United States
                  EnvironmentaLErotection
                  Agency          	
Air and  Energy  Engineering
Research Laboratory
Research Trangle Park, NC 27711
                  Research and Development
 EPA/600/S9-89/089    August 1990
v°/EPA         Project Summary
                   EPA/IFP  European
                   Workshop on  the Emission  of
                   Nitrous Oxide from  Fossil  Fuel
                   Combustion
                  Jeffrey V. Ryan and Ravi K. Srivastava
                   This report summarizes the pro-
                  ceedings Of an Environmental Pro-
                  tection Agency (EPA/lnstitut Francais
                  du Petrole  (IPP)  cosponsored
                  workshop addressing direct nitrous
                  oxide (N2O) emission from fossH-fuel
                  combustion. The third in a series, the
                  workshop  was held at the  IFP in
                  Rueil-Malmaison, France on June 1-2,
                  1988.
                   Increasing atmospheric  N2O
                  concentrations have been linked to
                  depletion of atmospheric  ozone (O3)
                  and to global climatic warming. The
                  combustion of fossil fuels has been
                  identified as a  potential  major
                  anthropogenic source of N2O.  This
                  workshop had two goals:  (1) to
                  exchange Information among various
                  international research and industrial
                  groups  that  are  involved in  N2O
                  chemistry,  modeling,  and  N2O
                  measurement; and (2)  to develop a
                  network for coordinating  future
                  related efforts.
                   The five  technical  sessions
                  addressed:  stratospheric  O3
                  depletion and global climate change,
                  mechanisms  of N2O formation and
                  destruction during combustion, N2O
                  measurment  techniques, full-scale
                  field data,  and practical conclusions
                  based on general discussion.
                    A sampling artifact discovered
                  during  EPRHundred  research
                  revealed that N2O  can  be generated
                  in  a  sample  container  in the
                  presence of nitrogen oxides (NOX),
                  sulfur dioxide (SO2),  and water. This
artifact potentially discredits much of
the N2O emissions data collected
from samples containing the above
compounds when  stored for some
time prior  to  analysis. Recent
sampling techniques that minimize
the artifact have produced data from
stationary sources that indicate that
direct emission of N2O from fossil -
fuel combustion may not be a major
contributor to the  measured annual
Increase. Limited data also indicate
that some specific sources (e.g., fluid
bed combustors) may be high  N2O
emitters. A  standardized sampling
protocol would help validate current
data.
  This Project  Summary  was
developed by EPA's Air and Energy
Engineering Research Laboratory,
Research Triangle  Park, NC, to
announce key findings of the research
project that Is fully documented  In a
separate report of the same title  (see
Project Report ordering information at
back).

Introduction
  This report summarizes activities at a
workshop  on direct  nitrous oxide  N20
emissions from fossil fuel combustion,
held in Rueil-Malmaison, France, on June
1-2, 1988. The workshop was the third in
a series on N2O emissions and was Co-
sponsored  by the U.S. Environmental
Protection Agency (EPA) and the Institut
Francais du Petrole (IFP). Its primary
focus was to assess and evaluate the role
that combustion of fossil  fuels plays in

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directly  emitting  N2O  into  the
atmosphere.  This  subject is  significant
because the ambient levels of N2O have
been reported   to be increasing   and
because  N20 has been  linked to
stratospheric ozone  (O3) depletion  and
global climatic warming. Another focus
was to establish an international  network
for exchanging  information related  to
N20 emissions.
  The  workshop  brought together  a
complementary group of experts involved
in  various aspects   of  N2O research.
Specifically discussed were the role of
N20  in  stratopheric  O3 depletion  and
global climate  change, the mechanisms
of  N2O formation/destruction  (involving
both  homogeneous  and  heterogeneous
reactions), and  the status of    N20
measurement techniques. Presentations
were also  made on emissions  data
collected from  a  variety of  stationary,
sub- and full-scale facilities, as well as on
data  from mobile sources. After these
presentations/discussions,  conclusions
were reached regarding  the  current
status   and future  direction  of   N20
research.
  This report documents both the formal
and  informal  material presented at the
workshop, and  it  covers vigorous
diccussion periods that  followed  formal
presentatations. It is an  account of the
proceedings  and  summarizes  the
workshop's content chronologically.

Atmospheric Concerns
  Representatives  of EPA, NASA, OECD,
and   Max Planck  Institute  presented
overviews of each  agency's  program
relating  to stratospheric ozone depletion
and global climate  change.
  EPA  believes that  human activities are
responsible for increases in atmospheric
gases that are causing  global  climate
change through warming (a result of the
greenhouse  effect)  and stratospheric
ozone (03) depletion. NASA believes that
in  the  last  100  years,  the  trace  gas
composition  of  the atmosphere  has
changed more than  in the previous 4.5
billion years, owing to increased  human
activity.  Carbon  dioxide   (C02),
chlorofluorocarbons (CFCs), and methane
(CH4) are anthropogenic  gases known to
participate in reactions  contributing to
climatic warming and ozone depletion.
  Nitrous  oxide (N20) is another trace
gas that contributes to both  stratospheric
ozone  depletion and climatic warming.
Ice core data show  steady  levels of N2O
until  the start of the industrial revolution
and    that   currently,   ambient
concentrations are increasing  at  an
annual  rate  of about 0.2  percent.
Although natural sources are thought to
comprise over  50 percent of  total
emissions, combustion  of fossil fuels and
biomass burning are   considered to be
major anthropogenic contributors.
  N2O  contributes to  the  greenhouse
effect through the absorption of  infrared
radiation. Global  temperatures  have
already  increased 0.6  °C since   1880,
and the four hottest years on record have
occurred in the 1980s. The  modeled
predictions  of global temperature,  using
recorded  data,   suggest   that
temperatures  may  rise by  as much as
5°C  worldwide by the  year  2030. About
10 percent  of this warming  may be due
to increased N2O  concentrations.  Many
global  features  are  expected  to  be
adversely affected  by   drastic climatic
changes. Global warming will melt polar
ice  caps, change   important weather
patterns, and  tax  human  health  and
society.

  Some scientists  suggest  that ozone,
the  only atmospheric  gas  that absorbs
ultraviolet radiation, may be  second only
to oxygen as the earth's most  important
gas.  A 50  percent  reduction  in
stratospheric ozone has been  observed
over  a  ten-year period over the South
Pole. This depletion probably represents
the largest geophysical perturbation ever
measured over so short a period.

  It has been determined that N2O plays
a key  role  in  stratospheric ozone
depletion.  A catalytic  loss  mechanism
involving the  oxides of nitrogen (NOX)
destroys  stratospheric  ozone.  It  is
interesting to  note that the  main source
of NO in the stratosphere originates from
N20.
  Currently,  the N20  data base  is
insufficient. There is a critical need to
foster research directed at developing a
better   inventory  of  N2O emissions
sources and  contributions, and to
improve understanding  of  both the
combustion processes related to  N20
emissions  and  control  options.
Accelerated research  is vital,  because
critical  decisions are  being  made to
control  NOX,  new  combustion devices
are  being designed  and built,  and
developing nations are  growing and
contributing to the N2O problem, all with
insufficient  information.
Mechanisms of N2O Formation
and Destruction During
Combustion

Basic  Kinetics
  Nancy Brown (Lawrence  Berkeley
Laboratory) described  her ongoing
investigation of the formation/destruction
chemistry of N20 in  premixed, laminar,
lean, atmospheric-pressure flames.The
study involves both  experiments and
modeling .
  For the experiments, CH4/air/nitrogen
compound       flames       and
H2/O2/argon/nitrogen compound flames
were chosen. The H2 flames were chosen
to  provide  results  without  the
complexities of carbon chemistry and to
allow a  comparison of results to model
predictions.  Experimental variables were
bulk flow rate (28-40 Lpm), to include the
effects of heat transfer  to the  burner,
equivalence ratio (0.75-0.9), and nitrogen
additive  (NH3, NO,  N20, and   N2).
Thermochemistry, probe, and quenching
effects were also studied.
   For modeling, she used  Sandia codes
Premix with full chemistry and transport,
Chemkin   with full chemistry,and
Thermochemistry-1987 Chemkin release.
For modeling,  actual  measured
temperature profiles  were used  rathe
than solutions of the energy equation.
  She  concluded  that agreement
between  the  experiment and modeling
was  satisfactory near 1,700 K, but  the
chemistry  at  temperatures less than
1,100 K  needs more  clarification.  Other
conclusions of  her research are:

  • N2O destruction results in  N2
    production.
  • Destruction  reactions need  to  be
    determined over  a  wide range of
    temperatures and product yields.
  • More information on N2O production
    reactions is needed.
  • Probe effects need to  be eliminated
    because  they  could  have  a
    significant  effect  on   N20
    measurements.

Gas Phase Kinetics
  John  Kramlich,  (Energy  and
Environmental Research  Corporation)
focused on the emissions of N20 from
industrial flames. He discussed were the
issues of N20 formation and  emission in
coal and oil  flames  and the effects of
firing  configuration  and pollution control
strategies  on  these emissions. This

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study has involved both experiments and
modeling.
  Figure 1 summarizes  the study with a
mechanism  overview and  admits that
predominant generation of N20 occurs in
the post-flame zone from conversion  of
HCN to N2O.  Presence of HCN in the
post  flame  can   be  credited  to
devolatilization of char-N and to free HCN
transported from the edge  of   volatile
flame in  stratified  flow. Some  N20  is
produced in the flame zone but is rapidly
destroyed to form N2.

 Heterogeneous  Reactions
  Gerard  de  Soete (IFP)  defined  a
heterogeneous reaction  as one between
two  different phases, as in gas to solid.
Heterogeneous reactions  implying N2O
as  a reactant  or  as  a  product are
numerous. Three examples are:
  1. Formation of N20 from  bound  N
    during heterogeneous char oxidation.
  2. Heterogeneous reduction of  N2O on
    char-bound  C  atoms   during
    heterogeneous char oxidation.
  3. Formation  of N20  during catalytic
    NO reduction (coupled with catalytic
    N2O  reduction), which may play a
    larger role in N20  emissions from
    mobile sources.
A  heterogeneous reaction  rate  can  be
expressed by:
where k, is is the rate  constant, enm  (a
fraction) expresses the dependence  of
the  covering  degree,  which   is
proportional to active sites  in the solid
involved in the  reaction, and  Py is the
dependence of partial pressure of one  or
more  reactant gaseous species.
  Thus  the  study,  focusing on
heterogeneous  reactions that imply N2O
as a  reactant or product,  involved two
tasks: (1) identification of the adsorption
and desorption reactions composing the
heterogeneous  mechanisms  and  their
reaction rates,  VjS;  and  (2)  a  time
resolved study of the reactions identified
in Task (1). This allowed determination  of
the  fractions leading to determination  of
the rate constants, kfs.
  The formation  of N20  during NO
catalytic reduction plays a  major role  in
emissions from mobile sources  using
three-way catalysts.
  Passing N2O  and NO over a typical
metal catalyst results in:
  1. Reduction  of NO at a much  lower
     temperature than N20, resulting  in
     the formation of N2O as  a function
     of temperature.
   2. Intermediate formation  of N2O
     when NO is  fed as  a function  of
     temperature.
  The above indicates that transformation
of N2O into NO is a minor reaction. In all
circumstances using graphite, N20 will
be reduced at a lower  temperature than
will NO, as opposed to when a metal
catalyst is  used with a reducing agent.
Since  N2O  reduces  at  a   lower
temperature than NO, little N20 is found
when  NO is  reduced.  Reduction  of NO
could  result in  formation  of  N20;
however, this reduction of NO  at the
temperature where N20 can be formed
occurs so fast that the N2O cannot be
seen in the gas. For graphite, this is true
in both the presence  and  absence  of
reducing gases. The situation is the same
during  heterogeneous reduction  of N2O
and NO on char-bound carbon atoms.
  Shown  in  Figure  2   are  the
experimentally  determined overall
reaction  rates of  C oxidation  and,  NO,
N20, and HCN formation as a function  of
temperature for  Eschweiler char.  The
subscript  e  in this figure implies  that
these reaction rates were obtained under
adsorption/desorption  equilibrium rates.
The  figure suggests a  rough
proportionality between Vc,  VNO.  and
VN,O.
  For  a  Cedar Grove char, plotted  in
Figure  3 are fractions  of  nitrogen
converting to NO and to N20 as functions
of fraction of carbon burnt. These  results
have been obtained for all fractions  of
carbon burnt and for temperatures up  to
1,400  K. As  a rough approximation, the
fractions of N  converted to NO and N20
seem  to be proportional to the fractions
of carbon burnt.  Thus  it  seems  that  a
constant fraction of N is formed into NO
and another  constant  fraction of N  is
converted into N20 in a heterogeneous
way. This is true  for  all  char burnout
fractions and at  all temperatures up  to
1.400K.
  Therefore, the  main reaction path  of
N20 formation from bound  nitrogen,
during  char combustion, at temperatures
below   1,400 K,  is  probably  not  a
formation   from  HCN, occurring  in the
gas phase, but a heterogeneous reaction
directly  linked to char oxidation.  This  is
suggested by reaction order with respect
to oxygen  of one  for  Vc  (overall
combustion  rate),  VNO  (overall  NO
formation  rate),  and VN o (overall N20
formation  rate), and similar temperature
dependence of their overall rate.
   Thus, based  on  this  study,  the
probable mechanisms involved  in
formation of N2O  from bound nitrogen
during  heterogeneous char oxidation are
shown  in Figure 4. The parentheses in
this figure imply solid bound groups.

Overall Chemical Information from
Laboratory Combustor
Experiments

  Jost  Wendt  (University of  Arizona)
gave results of ongoing  DOE-funded
research at  that  institution. The work
focused  on  optimizing   reburning
configurations  for NOX control.  A
secondary focus of the work was on  N20
measurements.  N2O was measured by
on-line  GC.ECD  following  a  sample
conditioning system.
  The experiments are  being conducted
on a premixed, down-fired combustor at a
firing rate of 27 kW to study NO and  N20
emissions  from  the  combustion  of
Beulah lignite and Utah #2  bituminous
coals. NO2 levels for both   coals were
found to be insignificant at less  than 2
ppm for stoichiometric  ratios (SR)
ranging from fuel  rich to  fuel  lean.
Measurements of NO and N20   as a
function of  residence time at fixed  fuel
lean  SRs,   with  combustion  gas
temperatures  in the range 850-1,290 K
for  Beulah coal and 1,050-1,525 K  for
Utah coal, showed N20  concentrations to
be  less than 5 ppm and  the  N2O/NO
concentration ratio to  be very  small.
Results, so far, have also indicated  that
there is little N20 formation under reburn
conditions using  natural gas   as  the
secondary fuel.
  William Linak (EPA/AEERL), presented
N20 emission  data from a  down-fired,
60,000  Btu/h  (18kW)  laboratory-scale
coal combustor with  a variable swirl
burner.    The  purpose  of  these
experiments  was  to change  NO
emissions through changes in the overall
turbulent diffusion flame type and thus to
determine if a correlation between  N2O
and NO  emissions was valid.   Bomb
samples were drawn  from  a post-
combustion  region under  stack type
conditions.   In  an attempt to  vary  the
NOX concentration, burner swirl and flame
shapes were  altered by changing axial
and radial air ratios and locations of the
injector  tube.  A  Utah  bituminous  coal
and a Montana subbituminous coal were
used in  these experiments,  the  first
having a higher organic content  but lower
moisture  level than  the other.  For each
coal, data were collected at  three (fuel

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                                         In Post-flame

                                                   Devolatilization   HCN
                                            Char-N 	»•
                                  N2O
                                             Free HCN
                         NH3

                         N2O
                                       At Edge of Volatile Flame
                                              Char Contains Char Nitrogen
                                              Stratified Flow May Contain HCN
                                        In Volatile Flame Zone
                                             Devolatilization
                         s
                         ^
       Figure 1. Mechanism overview.
lean) stoichiometric ratios and two  flame
shapes — one axial and one radial. Gas
samples were collected in stainless-steel
containers after refrigeration drying and
were analyzed for N2O by GC/ECD. The
widely  scattered data   show N2O
emissions of 10-250 ppm.  Experiments
using on-line N20 analyses  by GC/ECD,
indicated  N2O emissions  consistently
below 10  ppm. There  seems to be  no
correlation between N2O emissions and
NOX emissions.
  John Kramlich (EERC)  described  his
fluid bed model as a stirred reactor   for
bed particles releasing volatiles  such  as
HCN and CO, and as a plug-flow reactor
for the gases moving up through  the bed.
Initial  model results show that NO
concentration initially increased  because
of a  leaner  stoichiometry, reached  a
maximum  of about 200 ppm, and then
decreased in bed  region with relatively
less  lean  stoichiometries.  The final
stoichiometry was taken to be 1.25. The
results also  show that N20  emissions at
the end of  a  residence time of 0.5  s,
corresponding to  the beginning  of
freeboard part,  were  reasonably  high
(about 250 ppm).  The model predictions
for variations  in  excess  air,  bed
temperature, and fuel nitrogen speciation
are shown in Figure 5. The stoichiometry
in the bed was lean,  so an increase in
excess air  did not have much effect  on
N20 emissions, which are very  sensitive
to temperature in the  range 1,000-1,200
K. NH3 does  not  produce  much N2O;
HCN produces reasonably high  levels of
N2O; and a combination of NH3 and HCN
produces  intermediate  N2O levels.  All
these parametric effects, explored by the
model,  agree  with  N2O formation/
destruction chemistry understood so  far.
Model  predictions were also  made on
N20 emissions from  coal and natural gas
reburning.   The  results suggest  that
application  of  carefully  picked  gas
reburning conditions may decrease both
NO and N2O emissions.
  Alan Williams  (Leeds  University)
summarized  his own investigation.  His
measurements reveal that N20  is about
10-20% of the total  Nox for fluidized bed
and  drop-tube combustion, with grate
combustion  producing higher levels than
systems with sustained  high temperature
in  the post-.flame region . He  suggested
the mechanism of  N2O formation as
outlined   in    Figure  6  where coal
pyrolizes  to give tar + gases + char, all of
which  can produce N2O.  His   kinetic
calculations  reveal  that  the N20
contribution from the interaction of  NH3
+  NO was  only  about 5 ppm.   N20
yields from both tar and char combustion
were each  about   10%  of the   NO
produced. These results suggest that at
each stage of combustion, either single
or  staged, the  N20 is about 10%  (or
possibly  higher)  of the  NO  ( + N02)
produced, and  production  of  N20 is  a
strong function of temperature
  John Smart (International   Flame
Research Foundation) presented data on
his experiments on  a 4 MW  horizontal,
swirled  pulverized-coal-fired  furnace.
The  preliminary results  indicated that
HCN and NH3 found in the flame  at the
0.1m axial location were essentially gone
by the 0.2 m location. N20  values were
low at the 0.1 m location,  although  at 0.2
m  near peak values  were  achieved. N20
and  NOX in furnace exhaust (at  about
1,070 CC) were 43 and 720 ppm, (at 3.6
%  02).  The data suggest N20 formation
from fuel-bound N,  but further  work is
needed to characterize this hypothesis.
N2O Measuement Techniques
  The  second session  began  by
addressing  the  need  to develop
standardized sampling  and  analytical
techniques.    Given  the  measured
increase  in atmospheric N20 levels,  it
can  be  concluded that a  significant
anthropogenic source exists. The relative
importance of candidate sources such as
agriculture, biomass burning  and  fossil
fuel combustion and others is unclear at
this time.Therefore, a reliable, accurate
method  for  identifying  and  analyzing
these sources is crucial.  A standardized
sampling and analytical protocol is critical
in  verifying the reliability of  N2O  data
gathered  worldwide.  A wide variance in
sampling methodology is evident.  Grab
samples   have  been collected in  many
types  of  containers,  including glass,
stainless-steel, and Tedlar bags.  Sample
moisture  content  also  varies  greatly.
Furthermore, the development of an on-
line real time  analyzer  would eliminate
long analytical  delays  in  research

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                                                  Eschweiler Char
                                                  35 to 50  Microns
                                                  P02 '  29 Wa

                                                  (differential)
        --6
       h-8
                1                  1.2

Figure 2.  Reaction  rates  for Eschweiler char.
1.4
1.6

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                         0.6
                         0.4
                         0.2
                                  Cedar Grove Char
                                  P  = 1650  Pa
                                                               0.5
                      figure 3 . Cedar Grove char conversion of nitrogen.
              Oxidation of (-C) and (-H)
                              Nitrogen Species Involving Reactions
           Carbon Reactions:
           O2 + 2(-C) 1+ 2(-CO)
           (-CO) ^ CO * free site
           2(-CO) ^» CO2 * (-C ; * free site
                 (-CO
C0
                                 (-CO)
CO
CO2
Hydrogen Reactions:
2(-CH) ^ H2+2(-C)
H2  +  (-CO) 3-^ H20 * (-C;
H2O + (-C) "H H2+ (-CO)
 Formation of NO:
 O2 * (-c; * (-CN) 1-% (-co;  *  (-c/vo;
 (-c/vo; 2£ NO-I-(-C)
 (-CN) + (-CO;^J NO +2(-C)
 Formation of N2Q:
 2(-CNO)2-2*  (-CO) * N2O
 NO + (-CN)2£ N2O + (-C)
 (-CNO) *  (-CN) 2-$N2) +  2 (-C)
Heterogeneous Reduction of
   NO and N2O
NO + 2(-C)  ^» (-CO; + (-CN)
2(-CN)  N -^ 2 •» 2(-C;
A/O + (-CN) -^ /V20 *2 (-C;
N20 + (-C)1%N2 +  (-CO)
                                                 (-CO)
                                   CO2
                                                      18
                               N2O
                               w2o * (-co; ^ 2/vo * (-c;
                               NO + (-c; * (-CH; -»(-co; * (CH/V;
 Formation /Destruction of HCN:
 (-CH) + (-CN) ¥ HCN * (-C;
 «2  * r-c; * (-c/v; 2-%  (-CH) + (-CHN)
 (-CHN) ^» HCN + free site
 HCN + (-CN) 2*  N2 + (-CH)
 (HCN-* NO-I-...?)
 Formation/Destruction of NH3
 H2 + (-CHN) ^ NH3  +  (-C;
                  30
NH3+ (-CO)  +  (-CN) -» N2 + H2O +
   CH+ (-C)
(NH3 -» HCN....?)
(NH3-+NO...?)
Figure 4. Formation of N2 from bound nitrogen during heterogeneous char oxidation.

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       400
       300
       200
       TOO
                 Excess Air
Fluid Bed

   Bed
Temperature
Fuel Nitrogen
 Speciation
           0   10  20   30   40   1000    1100    1200
                Percent                     K
                    NH3   HCN NH3+HCN
Figure 5. Predictions under varied conditions-
                       Coal Particle
*F 	 1
Cyanogens
i
t

Oxycyanogens
\
p
A/Hj, NHz, NH
i
p




1
NO
>
V
r
•4-
1
f
    Figure 6.  NOxand N2O formation from coal..

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programs  as well as  the   problems
associated with grab sampling
  Limited methods of N20 measurement
are available.  Quantitation is usually
done by  gas chromatography using an
electron  capture  detector (GC/ECD).
Although suitable,  a disadvantage of GC
analysis  is  that a  true  real  time
measurement is not possible and that a
high skill level is required to perform the
analysis.
  Larry Muzio  (Fossil  Energy  Research
Corporation) reported on the  status of
the development  of an  on-line infrared
N2O analyzer. As a result of  his research
efforts, a  prototype  production  model
capable  of measuring  low  ppm
concentrations  with  high  precision is
currently being manufactured and  will be
field tested soon.
  Muzio (FERCo)  and Kramlich  (EERC)
presented  startling   results  of  a
collaborative study of interferences from
SO2 with  respect to N20, in  sample
containers under certain  conditions.
While conducting natural gas tests using
FERCo's  combustor,  high N2O  was
measured  while  doping with  ammonia (to
generate  NOX) and SO2  N20  samples
were collected in  glass  flasks using an
extraction  system  where moisture
removal   was  not  utilized  prior to
collection.  It was  discovered that, while
doping  with  2,500  ppm S02,N20
concentrations on  the order  of 300 ppm
were  observed,  while the condition
without S02 doping measured only about
1 ppm N20.
  Muzio and Kramlich began to suspect
that a reaction  in the sampling system
was the source of the  N20 artifact. At this
time, an attempt was made to  generate
N2O in the sample container. A synthetic
mixture containing N2, 02  C02 and NO
was placed in the flasks, one contaning
deionized H2O and no SO2 with the other
containing 1,500  ppm  SO2 and dilute
sulfuric acid. Over 150  ppm  N20  was
generated  from the SO2/sulfuric-acid
containing mixture while  virtually no N20
was measured  in the  mixture  lacking
these  components.    The test  was
performed again  without  adding S02.
This  time  no  N20  generation  was
observed,  isolating the importance of S02
in the artifact mechanism (see Figure 7).
  Tests were designed  to  determine if
the removal of  S02  or  moisture could
enable a  sample of uncompromised
integrity  to be  collected.  Sodium
hydroxide and  sodium  carbonate were
found to be effective  in neutralizing SO2
while having no evident effect on known
 N20  levels.  Passing  the  sample  gas
through  an  ice bath condenser reduced
the NO/SO2  interaction considerably,
although some  N20  generation  was
observed.
   Muzio stressed  the  impetus of the
artifact discovery  in regard  to  current
emission   data  bases  and  to  the
contribution from fossil fuel combustion
to the global N20 budget.

Full Scale Field Data
  The third session of the workshop
included a series of presentations on data
collected from both mobile and stationary
sources. The  presentations included
data from full-scale stationary utilities  in
the United States and  Europe.  The
presentations  provided  N20 emission
values measured  from different  research
facilities as well as industrial equipment
to provide a better  representation of N20
discharge levels and to assess the role of
fossil  fuel   combustion on  global  N2O
levels. Because of the sampling artifact
discussed  in the  previous session, each
presenter was  asked  to  include
information regarding  sampling  and
analytical techniques used, moisture and
sulfur content  of the sample, and any
efforts  taken  to  remove  these
constituents.
  European data represented about 70
different facilities  ranging  in  firing
capacities from 0.5 to 800 MW, with most
facilities in  the 100-600 MW range.  Data
from  circulating and stationary fluidized
bed combustors (FBCs) were included in
the presentations.  Data  from   coal
combustors  comprised  a  significant
portion of  the presentations,  although
emission data from peat,  distillate oil,
wood, refuse, and natural gas combustion
were also discussed.
  The European  data, excluding those
from FBCs, were  considerably lower than
U.S.   data  presented  from  similar
facilities. Figure 8  shows data  collected
from  full scale units using various  NOX
reduction methods  while firing European
brown coal  (RWE) that are plotted  along
with  data  presented  at the  Boulder,
Colorado  workshop.  Table  1  is  a
compilation of data presented  for easy
comparison.  Other data collected  using
on-line techniques  also  exhibited
extremely  low N20 values,  often  less
than 10 ppm.

Discussion To   Arrive at  Practical
Conclusions
  The remainder of the workshop was
designated  for open discussion of
material  presented and  for  reaching
practical conclusions on the direction  o
future research efforts.
  Steven Lanier (EERC)   offered the
following  conclusions to the participants
for discussion:
  1. A critical need exists to  develop and
    validate sampling and  analysis
    procedures.
  2. The  GC/ECD  method  of analysis
    appears   adequate,  but  the
    development  of a  continuous
    emission  monitor  for  N2O  is
    encouraged.
  3. Following validation, repeat sampling
    of utility boiler and  fuel classes,
    which have previously indicated high
    N20 emissions, is urgently  needed.
  4. Prediction  of  global N2O  increases
    based on  AP42 NOX factors is not
    scientifically justifiable.
  S.Mobile sources are a   minor
    contributor to the N2O emissions.
  6. European  data  indicate that direct
    N2O emissions  from coal-fired
    boilers  are a minor contributor  of
    N2O.
  7.Continued evaluation  of  N2O
    emissions  from  fluidized  bed
    combustors is encouraged.
  8. Other combustion sources  such  as
    catalytic   crackers  should  be
    evaluated.
  9. No clear consensus exists as to how
    NOX  combustion modifications will
    affect emissions
  A vigorous discussion period followed
Lanier's conclusions, showing    general
agreement  with them.  It was suggested
that  the possibility  of NO's  being
converted to N2O in the atmosphere  be
explored  as well.  It was also suggested
that  the  contribution from  other
combustion sources  should also  be
evaluated, biomass burning  in  particular.
The  participants agreed most   strongly
that  a  suitable  and  valid sampling
protocol should  be developed.
  K.  Hein (RWE) summarized the final
conclusions  reached  from  the
discussion:
  I.New information on N20  formation
    and destruction mechanisms  in stack
    gas samples precludes  earlier coal-
    and oil-fired boiler data.
  2. Assuming that the  European data are
    valid, the  direct emission  of  N2O
    from coal-fired  boilers  is a  minor
    contributor to  observed   global
    increases in N2O.
  3. Sampling,    handling,     and
    measurement techniques must  be
    thoroughly studied to  assess NO
    conversion to  N2O  in  sample

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                    200
                    TOO  -
Base Gas Mixture:
N2 86.2%
O2 4.3%
CO2 9.4%
NO 600 ppm

-

Liquid: H2O H2SO4(PH=2)
SO2 0 7500
    Figure 7. Synthetic gas mixtures in glass sample flask. 1. Title.
      200
      150
   Q.
   o"
      too
       50
                      250
500           750

         ppm
                         QAcurexJEPA
                         OHarvard
                         OMIT
                         &EPFU
                         VTU Delft (PFBC)
                         • RWE
1000
1250
Figure 8. Comparison with previous results.

-------
    containers characterizing catalytic
    effects.
  4. Repeat and extended measurements
    of NOX and  emissions from different
    combustion equipment types, fuel,
    etc.,  are  needed,  with  special
    attention to FBC  units  as  high
    emitters of N2O.
  5. All  other combustion  sources,
    including biomass burning, should be
    included in the evaluation of  global
    N20 emissions.


Summary
  Information presented at this workshop
suggests that N20  emissions have a
significant effect on both stratospheric 03
depletion  and global climate  change.
Studies  indicate an  annual increase in
N2O in  the  atmosphere of  0.2-0.3
percent, and isolating the source  of the
increase  is essential  to  prevent further
worldwide climate change.  There is still
some  question  as  to whether  the
combustion  of fossil fuels is directly
responsible  for the increase.  More
research is needed to find reliable and
accurate techniques for  establishing a
data base of  N20  emissions  from
combustion.
  The  mechanisms and conditions
involved  in N2O  combustion formation
and  destruction  are  not   well
characterized. N2O formation ispossible
in post-flame, temperature-dependent,
gas phase reactions.  Material presented
at the  workshop suggests that  volatile
HCN exposed to temperatures  between
1,150 and 1,500 K can  be converted to
N20 The possibility of this is supported
by  models  and  experiments.
Heterogeneous    N2O   ormation
mechanisms are also possible, but the
amount  of  N20  they  produce is less
thanobserved high stack emissions. The
use  of  catalysts  for  NOX  reduction
methodologies  has  not been  well
characterized  for N2O formation.  The
production  of  N20  is  temperature
dependent and  does not seem  to  be
significant in these reactions.
  Most of the information presented at
the  workshop  was  related to  N2O
measurement  techniques.  Muzio's
presentation  on  N2O generation  in
sample containers questions the  validity
and  accuracy of much of the reported
data.  A verifiable sampling technique is
essential  to assess the role of fossil-fuel
combustion in rising  concentrations of
atmospheric N20. Muzio pointed out that
NOx, S02, and N2O are involved in  the
artifact scenario. The removal of either of
these  components  could  halt  the
generation  of  N2O.  However,
considerable research is still  needed in
this  area, because these mechanisms
may also occur in the atmosphere. If this
is so, positive  identification  of  the
reaction  mechanism  is crucial,  which
opens an  entirely  new avenue  of
research.  Although sampling questions
still exist, the  analytical  methodologies
employed in  quantifying grab samples
are adequate. The development of an on-
line  continuous  N2O  monitor would  be
invaluable in combustion research.
  Substantial data was presented on the
N20 direct-emission levels from  various
European stationary utilities  employing
several  different  types  of combustion
techniques.  Fuels  other than coal were
included  in  these  presentations.
Considerably lower N20 emissions were
realized in relation to United States data.
In  the   presentations,  methods  of
sampling were also described. Much of
the European data include extensive
moisture  removal in  sampling. A
refrigeration condenser  was used,  and
desiccants were  employed.  Several
presentations  included  on-line
measurements, which showed very low
N2O concentration levels on  non-FBC
combustors.   The data presented  on
FBCs showed  significantly higher levels
of  N2O  emissions,  which supports
predictions by  computer modeling.  The
emission  of  N20  from  mobile  sources
appears to be very dependent on driving
styles. The conversion of NOX to N2O is
directly related to  catalyst temperature,
which is proportional to driving speed or
revolutions  per minute.   Lower
temperature catalysts  produce higher
N20 emissions.
  A general discussion period completed
the 2-day workshop, put in  perspective
the information presented, and enabled
participants to  set priorities for  research
and goals. Standardization of a practical
and accurate  sampling protocol  was
deemed most essential.  There is no way
to assess N20 emissions from fossil-fuel
combustion  unless  an   accurate
measurement  technique  is available.
Once a suitable  sampling protocol has
been installed, the utility boilers, catalytic
crackers, and other combustion sources
should be retested The combustion of
fuels other than coal and heavy distillates
should  be  considered,  particularly
biomass burning, where limited sampling
efforts have shown significant emissions.
A general consensus was reached that
direct emissions of N2O  from  the
combustion of  fossil fuels is  possibly not
the  major  source  of  N20   in  the
atmosphere, but  more research should
be conducted to support this conclusion.
                                                         10

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-------
  R. J. Ryan and R. Srivastasta are with Acurex Corp.,P.O. Box 13109, Re
  Triangle Park, NC 27709
  Joseph A. McSor/ey is the EPA Project Officer (see below).
  The complete report, entitled "EPA/IFP European Workshop on the Emisss
    Nitrous  Oxide From Fossil Fuel Combustion (Order No.PB90-126038
    $23.00 subject to change) will be available only from:
            National Technical Information Service
            5285 Port Royal Road
            Springfield, VA 22161
            Telephone: 703-487-4650
  The EPA Project Officer can be contacted at:
            Air and Energy Engineering Research Laboratory
            U.S. Environmental Protection Agency
            CResearch Triangle Park, NC 27711 Rin
United States                   Center for Environmental Research
Environmental Protection         Information
Agency                         Cincinnati OH 45268
Official Business
Penalty for Private Use $300

EPA/600/S9-89/089

-------