Journal of Loss Prevention in the Process Industries 15 (2002) 119127

www.elsevier.com/locate/jlp

Evaluations of kinetic parameters and critical runaway conditions

in the reaction system of hexamine-nitric acid to produce RDX in
a non-isothermal batch reactor
Kuo-Ming Luo *, Sheann-Huei Lin, Jih-Guang Chang, Tzung-Huei Huang
Department of Applied Chemistry, Chung Cheng Institute of Technology, National Defense University, Tashi, Taoyuan 33509, Taiwan

Abstract

In the production process of RDX from the reaction of hexamine and nitric acid, its reaction rate was evaluated and expressed
5671.062
as rA=1.234106e T CNOC1.28 A , where T is the reaction temperature, CA is the concentration of hexamine and CNO is the initial
concentration of added nitric acid. The critical condition of runaway reaction for the RDX production in a batch reactor is
c=20.4374.805/[1+exp(336.7b15.65)]. Its heat transfer coefficient at critical runaway condition was also estimated and
expressed as (hS/V)cr=(RqgACNOCnAO)/(Eb2e1/bfC). 2002 Elsevier Science Ltd. All rights reserved.

Keywords: RDX; Hexamine; Runaway reaction

1. Introduction extensively in mixtures with TNT, as so-called hexolite,

The explosive RDX is also known as Cyclo-trimethy-
lenetriamine, Hexogen, T4 or Cyclonite. Its nomencla-
ture is 1,3,5-trinitrohexahydro-sym-triazine or 1,3,5-trin-
itro-1,3,5-triazacyclohexane. This explosive has been
very important since World War II and has served as a
constituent of many explosive mixtures from which a
high power was required. The molecular formula of
RDX is C3H6N6O6 and its chemical structure is:
RDX was used in detonators and primers, and in detonat-
ing gains or boosters it is replacing tetryl. It was used
* Corresponding author.
E-mail address: luokm@cc04.ccit.edu.tw (K.-M. Luo).
semi-liquid, fusible explosive. The mixture of TNT,
RDX and aluminium is another kind of explosive. The
plastic explosives also contained RDX.
Although the RDX has been produced and used by
many countries for a long time, its production process
is not very safe so far. Numerous thermal runaway inci-
dents and explosion catastrophes have occurred in the
past. Unfortunately, its reactive hazard has not been
clearly identified. The critical runaway temperature and
unstable criterion at its reaction process are still
unknown. The industries have to control their operating
conditions very carefully to avoid the reaction system
becoming a runaway situation. Therefore, we evaluate
its reaction kinetic parameters from known production
data of RDX in this investigation. Then, we can deter-
mine the critical runaway conditions of RDX reaction in
a non-isothermal batch reactor using the transient energy
and mass balance equations and evaluated kinetic para-
meters by numerical techniques simultaneously. Conse-
quently, this critical runaway condition can be expressed
as a function of kinetic parameters of chemical reaction,
physical properties, and ambient temperature etc. Their
required heat transfer coefficients in this critical con-
dition can also be estimated.

0950-4230/02/$ - see front matter 2002 Elsevier Science Ltd. All rights reserved.
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120 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127

Nomenclature
A frequency factor of Arrehenius form, (L/mole)1.28min1
CAO initial concentration of hexamine, mole/L
CA reacted concentration of hexamine, mole/L
CP heat capacity, kJ/mole.K
CP,m overall heat capacity in reaction system, kJ/mole.K
E activation energy in the reaction of producing RDX, kJ/g mole.
h heat transfer coefficient, J/m2K s
Hof heat of formation, kJ/g mole
Hof,o overall heat of formation, kJ/g mole
Hof,p heat of formation for product, kJ/mole
Hof,r heat of formation for reactant, kJ/mole
K reaction rate constant of producing RDX, (mol/L)1n min1
mHNO3 weight percent concentration of nitrate acid, %
MHA molecular weight of hexamine, g/mole
MRDX molecular weight of RDX, g/mole
n reaction order in the reaction of producing RDX, .
NAO initial mole number of hexamine, mole
NNO initial mole number of nitric acid, mole
NRO initial mole number of RDX, mole
NRDX mole number of RDX after reacted, mole
NHA mole number of hexamine after reacted, mole
NHNO3 mole number of nitric acid after reacted, mole
rA reaction rate of hexamine, mol/(L.min)
Qd dilution heat, kJ/mole
Qd,o initial dilution heat of mixture, kJ/mole
Qd,m average dilution heat, kJ/mole
qg generation heat, kJ/mole
R universal gas constant, J/g mole.K
S external surface of cooling medium of reactor, m2
t reaction time, min.
T temperature of reaction system, K
Ta temperature of coolant, K
WHA feed weight of hexamine, g
WHNO3 feed weight of nitric acid, g
WRDX product weight of RDX, g
WT feed weight of hexamine and nitric acid, g
V volume of reactant, liter
xA fractional conversion of hexamine
xHNO3 fractional conversion of nitric acid
Y(%) yield percentage of weight RDX per gram of hexamine,

Greek symbols

b definition in Eq. (20)

r mixed density of reactant, g/cm3
q definition in Eq. (19)
qo dimensionless temperature at initial time
f definition in Eq. (21)
fc values of f at critical runaway condition
j definition in Eq. (22)
t definition in Eq. (23)
h definition in Eq. (24)
 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127 121

1.1. Evaluation of reaction kinetic parameters from NRDX WRDX/MRDX WRDX/222 7

batch reaction of RDX xA W (5)
NAO WHA/MHA 10/140 111 RDX

The chemical reaction rate is very sensitive and affec-

ted by the temperature variation in an exothermic reac- The yield of RDX, Y(%), is defined as the percentage
tion system. Runway reaction or thermal explosion of molar ratio of produced RDX to initial hexamine as:
occurs in this exothermic hexamine-nitric acid reaction NRDX WRDX/MRDX
system in its production process. If we consider this Y% 100% 100%100xA% (6)
NHA WHA/MHA
reaction system in a batch reactor, when the total gener-
ated heat rate of reactive system exceeds removed heat 700
WRDX%
rate of the ambient cooling medium, the whole system 111
is very easy to accumulate energy and raise temperature.
Then, this heat increasing system becomes unbalanced
In a batch reactor, the produced RDX, WRDX, at vari-
and a self-ignition reaction is triggered off. As soon as
ous reaction times, t, and reaction temperature, T, were
the temperature in this batch reactor reaches the critical
measured which were obtained from Dai, Yen and Chen
point, the reactive system becomes a runaway situation
(1996), and are listed in Table 1. Then, we can evaluate
or even explosion.
the values of xA and Y(%) using Eqs. (5) and (6), the
The chemical reaction of hexamine and nitric acid to
results are listed in the last two columns of Table 1.
produce the RDX is expressed as the following equation:
The reaction rate in the hexamine-nitric acid reaction
C6H12N4+10HNO3C3H6N6O6+3CH2(ONO2)2+NH4NO3+3H2O system can be expressed as the consumption of the tran-
(1)
(Hexamine) (RDX) sient molar number variation of hexamine in a control
reactant volume as:
This is the main reaction between the reactants of hex- 1 dNHA
amine and nitric acid. Besides, there is another side reac- (rA) (7)
V dt
tion between these two reactants and its reaction equ-
ation is:
NAO
C6H12N416HNO36CH2(ONO2)24NH4NO3 (2) If using the relation of CAO= and substituting Eq.
V
(3) into Eq. (7), we can express the reaction rate in terms
In a batch reactor for producing RDX, the feed of fractional conversion of hexamine reaction as:
weights of the nitric acid, WHNO, and the hexamine, WHA,
NAO dxA dxA
are equal to 110 and 10 g, respectively. The weight per- (rA) CAO (8)
centage concentration of nitric acid, mHNO3 (%), is equal V dt dt
to 98%. The average density of mixed reaction solution, where CAO is the initial concentration of hexamine. From
r, is equal to 1.5g/cm3. The reaction time and tempera- Eq. (8) we can rearrange and correlate the reaction time
ture were set and its production weight of RDX, WRDX,
was measured. Thus the yield rate of RDX, Y(%), and
the fractional conversion of hexamine, xA, can be esti- Table 1
mated from experimental data. The molar numbers of The producing weight of RDX and evaluated percentage of yields and
hexamine and RDX which can be expressed in terms the fractional conversion of hexamine at various reaction times and
of the fractional conversion of hexamine reaction and is temperaturesa
estimated from experimental data by the following corre-
T, C t, min WRDX Y (%) xA
lations:
NHANAO(1xA) (3) 25 600 13.20 83 0.83
10 360 13.10 83 0.83
and 0 120 13.00 82 0.82
10 45 12.95 82 0.82
NRDXNRONAOxANAOxA (4) 20 15 12.80 81 0.81
30 10 12.75 80 0.80
where NAO and NRO are the initial mole numbers of hex- 35 19 12.75 80 0.80
amine and RDX, respectively. The NHA and NRDX are the 40 5 12.50 79 0.79
mole numbers of hexamine and RDX after the system is 50 5 11.50 73 0.73
reacted, respectively. Owing to the value of NRO equal 60 5 9.97 63 0.63
to zero before reaction, from Eq. (4), the fractional con- a
(a) Concentration of feed nitric acid, mHNO3=98%. (b) Weight ratio
version of hexamine, xA, can be expressed as a function of feed nitric acid to hexamine, WHNO3:WHA=110g:10g. (c) Density of
of production RDX as: solution, rmix=1.5 g/cm3.
122 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127

as a function of fractional conversion and concentration Table 2

of hexamine in a batch reactor as: Evaluation of reaction kinetic parameters for the reaction of RDX pro-
duction from the experimental data of Table 1 and Fig. 1

xA CA

dxA dCA
tCAO (9)
rA rA Reaction rate rA
dCA E
AeRTCNOCnA
0 CAO dt

From the stoichiometry of reaction of Eq. (1), the

Total weight of solution W=WHA+WHNO3=10+110=120 g
weight ratio of nitric acid to hexamine, WHNO:WHA, is Density of solution rmix=1.5 g/cm3=1500 g/L
equal to 1063:222=2.84:1. The value of experimental
weight ratio, WHNO:WHA, in batch reactor as shown in
W 120
Table 1, is equal to 11:1. Thus, it is in great excess in Volume of solution V 0.08 L
rmix 1500
the feed quantity of nitric acid. The concentration of
nitric acid in this experiment is only a minor variation,
therefore it can be assumed as constant value. Conse- Concentration of nitric acid mHNO3=98%
quently, the reaction rate of hexamine in the nitric acid
system can be expressed as: WHNO3mHNO3 1100.98
Initial molar number of nitric NNO
MHNO3 63
rAkCNOCnA (10) acid
1.711 mole
where, n, k and CNO are the reaction order, the rate con-
stant and the initial concentration of nitric acid in this
hexamine-nitrite acid reaction system, respectively. Sub-
stituting Eq. (10) into Eq. (9) and integrating it, we can Initial molar number of hexamine NAO
WHA 10
0.071 mole
correlate the reaction time as a function of concen- MHA 140
tration as:
1
t [C1nCAO
1n
] (11) NNO 1.711
(n1)kCNO A Initial molar concentration of
CNO 21.388 mole/L
nitric acid V 0.08

Using the relation of CA=CAO(1xA), Eq. (11) can be

rewritten as
Initial molar concentration of 0.071
CAO 0.888 mole/L
C1n hexamine 0.08
[(1xA)1n1]
AO
t (12)
(n1)kCNO
Value of reaction order n=1.28

Express the rate constant in Arrheniuss form as

exp(15.782)
A 1.234
kAeE/RT (13) Frequency factor of kinetic
n1
(n1)CNOCAO

where A, E and T are the frequency factor, the activation

energy and the reaction temperature, respectively. Com-
parameters
106
L
mole
1.28
min1

bining Eqs. (12) and (13) to obtain

E=5671.0628.314=47.149
t C1n
AO e
E/RT
Activation energy
(14) kJ/mole
(1xA)1n1 CNO(n1)A

Taking the natural logarithm on the both sides of Eq.

(14) to obtain Table 1. The calculated results of CNO and CAO are equal

n t
(1xA)1n1
n
C

E
A(n1)CNO RT
1n
AO
(15)
to 21.388 and 0.888 mole/L, respectively. Then, we can
plot the evaluated values of n[t/(1xA)1n1] versus
1/T as shown in Fig. 1. However, the value of reaction
order n is still unknown. Thus we have to evaluate n
Table 2 shows the formulae which are used to calculate value by means of trial and error technique. When
the values of CAO and CNO from measured experimental n=1.28 as shown in Fig. 2, this plot can obtain the best
data and the evaluated kinetic parameters as listed in linear correlation which is:
 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127 123

The heat balance in this reactor is:

dT
rVCP,m q V(rA)hS(TTa) (17)
dt g

We can combine Eqs. (8) and (13) to obtain the rate

of fractional conversion by
dxA
AeE/RTCNOCAO
n1
(1xA)n (18)
Fig. 1. The manufacture process of RDX in a batch reactor. dt

Using the following dimensionless definition which

has been described by Frank-Kamenetskii (1969) and
modified by Luo, Lu and Hu (1997a, b), Luo and Chang
(1998) and Luo and Hu (1998)
E
q 2(TTa) (19)
RT a
RTa
b (20)
E
EqgVACNOCnAO 1
f eb (21)
RT 2ahS
n1 1
rCP,mVACNOCAO
j eb (22)
hS
Fig. 2. The evaluation of kinetic parameters in the batch reaction
system of hexamine-nitric acid to produce the RDX using Eq. (15). hSt
t (23)
rCP,mV

n t
(1xA) 1
1n
15.782
5671.062
T
(16) f EqgCAO
h 2
RqgCAO
2
j RT a rCP,m b ErCp,m
(24)

Thus, we can express Eqs. (18) and (17) in dimen-

Comparing Eqs. (15) and (16), we know that sionless form as
n[CAO
1n
/ACNO(n1)]=15.782 and E/R=5671.062 K,
respectively. Therefore, the values of reaction kinetic
parameters n, A and E are estimated and listed in
dxA
dt
jexp
q
bq+1
(1xA)n (25)

Table 2.
dq q
fexp (1xA)nq (26)
dt bq+1
2. Evaluation of critical runaway condition in
hexamine-nitric acid reaction system
In a batch reaction system of hexamine-nitric acid to
In order to estimate the critical runaway condition of produce the RDX, the variation of fractional conversion
hexamine-nitric acid reaction systems in a batch reactor, of hexamine was affected by its reaction temperature.
we have to calculate its transient variations of tempera- Their relationship can be correlated by combining Eqs.
tures and fractional conversions. Thus, we require the (10) and (13) to obtain the following term:

1
energy and mass balance equations to calculate both the (rA)eE/RT n
transient values of temperatures and fractional conver- xA1 (27)
ACNOCnAO
sions, simultaneously. The nitration process of hexamine
to product RDX in a batch reactor is shown in Fig. 1.
The inlet and outlet temperatures of the coolant medium Fig. 3 shows the calculations of the fractional conver-
are Ta and T, respectively. sion of hexamine, xA, versus the reaction temperature,
The transient energy and mass balance equations for T, using Eq. (27) and given values of A, E, n, CNO and
the production of RDX in a non-isothermal batch reactor CAO which are listed in Table 2. The reaction rates of
can be expressed as follows: hexamine are set as parameters that are varied from 0.01
124 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127

can be determined from the stoichiometry of chemical

reaction, combining Eqs. (1) and (2), the overall reaction
for the production of RDX is
1 9
C6H12N413HNO3 RDX CH2(ONO2) (28)
2 2
5 3
NH4NO3 H2O
2 2

The overall heat of formation is

1
H0f,oniH0f,iNproductH0f,pNreactantH0f,r (71.546)
2
9 5 3
(199.158) (365.263) (285.830) (29)
Fig. 3. The relationship of fractional conversion and reaction tem- 2 2 2
perature at various reaction rates for the hexamine-nitric acid system
in a batch reactor. 136.81713(173.218)87.324 kJ/mole

to 100 (mole/L min) in this calculation. Each curve rep- The heat of dilution (Hale, 1925) for the mixture
resents the same reaction rate of hexamine. The higher includes the dilution of nitric acid and hexamine which
reaction temperature leads to the higher fractional con- can be expressed as
version for each reaction rate profile. However, the lower NHA
reaction rate leads to the higher fractional conversion at Qd,mxAQd,HAxHNO3Qd,HNO3 Q
NHA+NHNO d,HA
a given reaction temperature. 3

The values of fractional conversions of hexamine are HHNO3 0.071

affected by the variation of reaction temperature. At the Qd,HNO3 (20.083) (30)
same time, the reaction temperatures in the hexamine- NHA+NHNO3 0.071+1.711
nitric acid reaction system are also affected by the 1.711
chemical consumption of hexamine. In order to evaluate (2.931)3.614 (kJ/mole)
0.07+1.711
the transient reaction temperature and fractional conver-
sion in the hexamine-nitric acid reaction system, we have
to solve Eqs. (25) and (26) simultaneously. The required Thus, we can evaluate the generation heat qg per mole
heat capacities and generation heats in the calculations hexamine by adding up Eqs. (29) and (30) as
of xA(t) and q(t) have to be evaluated from the average
qg[H0f,0Qd,m][87.3243.614] (31)
values of mixture components in the nitric acid-hexam-
ine reaction system. Table 3 shows the values of heat 90.938 (kJ/mole)
capacities (Cp), for each component in this reaction sys-
tem, heat of formation (H0f) and heat of dilution (Qd) The initial dilution heat of nitric acid and hexamine is
which were obtained from Dai et al. (1996).
Qd,0NHAQd,HANHNO3Qd,HNO3(0.071)( (32)
2.1. Evaluating the values of qg, CP,m and qo
20.083)(1.711)(2.931)6.441 kJ
The generation heat in the hexamine-nitric acid reac-
tion system includes the heat of formation and dilution At initial time, the heat of dilution can also be
heat of nitric acid and hexamine. The heat of formation expressed as mixing of nitric acid and hexamine as

Table 3
Heat capacities and heat of formations in the reaction of hexamine-nitric acid system and dilution heat of hexamine and nitric acid

Property Chemical C6H12N4 HNO3 C3H6N6O6 CH2(ONO2)2 NH4NO3 H2O

Hfo KJ/mole 136.817 173.218 71.546 199.158 365.263 285.830

CP KJ/mole.K 0.176 0.125 0.307 0.227 0.141 0.075
KJ/kg.K 1.256 1.989 1.382 1.926 1.759 4.187
Qd KJ/mole 20.083 2.931
 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127
Qd,0(WHACp,HAWHNO3Cp,HNO3)(TTa)
WTCP,m(TTa)
Thus, the value of (TTa) at initial time is
Qd,0
(TTa)initial
WHACp,HA+WHNO3Cp,HNO3
27.841 K
If we set the values of Ta is equal to 25C, the dimen-
sionless temperature at initial time can also be determ-
ined as
E 47149
q0 2
(TTa)initial (27.841)
RT a 8.314298.162
1.776
These values of CP,m, qg and qo should be used in the
calculation for the critical condition.
A typical calculation in this batch reaction system for
f=0.95, b=0.053 and j=0.533 is shown in Fig. 4. The
dimensionless reaction temperature profile increases in
the beginning but decreases at the end of chemical reac-
tion. There is a maximum temperature point, i.e.
q=qmax=2.17, at the dimensionless reaction time
t=tmax=0.318. Another calculation shows the variation
of fractional conversion of hexamine profile increases
very fast at the starting time of reaction. It reaches
almost a constant value after the reaction time is greater
than the value of tmax.
However, the transient temperature profiles do not
always behave the same as in Fig. 4. Some of the dimen-
sionless temperature profiles go to the maximum point
qmax very quickly and sharply. The reaction temperatures
may increase very quickly to a higher degree in a reac-
tion time. Sometimes they decrease directly to a low
Fig. 4. The relationships of q and xA versus t for the production of
RDX in a non-isothermal batch reactor.
125
(33) degree after the chemical reaction is proceeded. Fig. 5
shows the calculations of dimensionless reaction tem-
perature q versus the dimensionless reaction time t with
various values of f as parameters in a batch reactor of
hexamine-nitric acid reaction system. The values of f
for the curves of A, B and C are equal to 200, 140 and
100, respectively. These three curves of dq/dt increase
(34)
to an infinite large value when the dimensionless reac-
tion time, t, reaches some confined value. These mean
that dq/dt at confined time. This phenomenon in the
reaction system is a runaway reaction. The values of f
for the curves of E, F and G are equal to 20, 5 and 1,
respectively. The situation of dq/dt never happens
for these three curves. Thus, the conditions for these
three curves belong to safe reaction. The dashed curve
(35) D is the value of f which is equal to 60.712. This curve
is the critical curve for the reaction system either goes
to the runaway or safe reaction when the values of f are
larger or less than the value of this critical value of
60.712. We define the value of f at this critical curve
as fC for a given b. When ffC, the reaction system
goes to the runaway situation. Otherwise, when ffC,
the reaction system is safe.
The transient fractional conversions of hexamine cor-
responding to each value of f is shown in Fig. 6. The
values of xA increases to unity very quickly when the
values of j are relatively higher. When the values of j
are relatively lower, the values of xA grew gently to
unity. For a given value of b, the value of f at the critical
condition of runaway reaction, fC, can be obtained by
means of trial and error iterations. When the value of b
is changed, the value of fC is also changed. Fig. 7 shows
the variations of fC are varied along the increasing of
b. We can express fC as a function of b by means of
mathematical curve fitting in this calculated fCb data
and obtain the following equation as:
Fig. 5. The affection of f value on the q trajectories along the vari-
ation of t for the production of RDX in a non-isothermal batch reactor.
126 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127

hS
V

cr
RqgACNOCnAO
Eb2e1/bfC
(37)

Fig. 8 shows the required critical values of heat trans-

fer per unit volume of batch reactor in the hexamine-
nitric acid batch reaction system. The calculated curve
of (hS/V)cr using Eq. (37) is the watershed of safety and
runaway situation. Below this curve, the reaction
belongs to runaway region. Another region above this
critical curve belongs to safe reaction region.

3. Conclusion

Fig. 6. The affection of j value on the Xa trajectories along the vari- In the reaction of hexamine-nitric acid system to pro-
ation of t for the production of RDX in a non-isothermal batch reactor. duce RDX in a batch reactor, its reaction rate is
5671.062
rA1.234106e T CNOC1.28
A

The batch reaction system of RDX production being

either runaway or safe can be evaluated from the values
of f. This system is safe when the values of f is less
than fC. On the contrary, this system is runaway if the
values of f are larger than fC. The values of fC at the
critical runaway condition in a batch reaction of RDX
is a function of b and expressed as:
fC20.4374.805/[1exp(336.7b15.65)]

For a reactor design of RDX production, the values

of heat transfer are important for its safety. Its required
heat transfer per unit volume of reactor at critical con-
dition is determined by the term:

Fig. 7. The relationship of fc and b at the critical runaway condition
for the production of RDX in a non-isothermal batch reactor. hS RqgACNOCnAO

V cr b2Ee1/bfC
4.805
fC20.437 (36)
1+exp(336.7b15.65)

From this equation, we can evaluate the value of fC

at the runaway condition for various values of b. Thus,
when the value of f in a hexamine-nitric acid batch reac-
tion system is determined, we can evaluate whether a
reaction system is runaway or safe by the following cri-
teria:
ffC reaction system goes to runaway.
f=fC critical runaway.
ffC reaction system is safe.

By combining Eqs. (28) and (21), the critical value

of heat transfer coefficient in a control volume can be Fig. 8. The critical required heat transfer coefficient per unit volume
expressed as reactor for the production of RDX.
 K.-M. Luo et al. / Journal of Loss Prevention in the Process Industries 15 (2002) 119127
For safe production of RDX, the values of (hS/V) must
be greater than the values of (hS/V)cr.
Acknowledgements
The authors gratefully acknowledge the support of the
National Science Council of the Republic of China under
grant NSC 89-2214-E014-001.
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