Powder Technology 205 (2011) 81–86

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Powder Technology
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / p ow t e c

Dust/gas mixtures explosion regimes

A. Garcia-Agreda a, A. Di Benedetto b,⁎, P. Russo c, E. Salzano b, R. Sanchirico b
a
Dipartimento di Ingegneria Chimica, Università di Napoli, Italy
b
Istituto di Ricerche sulla Combustione, Consiglio Nazionale delle Ricerche, Napoli, Italy
c
Dipartimento di Ingegneria Chimica e Alimentare, Università di Salerno, Fisciano (SA), Italy

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

Article history: The explosion features of nicotinic acid dust in atmosphere of methane and air at different concentrations of
Received 4 February 2010 either dust or gaseous fuel are studied. Experimental measurements of the pressure history, deflagration
Received in revised form 15 July 2010 index and flammability limits are performed by the standard 20 l Siwek bomb though adapted for such hybrid
Accepted 30 August 2010
mixtures.
Available online 7 September 2010
Data show non linear effect of explosion severity and the synergistic effects when hybrid mixtures explode.
Results allow the definition of five different regimes of the gas/dust/air mixture explosion in the plane dust
Keywords:
Dust explosion
concentration vs. fuel concentration.
Hybrid explosion © 2010 Elsevier B.V. All rights reserved.
Nicotinic acid
Deflagration index

1. Introduction
More than one century ago, in 1885, Engler [1] observed that
mixing coal dusts with methane at a concentration lower than the
methane lower flammability limit (i.e. 2.5% in air), would allow the
explosion of the dust/gas mixture, hence producing unexpected
hazardous conditions.
Since that, many studies have been performed to reveal the origin
of such behaviour and also to measure the ignition propensity of such
dust/gas mixtures frequently named “hybrid” mixtures [2–11].
The most extensive work on hybrid mixtures has involved the
measurements of the lean flammability limits of coal dust with
methane addition [7,12]. For these mixtures, it was found that dust
concentration required for flammability conditions may be predicted
by Le Chatelier's Law, originally developed and adopted for homoge-
neous gas mixtures [13]. This curve is a straight line between the lean
flammability limits for pure coal dust and pure methane, and the
weighting factor for each fuel is its content in the mixture.
Le Chatelier's law was derived by the concept of a constant limit
flame temperature for a given class of fuels. In the case of methane and
coal dust mixtures such temperatures are comparable and then the
linear trend is valid.
However, Cashdollar [8] has found some deviation from Le
Chatelier's rule when methane mixes with Pocahontas coal, which is
characterized by low content of volatiles. Bartknecht [4] has also
⁎ Corresponding author.
E-mail address: dibenede@irc.cnr.it (A. Di Benedetto).
shown that if methane or propane is admixed to PVC dust in air, the
lower explosion limit of the dust/gas/air mixture decreases with
increasing the gas concentration by a second order equation which is
known as the curve for flammability limit of hybrid mixtures.
The data of Gaug, as referred by Hertzberg & Cashdollar [14], for
hydrogen addition to cornstarch dust, also have showed significant
deviation from Le Chatelier's relationship, thus indicating that a
higher amount of dust is required to render the system flammable
with respect to that predicted on the basis of Le Chatelier's Law.
Concerning the explosion severity, the explosion parameters
(maximum pressure and deflagration index) have been mea-
sured extensively at changing the dust and gas concentrations
[11,15–18]. But it is not yet clarified whether the dust or the gas is
driving the explosion phenomena at changing the dust/gas ratio and
the fuel/air ratio.
Dufaud et al. [15,16] have studied the influence of pharmaceutical
dusts and their associated solvent (ethanol, di-isopropyl ether,
toluene) concentrations on maximum pressure and maximum rate
of pressure rise. Their results on hybrid mixtures have highlighted a
promotion effect on the combustion kinetics and on the rate of
pressure rise for poor mixtures. Furthermore, they have noticed that
the maximum value of the deflagration index is found for dust/gas (or
dust/vapors) rather than for the pure fuels, thus concluding that there
are more than simple additive effects on explosion severity.
These studies were performed in the equipment ad hoc developed
for dust explosion tests in which ignition of the dust/air suspension is
performed by using two chemical igniters of total 10 kJ. The
contribution of the gas in the gas/dust/air mixtures with respect to
explosion severity and ignitability may be significantly influenced by
such ignition energy.

0032-5910/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.powtec.2010.08.069
82 A. Garcia-Agreda et al. / Powder Technology 205 (2011) 81–86

Denkevits [11] has studied the ignitability of the dust constituent

and its influence on the hybrid explosion severity of the graphite/
hydrogen/air mixtures by adopting a weak electric spark. He found
that the use of low-energy sparks allowed the identification of
different stages of explosion evolution at changing the hydrogen
content, which cannot be deduced by the simple combination of the
behaviour of the two components.
In this framework, the authors make some efforts aiming at
clarifying the synergetic effects of dust and gas in air during explosion.
We have previously investigated the effect of particle size on both
dust and hybrid mixture explosions and proposed a way to predict KSt
for hybrid mixtures [19–21]. We have underlined the avoidance of
both fine dust sizes and hybrid mixtures is a beneficial approach in the
process industries to reduce the risk arising from the hazards posed by
combustible dusts and their mixtures with flammable gases.
More recently we have studied the effect of the initial turbulence,
by varying the ignition delay time, on the explosion of a model hybrid
mixture at varying the gas content in mild ignition conditions [22].
The model gas/dust mixture here used is composed by CH4 and
nicotinic acid whose single behaviour is well identified and quantified Fig. 1. Scheme of the 20 l bomb.
in the literature.
The present paper is focused on the identification of explosion
regimes for the same model gas/dust/air mixture by using a weak circulating crio-thermostat for the temperature control (Julabo
electric spark ignition. More specifically, the paper is addressed to the CF31). In all runs water was used as the cooling fluid, at 25 °C.
quantification of the severity of explosion of hybrid mixtures in terms The partial pressure method is used for the feed of the methane gas
of maximum pressure and deflagration index and to the definition of in the bomb. It consists of the following steps: i) the sphere is
the most severe zones in the dust/gas concentration plane plot. evacuated up to PA = −0.8 barg; ii) pure methane is fed until the
Explosion experiments were performed in the 20 l Siwek bomb, required pressure (PB) to obtain a given methane concentration in air;
but using a weak electric spark ignition source instead of standard iii) air is fed up to PC = −0.6 barg. The values of set pressure at
chemical igniters. The strong ignition energy of chemical igniters may different methane concentrations are reported in Table 1. Dry air is fed
indeed in some cases hide some interplay phenomena between dust in the dust container (with or without dust) up to 20 barg pressure.
and gaseous fuel, overdriving the explosion behaviour. While it is Then outlet valve (V2) is opened reaching the initial pressure
strictly demanding that the explosion investigation has to be (P0 = 0.0 barg) in the sphere.
performed in the same experimental conditions for comparing the Pressures were measured by means of the manometer M (Dwyer
explosion behaviours of dust alone, of gas alone and of a mixture of Series 626).
them. Finally, the results of this work may be generalized and utilized Minor hardware modifications on KSEP 320 have allowed the
as guidelines for estimating and predicting the performances of dust/ possibility of varying the spark delay time (tV). This parameter is
gas mixtures from those of pure compounds. crucial because it determines the turbulence level when spark is
triggered. tv is defined as the time at which the primary coil of the
2. Methods high voltage transformer is energized with respect to the time at
which the pressure signals measured by PT1 and PT2 start to increase.
2.1. Experimental In this paper the tests were all performed at tv = 0. We selected tv = 0
to avoid methane/dust un-mixedness and stratification. The fuel
The experiments have been performed in the standard 20 l mixtures are made of nicotinic acid supplied by Sigma Aldrich and
apparatus manufactured by Adolf Kühner AG (CH). The system has methane.
been modified to be used for hybrid mixtures; this modification Nicotinic acid, used as received, has been characterized by laser
consists essentially in the addition of the feed line for the gases. A diffraction granulometry using di-ethyl ether as the disperdant
scheme of the setup is reported in Fig. 1. solvent (Malvern Instruments Mastersizer 2000); scanning electron
The equipment is made of a stainless steel spherical bomb surrounded microscopy (Philips mod. XL30); simultaneous TG/DSC analysis (TA
by a water jacket for the control of the internal wall temperature. Instruments SDTQ600).
A flange on the top of combustion chamber allows for the insertion of The explosion experiments have been performed varying the
two electric rods, in order to reach the center of the sphere for spark methane concentration (v/v-%) in the range 1.0–10% and for the
electrodes. In the present study, a permanent spark generator capable to nicotinic acid in the range 30–250 g m−3.
supply 15 kV, 30 mA as produced also by Kühner (KSEP 320) has been
used. The spark electrodes were two rounded tungsten rod (diameter
2 mm) whose tips were spaced at the standard distance of 6 mm. Table 1
At the bottom and right side of the bomb, the outlet valve V2 and Set pressures for preparation of the methane/air mixture in the bomb.
the two piezoelectric transducer PT1, PT2 (Kistler Type 701A) are
CH4 SET (%v/v) PA (bar g) PB (bar g) PC (bar g) P0 (bar g)
installed. The outlet valve is connected to a rebound nozzle placed at
the bottom of the bomb for the dispersion of the dust/air mixture. 1 −0.80 −0.79 −0.60 0.0
1.6 −0.80 −0.78 −0.60 0.0
The input section of the outlet valve is connected to the sample
2.3 −0.80 −0.78 −0.60 0.0
container SC (VSC = 0.6 l). All the timing sequences and the 3 −0.80 −0.77 −0.60 0.0
acquisition of the pressure signals are performed by means of the 3.6 −0.80 −0.76 −0.60 0.0
electronic module KSEP 332, which is interfaced by a desktop 6 −0.80 −0.74 −0.60 0.0
computer for the remote control of the system. The system is also 7.3 −0.80 −0.73 −0.60 0.0
10 −0.80 −0.70 −0.60 0.0
connected to a vacuum pump (Vacuubrand RZ9) and to a re-
 A. Garcia-Agreda et al. / Powder Technology 205 (2011) 81–86
Experiments were carried out in triplicate: the standard deviation
and the accuracy of our data are Pmax ≤ ± 5% and KSt ≤ ± 15%.
2.2. Theoretical evaluation
The measured peak pressures of the mixtures dust/air and
methane/air were compared with the theoretical adiabatic pressure.
Such parameter was computed by means of the CEA (Chemical
Equilibrium with Applications) thermo-equilibrium code [23].
Furthermore, we calculated the equilibrium volatile content and the
volatile product distribution of nicotinic acid by using the CEA code.
The CEA code allows the calculation of the equilibrium conditions
by minimizing Helmholtz energy at constant temperature and
volume; or by minimization of Gibbs free energy, for the chemical
equilibrium at constant temperature and pressure.
3. Results
In the following we report the explosion results obtained in our
equipment for each fuel (methane and nicotinic acid) and then we
discuss the results of the explosion behaviour of their mixture at
changing the CH4/nicotinic acid ratio.
3.1. Methane explosion
The explosion behaviour of methane has been widely studied and
it is well known in the literature.
Conversely, few papers deal with the explosion behaviour measure-
ments of methane/air mixtures in the standard conditions of dust/air
explosion in the 20 l bomb, at quiescent conditions [24–27].
In the present work the ignition of methane/air mixtures is
performed at the same conditions as the dust runs (gas mixture
injection and tv = 0; spark ignition) in order to allow the comparison
between the pure fuel behaviour and the gas/dust/air behaviour.
Fig. 2 shows the maximum pressure and the deflagration index as
measured for the methane/air explosion with respect to the fuel
concentration. The literature data for the deflagration index as reported
by Senecal [27], Bartcknect [28] and NFPA [29] are also given. These
values were obtained in apparatus different from the 20 l spherical
bomb and are significantly lower than those found in our experiments.
Fig. 2. Maximum explosion pressure and deflagration index as function of methane
concentration. KG of methane from experiments (spark ignition, tv = 0) and literature
data.
83
The data of the deflagration index from Dahoe & de Goey [24],
Cashdollar et al. [25] and Mashuga & Crowl [26] are also shown, but a
significant difference is found due to the highly turbulent conditions,
which establish inside the bomb at a delay time tv = 0 used in the
present paper.
The adiabatic pressure as calculated by means of the CEA code is
also shown. The calculated values are higher than the peak pressure
measured due to the effect of heat losses.
3.2. Nicotinic acid explosion
The nicotinic acid is an organic compound classified as a B-vitamin.
It belongs to the B-vitamin sub-class known as Niacin (Vitamin B3),
with the molecular formula C6H5NO2 (Fig. 3). It is used mainly in
pharmaceutical industries and also is a reference dust for testing dust
explosion.
The sample structure has been analysed by means of scanning
electron microscopy. SEM images of nicotinic acid, reported in Fig. 4 at
two different magnifications, show that the sample is composed of
smooth-faced prismatic particles.
Details of the granulometric distribution of the nicotinic acid are
given in Table 2.
The simultaneous TGA-DSC test (N2 flow rate of 100 ml/min;
heating rate of 20 °C/min) carried out on the nicotinic acid sample
revealed the absence of moisture in the dust. Furthermore, in the
explosion tests we used cylinder dry air rather than ambient air.
The complete combustion of the nicotinic acid is the following:
2C6 H5 NO2 þ 25=2O2 →12CO2 þ 5H2 O þ N2 : ð1Þ
From this equation, it is possible to calculate the stoichiometric
dust concentration, which results in C = 168 g/m3.
In Fig. 5 the maximum pressure (Pmax,) attained in the sphere and
the deflagration index (KSt) are shown as a function of the dust
concentration. It appears that the maximum value of both Pmax and KSt
is attained at about C = 600 g/m3, which is much higher than the
calculated stoichiometric value, C = 168 g/m3. These data are similar
to those found in the literature [15,30–32] and reported in Table 3. In a
previous paper Di Benedetto and Russo [33] showed that the
explosion of dust can be modelled as the explosion of its volatiles.
In order to get insights into this difference, we have calculated the
thermodynamic distribution of the volatiles of nicotinic acid by using
the CEA code. In this regard, we have found that in the range of
temperatures from 700 °C to 1800 °C the volatile content ranges from
25% up to 26% in weight. This result definitely agrees with the ratio
between the stoichiometric dust concentration and the value at which
the maximum pressure and deflagration index occur (168/
600=0.28). In the following the experimental data are compared
with the thermodynamic values estimated at the respective equiva-
lent dust concentration Ceq calculated as follows:
Ceq = C = f ð2Þ
where C is the experimental concentration, and f is the fuel volatiles
content of nicotinic acid in the temperature ranges of interest
Fig. 3. Structural formula of nicotinic acid.
84 A. Garcia-Agreda et al. / Powder Technology 205 (2011) 81–86
Fig. 4. SEM images of nicotinic acid at 2500 × (up) and 8000 × (down) magnification.
(f = 0.26). The factor f is here defined as the dust “equivalent”
concentration, according to the volatile content.
In the experimental conditions of this work we found that the
minimum explosive concentration (MEC) of the nicotinic acid is equal
to 125 g/m3. This value is higher than those found in the literature
(Table 3); this difference is probably related to the weak ignition here
used (spark ignition instead of chemical igniters).
In Fig. 5 the adiabatic pressure as computed by CEA is also showed.
These data are shifted in the concentration range by the factor f
(Eq. (2)).
3.3. Explosion of nicotinic acid/methane air mixtures
The explosion behaviour of the methane/nicotinic acid mixture in
air has been investigated in the conditions close to the minimum
concentration values of both methane (1% up to 7.3%) and nicotinic
acid (30 g/m3 up to 250 g/m3).
In Fig. 6 the maximum pressure is plotted vs. the methane
concentration at six values of the nicotinic acid concentration in the
range C = 0–250 g/m3.
When the dust concentration is lower than MEC = 125 g/m3
(C = 0, 30 and 60 g/m3), ignition is observed at CH4 concentration
higher than 3.6%. On further increasing the methane content the
mixture is ignited, even if both the fuels are below their flammability
(or explosibility) limits.
At MEC = 125 g/m3, the maximum pressure is slightly dependent
on the methane content. At higher values of dust concentration (190,
or 250 g/m3) the maximum pressure seems to be almost independent
on the methane content.
From these results it appears that when methane concentration is
lower than lower flammable limit (LFL) the thermodynamic para-
meters become less sensitive to the methane content when dust
concentration goes from non-flammable concentration (C b MEC) to
flammable concentration (C N MEC).
Table 2
Granulometric distribution of nicotinic acid.
Percentile diameter (μm)
D (0,1)
D (0,5)
D (0,9)
Surface weighted mean diameter (μm)
D (3, 2)
Volume weighted mean diameter (μm)
D (4, 3)
In Fig. 7 the corresponding data of the deflagration index are given.
The results plotted suggest that in the range of concentrations
investigated, the presence of methane in a cloud of nicotinic acid
makes the dust more violent and reactive than the pure nicotinic acid.
Conversely, in the conditions here investigated, it seems that the
methane/air mixture explosions (C = 0) are much more severe than
that of the methane/nicotinic acid/air mixtures.
At dust concentrations below the MEC (C = 30 and 60 g/m3), the
nicotinic acid alone is unable to ignite, but the presence of methane
activates the explosive reaction. At dust concentration equal to the
MEC (C = 125 g/m3), the presence of methane has a significant impact
on the violence of explosion: the deflagration index increases (from
20 to 470 bar m/s) about 20 times when increasing the methane
content from zero up to the LFL (6%).
At values of the dust concentration higher than the MEC value
(C = 190 and 250 g/m3), the presence of methane increases the
violence of explosion, but its influence is less significant (the
deflagration index goes from 80 up to 490 bar m/s and 120 up to
410 bar m/s respectively). As a result, the sensitivity of nicotinic acid/
methane/air mixtures to methane content in the non-flammable
region of methane (bLFL) decreases when the dust concentration is in
the flammable region.
It is worth noting that an inversion occurs: at dust concentration
higher than MEC and at low values of the methane content, the
highest value of the deflagration index is at the lowest dust
concentration; conversely, at high values of the methane content,
5.56
32.00
93.06
14.37
Fig. 5. Maximum pressure and deflagration index as a function of the dust
41.43
concentration. (Nicotinic acid, spark ignition, tv = 0).
 A. Garcia-Agreda et al. / Powder Technology 205 (2011) 81–86
Table 3
Literature data of nicotinic acid.
Pmax (bar) KSt (bar m/s) MEC (g/m3) C@ max (g/m3) Ignition Ref.
8.4 214 60 500 2 × 5 kJ
8.0 ± 10% 241 ± 10% – 520 (Pmax) 690 (Kst) 2 × 5 kJ
8.1 ± 10% 232 ± 10% – 680 (Pmax) 880 (Kst) 2 × 5 kJ
8.3 ± 10% 236 ± 10% – – 2 × 5 kJ
7.2 ± 5% 179 ± 15% 125 600 spark
the highest value of the deflagration index is at the lowest value of the
dust concentration.
From these results it can be concluded that methane and nicotinic
acid have comparable thermodynamic pressure and then temperature
(Fig. 6). Conversely, the kinetic behaviours (Fig. 7) are quite different.
3.4. Niacin/methane/air explosion regimes
In order to rationalise all the data, we have developed the map of
the explosion behaviour of the CH4/nicotinic acid/air mixtures, where
methane content (vol.%/LFL) and dust concentration (C/MEC) are
respectively the x- and y-axes (Fig. 8). In the figure, the measured data
of the deflagration index are represented by the solid circles whose
diameter increases proportionally to the value of Kst. White circles
refer to experiments where explosion does not occur.
In the same figure, Le Chatelier's line and Bartknecht curve are also
shown. These curves delimit the explosive vs. the non-explosive
region. Finally, the stoichiometric line (red curve) is also plotted. The
equation of this line is the following:
C = MEC = 4:8–3:03yCH4 = LFL
The white circle symbols lay all below Le Chatelier's line, which
limits the non-flammable zone. All the other points represent
explosion conditions. Le Chatelier's line well separates the explosive
from the non-explosive region since as shown in Fig. 8, the adiabatic
pressure of methane/air and nicotinic acid/air mixtures (and then
temperature) are quite similar.
In the plot of Fig. 8, five zones may be identified. The no-explosion
zone lays below Le Chatelier's curve.
Above this line the synergic explosion behaviour zone is present.
This zone is limited by Le Chatelier's curve and the LFL and MEC lines.
The dust (fuel) driven explosion zone is the region in which the dust
(fuel) concentration is higher than the MEC (LFL) and the methane
(dust) concentration is lower than the LFL (MEC).
Fig. 6. Maximum pressure as a function of the methane content at different values of the
nicotinic acid concentration ( spark ignition, tv = 0).
85
[16]
[30]
[31]
[32]
this work
Fig. 7. Deflagration index as a function of the methane content at different values of the
nicotinic acid concentration (spark ignition, tv = 0).
Finally, the dual-fuel explosion zone is above both LFL and MEC
concentrations. In this zone both methane and nicotinic acid
contribute to the explosion.
From the data of Fig. 8 it appears that the maximum values of the
deflagration index lay close to the stoichiometric line. When
approaching this line the diameter of the solid circles increases. It is
also worth noting that in the region where the oxygen is controlling
the kinetics of explosion, the diameter of the circle is almost
insensitive to both the dust and methane concentrations.
ð3Þ 4. Conclusions
In this work measurements of explosivity of methane/nicotinic
acid/air mixtures are carried out in a modified spherical bomb. The
experiments have been performed varying the methane concentra-
tion in the range 1.0–10% and for the nicotinic acid in the range 30–
250 g m−3. A spark ignition was used.
From the results obtained the following conclusions may be
drawn:
1. the volatile content of the dust significantly affects the stoichio-
metric and the minimum explosive concentration;
2. the adiabatic pressure of methane and nicotinic acid are compa-
rable and then their mixture verify Le Chatelier's criterion for
flammability: the methane/nicotinic acid mixture may be defined
as a similar mixture;
Fig. 8. Explosion regimes in the plane methane content/nicotinic acid concentration.
86 A. Garcia-Agreda et al. / Powder Technology 205 (2011) 81–86
3. the explosion behaviour of the methane/nicotinic acid mixture
may be classified in five different regimes in the plane dust
concentration vs. fuel concentration;
4. these results may be extended to all the gas/dust/air mixtures
which are similar.
Acknowledgement
The authors wish to acknowledge Mr. Andrea Bizzarro for his
technical support.
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