Development of a novel mining explosive

formulation to eliminate nitrogen oxide fumes

M. Araos and I. Onederra*
Post-blast nitrogen oxide fumes (NOx) from coal overburden blasting may occur in a variety of
geological conditions with the use of bulk ammonium nitrate (AN) based explosive products. In
Australia, government directives to stop blasting activities because of NOx fume incidences have
led to costly delays in production, which has directly impacted on the ability of operations to meet
production targets. Nitrogen oxide and nitrogen dioxide can cause serious health risks to persons
exposed, with excessive levels of NO2 also affecting the viability of flora and root systems. A
number of research projects in Australia have focussed on minimising the risk of NOx fumes by
better understanding the behaviour of current explosive products. The main outcomes from these
projects have been the development and implementation of guidelines or administrative controls
to minimise the NOx fume risk and reduce the potential exposure to the hazard. This paper
describes preliminary work to provide a step-change solution that has the potential to completely
eliminate the NOx hazard. A novel formulation that substitutes the use of AN with oxygenated
water (OW) as the main oxidising agent has been developed and recently patented as part of a
PhD program at The University of Queensland. The detonation properties of mixtures made with
OW and fuel were studied. Unconfined velocities of detonation (VODs) tests of OW sensitised
mixtures were conducted. It was found that for reliable detonation to occur, a minimum level of
sensitisation must be accomplished. Adequately sensitised mixtures, with a water content of 47%
by weight, were able to detonate at velocities in the range of 2600–5000 m s21, with a critical
diameter of the order of 23 mm. The recorded detonation velocities were clearly dependent on the
mixture density and charge diameter, similar to the non-ideal behaviour of AN-based commercial
explosives.
Keywords: Nitrogen oxide fumes, Blasting agent, Explosive formulation, Detonation velocity, Oxygenated water

Introduction A comprehensive review of the literature in conjunction

Post-blast fumes are toxic nitrogen oxides, a direct
product of the detonation process, which can be easily
identified as the resultant yellow to orange to purple
post-blast clouds. These nitrogen oxides are produced by
the burning reaction and then the secondary oxidation
of NO to NO2 as the blast fumes mix with air.
With a growing number of coal mines operating in
close proximity to towns, there is significant concern
over the detrimental effects of post-blast fumes on the
surrounding communities. Exposure to these toxic gases
can have a range of negative effects on the health and
safety of exposed persons and on the surrounding
environment.
School of Mechanical and Mining Engineering, CRCMining, The University
of Queensland, Building 103–2436, Moggill Road, Pinjarra Hills, Qld 4069,
Australia
*Corresponding author, email i.onederra@uq.edu.au
with an industry survey conducted and published by
Onederra et al. (2012) indicated that fume incidences are
associated with a complex set of factors that are very
difficult to isolate in an operational environment. From
laboratory scale tests, there is a general agreement that
the conditions leading to fumes are associated with fuel
deficiencies or incomplete detonation of the explosive
product. From a practical perspective, this can be due to
one or a combination of factors such as explosive product
characteristics; confinement effects; ground conditions;
inappropriate blast design parameters; explosive product
selection; poor on-bench loading practices and potential
contamination of explosive product in the blasthole.
Mining companies, explosives suppliers and government
regulatory agencies have worked together to address the
NOx issue by implementing procedures, code of practices
and guidance (Rio Tinto Coal, 2011; AEISG, 2011;
Queensland Explosives Inspectorate (Australia), 2011).
It should be noted that AN-based commercial
explosives will always produce NOx, either in low
amounts (when explosives products properly detonate)

ß 2015 Institute of Materials, Minerals and Mining

Published by Maney on behalf of the Institute
Received 11 June 2014; accepted 23 July 2014
16 DOI 10.1179/1743286314Y.0000000074 Mining Technology 2015 VOL 124 NO 1
 Araos and Onederra A mining explosive formulation to eliminate NOx fumes

mixtures of OW/glycerol/water in different ratios were

1 Ternary diagram for the detonation range of oxyge-
nated water (OW)/glycerol/water mixtures
or large amounts (as per the above reasons). It is worth
noting that since the introduction of AN to make
Ammonium Nitrate and Fuel Oil (ANFO) or make
variants such as emulsions or water gels, research and
development of new explosive formulations for civil and
mining applications has been virtually at a stand-still.
Explosive suppliers have established AN as their key
commodity and investment into new AN plants has been
steadily increasing, particularly in countries where
mineral extraction activity has been the strongest (e.g.
South America, Australia and Africa).
In order to eliminate the NOx hazard, oxygenated
water (H2O2, hydrogen peroxide, OW), a chemical that
has the potential to replace the AN and thus the nitrogen
in the chemical structure of current explosives, is used. In
addition to the elimination of NOx fumes, other future
benefits may include the elimination of the potential risk
of discharge of AN into groundwater systems, particu-
larly when mining below the water table, and potential
improvements in overall community safety associated
with manufacturing and transportation processes.
Oxygenated water based explosives
Oxygenated water is a powerful oxidant that is produced
in large amounts around the world. The production as
of 2010 was of 2 600 000 t (SOLVAY Presentation,
2010). The main applications of OW are in the paper
mill industry, detergents, synthesis, propellants, etc.
Because of its oxidising behaviour, OW could also be
used as an explosive. In fact, the first evidence that
mixtures of OW and fuel were able to detonate dates
back to 1947 (Shanley, 1948). This work proved that
able to detonate. Results from this work are shown in
the ternary diagram in Fig. 1.
The green dashed area displays the zone at which the
OW/glycerol/water mixtures would detonate. The red
line shows the stoichiometric ratio for OW/glycerol
mixtures (i.e. oxygen balance50). Although Shanley’s
document does not provide velocity of detonation
(VOD) data, the mixtures detonated when loaded in
tubes that offered strong confinement (i.e. lead tubes).
A few years later, a patent using OW/fuel-based
mixtures was granted to Baker (Baker and Groves,
1962) In this patent, a range of different combustibles
were used (e.g. wood products, hulls and metals).
Mixtures of OW and gel-forming materials (corn starch)
were disclosed. The mixtures were sensitive to detonator
No. 6, however no VOD measurements were disclosed.
In 1990, mixtures of OW and resins were patented as
packaged explosives (Bouillet et al., 1990). Examples
provided in the patent showed that some of the mixtures
detonated at velocities above 6000 m s21 in 33 mm
diameter PVC tubes. Finally, a team at Los Alamos
National Laboratory showed that OW, at high concen-
trations, was able to detonate without fuel and without
sensitisation (Sheffield et al., 2010). The above work
indicated that both concentrated OW and OW/fuel-
based mixtures had the potential to detonate under
strong or weak confinement. Despite this, there has been
little evidence of work conducted that evaluates the
detonation properties of relatively low concentration of
OW and fuel based mixtures together with void
sensitisation techniques. These techniques incorporate
voids (hot spots) into the bulk of the explosive and have
been widely used in mining explosives to increase their
sensitivity and change their detonation characteristics.
The mechanisms that support initiation to detonation
with void sensitisation are well known (Bowden et al.,
1947). Nowadays, this technique is commonly used with
AN-based blasting agents. Voids can be provided by gas
bubbles injection (Ferguson and Hopler, 1966), glass or
Table 2 Example of formulations
% %
Oxidiser
OW (44%) 83.0 83.0
Fuel
Glycerol 14.0
Sugar 14.0
Viscosity modifier 3.0 3.0
OB 22.2 20.9
Density (g mL21) 1.19 1.20

Table 1 Energetic content comparison between OW/fuel- and ammonium nitrate-based mixtures

OW/fuel-based mixtures

44% 60% 80% ANFO ANE

Density/g mL21
0.79 0.78 0.86 0.80 0.88
Ideal VOD/km s21 3.899 4.002 4.439 4.848 4.468
Heat of reaction/MJ kg21 1.833 2.963 4.177 3.904 2.345
Relative weight strength (RWS) 44 65 93 100 64
Relative bulk strength (RBS) 44 64 100 100 71
OW: oxygenated water; VOD: velocity of detonation; ANE: ammonium nitrate emulsion.

Mining Technology 2015 VOL 124 NO 1 17

Araos and Onederra A mining explosive formulation to eliminate NOx fumes
2 Set-up of unconfined velocity of detonation (VOD) tests
plastic microballoons and/or perlite (Mullay, 1978),
materials that have air entrapped (Edamura et al.,
1985) or gas bubbles generated in the bulk of explosives
(Alfred, 1968; Edmonds et al., 1981).
The combined knowledge of OW as an oxidiser and
void sensitisation helped drive the idea that there was a
potential to develop an OW/fuel-based mixture that
could be prepared with low concentrations of OW
solution (Araos, 2013). A new formulation was subse-
quently developed and the following research questions
were posed:
N Would the mixture detonate under no confinement
and low OW content?
N Would the mixture detonate at different densities?
N If the mixtures detonate, how would they behave (as a
non-ideal or ideal explosive)?
This paper discusses the preliminary results of research
conducted to answer the above questions.
Preliminary analysis based on ideal
detonation theory
Results of the theoretical energy content for the OW/
fuel-based mixture (made with different OW strength
solutions), AN emulsion (ANE) and ANFO at densities
of approximately 0?80 g mL21 are given in Table 1. The
3 Velocity of detonation (VOD) trace for 23 mm diameter pipe at 0?79 g mL21
18 Mining Technology 2015 VOL 124 NO 1
ANE example was assumed to have a 74% of AN in the
total formula (i.e. prepared with AN solution 80% by
weight and assuming 7% of fuel phase). The heat
of formation (nHfu) for OW is 244?84 kCal mol21
(Cooper, 1996).
As shown, the heat of reactions of the OW/fuel-based
mixture (concentrations below 80% OW by weight)
is clearly lower than the one for ANFO at densities
0?80 g mL21. However, the comparison may not be
straightforward. For example, for a situation under
confinement, the reaction of the OW/fuel-based mixtures
will release only CO2 and H2O. Instead, AN-based
explosives release CO2, H2O and N2. How this will affect
the breakage performance of the product during blasting
practices is difficult to anticipate at this stage of the
research. In addition, traditional AN-based mining
explosives have up to 20% of water by weight. In the
case of OW/fuel-based explosives, the water content
could be higher. This theoretical analysis raised a
number of different questions which could only be
answered experimentally. The first stage of experiments
is discussed in the following sections.
Formulations and experimental set-up
Unconfined VOD was measured to determine if the
product would detonate; and if that was the case, how
 Araos and Onederra A mining explosive formulation to eliminate NOx fumes

4 Unconfined velocity of detonation (VOD) test of oxygenated water (OW)/fuel-based mixture

the density and diameter of the charge would in- thickness and 400 mm in length). Pipes with the
fluence it. The density of the OW solution used was explosive were loaded and fired the same day. The
1?18 g mL21. According to density tables (Huckaba and VOD was continuously measured using the MREL-
Keyes, 1948), the density indicated that the total Microtrap data acquisition system. The VOD cable was
concentration of the sourced OW was in the neighbour- externally attached to the PVC pipe and charges were
hood of 44% w/w. OW was mixed with glycerol (fuel). initiated with a 50 g pentolite booster. The booster was
Sugar, another type of fuel, was also tested to see if it initiated with an electric detonator. Figure 2 illustrates
was able to influence the detonation properties of the the set-up of the one of the firing tests.
final product.
A viscosity modifier was added to the OW/fuel-based Detonation test results
mixtures. The reason for this is that the sensitisation was
The initial density (or unsensitised density) of the OW/
achieved by using glass microballoons (GMB). The
fuel-based mixture, made with glycerol, was 1?19 g mL21.
viscosity modifier keeps the GMB dispersed throughout
It is worth noting that before these tests there was no
the explosion and prevents them from ‘floating’.
The sensitising agent used was GMB Q-Cel 520 (density Table 4 Velocity of detonation (VOD) results at different
0?13-0?15 g mL21). The sensitising agent was added in densities for sugar and glycerol
different amounts to target five predetermined densities
(0?80, 0?90, 1?00, 1?05 and 1?12 g mL21). It was noticed Sugar Glycerol
that the more GMB were incorporated, the higher the
viscosity of the final product and the longer the mixing Density/g mL21 VOD/m s21 Density/g mL21 VOD/m s21
took to achieve a good homogenisation of GMB in the 1.07 2620
product. A summary of the mixtures prepared is given in 1.04 3597 1.04 3357
Table 2. 0.98 4214 0.97 4323
The OW/fuel-based mixtures were loaded into PVC 0.87 3550 0.82 3164
tubes (23, 44 and 87 mm inner diameter, 1 mm wall 0.82 3152 0.79 2925

Table 3 Velocity of detonation (VOD) results at different diameters and densities

23 mm 44 mm 87 mm

Density/g mL21 VOD/m s2-1 Density/g mL21 VOD/m s2-1 Density/g mL21 VOD/m s2-1

1.12 F 1.12 F 1.12 2935

1.07 2620
1.04 F 1.04 3357 1.04 5074
0.97 F 0.97 4323 0.98 4852
0.90 2595
0.84 2880 0.82 3164 0.84 3800
0.79 2777 0.79 2925 0.79 3380

Mining Technology 2015 VOL 124 NO 1 19

Araos and Onederra A mining explosive formulation to eliminate NOx fumes

5 Density v. velocity of detonation (VOD) for different diameters and densities

6 Plot of density v. velocity of detonation (VOD) for ammonium perchlorate (AP), ammonium nitrate emulsions (ANE)
and oxygenated water (OW) tests

literature available on sensitised OW/fuel-based mixture of 44 mm charges, a density of 1?07 g mL21 was prepared
and therefore we tried to be cautious with the test regime. (at 44 mm diameter, the charge failed at 1?12 g mL2-1, but
Glass microballoons were used to slightly drop the density detonated at 1?04 g mL21). The intention of this new set of
from 1?19 to 1?12 g mL21. Then the OW/fuel-based tests was to find densities at which the products were able
mixtures were tested from small to large diameters. to detonate, and thus have enough data to evaluate the
At density 1?12 g mL21, the OW/fuel-based mixture unconfined VOD, diameter and density relation.
did not detonate in either 23 or 44 mm diameter. The Table 3 displays a summary of the results.
mixture, however, when tested in 87 mm, did detonate. After the above tests, the OW/fuel-based mixtures
Figure 3 shows a sample of typical VOD trace resulting made with sugar as fuel were fired. All the samples
from one of the tests. As shown, the traces obtained were detonated in 44 mm diameter pipes. The VOD results
well defined and it was easy to identify if the explosive are summarised in Table 4.
detonated or not. Figure 4 shows an example of an
unconfined VOD test with one of the OW/fuel-based Data analysis and discussion
mixtures prepared. The initial density of the product (unsensitised) was
A second round of tests was conducted with the OW/ 1?19 g mL21. From the results of the first series of tests
fuel-based mixture at density 1?04 g mL21. At this time, with sensitised product (density 1?12 g mL21 in PVC
the mixture detonated in 44 and 87 mm diameter and pipes 23, 44 and 87 mm), we observed that the product
failed in 23 mm.
The mixture in 23 mm also failed to detonate when Table 5 Velocity of detonation (VOD) and inverse
tested at density 0?98 g mL21. However, the mixture diameter results for two densities
began detonating at density 0?84 g mL21. The mixture
VOD/m s21
in diameters of 44 and 87 mm detonated at densities of
0?98 and 0?84 g mL21, respectively.
Diameter/mm (1/D)/mm21 0.84 g mL21 0.79 g mL21
Additional charges, for 23 mm and 44 mm diameters,
were prepared with the OW/fuel-based mixture. For 23 0.0435 2880 2777
23 mm, a charge with a density of 0?90 g mL2-1 was 44 0.0227 3164 2925
made (noting that for 23 mm, the charge failed at 87 0.0115 3800 3380
‘ 0.0000 3770 3347
0?98 g mL21 and detonated at 0?84 g mL21). In the case

20 Mining Technology 2015 VOL 124 NO 1


7 Plot of (1/diameter) v. velocity of detonation (VOD) for two densities
needed a minimum diameter to detonate (in this case
around 87 mm). The OW/fuel-based mixtures loaded and
tested in smaller diameter (23 and 44 mm) did not sustain
the detonation. At this stage, results were strongly
indicating that the detonation of the product would
depend on the diameter of the charge. Because the
product did not detonate at densities 1?12 g mL2-1 and
in 23 and 44 diameters, we can infer with a high degree
of certainty that the unsensitised product (density
1?19 g mL21) in those diameters will not detonate. This
is also important as it was indicated that the detonation
depended on the degree of void sensitisation.
When the density of the OW/fuel-based mixture was
dropped by the incorporation of more GMB, to density
of 1?04 g mL21, the OW/fuel-based mixtures in 44 mm
diameter began detonating. On the other hand, the
mixture at 23 mm did not detonate at that density of
0?98 g mL21 or even lower. However, by decreasing the
density further, to 0?84, the mixtures loaded in 23 mm did
detonate. These results confirm that the detonation
properties of the OW/fuel-based mixtures would also
depend on its density. This finding is described in Fig. 5.
As the density moves down from 1?12 to around
0?80 g mL21, the mixture began detonating (regardless
of the diameter of the test). The VOD increased to a
maximum, and then it drops at lower densities. The
analysis in Fig. 5 also confirms the VOD dependence with
the diameter of the charge.
8 Density v. theoretical velocity of detonation (VOD) at infinite diameter and infinite VOD for 0?79 and 0?86 g mL21,
respectively (calculated from extrapolation)
Araos and Onederra A mining explosive formulation to eliminate NOx fumes
The two above observations confirmed that the newly
proposed OW/fuel-based mixtures behave as a non-ideal
explosive (Price, 1966). Figure 6 shows the plot of
density v. VOD for examples of non-ideal explosives
(Clairmont et al., 1967; Lee et al., 1989) as well as the
results obtained from this study. Note that these re-
sults are for 76?2, 77?9 and 87?0 mm diameter tubes
[ammonium perchlorate (AP), ANE, and OW respec-
tively]. Also, AP (in Clairmont’s wok) was detonated
using no fuel (hence it has lower overall VOD). The
similarity of the curves density v. VOD for these three
explosives is clear and we could infer that OW/fuel
mixtures belong to the non-ideal class of explosives.
The data obtained from the tests allowed us to plot
the inverse of diameter (1/D (mm21)) v. VOD (m s21) in
order to obtain the VOD at infinite diameter, for density
0?79 and 0?84 g mL21. Note that the values in bold in
Table 5 were calculated by extrapolating the fitted line
for each density data.
The plot in Fig. 7 shows the calculated VOD at
infinite diameter. As expected the VOD depends on the
charge diameter.
The relationship between VOD and charge diameter
was already described by Eyring et al. (1949). At larger
diameter the VOD increases and by extrapolation, the
VOD at infinite diameter could be found – as we did in
our case. At low diameter, usually the curve veers off the
straight line as the VOD decays rapidly (right hand side
Mining Technology 2015 VOL 124 NO 1 21
Araos and Onederra A mining explosive formulation to eliminate NOx fumes
9 Density v. velocity of detonation (VOD) curve, for oxygenated water (OW)/fuel mixtures using different fuels
of the plot). At this stage, the lack of data from our
experiments does not allow us to see that part of the
curve. More testing will be conducted in the future to
confirm whether or not the OW/fuel-based mixtures
follow that trend.
Figure 8 displays the theoretical VOD at infinite dia-
meter for the density range between 0?67 and 1?20 g mL21.
The theoretical VOD for OW/fuel-based mixtures at
different densities was calculated using ideal detonation
theory.
As shown in Fig. 8, the calculated VOD at infinite
charge diameter (for products at densities 0?79 and
0?84 g mL21) is lower than the theoretical VOD
calculated from thermodynamic data. This needs further
investigation.
It is worth noting that the OW/fuel-based mixtures
detonated with a 47% by weight of water in the formula.
Previous studies conducted by Allum et al. (1997) in AN-
based emulsions showed that those products were able
to detonate with up to 35% of water and density of
0?86 g mL21, in polypropylene pipes (unconfined) having
a diameter of 39 mm. That work did neither study lower
densities nor smaller diameters. In our case, the product
detonated unconfined (PVC tubes) in a diameter of
23 mm with a density of 0?79 g mL21. It is possible that
the lower density of the OW/fuel-based mixtures (which
means much more hot spots present to sustain the reac-
tion) tested in this study may have contributed in the
detonation process. At this stage, we can assume that the
OW/fuel-based mixture from this study could have a lower
critical diameter than 23 mm (at density 0?79 g mL21)
and that may be room to increase the water content of the
OW/fuel-based mixtures. Tests also showed no difference
in the VOD when other types of fuels are used in the OW/
fuel mixtures. A density v. VOD plot for tests with glycerol
and sugar for a diameter of 44 mm is given in Fig. 9.
Conclusion and future work
Previous work has shown that OW/fuel-based mix-
tures can detonate either under strong confinement or
using a high concentration of OW solution. There was,
however, little evidence of work conducted that
evaluates the detonation properties of relatively low
concentration of OW and fuel based mixtures together
with void sensitisation. A new formulation has been
22 Mining Technology 2015 VOL 124 NO 1
developed and patented that incorporates the above
characteristics.
Tests conducted with this novel mixture have indi-
cated the following:
N At small diameters (below 44 mm), in unconfined
conditions, unsensitised OW/fuel-based mixtures are
unable to detonate.
N The sensitised OW/fuel-based mixtures behave as
non-ideal explosives. This was confirmed by the fact
that the VOD depends on both density and diameter
of the charge. However, the VOD at infinite diameter,
for densities 0?79 and 0?84 g mL21, does not agree
well with theoretical calculations.
N The mixtures are able to detonate even in the presence
of large amounts of water (47% by weight in the total
formula).
Further work is required to fully characterise a range of
mixtures at different densities; conduct chemical stabi-
lity analysis; provide feedback on their safety character-
istics and conduct controlled and fully instrumented
tests to evaluate breakage performance. In addition to
important occupational health, safety and environment
(OHSE) benefits, further research and development
could lead to other significant benefits to industry,
including:
N Delivering cost savings in open pit coal mining
through reductions in the use of AN.
N Providing mine sites with a viable alternative to
increase productivity and competition in the mining
explosive market.
N Improvements in overall community safety. Currently,
approximately 2?5m t year21 of AN and ANE are
transported within Australia. Potential on site manu-
facturing of OW based products currently under
investigation could reduce the interface with the
public. Transport of explosives by roads is of great
concern to government regulators
N Contribution to sustainable practices by eliminating the
potential risk of discharge of AN into groundwater
systems, particularly when mining below the water
table.
Acknowledgement
The authors would like to thank Mark Anger for
providing support during on-site tests.

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