oxygen Total oxygen Total mass of
concentration consumption deposition
(ppm) (ppm) (mg)
Deoxidized-level b1 b1 3.53
Normal-level 10 6.34 5.13
High-level 32 18.2 14.35
the oxygen consumption data. The same Arrhenius parameters were
used for the normal and high-level cases.

 Z T out
O2c a
ln A expE=RT dTb 1
O2in T out 300 300
In Eq. (1), A, E/R, a, and b are 101, 982 K, 32.98, and 4.943, respec-
tively. Tout is the thermodynamic outlet fuel temperature, and the sub-
scripts c and in denote consumed oxygen and initial oxygen
concentration, respectively.
On the one hand, the oxygen consumption increases greatly above
200 C, which indicates a more violent oxidation deposition reactions
in both cases, on the other hand, the oxygen in the high-level case is
consumed faster than that in the normal case at temperatures below
200 C. When the temperature is above 325 C, however, the oxygen
consumption fraction of high level is lower than that of the normal
level. Because the oxidation deposition is not completely linear enlarged
with the increase in the concentration of the dissolved oxygen in the
fuel. Under certain conditions of temperature and pressure, there
maybe a peak of surface fouling and the deposition reactions can be
more violent with less dissolved oxygen concentration. The similar re-
sults were also observed in the experiments of Ervin and Williams [23].
As displayed in Fig. 3, the deposition in the high-level case is far
greater than in the other two cases. The deposition rate for the high-
level case is the fastest and increases stably along the tube, due to the
sufcient dissolved oxygen in the fuel. Deoxidization is an effective
way to decrease deposition along the tube, because dissolved oxygen
is not present to trigger hydroperoxide formation and stimulate free-
radical reactions. When the amount of oxygen is limited, the dominant
radical species changes from the peroxy radical to a mixture of peroxy,
alkoxy (RO) and alkyl (vinyl) radicals (R). Furthermore, the deposits
formed in the air-saturated fuel experiment contain mostly spherical
particles, whereas for the deoxidized fuel, it takes the form of a fused,
amorphous varnish [35]. Oxygen is therefore essential, not only because
of its effect on the chemistry of deposit formation, but also in terms of
morphology.
It is revealed in Fig. 3 that there are higher amounts of deposits at the
tube inlet in all cases, because of the entrance effect which is deter-
mined by the temperature gradient and the boundary layer. A thermal
boundary layer is established as a result of heating of the wall when
the uid enters the tube. The viscosity of the uid in contact with the re-
actor surface resists the motion of adjacent uid layers and slows them
down gradually. The thickness of the boundary layer gradually increases
in the ow direction until the boundary reaches the pipe center and lls
the entire pipe. The increasing thickness of the boundary layer acceler-
ates the ow of the central portion. The length from the pipe entrance to
the point at which the wall shear stress reaches about 2% of the fully de-
veloped value is called the thermal entrance length, L*. In a laminar
Pressure (MPa) Maximum fuel temperature at outlet (C)
410
 X. Pei, L. Hou / Fuel Processing Technology 142 (2016) 8691
Fig. 2. The oxygen consumption fraction with the outlet fuel temperature.
ow, the non-dimensional hydrodynamic entry is given by L 0.05dRe
[36]. The ow at normal temperature (27 C) of reactor inlet is laminar
as Reynolds number (Re) in 751 and the mass ow rate of 1 g/s, there-
fore L* is 75.1 mm.
To investigate the inuence of the inlet Re on the entrance effect, an
experiment with a high Re, i.e., 3746, was performed by increasing the
fuel temperature at the inlet. As plotted in Fig. 4, the inlet Re was
changed by increasing the inlet temperature. For Re of 751, the deposi-
tion rate in the section up to nearly 60 mm from the inlet is nearly three
times as much as those in the other sections. This length is less than the
empirical L* calculated above in that the heat is transferred radially up-
stream inducing a gradual increase in the inlet temperature to above
100 C. The ow at this temperature is transition ow with Re at
1850. The Re is calculated based on the viscosity coefcient and density
that are varied with the fuel temperatures [30]. This value is just be-
tween laminar ow and turbulent ow. Growth of the boundary layer
for turbulent ow is faster than that for laminar ow, resulting in a
shorter L*, i.e., about 2545d, mainly because of ow disturbance. The
entry length for transition ow in this experiment is therefore between
those for the turbulent and laminar ow.
Fig. 3. The deposition rate distribution along the tube.
89
Fig. 4. The deposition rates for different inlet Re numbers along the tube.
In Fig. 4, the turbulence inlet condition mitigates the entrance effect
and leads to an observable decrease in deposit formation at the inlet, be-
cause the intense mixing during random uctuations outweighs the ef-
fect of molecular diffusion.
In the thermal entrance region, the wall shear stress is the highest at
the tube inlet, where the boundary layer thickness is the smallest, and it
decreases along the ow direction; this induces a long residence time
for the ow and enhances deposition. Also, as the initially thin thermal
boundary layer develops near the heated wall of the inlet, the radial
temperature gradient is large at the inlet wall but decreases with in-
creasing axial distance. Not only the reactions but also the deposit mor-
phology are different. In the stable heated sections, the deposit layers
have micro-spheroidal structures, whereas in the gradient temperature
section, a lm with no perceptible small-scale structure, which con-
forms to the micro-geometry of the underlying stainless-steel surface,
is formed. Laminar ow, high wall shear stress and temperature gradi-
ent, and prolonged residence time near the wall all stimulate formation
of oxidized deposits near the entrance of the reactor tube.
As given in Fig. 5, it is obvious that there are some uctuations in
both the wall temperature and mass of deposits along the tube. The ex-
tent of the wall temperature uctuation increases with heating. In addi-
tion the region with the peak wall temperature approximately coincides
with the area of high coke deposition. In this case, deposition on the
inner surface increases the wall temperature. In Fig. 6, the wall temper-
ature, corresponding to a high level deposition at location B in Fig. 5,
increases faster than the one at location A during heating process.
Fig. 5. Wall temperature and deposition proles at different time and locations.
90 X. Pei, L. Hou / Fuel Processing Technology 142 (2016) 8691
Fig. 6. Wall temperature distributions at the location A and B with time.
Hence, it is demonstrated that the formation of a large amount of de-
posits results in an increase in the coke thermal resistance, which hin-
ders heat transfer in this region. In addition, the rough surface of the
coke deposit is an irregular porous medium, which may increase coke
adsorption on the wall.
It can be observed in Fig. 7 that the variation trends in fuel temper-
ature for the three cases are similar and the temperature gradually ap-
proach 405 C at the ends of the three tests; this indicates that the
heat sinks of the three fuel samples are the same. For the wall tempera-
ture distribution, a difference is gradually distinguished after 20 min
and the wall temperature in the high-level case becomes higher than
those in the other two cases. The different proles of the average wall
temperature along the tube in the three cases result from the oxidation
deposition, which affects heat transfer. The wall temperature is higher
and increases faster than the fuel temperature. The temperature of the
fuel near wall after 45 min is above the pseudo-critical temperature
which is about 400C at supercritical pressure of 3 MPa [30]. When
the ow state is close to the critical point, small changes in pressure or
temperature result in large changes in the thermal properties and the
fuel becomes a supercritical uid with gas-like diffusivity, density and
viscosity. The bigger difference between the wall and fuel temperatures
indicates that the supercritical physical properties of the fuel will accel-
erate the oxidation deposition reaction. At the ends of the tests, there
Fig. 7. The average wall and outlet fuel temperatures for various oxygen concentrations.
was a difference of about 50 C between the wall and fuel temperatures
for the deoxidized and air-saturated cases, and of nearly 100 C in the
high- level case due to the larger amount of oxidation deposition.
Thus, the fuel deoxidization not only reduces thermal oxidative deposi-
tion but also improves the heat transfer effect.
In Fig. 8, Nu is the ratio of convective to conductive heat transfer
across the boundary and used to evaluate the convective heat transfer
intensity. To clarify the difference among the experiments, the Nu pro-
les for various oxygen concentrations were exponential tted to the
measured values. The Nu proles in all three cases increase along the
tube. Heat transfer is slightly enhanced at the end of the reactor because
of heat dissipation at the outlet. The differences among the Nu values
gradually become clearer, especially in the deoxidized case. As analyz-
ing the Fig. 3 and Fig. 8 together, the conclusion can be drawn that the
heat transfer deteriorates with increasing deposition rate. The average
Nu along the tube for the deoxidized case is 2.2 times higher than that
for the high-level case, and 1.7 times more than that for the air-saturat-
ed case. Coke deposition on the inner wall therefore weakens heat
transfer between the wall and the fuel.
4. Conclusion
A detailed experimental investigation of the thermal oxidation de-
position characteristics of RP-3 was performed to evaluate the impor-
tance of the oxygen concentration. The results revealed that a lower
inlet level of dissolved oxygen reduced oxidation coking deposition in
the tube. The oxygen consumption fraction change was pseudo-rst-
order with respect to the fuel outlet temperature and increased greatly
above 200 C. Investigation of the entrance effect indicated that under
the range of Reynolds number in the experiments, less amounts of de-
posits were produced in turbulent ow than those in laminar ow.
Coke deposition on the inner surface affected heat transfer between
the surface and the fuel. Accordingly, fuel deoxidization not only re-
duces thermal oxidative deposition but also improves heat transfer.
Acknowledgments
The nancial assistances provided by the National Natural Science
Foundation of China (51176093) and Tsinghua University Initiative Sci-
entic Research Program (20131089265) are gratefully acknowledged.
Fig. 8. Distributions of tted Nu number along the tube.
 X. Pei, L. Hou / Fuel Processing Technology 142 (2016) 8691
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