600284051
       GASEOUS EMISSIONS FROM EXCESS AIR COMBUSTION
               OF  EXPLOSIVES AND PROPELLANTS
                            by
      Janet  Mahannah,  Donald  Schubert,  and  Carl  Culp
              Atlantic Research Corporation
                Alexandria, Virginia  22314

                           and

                      Terry Schomer
                     IT  Enviroscience
                   Knoxville, TN 37923
                 Contract No. 68-03-3069
                     Project Officer

                     John E. Brugger
        Oil and Hazardous Materials Spills Branch
.Municipal  Environmental  Research  Laboratory  (Cincinnati)
           U.S.  Environmental Protection Agency
                 Edison,  New Jersey 08837
       MUNICIPAL ENVIRONMENTAL RESEARCH LABORATORY
           OFFICE OF  RESEARCH AND  DEVELOPMENT
          U.S.  ENVIRONMENTAL PROTECTION AGENCY
                 CINCINNATI, OHIO  45268

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                                  DISCLAIMER

The information in this document has been funded wholly or  in  part  by  the
United States Environmental Protection Agency under Contract No. 68-03-3069
to IT Corporation.  It has been subject to  the Agency's peer and
administrative review, and it has been approved for publication as  an  EPA
document.  Mention of trade names or commercial products does  not
constitute endorsement or recommendation for use.

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                                   FOREWORD
    The U.S. Environmental Protection Agency was created because of
increasing public and government concern about the dangers of pollution to
the health and welfare of the American people.  Noxious air, foul water,
and spoiled land are tragic testimonies to the deterioration of our natural
environment.  The complexity of that environment and the interplay of its
components require a concentrated and integrated attack on the problem.

    Research and development is that necessary first step in problem
solution, and it involves defining the problem, measuring its impact, and
searching for solutions.  The Municipal Environmental Research Laboratory
develops new and improved technology and systems to prevent, treat, and
manage wastewater and solid and hazardous waste pollutant discharges from
municipal and community sources, to preserve and treat public drinking
water supplies, and to minimize the adverse economic, social, health, and
aesthetic effects of pollution.  This publication is one of the products of
that research and is a most vital communications link between the
researcher and the user community.

    The safe disposal of high energy materials (explosives, propellants) is
an ongoing problem for both military and commercial manufacturers and
users.  That such disposal practices are environmentally acceptable and
have minimal impact present additional constraints requiring the
application of unusual and innovative approaches.  This project was an
effort to develop and evaluate one such approach for this difficult area.


                                          Francis T. Mayo
                                          Director
                                          Municipal Environmental Research
                                          Laboratory
                                     m

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                                   ABSTRACT
     The purpose of  this  short-term  project  was  to  determine  the  levels  of
nitric oxide  (NO),  nitrogen  dioxide (N02),  and  carbon  monoxide  (CO)  in
the  off-gases  from  the open  burning of  high explosives in  excess air.   The
ultimate  goal  is  to develop  and  demonstrate an  improved technique for open
air  burning of surplus,  waste, over-age,  and out-of-specification high
explosives  (including propellants)  so that  the  level of released
particulates  and  noxious gases is much  reduced  from  the level  that is
common when the explosive is  destroyed  by detonation or conventional open
air  burning.   Data  are available on the composition  of gases and vapors
released  from  explosives in  actual  use  situations  (blasting, rocket
propulsion) in which all  (or  most)  of the oxygen  is  provided by  the
explosive itself; but there  are  little  data available  on the combustion
products  formed during burning (or  incineration)  in  excess air.   Previous
work  (DOE) showed that a gravel  and sand  filter installed  in the roof of a
bunker significantly reduced  the level  of particulates emitted during the
excess air combustion of high explosives  but few  NOx or CO measurements
were  reported.
     In the project herein  reported,  two  HMX-^HsOsNs) -based  propellants,
Chaparral 6678  (200 to 538  q)  and  Arcadene  31 3B  (65  to  162  g),  were  burned
in a specially  built,  1.3 m^-steel  chamber  fitted with  internal  baffles
and a top-side  30-cm  (12-in.)-deep,  layered,  sand-on-gravel  bed  (ca.  0.8
m2 (1 yd2) in area) also containing  a 2.5-cm  (l-in.)-layer  of  damp
granulated activated  carbon.   A  blower furnished 1 to 6  nvVmin  (35 to 210
acfm) of air to the chamber to ensure smooth  combustion  and  to  force  the
off-gases, vapors, and particulates  through the  filter  bed.  Thermocouples
and gas analysis probes were  installed above  and below  the  filter to
monitor gas/vapor temperatures and  compositions.

    More than 50 burns were conducted merely  to  determine the  optimum
quantities of explosive, air  flowrates, position of  baffles, and loca-
tion of the sensors.  Nonetheless,  the results of the 15 tests-of-record
were quite variable.  The NO  concentration was both  the  most prominent and
reproducible for the  components  sampled.  Little N0£ was observed.   CO
production fluctuated widely  for reasons  that are incompletely  understood
but that may relate to inadequate mixing  of the  gases,  fluctuating contact
between air and uneven burning of the propel 1 ant.  NO reductions across the
filter were 25 to 70% for Arcadene  and 10 to  57% for Chapparal;  CO
reductions were 38 to 81% for Arcadene and 33 to 91% for Chaparral.

    Note that, when HMX explodes in  the absence of air,  one mole (MW  = 296)
should stoichiometrically yield 4 moles each of N2, CO,  and H20, which
is equivalent to 270 L (@STP) and, assuming the water exists as  steam,
corresponds to 330,000 ppm of CO.  For the samples tested,  assuming  burn

                                      iv

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times of 1 min @ 2.4 m3/min of added  air, the  average  CO  level  should  be
about 40,000 ppm, assuming no conversion to C02.   In this work,
time-averaged, maximum concentrations for CO are  less  than 400  ppm, which
indicates considerable conversion of  CO to C02.   On the other hand, the
quantity of NOX produced may be higher in open air burning than  during
explosions.

    The project demonstrated that the filter used  is effective  in  partially
eliminating NO and CO emissions and verified that  particulates  are trapped
by the filter.  Additional work—including the incorporation of  catalysts
in the bed and the addition of NO-control gases (e.g., NH3)—should be
undertaken.

    This report was submitted in fulfillment of Job Order R-52  (IT Purchase
Order No. E10-81-1) of EPA Contract 68-03-3069 with IT Corporation.
Atlantic Research Corporation was awarded a subcontract to perform the
experimental work and produce a report on the  data.  The  report  covers the
period from October, 1981 to December, 1981 (experimental work); work was
completed as of June, 1982.
                                      iv

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                                   CONTENTS
Foreword	    i i i
Abstract	     iv
Figures	     vi
Tables	     vi
Acknowledgement	,	    vii

        1.  Introduction	'	      1
        2.  Conclusions and Recommendations	      5
        3.  System Preparation	      7
                  Equipment	      7
                  Explosives and Gases	     11
                  Procedures	     11
        4.  Experimental Procedures	     13
                  Preliminary Test Burns	     15
        5.  Results and Discussion	     16

References	     21

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                                   FIGURES
Number

   1
   2
   3
   4
Schematic of combustion chamber	
Combustion chamber	
Experimental set-up	
Slab of Chaparral propellant prepared for ignition,
Page

  8
  9
 10
 14
                                    TABLES

Number

   1     Approximate Composition of Chaparral Propellant.
   2     Arcadene 31 IB (C-4) Composition	,
   3     Combustion of Chaparral 6678 and Arcadene 311B.,
   4     Combustion of Chaparral 	
   5     Combustion of Arcadene 31 IB (C-4)	
   6     Yield of Gaseous Products  from the Isothermal
            Degradation of HMX	
   7     Composition of PBX 9404	
   8     Selected Data from High Explosive Incineration..
                                                                 12
                                                                 12
                                                                 17
                                                                 18
                                                                 18

                                                                 19
                                                                 20
                                                                 20
                                     VI

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                               ACKNOWLEDGEMENTS

    The authors gratefully acknowledge  the  assistance  and  encouragement
provided by numerous colleagues.   In  particular, we most sincerely
appreciate the effort and cooperation that  we  received from  the  following:
Dr. Wei Shing Chang, Bureau of Explosives,  Association of  American
Railroads, Edison, N.J.; Dr. Judith F.  Kitchens, Atlantic  Research  Corp.,
Alexandria, VA; M. Sproul and Dr.  R.D.  Worley, Mason and Hanger-Silas  Mason
and Co., Inc., Lexington, KY; D. Burch,  Naval  Weapons  Support  Center,  U.S.
Navy, Washington, D.C.; A. Heinman, Naval Weapons  Station, U.S.  Navy,  Earle,
N.J.; K. Range, Naval Sea System Command, U.S. Navy, Washington,  D.C., and
Dr. Herbert Skovronek, Consultant.  Special thanks are due to  Ms. Darlene
Williams and Ms. Joanne Cuoghi, IT Corp., Edison,  N.J.  who—with  great
patience—edited and typed numerous drafts  and the final manuscript.
                                      VII

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                                   SECTION 1

                                  INTRODUCTION

   The proper handling  of  explosives  and  propellantsU,2,3),  for  both
military and commercial  uses,  requires—among  other  considerations—that
excess materials, products outside of specifications,  and  out-of-date
materials be disposed of safely.  Often the  very  properties that  make  such
waste materials unsuitable for use also increase  the risks inherent in  their
disposal.  The sensitivity and high energy of  explosive  materials impose
unique constraints  and  limitations on suitable and cost-effective, particu-
late and noxious gas emission-control equipment that may be used  in
conjunction with available disposal systems.

   Among the conventional methods of  disposal  for high explosives detona-
tion, open burning, and  incineration  in a variety of specially  designed
chambers are the most widely used procedures.   Traditionally, excluding
incineration, these processes  have been carried out  in remote areas without
any control of the  gaseous or  particulate emissions  generated by  the
destruction.  Recently,  however, there has been interest in assuring that
such operations do  not  contribute to  air or  water pollution.

   At this time, detonation and open  burning are  the preferred  methods, of
disposal since these require minimum  handling  of  sensitive materials and
allow the materials to  be destroyed with the least likelihood of  creating an
unsafe situation, as might occur in a confining chamber  i.e., incinerator.
Both procedures are convenient, very  economical,  and relatively safe.   Al-
though the processes are, wherever possible, carried out in remote
locations, detonation can result in excessive  noise  and  disturbing shocks,
and both processes  produce uncontrolled emissions of particulate  matter and
noxious gases such  as NO,  N02, CO, N20, and  even  HCN.  The technology  is
such that control of emissions cannot be accomplished  readily.  Where  large
quantities of explosives and propellants must  be disposed  of, such emissions
may be a nuisance, exceed allowable emissions, or contribute  to excessive
ambient air levels  of the pollutants  and possibly to acid  rain  formation.

   Incineration, which  involves the controlled thermal oxidation  of sensitive
materials in a chamber,  allows more precise  control  of the process and
emissions.  However, this processing  route is  more expensive  in both capital
and operating costs, partially because of the  special handling  requirements
and partially because of the control  equipment needed to minimize emission
of combustion products.

   Low cost control  of emissions from incineration and other  combustion
processes (excluding detonation) would make  such alternatives more
attractive to industry and public groups.  This study evaluated one such

                                       1

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 method(4), which  was  originally examined  as  a  means  of controlling
 participate  emissions,  for  also reducing  gaseous  emissions  of NO,  N02,
 and   CO  from the  combustion  of  explosives.   Fundamental  studies  have
 demonstrated that N2, H20,  and  CO are  the major  gaseous  combustion
 products  from the actual  use of high explosives  and  propellents, while  NO,
 N20,  N02, C02,  and HCN  are  other possible products.   Depending on  the
 formulation  of  the explosive, particulates can be released  in significant
 quantities.   The  effectiveness  of the  system used in this  project  is based
 on the reduction  in concentration of particulates,  NO, and  CO when the
 combustion occurs with  excess air and  the combustion products then pass
 through  a sand/gravel filter bed.

     In general, explosive (and  pyrotechnic)  materials consist of solid  or
 liquid compounds  or mixtures that,  when shocked  or  ignited,  quite  rapidly
 release  heat and  convert  almost completely to  hot gases, vapors, and
 particulates  with  no  requirement for oxygen  other than'what  is self-
 contained.   Typical detonators  (initiating explosives) include lead
 azide  (Pb(N3)2) and PETN  (CsH8N40i2),  which  create  shocks  to set off high ex-
 plosives  such  as  RDX  (C^ti^Q^) or  Dynamite  (CaHsNsOg with  24.5% diato-
 maceous  earth  and 0.5%  sodium carbonate). A good example  of a low
 explosive is  black  powder (74%  KN03, 15.6% charcoal, 10.4%  S).  High
 explosives include many formulated  blasting  agents  (ammonium nitrate (94%)
 + fuel oil (6%))  and  propellents (HMX  compositions)  used industrally or in
 munitions or  rocketry,  where extreme brisance  (shattering)  is not  needed or
 required.  (Grenades, shells, bombs, and  remotely guided missile warheads
 require  high  explosives designed for metal shattering; the  propellant that
 drives a  round  from a cannon does  not.)   The major  products  generated by
 typical  explosives are  nitrogen, steam, and  carbon monoxide, as well as
 particulates  from incomplete combustion or,  more  generally,  from the
 special  additives  in  formulated explosives.

     In low explosives,  the  sound accompanying  the release of energy
 resembles a  "whoosh", initiation is usually  by ignition, time of conversion
 to gaseous products is  measured in  milliseconds,  velocity of combustion is
 ca. 5 to  7.5 cm/sec (2  to 3  in./sec),  flame-front velocity  is 500  to 1600
 m/sec  (1/3 to  1 mile/sec),  and  pressure of the explosion is  up to  3.4x10^
 kN/m2  (50,000 psi).  For  detonators or high  explosives,  the  sound
 resmbles a boom or clap,  initiation is by shock  (as  from a  detonator) heat,
 or a spark,  conversion  time  is  measured in microseconds, velocity  of
 consumption of  1600 to  10000 m/sec  (1  to  6 miles/sec), velocity of the
 flame front  is similar, and  pressure ranges  from  3.4 x 10^  to 2.7  x 10?
 kN/m2  (50,000 to  40,000,000  psi).  All explosives produce overpressures
 in the atmosphere  and the detonators generate  shock  waves.

    Explosives generally  fill their containers more  or less  completely  so
 that, when the explosion  occurs,  the great energy release  (heat) and change
 in PV (pressure x volume  product) produce hot, high  pressure gases from the
 solid explosive; extreme, disintegrative  or  propulsive forces are
 unleashed.  For propellants  (especially for  rocketry), controlled  burning
 is required so that steady,  predictable thrust can be  generated  (the newly
released gases and particulates  react  against  what has already been
released (Newton's 3rd  law); solids, including metal  powders,  are  added for
 a variety of reasons).
                                      2

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    Consider  RDX  (Cyclonite,  C3HeN606,  hexahydro-1,3,5-trinitro-l,3,5-
 triazine)  and  HMX  (C^sOsNSt  octahydro-1,3,5,7-tetranitro-l,3,5,7-
 tetrazine). Assuming  the  nitrogen  forms  N2  gas  and  the  hydrogen  forms
 H20 (steam),  there  is  just  enough  oxygen  remaining  to form  CO.   When one  con-
 siders kinetics,  equilibria,  and side  reactions,  it is  not  surprising that
 N20, NO, N02, C  (soot), HCN,  as well as  some  free radicals  are also
 formed: N, H, and 0 atoms and  OH radicals.

    On the other  hand, nitroglycerine  ^3^309)  stoichiometrically should
 form 1.5 N2,  2.5  H20,  and 3 C02 with one  0.5  0  left over  (perhaps  to form
 0.5 N20).  (Note  absence  of CO.)   For  most  high explosives,  however, CO
 is a major product, which is  advantageous since less  (bound)  oxygen is
 required than to  form  C02 and  either gas  will occupy the  same volume,
 with CO behaving  more  ideally  as a gas  and  thus exerting  more pressure.

    Black  powder  (gunpowder),  a low explosive,  is generally formulated to
 form K2$,  N2, C02, and CO,  but S02, K2S04,  K2$, and other compounds have  also
 been identified.

    In passing, one should  note the existence of  hypergolic materials,
 which are  separated materials  that react  vigorously on  mixing (the rocket
 fuel composed of  nitrogen tetroxide ^04)  and  a  mixture  of hydrazine
 (N2H4) and substituted hydrazines  [(CH3)2N-NH2] is  an example).   A variety
 of combinations of hydrogen,  oxygen, fluorine,  boron, and peroxides form
 hypergolics that  are commonly  used in  rocketry—no  further  consideration  is
 given to hypergolics herein.

    To return to  the high explosives and  propellants that are formulated
 from HMX, RDX, Dynamite,  nitrocellulose,  etc.,  the  disposal  problem being
 addressed  is twofold:  (1)  to  reduce or eliminate the nitrogen oxides and
 CO released during destruction and (2)  to remove  the particulates  that may
 form intentionally (as part of the formulation) or  from kinetic/thermo-
 dynamic considerations.  Water, CO, and N2  are  odorless,  and  C02 is almost
 so, so that the odor associated with the  use  or destruction  of explosives
 comes from other  gases such as NO,  N02, NOX,  sulfur oxides,  etc.   In the
 case of ANFO  (ammonium nitrate and fuel oil)  explosives or  of ammonium
 perchlorate, the  gaseous  products  may  be  especially irritating to  humans
 and may contribute to formation of photochemical  smog.

    One should not be  left  with the impression  that burning  of explosives
 without application of air  pollution control  systems is the  universal
 practice.  Rounds and detonators (including components  of mines  and shells)
 are often incinerated at a  safe feed rate in  thick  wall furnaces  to collect
 the metal (brass, lead, steel) for recovery.    Detonators are frequently
 disposed of by dropping them  (also at  a controlled  rate)  into heated pans
 in an incinerator.  The off-gases  and  particulates  usually  pass  through
 cyclones and bag houses.  The  most commonly regulated emissions  are
 particulates and NOX.(3)

    A major advance was the work by DOE (4) that  showed quantities of cer-
tain propellants could be burned with excess  air  in  bunkers  equipped with
gravel/sand tops for removal of the major fraction  of particulates.  Under

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 the  proper design  conditions,  existing  participate  emission  regulations
 could readily be met.

     With this work  as  a  starting  point,  the  intent  of  this project  was to
 find a way of conducting open  burning so that  the  level  of NOX)  CO,  and
 even SOX could  also  be lowered to levels that  are more  commonly  accepted,
 such as those from  power plants or  automobiles.

     By their very  design,  some high  explosives  produce  CO  in quantity; CO
 is not readily  converted to  COg unless  excess  oxygen and possibly
 catalysts are present.   (Note  that  at thermodynamic equilibrium, C,  CO,  and
 C02 must co-exist.)  The problem  with NO is  perhaps more difficult  since
 the conversion  of  NO to  N02  is slow  and, further, high  temperatures  favor
 the formation of nitrogen  oxides  from the nitrogen  gas  that  is almost
 always a principal  product of  the decomposition  of  explosives  (in actual
 use or during disposal).   The  nitrogen/oxygen  reaction'is complex;  but,  one
 can generally expect NOX to  become  a problem at  temperatures of  1200-
 1500 °C.  Unfortunately,  there are many  temperatures to be considered
 (flame, gas, wall,  product)  and the  formation  and dissociation of NOX  is
 condition-dependent.

     In this project, the goal  was to obtain  some baseline data on what
 levels of CO and NOX one might expect during open burning of explosives
 in excess air.  A next phase would consider  improved ameliorative measures
 (only a thin layer of granular activated charcoal  (GAC)  was  used in  this
 work and GAC is not  a really good adsorber for CO and  NO).

    The work was conducted at  a very low level of funding; the results,
 though not of the highest  quality, do indicate that there are significant
 differences in  the products of the decomposition of explosives in actual
 use (or in the  in-field  detonation of surplus  material)  and  in controlled,
 excess air burning.  The work  was not performed  in  an  incinerator,  as that
 term is commonly understood.   The quantity of material  burned was selected
 so that no explosion (but, rather, free  burning) took  place.  The ultimate
 goal  is to determine what  simple,  cheap,  air pollution  systems can  be used
 to reduce the level  of undesirable emissions.

    Note should be taken  that  it  is  not  always practical or  expedient to
make any attempt whatsoever to protect the environment  when  explosives must
 be disposed of.  Bomb squads are  no  more  subject to arrest for violation of
 air pollution regulations  than  are owners or tenants whose buildings burn,
 each  group having in common the "permission" to  allow  air to become
 "dirty"—albeit for  different  reasons.

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                                   SECTION 2

                        CONCLUSIONS AND RECOMMENDATIONS

    The  results  of  tests  on  the  excess  air combustion  of high  explosives  in
a steel  chamber  fitted  with  a  charcoal -containing  sand and gravel  filter  (1)
indicate that  the levels  of  the  evolved nitric oxide (NO) and  carbon
monoxide (CO)  are effectively  lowered,  and (2) verify  a prior  observation
that particulates are efficiently  removed.

    By the reaction  of  CO with Og  in  the  air,  the  level  (quantity)  of CO
is much  reduced  over what is common during confined combustion (propellants)
or during explosions.   The filter  is  effective in  further reducing  the level
of noxious gas  (CO,  NO, etc.)  concentration  during passage through  the
composite bed.

    Definitive values for the  achievable  reduction of  each gas level  cannot
be presented because of the  wide variation in  data.  Specifically,  NO
reductions by  the filter  ranged  from  25 to 67% for Arcadene 31 IB and  10 to
57% for  Chaparral; CO reductions ranged from 38 to 81% for Arcadene 311B  and
from 33  to 91% for Chaparral.  (Arcadene  and Chaparral  are
based propel 1 ant formulations.)
    Little or no N0£ results  from  the  combustion  of either  Arcadene  311B
or Chaparral under the conditions  existing  in  the chamber used  in  this
study.  Low N0£ generation  has  also  been  reported by other  investigators.
    The variations  in removal of  NO  and  CO  may  be  due,  at  least  in  part,  to
the design of the excess  air  inlet system and the  resulting  uneven  burning
of the propel lant and inadequate  mixing  of  the  gases  in the  chamber.   These
problems could be avoided by  modifying the  design  of  the chamber and  by
developing more effective means of providing air to the sample.   For
example, better mixing of the gases  and  a more  even burn might be achieved
by providing underflow and/or tangential air flow  to  the chamber.
Investigation of these factors should be a  major consideration in any
future study.

    Future work should be directed toward applying known or  novel
technology to changing the composition of the gases emitted  to the
atmosphere.  A nickel oxide catalyst is  reported(S) to  accelerate the
reaction of NO with CO:

                      2NO  +   2CO   Nl'°  > 2C02   +  N£.

Nickel catalysts have been used successfully in a  fluidized  bed  incinera-
tor for the disposal of explosive wastes;   NO,  N02, and CO emissions  were

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reduced substantially^).  Additions of catalysts to the filter bed should
be evaluated as a means of reducing NO, N02, and CO emissions.

    Similarly, while NO is a relatively difficult air pollutant to remove
from a gas stream, N02 much more readily dissolves in water (ultimately
forming nitric acid) and can be adsorbed on activated carbon  though
adsorption is poor for N02, but better than for CO and NO.   Therefore,  it
would be advantageous to explore methods for rapidly converting NO to
N02, such as by the addition of copper or other oxidation catalysts to
the filter bed, or of determining whether catalyzed reduction (using NH3)
can be effectively applied.

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                                   SECTION 3

                              SYSTEM PREPARATION

EQUIPMENT

   A schematic and a photograph of the combustion chamber are shown  in
Figures 1 and 2, respectively.  The chamber was constructed of 3.2-mm
(1/8-in)-thick steel.  A 9-gauge  (1.9-cm, 0.75-in.), slot-expanded
sheet-metal grating located 30 cm  (12 in.) from the top of the chamber
provided the support for the sand  and gravel filter.  Hardware cloth was
placed over this grating to prevent loss  through the grating of smaller
particles such as pea gravel and sand.  The filter bed consisted of  the
following layers (bottom-to-top):  10 cm (4 in.) of road gravel, 5 cm (2 in.)
of pea gravel, 2 cm (0.8 in.) of activated carbon, and 13 cm (5.2 in.) of
sand.  A 5-cm (2-in.j-thick layer of gravel was placed on the floor  of the
combustion chamber to provide a base for  the propellant samples and  to
thermally insulate the bottom of the chamber and prevent warping; a  drum lid
provided the actual support for the propellant charge.  A thermocouple
placed immediately below the filter was used to determine the chamber
temperature during each combustion test.  One set of gas analyzer probes for
NO, N02, and CO was placed below the filter to measure the gases resulting
from the combustion process, and another  set of probes was located above the
filter to determine concentrations after  passage through the filter.  The
probes were connected to the analyzers by 4.5-m (15-ft)-lengths of
polypropylene tubing.  A photograph of the experimental set-up is shown in
Figure 3.

   The following instruments and auxiliary equipment were used in the tests:

   o    Portable, direct-reading gas analyzers, InterScan Corporation,
        two each:
            Nitric oxide (NO), 0 to 500 ppm.
            Carbon monoxide (CO), 0 to 3000 ppm.
            Nitrogen dioxide (N02), 0 to 500 ppm.

   o    Strip chart recorders:
            6-Channel, Brush-Gould Model No. 260 (to record output of gas
            analyzers).
            Single channel, Sargent Model  SR (to record output
            of thermocouple).

   o    Air flow meter,  0 to 18 m3/min (0 to 600 cfm),
        Datamatrics Model 100VT.

   o    Battery charger, 12 VDC,  plus nichrome wire for ignition.

                                      7

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               Exhaust
                                 30  cm (12")  sq. opening
                                 Sanpltng Line
                                 Co Monitor
                                                   BoCcom Sampling Lines
                                                   to Monitor
                                 Sampling Line
                                 co Monitor
                                                                     Blower
 30 x 51 cm
(12"v x
   20" Ig)
             Cover.
             Place
                    89 cm
SI en            (35" so.)
(32") sq. opening
      Figure  1.   Schematic of  combustion chamber.
                                8

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1.  Combustion chamber
2.  Duct from blower to chamber
3.  Polypropylene tubing from chamber to gas analyzers
4.  Ignition wire
                Figure 2.  Combustion chamber.

                               9

-------
1.  Combustion chamber
2.  Gas analyzers
3.  6-Channel strip chart recorder
4.  Steel shield
5.  Vent
                Figure  3.   Experimental  set-up.

                              10

-------
   o     Thermocouples,  type  K,  Chrome! -Al umel ,  Omega  Engineering.

   o     Inlet filters for  gas detectors
             gauze  and activated  charcoal,  sealed  canister  type,  Koby.
             coalescer/microfiber glass  type,  Balston.
             swinnex/Teflon element  type,  Millipore.

   *     Tedlar gas sample  bags,  1  liter.

   *     Blower, 20-cm (8-in.) fan,  0.5  hp  motor,  1.9-cm (0.75-in. )-Hg  static
         pressure,  Brundage Model  SW-8-815.

   *     Ducting, aluminum, 20 cm (8 in.)  diameter (fan  to  incinerator).

EXPLOSIVES AND GASES

   Two different propellants, Chaparral 6678  and  Arcadene  311B (C-4),  were
used in  the  study  to evaluate the  effectiveness of the  filter.  General  com-
positions of these two  materials are given  in Tables  1  and 2,  respectively.
In addition, black powder  (74%  potassium  nitrate, 15.6% charcoal,  and  10.4%
sulfur)  was  used to study  the air  flow  patterns in the  combustion  chamber.

   The analyzers were calibrated as described in  the  next  paragraph  with EPA
Protocol gases ( 1% certified)  prepared by Scott  Specialty Gases and having
the following compositions:

         CO in air, 350  ppm;
         CO in air, 2000 ppm;
         NO in H2,  22 ppm;  and
             in air, 250 ppm.
PROCEDURES

   The gas analyzers were calibrated  by  attaching  a  gas  bag  filled  with  the
appropriate Protocol gas to the  gas  inlet  of  the analyzer.   Gas  was allowed
to pass through the sensor for approximately  1  min.   For the calibration, the
span control was adjusted so  that  the meter reading  corresponded to the
known gas concentration.  Since  the response  of the  instrument
was — according to the manufacture! — linear with concentration, calibration
of each type of analyzer at a single  gas concentration was deemed sufficient.

   The combustion chamber was prepared for air  flow  optimization tests by re-
placing the steel cover plate with one constructed of plywood and having a
PlexiglasTM window.  The filter  bed was  prepared as  it would be  for an
actual burn.  Air flow was provided by the blower, and smoke — used  in
observing the air flow patterns—was  generated  by  igniting a small  quantity
(approximately 20 g) of black powder  in  the chamber.  A  temporary plywood
deflector was placed in a different position  within  the  chamber  for each
run.  When thorough mixing of the  smoke  within  the chamber appeared to have
been achieved, the deflector  position  was  noted so that  a permanent steel
baffle could be attached at that position.

                                       11

-------
        TABLE 1.  APPROXIMATE COMPOSITION OF CHAPARRAL 6678 PROPELLANT
             Component                                Weight % of Total
HMX (octahydro-1,3,5,7-tetranitro-^l ,3,5,7-tetrazine)*        60
Nitroplasticizers                                            27
Polyester resins                                              6
Nitrocellulose                                                1.5
Caprolactone polyol                                           1.5
Other (minor constituents)                                    4.0
   2-Nitrodiphenylamine
   4-Ni trodi phenylami ne
   N-Methyl-p-nitroani1ine
   Diisocyanate
   Carbon black
   Zirconium carbide
   Tin oxide
   Lead  sesquioxide
   Triphenylbismuth
* Cyclotetramethylenetetranitramine
                   TABLE  2.   ARCAOENE  31 IB  (C-4)  COMPOSITION
          Component                                Weight % of Total
            HMX                                            84.80
            Carbon black                                    0.05
            Curative and binder                            15.15
                                      12

-------
                                   SECTION  4

                            EXPERIMENTAL  PROCEDURES

   The chamber was  prepared for  the  ignition  of  the  propellants  by  assuring
that the bed contained  sufficient  moisture to be "damp".   The  bed was  kept
moist for two reasons;  first,  to maintain  structural  integrity and,  second,
so that NO and N0£  (if  present)  could  be absorbed and,  possibly,
converted to nitrogen-containing acids.  The  reactions  of  NO and N02 with
oxygen and water to form nitric  and  nitrous acids are complex  and will  not
be discussed.  (Activated  carbon was included in the bed because it  is
known to adsorb N02;  NO is  not significantly  adsorbed,  nor is  CO.)

   The cast propellant  blocks  had  the  consistency of soft  rubber and were
easily sliced with  a  knife.  The blocks  were  cut into slabs measuring
approximately 15 x  10 x 2.5  cm (6  x  5  x  1  in.) for each test.  Each  slab
was weighed and then  prepared  for  ignition by placing a 20-cm  (8-in.)-length
of nichrome wire into a cut  made near  one  end of the slab. The  ends of the
nichrome wire were  attached  to leads of  the battery  charger by means of
alligator clips.  (Hot  nichrome  wire can ignite  the  propellants  used.)  A
sketch of a slab of Chaparral  (approximately  500 g)  prepared in  this manner
is shown in Figure 4.   In  preparation  for  the test,  the sample was  placed
in the chamber, and the metal  cover  plate  was bolted over  the  chamber
sidewall opening (Figure 1).

   Before the actual  ignition  of the propellant  samples, the gas analyzers
were wired to the six-channel  strip  chart  recorder and  activated.   The
analyzers were zeroed,  and  chart speed and analyzer  output sensitivities
were selected.  The single-channel recorder for  chamber temperatures was
plugged in and turned on.   The blower  providing  air  to  the chamber was  also
turned on.

   When the above procedures were  complete, the  propellant sample was
ignited by switching the battery charger on and  allowing current to  flow
through the nichrome wire embedded in  the  propellent sample until the
generation of smoke—or a rise in  temperature—indicated that  ignition  had
taken place.  The battery charger  was  then switched  off.   Exhaust rates
were measured during the burning of  the  propellant by holding  the probe of
a portable, hand-held air flow monitor over the  exhaust stack  of the
chamber.  Temperature and gas  concentration data were collected until  NO,
N0£, and CO concentrations  above and below the filter returned to zero.
The time until gas evolution ceased  was  recorded  in  some tests.

   Gas concentration data were obtained  in terms of  peak concentrations
and, in certain cases,  also  as time-averaged  concentrations.   According to
the manufacturer, the voltage  output of  the analyzer  is proportional to gas
                                      13

-------
\
                                                                                      c
                                                                                      o
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-------
concentration.  Time-averaged concentrations,  i.e.,  the  average  concen-
trations over the time during which  gas was  evolved,  were  determined  by
measuring the area under  a  plot of the gas concentration against time on
the recorder chart with a calibrated  planimeter.   The measured area was
then divided by the total time during which  gas was  emitted  to yield  the
average concentration.

PRELIMINARY TEST BURNS

   A series of preliminary  test burns was carried  out to determine the
minimum sample size needed  to produce measurable concentrations  of CO and
NOX and to select the appropriate analyzer output  sensitivities.  For
example, an initial test  burn of 100  g of Chaparral  produced  negligible
NOX and CO emissions; therefore, sample size was increased.   Chaparral
samples in the range of 200 to 500 g  were found to produce adequate gas
volumes.  Smaller samples of C-4 (approximately 100  to' 200 g) were found to
be adequate, because of the higher content of  HMX  explosive  in this
propel!ant.

   The preliminary test burn data were also  used to  optimize  burn
conditions.  The goals of this optimization  were to  provide  sufficient
combustion air and yet to maximize the residence time of the  gases in the
filter bed.  To meet these  requirements, the blower  that provided air to
the chamber was  modified to allow the air flow to be decreased.  This was
accomplished by systematically restricting the air intake  to  the  blower.
At each change (reduction)  in air flow, the  rate of  air flow  was  measured
at the inlet to the combustion chamber.  This  procedure was repeated  until
the levels of CO within the chamber  (below the filter bed) began  to
increase, indicating insufficient excess air to ensure combustion of  the CO
to C02.  This air flow (2.4 m3/min (85 ft3/min)) rate was  then used
for all the burns of record.
                                      15

-------
TABLE 3.   COMBUSTION OF  CHAPARRAL  AND ARCAOENE 311B  (C-4)
Burn Propel lant
*
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
C-4
C-4
C-4
C-4
Chaparral
Chaparral
C-4
C-4
C-4
C-4
C-4
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
Chaparral
C-4
C-4
C-4
Chaparral
Chaparral
Chaparral
C-4
C-4
C-4
C-4
C-4
Chaparral
Chaparral
Chaparral
Propel lant
Weight
(a)
450
340
450
450
225
225
225
225
225
630
180
180
180
180
180
180
545
545
480
446
474
211
498
493
248
435
476
522
162
65
70
503
493
528
129
114
114
103
84
200
500
500
Air Flow
Rate
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
6.4
3.9
2.9
.0
.0
.0
.0
.0
.0
.5
2.
2.
2.
2.
2.
2.
2.4
2.4
2.4
2.4
2.4
2.4
2.4
2.4
2.4
Chamber

Maximum
Bottom
Gas Concentrations (ppm)
Top
Temperature NO CO NOg
.
-
-
-
-
.
.
-
180
299
136
147
166
173
155
130
311
342
370
366
326
282
355
420
278
370
318
370
194
92
172
376
394
416
.
131
139
153
-
190
380
•

250
250
250
250
250
250
_
360
370
125
375
320
360
200
200
260
140
>500
>500
500
>500
210
>500
>500
1250
950
525
525
150
1300
600
350
300
700
450
400
1100
1150
200
200
200
>3000
.
175
>3000
0
0
0
-
•0
>3000
0
0
0
0
0
0
0
0
0
0
0
0
>3000
600
450
2100
975
1050
150
.
0
0
0
0
600
0
0
30
450
9
30
45
.
-
5
5
10
30
125
-
50
15
-
50
40
10
10
15
15
10
5
0
0
0
0
0
0
0
0
5
5
.
0
0
10
0
0
0
0
2
20
0
0
0
NO CO
.
205
250
250
200
250
250
-
200
190
80
210
170
130
130
120
120
150
180
200
130
110
230
175
175
175
225
275
250
125
600
400
300
300
250
100
100
250
325
100
150
150
>3000
0
0
>3000
0
0
0
-
0
0
0
1200
0
0
0
0
0
0
0
0
0
0
>3000
900
300
750
300
225
75
.
600
0
0
0
150
0
0
0
270
0
15
15
N02
.
0
10
10
5
10
0
-
25
0
0
0
0
0
0
0
0
0
0
0
0
0
0
2
0
0
0
0
0
.
55
10
0
0
20
0
0
5
15
0
0
0
                          17

-------










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 for CO  the  range  was  33  to  91%.   The  percent  reduction  in  NO generated  by
 the excess  air  destruction  of  C-4 ranged  between  25  and  67%, and  the  CO
 reduction ranged  from 38 to 81%.   Insufficient  mixing of gases  and  uneven
 burning, as discussed earlier, may be responsible for these  variations.
 Nevertheless,  it  is significant  that  reductions in both  NO and  CO did occur
 consistently.

    The absence of significant concentrations of  N02 was expected.  Other
 studies(3)  under  different  conditions have  shown  that the  primary
 isothermal  degradation products  of HMX are  N20, N£,  NO,  CO,  C02,  and  HCN.
 For example, the  yield of gaseous products  from the  isothermal  decomposition
 of HMX  (7)  at  selected temperatures  is shown  in Table 6.  It should be
 noted that  these  values  are the  result of isothermal degradation  of HMX,
 not an  incinerative process such  as  used  in the present  study;  therefore,
 the results should only  be  used  as indicative of  the relative amounts of
 off-gases.  These values also  do  confirm  the  observed absence of  N02  in
 the current study.

       TABLE 6.  YIELD OF SELECTED GASEOUS PRODUCTS FROM THE  ISOTHERMAL
                              DEGRADATION OF HMX
Temp.
(OC)
226
250
258
N20

2.52
2.58
2.57
N2
(moles gas
0.47
0.46
0.47
NO
CO
CO?
HCN
produced/mole HMX charged)
0.42
0.50
0.55
0.40
0.47
0.47
0.56
0.41
0.54
0.02
0.04
0.07
    Exhaust rates were also  determined  for  two  samples  at  the  established
blower rate.  The burning of a  522  g  sample  of  Chaparral gave  a  peak
exhaust rate of 1.4 m3/min while  162  g  of C-4 produced  a peak  exhaust
rate of 1.8 m3/min.  These values again  reflect the  higher HMX content  of
the C-4 propel 1 ant.

    Over the period of 1971  to  1976,  Mason  and  Hanger-Silas Mason  Co.,  Inc.,
investigated various methods  for  the  disposal of high explosives.   As part
of that study, PBX 9404, an  HMX-based,  plastic-bonded explosive  ("PBX"),
with the composition shown in Table 7,  was  thermally decomposed  in a
closed-pit chamber (bunker)  designed  to  accommodate  approximately  450 kg
(1000 Ib) of explosive.  As  part  of that study,  a  sand  filter  placed above
the chamber was evaluated, primarily  for the control of particulate
emissions.  Because of the similarities  between  the  Mason  and  Hanger work
and the present study, a comparison between  the results of the two is of
interest.  Data selected and  adapted  from the earlier study (4)  are
presented in Table 8.  Maximum  values for NOX emissions were of  the same
order of magnitude as those  found in  the current study, but the  levels  of
CO reported by Mason and Hanger were  much higher than those found  in the


                                      19

-------
                      Table 7.  COMPOSITION OF PBX 9404*
     Component
  % of Total
HMX
Nitrocellulose
CEF
Diphenylamine
94 ±
3
3
0.1
0.5


± 0.01
       *   Reference 8.

Hanger were much higher than those found  in the current study, probably be-
cause the large volume of excess air  introduced in the current study con-
verted more CO to C02.  Although percent  reduction values after passage
through the filter are not given in the Mason and Hanger report, the
authors did note that slight decreases in NOX and CO emissions
were measured as the gases passed through the filter.  The authors also
found that, at most, 10% of the NOX was in the form of N02, and that the
major component of the NOX was NO.  Temperatures of the chamber, also
noted in Table 8, were obtained on an I-beam support above the pit; they are
of the same order of magnitude as those measured in the current study.

          TABLE 8.  SELECTED DATA FROM HIGH EXPLOSIVE INCINERATION*
             Amount        Burn
Burn No.   of HE (kg)   Time (min)   Temp, (oc)**
Peak Gas Concentrations
NOX (ppm)   CO (ppm)
40
41
45
47
48
52
463
457
463
463
457
463
1.08
1.17
1.19
1.19
1.28
1.11
370
370
370
320
350
340
275
277
500
502
375
476
60,000
44,000
18,000
5,000
1 1 ,000
3,900
*  Reference 4.
** Temperature of I-beam located in incinerator.

                                      20

-------
                                  REFERENCES

1.  Cook, M.A., The Science of High Explosives, Krieger, Huntington, NY
    1971.

2.  Cook, M.A., The Science of Industrial Explosives,  IRECO Chemicals, Salt
    Lake City, UT. 1974.

3.  Chang, W.S., and J.F. Kitchens.  Environmental Considerations in the
    Safe Disposal of Explosives.  In: Proceedings of the 1982 Hazardous
    Materials Spills Conference, Government Institutes, Inc., Rockville, MD
    1982, pp. 94-101.

4.  Mason and Hanger-Silas Mason Co., Inc.  Disposal of Waste or Excess
    High Explosives.  MHSMP-76-51.  U.S. Energy Research and Development
    Administration, Albuquerque, NM  1977.

5.  Carroll, J.W., T.L. Guinivan, R.M. Tuggle, K.E. Williams, and D.L.
    Lillian.  Assessment of Hazardous Air Pollutants from Disposal of
    Munitions in a Prototype Fluidized Bed  Incinerator.  Am. Indus. Hyg.
    Ass'n. J., 40(2):147-158, 1979.

6.  Scola, R. and J.S. Santos.  Fluidized Bed Incinerator for Disposal of
    Propellants and Explosives.  ARLCD-TR-78032, U.S. Army, 1978.

7.  Suryanarayana, B. and R.J. Graybush.  Thermal Decomposition of
    l,3,5,7-Tetranitro-l,3,5,7-tetraazacyclooctane (HMX):  A Mass
    Spectrometric Study of the Products from HMX.  Ind. Chem. Beige., 32
    (3):647-650, 1967.

8.  Kitchens, J.F., W.E. Harward, III, D.M. Lauter, R.S. Wentsel, and R.S.
    Valentine.  Preliminary Problem Definition Study of 48 Munitions-Related
    Chemicals.  Vol. I.  Explosives-Related Chemicals.  Atlantic Research
    Corporation, Alexandria, VA  1978, 29 pp.
                                      21

-------
                                           TECHNICAL REPORT DATA
                                  (/'lease read Instructions on the reverse before com/ilcting)
 1 . Rt PORT NO.
                                    2.
                                                                       3. RECIPIENT'S ACCESSION NO.
 4. TITLE AND SUBTITLE
                                                                       5. REPORT DATE
  GASEOUS EMISSIONS  FROM  EXCESS AIR COMBUSTION
  OF  PROPELLANTS  AND  EXPLOSIVES
                               6. PERFORMING ORGANIZATION CODE
 7. AUTHOR(S)
  Janet  Mahannah,  Donald  Schubert,  Carl  Gulp,  and
  Terry  Schomer
                                                                       8. PERFORMING ORGANIZATION REPORT NO.
 9. PERFORMING ORGANIZATION NAME AND ADDRESS
  Atlantic Research Corporation
  5390 Cherokee Avenue
  Alexandria,  VA  22314
and   IT  Corporation
       312 Directors  Ur.
       Knoxville,  TN  37923
10. PROGRAM ELEMENT NO.

         CBRD1A
11. CONTRACT/GRANT NO.

           68-03-3069
 12. SPONSORING AGENCY NAME AND ADDRESS
  Municipal  Environmental  Research  Laboratory—Cin.,  OH
  Office  of  Research  and  Development
  U.S. Environmental  Protection Agency
  Cincinnati,OH 45268
                               13. TYPE OF REPORT AND PERIOD COVERED
                                         Final  10/81-6/82	
                               14. SPONSORING AGENCY CODE
                                         EPA-600/14
 15. SUPPLEMENTARY NOTES
  Project  Officer:  John E.  Brugger  (201) 321-6634
 16. ABSTRACT
                      -^f ^1s/Mn°l^t"tern'  Pr°J'ect was to determine the levels of nitric oxide
                  ), nitrogen dioxide  (N02), and carbon monoxide (CO) in  the off-gases from the open
               burning  of explosives in excess  air.  The ultimate goal  is to reduce  the level  of NO,
               CO, and  particulates emitted during the destruction of surplus, waste, and off-spec
               explosives.  Previous work (OOE) showed that  a gravel/sand filter in  the roof of a '
               bunker reduced the level of particulates emitted during  excess air combustion of
               SM^^U"^ (?"ly 1imited N°x or co measurements were reported).  In  this project, two
               HMX-(C4H808N8)-based propellants (Chaparrel.  200 to 538  g, and Arcadene 313B, 65 to
               162 g) were burned in a 1.3 m3-steel chamber  fitted with a 30-cm-deep sand and
               gravel filter.  Air (1 to 6 m3/min) was blown into the chamber to ensure combus-
               tion  and to force the gases through the filter, which included a 2-cm layer of damp
               activated carbon.  The NO-concentration was the predominant and most  reproducible
               for the components measured.   Little N02 was observed.  CO-production fluctuated
               widely, probably due to inadequate mixing of  the gases within the chamber and uneven
               burning.  The  NO and CO concentrations decreased across  the filter.   NO-reductions
               were  25 to 67% for Arcadene and 10 to 57% for Chaparral;  CO-reductions were from
               38  to SIX for  Arcadene and 33 to 91% for Chaparral.   The project demonstrated that
               the filter is  effective  in partially eliminating NO  and CO emissions, but that
               additional work,  including the incorporation of catalysts in the bed and the
               introduction of NO-control  gases (e.g.,  NH3),  should  be undertaken.
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