ISSN 0012-5016, Doklady Physical Chemistry, 2007, Vol. 416, Part 2, pp. 265–270. © Pleiades Publishing, Ltd., 2007.

Original Russian Text © A.A. Koptelov, Yu.M. Milekhin, S.A. Gusev, 2007, published in Doklady Akademii Nauk, 2007, Vol. 416, No. 4, pp. 496–501.

PHYSICAL
CHEMISTRY

Application of Thermal Analysis Methods to Studying

the Kinetics of Thermal Decomposition of Energetic Materials
A. A. Koptelov, Yu. M. Milekhin, and S. A. Gusev
Presented by Academician Yu.D. Tret’yakov May 21, 2007

Received May 21, 2007

DOI: 10.1134/S0012501607100016

Studies of the formal kinetics of thermal decompo- By DSC, DTA, and TG methods, they obtained 38 dif-
sition of energetic materials in the condensed phase are ferent values of E and Z, which range from 125 to
necessary for estimating the reaction rates under the 216 kJ/mol, depending on η and T.
conditions of their synthesis, storage, processing, and
use and also for solving a number of basic problems of Using these kinetic constants, let us estimate the
chemical physics [1]. Although experimental equip- critical temperatures Tcr for HMX samples shaped as
ment is continuously being improved, the published flat plates with a half-thickness r of 2.5 × 10–3 to
data on the kinetic parameters of thermal decomposi- 1.0 mm. In an isothermal experiment, Tcr is found from
tion of energetic materials show very wide scatters. In the equation
our opinion, these scatters are largely determined by
subjective factors, first of all, insufficiently detailed r ρQZE
2
δ* exp ⎛ ----------⎞ = -------------------
E
design of experiments. Among methods for studying -. (2)
⎝ RT cr⎠ λRT cr
2
the kinetics of transformation of energetic materials on
heating, the most informative are thermal analysis (TA)
methods: differential scanning calorimetry (DSC), dif-
ferential thermal analysis (DTA), and dynamic and iso- Table 1. Kinetic parameters of thermal decomposition of
thermal thermogravimetry (TG). The purpose of this HMX in the condensed phase (monomolecular reaction) [2−4]
work is to analyze the sources of errors in determining
Ti – T *f , E, Z,
the kinetic parameters of thermal decomposition of No. Method
K kJ/mol s–1
energetic materials from thermal analysis data and to
find the experimental conditions under which these 1 DSC 504–547 220.6 5.00 × 1019
errors are minimal. The quantitative data presented 2 DSC, DTA, TG 473–533 165.0 2.00 × 1013
below on decomposition kinetics mainly describe octo-
gen (HMX); however, the conclusions drawn are also 3 IR spectroscopy 439–467 204.3 6.31 × 1019
equally applicable to other types of energetic materials. 4 DTA 502–542 187.1 7.94 × 1015
The scatter of experimental values of the kinetic 5 Chromatography 503–543 221.4 2.51 × 1018
constants for thermal decomposition of HMX in the 6 TG (O2) 502–542 208.0 1.26 × 1017
condensed phase can be illustrated by the monomolec- 7 TG (air) 502–542 205.1 1.00 × 1017
ular reaction data (Table 1): 8 DTA (N2 , 3.5 MPa) 502–542 108.4 3.16 × 108
9 TG (N2, 105 MPa) 502–542 146.9 3.16 × 1011
------ = Z exp ⎛ – -------⎞ ( 1 – η ),
dη E
(1) 6.31 × 1018
dτ ⎝ RT ⎠ 10 DSC 544–558 214.6
11 Barometry 403–453 158.6 1.58 × 109
where η is the degree of decomposition, τ is time, E is 12 Barometry 534–549 205.1 6.31 × 1017
the activation energy, and Z is the preexponential factor.
13 DTA 433–523 113.0 1.00 × 1010
In our calculations, along with the data in Table 1, 14 DTA 458–533 172.5 2.00 × 1014
we also used other estimates for the first-order reaction,
which were taken from Burnham and Weese’s work [4]. 15 Barometry 453–458 171.6 6.31 × 1012
16 Barometry 423–443 150.7 6.31 × 1010
Soyuz Federal Center for Dual-Use Technologies, 17 Barometry 449–503 158.6 1.58 × 1011
ul. Akademika Zhukova 42, Dzerzhinskii,
Moscow oblast, 140090 Russia * Initial and final values of the investigation temperature range.

265
266 KOPTELOV et al.

Table 2. Names and numerical values of the parameters of Eqs. (2) and (3)
Characteristic Notation Dimension Numerical value
Sample half-thickness r m from 2.5 × 10–6 to 1.0 × 10–3
Sample density ρ kg/m3 1340*
Thermal conductivity of HMX λ W/(m K) 0.29 [15]
Specific heat of HMX decomposition Q J/kg 2.0 × 106 [15]
Sample surface area S m2 1.6 × 10–5
Specific heat of HMX C J/(kg K) 391 + 2.09T [8]
Initial weight of sample m0 kg from 1.0 × 10–7 to 5.0 × 10–5
Specific heat of aluminum container (crucible) Ct J/(kg K) 785 + 0.42T
Container weight mt kg 6.5 × 10–5
Biot number Bi** – from 7.0 × 10–3 to 3.0
Initial temperature of sample T0 K 293
* ρ = kρ0 , where ρ0 = 1810 kg/m3 [15] and k = 0.74 (closest packing of identical spheres).
r
** Bi = ----------- .
ΨSλ

Table 3. Most probable values of the critical temperatures at various characteristic sizes of samples of an energetic material
with characteristics identical to those of HMX
r, mm 2.48 × 10–3 6.74 × 10–3 1.83 × 10–2 4.98 × 10–2 0.135 0.368 1.00
T cr , K 614 596 584 564 547 529 509
σ, K 19 11 21 20 14 6 9

The names and numerical values of the parameters of
Eq. (2) that were used in our calculations are presented
in Table 2. We can write δ* = ϕ(Bi)δ0 [5], where, for the
planar geometry, we have δ0 = 0.88; the function ϕ(Bi)
for arbitrary Biot numbers can be calculated as
2
Bi Bi + 4 – Bi – 2
ϕ ( Bi ) = ----- ( Bi + 4 – Bi ) exp ----------------------------------------- .
2
2 Bi
The results of calculating Tcr are shown in Fig. 1.
Table 3 presents the most probable values of the critical
temperatures T cr and the root-mean-square deviations σ,
which were calculated under the assumption that the
distribution is Gaussian. The found Tcr values corre-
spond best to the values E0 = 165 kJ/mol and Z0 =
2.0 × 1013 s–1, which were recommended [6] for use in
“global kinetics” models (Fig. 1, curve 2). These E and
Z data were further used as calculation reference val-
ues. The data found from barometric experiments
(Fig. 1, curves 11, 15–17) and by IR spectroscopy
(Fig. 1, curve 3) are farther than ±2σ from the T cr val-
ues (the exception is barometric curve 12). Some
causes of the inaccuracy of determining the kinetic con-
stants by barometric methods have been considered in
the literature [1, 7].
The experimental data indicate that the HMX sam-
ples decompose with acceleration (are ignited) either
directly at the onset of melting or after partial melting
[4, 8]. An abrupt increase in the decomposition reaction
rate in the formation of the liquid phase is also charac-
teristic of other energetic materials. Therefore, the cal-
culated Tcr values exceeding the melting point Tm
(for HMX, ~550 K) are conditional. Previously deter-
mined [8] extremely high (1100–8800 kJ/mol) E values
are likely to be related to attempts to describe the
decomposition curves in the melting zone.
Let us consider the possibilities of the DSC method
in studying the kinetics of decomposition of energetic
materials in the solid phase. DSC devices record the
power q (W) of heat release (absorption) on heating a
test sample. According to a mathematical model of
DSC [9], the set of equations describing the thermal
decomposition of energetic materials in the dynamic
heating mode has the form
dq dT
Ψ Σ C s ------ = – q + ( C s – C r ) ---------p
dτ dτ
(3)
– m 0 QZ exp ⎛ – ---------⎞ f ( η ),
E
⎝ RT s⎠
------ = Z exp ⎛ – ---------⎞ f ( η ).
dη E
(4)
dτ ⎝ RT s⎠

DOKLADY PHYSICAL CHEMISTRY Vol. 416 Part 2 2007

 APPLICATION OF THERMAL ANALYSIS METHODS TO STUDYING THE KINETICS 267

Here, Cs = Cm + Ctmt, Cr = Ctmt, dTp/dτ = b is the pro- Tcr, K

grammed heating rate, Tp is the heating temperature, 700
and m ≈ m0(1 – η) is the current weight of the sample of
energetic material; the names and numerical values of
the other quantities are presented in Table 2. The valid- 1
ity of using Eq. (3) is confirmed by available experi- 2
mental data. The heat resistance ΨΣ in Eq. (3) is gener- 3
ally a complex function of heat-transfer conditions and 650 4
temperature differences in the sample–container–tem- 5
perature sensor–heater system. We restrict our consid- 6
7
eration to the case where ΨΣ = Ψ, where Ψ is limited by 8
the device; then, in Eqs. (3) and (4), Ts = Tp – qΨ = 9
T0 + bτ – qΨ. The minimal value Ψ = Ψ0 for “classical” 10
DSC devices (Perkin-Elmer) that was found in studying 600 11
the melting of metals was estimated at 75 K/W [10]. 12
The position of the baseline for q in the model consid- 13
ered is determined by solving the set of Eqs. (3) and (4) 14
at m0 = 0, and in a real experiment, by the method of 15
16
successive approximations [11]. In measurements in 17
the mode b = const, it is most convenient to compare 550
quantities of the same scale, namely, the “true” rate of
change in η with an increase in temperature

W ≡ ------ = --- exp ⎛ – -------⎞ f ( η )

dη Z E
dT b ⎝ RT ⎠
and the “normalized” DSC signal
q
W* = – -------------- .
Qm 0 b
Solving the set of Eqs. (3) and (4) under the initial
conditions T(0) = 0 and η(0) = 0 at given initial E0 and
Z0 values gave W i* (Ti) values. The kinetic constants E
and Z at f(η) = 1 – η were determined as the parameters
at which the data W i* are best approximated by the
function W(T) found from the integral form of Eq. (5).
For f (η) of more complex form, we used data process-
ing methods proposed before [4, 5]. The criterion of
quality of thermograms obtained in the numerical
experiment was the relative deviations ε of the calcu-
lated constants E and Z from E0 and Z0. The character
of the influence of b, m0Q, and Ψ on the ratio between
W* and W becomes clearer after minor transformations
of Eq. (3) using the inequality |qΨ|
Tp, which is valid
for small samples:
⎧ Qm 0 bΨE ⎫
W* ≈ W exp ⎨ W* ----------------------
2
-⎬
⎩ RT p ⎭
dW* Cm
– ΨC s b ----------- – ----------- .
dT Qm 0
Equation (7) shows that the representation of the
kinetic curve (W* → W) by the DSC signal is the more
accurate the better the conditions m0QbΨ → 0 and
ΨCsb → 0 are met. An increase in b, m0Q, and Ψ causes
a progressive increase in the deviation of the curves
(5)
500
–6 –4 –2 0
lnr[mm]
(6)
Fig. 1. Critical ignition temperature versus logarithm of the
half-thickness of an HMX sample shaped as a flat plate at
various kinetic parameters of the monomolecular reaction
of thermal decomposition. The numbering of curves in the
figure corresponds to the numbering of methods in Table 1.
W*(T) from the curves W(T), which describe the “pure”
kinetics, and, correspondingly, in the errors in deter-
mining the kinetic constants. In the example given in
Fig. 2, the error of determining E at Ψ = 750 K/W, m0 =
10 mg, and b = 0.015 K/s is ε = (E/E0 – 1) × 100% ≈ 16%.
The maximum admissible heating rate in studying
the decomposition of energetic materials in the solid
phase should be taken to be that at which, before the
onset of melting, the degree of decomposition is η ≈ 1.
From this condition, solving the set of Eqs. (3) and (4),
we obtain that the maximal b value in studying the ther-
mal decomposition of HMX in the solid phase should
not exceed 0.015 K/s (~1.0 K/min). The minimal
admissible heating rate can be estimated from the con-
dition that the signal-to-noise ratio N is suitable, which
(7)
can be written as
q max ≥ q*N min , (8)
Here, qmax is the maximal heat release power in the
sample, q* is the device sensitivity, and Nmin is the min-
imum admissible N value. Taking Nmin = 100 and qmax =
1 µW, we obtain q* = 0.1 mW. For base characteristics
of the sample, these values correspond to bmin =

DOKLADY PHYSICAL CHEMISTRY Vol. 416 Part 2 2007

268 KOPTELOV et al.

W*, W, K–1 m0, mg

102
4
0.03

5
101 5
1
0.02 4

3 100 3
0.01
2
2
1
0 10–1
450 500 550 10–3 10–2 b, K/s
T, K
Fig. 3. Approximate admissible region of heating rates and
Fig. 2. Functions W and W* versus programmed tempera- sample weights in studying the kinetics of thermal decom-
ture at m0 = 10 mg (2r = 0.46 mm), b = 0.0167 K/s, and Ψ = position of HMX by DSC. Straight lines 1 and 2 are deter-
750 K/W: (1) W*(T) calculated using Eqs. (3), (4), and (6); mined by the device sensitivity. The position of straight line
(2) baseline; (3) W*(T) corrected for the baseline drift; 3 was found from the condition that samples must not melt.
(4) best approximation of curve 3 by the function W(T) = Straight lines 4 (Ψ = 75 K/W) and 5 (Ψ = 750 K/W) corre-
T spond to the relative deviation ε ≈ 5% of the calculated E
⎛ Z ⎞
--- exp ⎛ – -------⎞ exp ⎜ – --- ∫ exp – ------ dζ⎟
Z E E and lnZ values from given E0 and lnZ0 values.
(corresponds to
b ⎝ RT ⎠ ⎝ T b Rζ ⎠
0

E = 192.3 kJ/mol and Z = 1.72 × 1016 s–1); and (5) W(T) cal-
culated at E = E0 and Z = Z0.
0.0017 K/s (~0.1 K/min). These estimates of the admis-
sible range of b for HMX are in good agreement with
experimental data [4, 5].
Figure 3 shows the admissible region of studying
the thermal decomposition of HMX in the solid phase
in m0–b coordinates. The upper boundary for m0 was
found from the condition that the value ε ≈ 5% for the
calculated E and/or lnZ values should not be exceeded.
Samples of relatively large weight may be unsuitable
because of the possible creation of conditions of a
dynamic mode of thermal self-ignition. There exists a
critical heating rate above which the kinetic factor can-
not prevent explosion [12]. The absence of thermal
explosion is guaranteed by satisfying the condition
Ω = Cb exp ⎛ ----------⎞ / ( QZ ) ≤ Ω*,
E it can also vary, depending on the fractional composi-
(9)
⎝ RT cr⎠
where Ω is the dimensionless heating rate and Ω* is its
critical value. For a first-order reaction in the quasi-sta-
e γ
2
tionary approximation, we have Ω* = -------------- , where
1 – γe
2 forms on their surface [13]. The totality of physico-
CRT
γ = --------------cr- .
QE
The calculations were performed for the most prob-
able Tcr found above for HMX and their corresponding
sample thicknesses 2r; the other parameters were taken
from Table 2. The maximum admissible weights (m0 =
2ρrS) of samples of energetic materials that correspond
to Ω = Ω* and the thicknesses of such samples at vari-
ous b are presented below.
b, K/s 0.01 0.1 0.5 1.0 5.0
m0 , mg >50 15.6 4.6 2.6 0.7
2r, mm >2 0.73 0.21 0.12 0.033
It is seen that the conditions under which there is no
thermal explosion in the mode b = const in DSC devices
are reachable; therefore, the factor that limits the heat-
ing rate in studying energetic materials by DSC is pri-
marily the distortion of the position and shape of the
device output signal (with respect to the curve describ-
ing the “true” decomposition kinetics) because of finite
heat resistance. In DSC study of solid-phase energetic
materials, powder samples are typically used. In this
case, not only can Ψ significantly exceed 75 K/W, but
tion of the sample, the packing density in the container,
T, and b, which, in real experiments, can lead to very
large errors and scatters in estimating the kinetic con-
stants.
In combustion of most individual energetic materi-
als, a melt film (more precisely, a two-phase region)
chemical processes in this region along with the heat
transfer from the gas phase determines the combustion
rate v of energetic materials. The transformations in the
solid phase occur at much lower rates and are likely to
have no noticeable effect on the character of combus-
tion [13]. A necessary condition for studying the kinet-

DOKLADY PHYSICAL CHEMISTRY Vol. 416 Part 2 2007

 APPLICATION OF THERMAL ANALYSIS METHODS TO STUDYING THE KINETICS 269

ics of decomposition of energetic materials in the melt η

is to reach quite high heating rates. The lower estimate 1.0 6
of b on the surface of energetic materials in steady com- 5
bustion can be written as 5'
0.8
2 B
v 4
b min ≈ ( T w – T 0 ) ------ ,
a 0.6 4'
where Tw is the temperature on the combustion surface 3
2
and a is the thermal diffusivity. For HMX, Tw ≈ 700 K 0.4 3'
2'
and a ≈ 1.0 × 10–7 m2/s. Taking v ≈ 4 × 10–4 m/s at a
pressure of p1 = 0.1 MPa and v ≈ 10–2 m/s at p2 =
0.2
6.0 MPa [14], we obtain bmin = 6.4 × 102 and 4 × 105 K/s, 1
respectively. The actual rates of heating of the surface
of energetic materials can exceed 106 K/s [13]. Kinetic
0 2000 4000 6000 8000 10000
studies at such b using available TA devices are impos- τ, s
sible. Even at b = 1.0 K/s, the error in determining E for
a nonmelting energetic material with characteristics
Fig. 4. Degree of decomposition of HMX samples of weight
identical to those of HMX using an “ideal” DSC device m0 = 1 mg at Ψ = Ψ0 versus thermostating time as calcu-
with Ψ = 75 K/W exceeds 6–10%. lated using (1–6) Eqs. (10) and (11) and (2'–5') Eq. (12) at
Let us evaluate the possibilities of studying the T = (1) 473, (2, 2') 493, (3, 3') 503, (4, 4') 513, (5, 5') 533,
and (6) 548 K. The time for DSC curves 1–6 is counted
kinetics of thermal decomposition of energetic materi- from the moment of reaching the isothermal mode at a rate
als by the DSC method in the isothermal mode. The of b = 0.1 K/s. The admissible time region q is to the left of
temperature is limited from below for the signal-to- line B.
noise ratio N to be high enough and from above lest the
degree of sample decomposition before reaching the
mode T = const be too high. Let us assume that we can (when the mode T = const is reached instantaneously)
create the following sample heating mode: (1) linear at T = 493, 503, 513, and 533 K; the calculation was
heating (b = const) until a given programmed tempera- performed using the formula
ture Tp is reached at the moment of time τb (when the
degree of decomposition is ηb and the heat flux power ⎧ E ⎫
is qb) and (2) treatment of the sample at Tp = const from η = 1 – exp ⎨ – Z exp ⎛ – -------⎞ τ ⎬. (12)
⎝ RT ⎠
the moment of time τb for a time that ensures a suffi- ⎩ ⎭
ciently informative change in η. The first stage is
described by Eqs. (3) and (4) under the initial condi- The minimal temperature at which the measurement
tions q(0) = 0 and η(0) = 0. The second stage is charac- accuracy is satisfactory is found from the condition q ≥
terized by the set of equations q*Nmin. At the above q* and Nmin, a suitable q value for
Qm0 = 2 J is reached at Tp ≥ 493 K (when q ≥ 0.1 mW
ΨC s ------ = – q – m 0 QZ exp ⎛ – ----------------------------⎞ f ( η ), (10)
dq E for η ≤ 0.24). At the other Tp, the admissible signal lev-
dτ ⎝ R [ T p – qΨ ]⎠ els correspond to times τ limited from the right by bro-
ken line B in Fig. 4. Assuming |qΨ|
Tp and introduc-
------ = Z exp ⎛ – ----------------------------⎞ f ( η )
dη E dη q
(11)
dτ ⎝ R [ T p – qΨ ]⎠ ing the notation V ≡ ------ and V* ≡ – ----------- , we transform
dτ m0 Q
under the initial conditions q(0) = qb and η(0) = ηb, Eq. (10) to the form
where time is counted from the moment of reaching the
isothermal mode. Calculation at a rate of reaching the ⎧ Em 0 QΨ ⎫ dV *
isothermal mode of b = 0.1 K/s for HMX samples at 2
- ⎬ – ΨC s ----------.
V * ≈ V exp ⎨ V * ------------------- (13)
⎩ RT p ⎭ dτ
E = E0, Z = Z0, and f(η) = 1 – η gives the following val-
ues for qb and ηb at various T = Tp:
Equation (13) implies that the description of the rate
Tp , K 473 493 513 533 548 of change in the degree of decomposition of energetic
materials by the experimental function V* is the more
qb , W 1.26 × 10–4 2.1 × 10–5 –4.4 × 10–4 –2.1 × 10–3 –4.3 × 10–3 accurate the smaller the ΨCs and Em0QΨ values. The
ηb 0.0013 0.0077 0.0388 0.1686 0.4196 errors in determining E in the isothermal mode depend
very strongly on the errors in determining the current
Figure 4 illustrates the dependence η(τ) at various degree of decomposition δη. For example, in calculat-
Tp (time is counted from τb). Figure 4 also presents the ing E from two curves η(τ), ε may exceed 5% even at
η versus time curves describing the “pure” kinetics δη = 0.025.

DOKLADY PHYSICAL CHEMISTRY Vol. 416 Part 2 2007

270 KOPTELOV et al.
Analogues of W* in studying the kinetics of decom-
position of energetic materials in the mode b = const by
DTA and TG methods are the functions W 1* = 3.
(Ts − Tr)/(Qm0bΨ) and W 2* = (Ts – Tp)/(Qm0bΨ), 4.
respectively; the latter formula follows from analyzing
a TG model [9] that assumes Newtonian heat transfer in 5.
the sample–heater system. Unlike the DSC model, the
heat resistances Ψ in these formulas appear explicitly, 6.
generally take much higher values than in DSC devices,
and are nonlinear functions of temperature. These basic
features of DTA and TG pose additional problems in 7.
analyzing experimental thermograms and are sources
of serious errors in determining kinetic constants. 8.
Thus, satisfactory accuracy in determining the
kinetic constants for the reaction of thermal decompo-
sition of energetic materials in the condensed phase by
9.
TA methods is reached within very narrow ranges of
heating rates and temperatures. Significant limitations
are also imposed on the size and weight of samples and 10.
the quality and reproducibility of heat-transfer condi-
tions in the sample–measuring cell system. Violation of
these limitations is one of the most obvious causes of 11.
the wide scatters of published estimates of kinetic con-
stants. 12.
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