PB83-117069
    Mechanisms of NOx Formation and Control
    Alternative and Petroleum-Derived Liquid Fuels
   Energy and Environmental  Research Corp.
   Santa Ana, CA
   Prepared for

   Industrial Environmental Research  Lab.
   Research Triangle Park, NC
   1981
U.S. D«?ertiRKit of Commerce
Nations! Technical Information Service

-------
                                TECHNICAL REPORT DATA
                         (Pleetr rend lasuuctiunt on the went btfort compte'
1. REPORT NO.
  EPA-600/D-82-344
PUBLISHED PAPER
                               PB83-117069
4. TITLE AND SUBTITLE
Mechanisms of NOx Formation and Control:
  Alternative and Petroleum-de rived Liquid Fuels
                         5. REPORT DATE
                          1981
                         6. PERFORMING ORGANIZATION CODE
?. AUTHOR(S)
G.England, M. Heap, D. Pershing, and R.Nihart
  (EERC); and G.B.Martin (EPA)	
                                                     8. PERFORMING ORGANIZATION REPORT NO,
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Energy and Environmental Research Corporation
8001 Irvine  Boulevard
Santa Ana,  California 92705
                                                      10. PROGRAM ELEMENT NO.
                         11. CONTRACT/GRANT NO.

                         68-02-3125
12. SPONSORING AGENCY NAME AND ADDRESS
 EPA, Office of Research and Development
 Industrial Environmental Research Laboratory
 Research Triangle Park, NC  27711
                         13. TYPE OF REPORT AND PERIOD COVERED
                         Symposium paper; 1981	
                         14. SPONSORING AGENCY CODE
                          EPA/600/13
is. SUPPLEMENTARY MOTES ERL-RTP author Martin's mail drop is 62; his phone is 919/541-
7504. Paper was published in Eighteenth Symposium (International) on Combustion,
The Combustion Institute. 1981. DP 163-174.	
 s. ABSTRACT
              paper gives results of burning petroleum-, coal-, and shale-derived
liquid fuels in a downf ired tunnel furnace to assess the impact of fuel properties on
the formation and control of NOx emissions. A nitrogen-free oxidant mixture (Ar,
CO2, O2) was used to isolate fuel NOx formation. Under excess air conditions, fuel
NOx correlated well with total fuel nitrogen content for both the petroleum and alter-
nate fuels. Under staged combustion conditions, the  influence of fuel nitrogen content
was much less pronounced but equally highly correlated except for coal-derived
liquid. Exhaust NOx emissions were directly related to the amount of oxidizable
nitrogen species  leaving the first stage. NO, HCN, and NH3 concentrations were
measured in the fuel-rich zone of the staged combustor as a function of stoichiometry
for seven liquid fuels and one CH4/NH3 mixture. Similar characteristics  were obser-
ved for all liquid fuels. As  the first stage stoichiometry (SRI) was reduced,  NO con-
centrations at the first stage exit decreased; however, below SRI  = 0. 8, HCN and
NH3 concentrations increased.  Thus, the total fixed nitrogen (TFN = NO + HCN +
NH3) concentration passed through a minimum. Experimental data also indicated that
increasing the temperature of the fuel-rich zone decreased TFN concentration which
resulted in reduced exhaust NOx emissions.
17.
                             KEY WORDS AND DOCUMENT ANALYSIS
                DESCRIPTORS
                                          b.lDENTIFIERS/OPEN ENDED TERMS
                                     C. COSATI 1-ield/GlOUp
Pollution
Fossil Fuels
Combustion
Nitrogen Oxides
Stoichiometry
             Pollution Control
             Stationary Sources
13B
21D
21B
07B
07D
18. DISTRIBUTION STATEMENT
 Release to Public
                                          19. SECURITY CLASS I This Report)
                                          Unclassified
                                     ii.NO. OF PAGES.
                                        13.
             JO. SECURITY CLASS (This page)
             Unclassified
                                     22. PRICE
EPA Form 2220-1 (»-73)

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                                                                          EPA-600/D-82-344
                                                                          PUBLISHED  PAPER
Eighteenth Symposium (International) on Combustion      The Combustion Institute. 1981

                                    pgs.  163-174
  MECHANISMS OF NO, FORMATION AND CONTROL:  ALTERNATIVE
                 AND PETROLEUM-DERIVED LIQUID FUELS


                G. C. ENGLAND,' M. P. HEAP, D. W. H3RSHING, R. K. NIHART
  Energy and Environmental Research Corporation. 80O1  Irvine Boulevard. Santa Ana. California 92705
                                         G. B. MARTIN
        l). S. Environmental Protection Agency, Industrial Environmental Research Laboratory,
                           Research Triangle Park, North Carolina 27711
        Petroleum-, coal- and shale-derived liquid fuels were burned in a downfircd tunnel furnace
      to assess the  impact of fuel properties on the formation and control of NO, emissions. A
      nitrogen-free oxidant mixture (Ar. CO2, O2) was used to isolate fuel NO. formation. Under
      excess air conditions fuel NO, correlated well with total  fuel nitrogen content for both the
      petroleum and alternate fuels.  Under staged  combustion conditions the influence of fuel
      nitrogen  content was  much less pronounced but equally  highly  correlated except in  the
      case of a coal-derived liquid.
        Exhaust NO, emissions were found to  be  directly related to the amount of oxidizable
      nitrogen  species  leaving the first stage. NO,  HCN and NH3 concentrations were measured
      in the fuel-rich zcnc of the staged combustor as a function of stoichiometry for seven  liquid
      fuels and one CH4/NH3  mixture. Similar characteristics were observed  for all liquid fuels.
      As the first stage stoichiometry  (SR,)  was reduced, NO concentrations at the first  stage
      exit decreased, but below SR, = 0.8 HCN and Nil, concentrations increased. Thus,  the
      total fixed nitrogen (TFN = NO + HCN + NH3) concentration  passed through a minimum
      Experimental data also indicated that increasing the temperature of the fuel-rich zone decreased
      TFN concentration which resulted in  reduced exhaust NO. emissions.
                  Introduction                     of the controlling mechanisms and the trade-off with
                                                  smoke  emissions. This paper summarizes a series
  Increased coal utilization provides a partial solu-    of experimental investigations carried out at atmo-
tion to current energy problems; however, the need    spheric pressure  to define the  influence  of fuel
for a balanced fuel economy and realities of retrofit    properties and combustor design parameters on NO,
capability necessitate that in the future many indus-    formation. Twenty-six petroleum-, shale- and coal-
trial users will be required to burn heavy liquid    derived liquid fuels were burned in a refractory-
fuels, both petroleum-  and coal- or shale-derived.    lined tunnel furnace. In-flame measurements were
Since these fuels, particularly the alternativeliquids,    made to quantify the influence of temperature and
have  relatively high fuel  nitrogen contents, there    stoichiometry on  the fate of fuel nitrogen species.
is potential for increased  nitrogen oxides (NO.)    The ultimate objective of the study was to provide
emissions unless preventative measures are taken.'"    design  criteria for full-scale lo .v emission oil burners
  Staged combustion has proved to be an effective    suitable for a wide range of fuels.  The approach
NO,  control   technique  for  residual  oil-fired    was to  divide the overall heat release process into
systems."1"'" However, optimization has proven    a series of zones: 1) a fuel vaporization  region; 2)
to be difficult because  of a limited  understanding    a fuel-rich hold-up zone;  3) a second stage  air
                                                  addition zone; and 4) a burnout zone. The  results
  "Author  to  whom correspondence should  be    presented  in this  paper aie mainly concerned with
directed.                                          the optimization of the fuel-rich hold-up zone.

                                              103

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164
COMBUSTION GENERATED POLLUTION
             Experimental Systems

Tunnel Furnaces

  The fuel comparison tests in this study were done
in a  downfired,  tunnel  furnace which has  been
described in detail  previously.7 The vertical  com-
bustion chamber was 2.1 m long and 20 cm in inside
diameter. The overall outer diameter was approxi-
mately 81 cm and the walls consisted of insulating
and high temperature castable refractories. All air-
streams were metered with precision rotameters and
the artificial atmospheres were supplied from high
pressure  cylinders.
  The staged combustion tests were conducted in
a separate but similar tunnel furnace illustrated in
Fig.   1.  In  this  system  the  vertical  combustion
chamber  was 2.3 m long and 15.2 cm in  inside
diameter. The walls contained slots which allowed
insertion of stainless steel cooling  coils, thus, the
temperature profile  within the  furnace could be
significantly changed by varying the location and
number  of these  coils.  The slots  were also used
for inserting a refractory choke/secondary air  injec-
tion system. A 5 cm  inside diameter choke was used
to prevent recirculation of second stage air into the
first  stage. The secondary  air injector  was a 10.2
                    FUEL »
                  ATOMIZING AIR
                            PRIMARY AIR
      RESIDENCE
        TIME
METERS SECONDS
     0-1 O-i
        0.5-
    1.0-
    1.5-
    2.0-
         I.O-J
                                 i_ INSULATINQ
                              ^//f  REFRACTORIES
  Fic. 1. Furnace configuration showing approxi-
mate residence time for SR, = 0.78.
                       cm diameter stainless steel ring with 24 6.3 mm
                       diameter holes drilled  parallel  to the axis  of the
                       furnace. The injector was designed to provide grad-
                       ual mixing of the secondary air with  the primary
                       combustion products. The velocity ratio of the sec-
                       ondary air to the incoming combustion  products
                       was approximately 2-to-l at a first-stage stoichiome-
                       try of 0.8. In some tests a second refractory choke
                       was also inserted near the top of the furnace to
                       shield the initial fuel vaporization zone from cooling
                       coils in the first stage. This "radiation choke" made
                       it possible  to vary temperatures in the  fuel-rich
                       hold-up zone without influencing the rate of droplet
                       vaporization and initial combustion.
                         The full-load firing rate in all experiments (both
                       furnaces) was 0.53 cc/sec. In both systems the fuel
                       injector consisted of  a 19 mm diameter  stainless
                       steel  tube containing an atomizing air supply tube,
                       fuel  supply  tube, a cartridge  heater for  final oil
                       temperature control, and a chromel/altimel thermo-
                       couple for accurate measurement of oil temperature.
                       A commercial,  ultrasonic  oil  atomizer was used
                       because it provided excellent  atomization  of  the
                       heavy fuel  oils at  relatively low flow rates even
                       though the atomizer is designed for lighter oils. The
                       spray from this atomizer has been characterized in
                       a separate study -using a laser diffraction drop size
                       analyzer and produces a very  narrow  distr'bution
                       of drop sizes centered at 20 u,m under the operating
                       condition of these experiments. .

                       Analytical System

                         Exhaust  concentrations were monitored contin-
                       uously  using a chemiluminescent analyzer for NO
                       and NO,, an NDIR analyzer for CO  and CO2, a
                       paramagnetic analyzer  for O2, and an FID analyzer
                       for total hydrocarbons (THC).  The flue  gas was
                       withdrawn from the exhaust stack'through a water-
                       cooled,  stainless  steel  probe1  using  a  stainless
                       steel/Teflon sampling pump. Sample conditioning
                       prior to the instrumentation consisted of an ice bath
                       water condenser and  glass wool and Teflon fiber
                       filters.  All  sample lines were 6.3 mm Teflon and
                       all  fittings Type 316 stainless steel.
                         In-flame temperature measurements were  made
                       using a standard 19 mm diameter suction pyrometer
                       containing a platinum-platinum/rhodium thermo-
                       couple. In-flame gas samples were withdrawn with
                       a long, stainless steel  water-quench probe.  HCN
                       and NH, were absorbed in a series of impingers
                       ana concentrations determined using  specific  ion
                       electrodes. Sulfide ion interference was minimized
                       by. the addition of iead carbonate."

                       Fuels

                         An  independent   laboratory  determined  the
                       characteristics of the liquid fuels used in this study
                       which are given in Table I.

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                   ALTERNATE AND PETROLEUM-DERIVED LIQUID FUELS
                                                                                               165
       !      Fuel Effects-Excess Air

  Figure 2 is a composite  plot of total and fuel
NO, emissions fcr all of the fuels tested at 5 percent
exce:B O2, 405°K air preheat and 0.53 cc/sec firing
rate. All data were obtained with the ultrasonic
nozzle and an air atomization pressure of 103 kPa
(gage). Fuel viscosity was maintained  at 12 ± 1.5
cs by appropriate selection of fuel temperature. Total
NO. refers to emissions produced with air as the
oxidunt. Fuel NO, is defined as the emissions mea-
sured when molecular nitrogen was excluded and
the fuel burned in an atmosphere composed of argon,
carbon dioxide and oxygen.7 Results obtained with
petroleum-derived fuels are presented in Figure 2a.
Both,  total  and fuel NO, emissions increase with
increasing  fuel  nitrogen content. Distillate oils
doped with pyridine and thiophene (slashed sym-
bols) correlate well with the  actual heavy petroleum
liquids under the conditions of these tests (fine oil
atomization,  rapid  mixing burner). The difference
between total and  fuel NO, data is defined to be
thermal NO, and is approximately constant for all
the heavy  residual oils. However, thermal  NO,
produced from distillate oils is consistently higher
than that produced from residual oils.
  A comparison of total and fuel NO, produced with
alternative and petroleum-derived fuels is presented
in Figure 2b. In general, alternative fuels have higher
nitrogen contents than petroleum-derived fuels and,
therefore, produce higher fuel NO, emissions. With
few exceptions,  fuel NO, emissions  from  both al-
ternative  and petroleum-derived fuels appear to
correlate well on the basis of fuel nitrogen content.
Total NO, emissions from alternative fuels (dashed
line) are higher  than from pure pedoleum-derived
fuels, suggesting a  greater production of thermal
NO,.  This may  be because the  alternative fuels
contain significantly larger fractions of light hydro-
carbons which cause higher peak flame temperatures
since more fuel  is burned prior to vitiation of the
combustion air with recirculated combustion prod-
ucts,  or because the  relatively high vaporization
rates produce higher local combustion intensities.


              Staged Combustion

First  Stage Stoichiometry

  During fuel-rich  combustion the  original  fuel
nitrogen species are  ultimately converted to  N2,
    1000
    BOO
  geoo
  g
  5"
   : 400
    200
                                                   2400
                                                   2000
                                                   1600
 1200
                                                    BOO
                                                    40O
                0.2      0.4      O.6       0.8         6      0.3

                                          FUEL NITROGEN (WTX)
                                                                     1.0
                                                                            1.3
                                                                                   2.0
                                                                                          2.5
                                                                           (b)
  Fie. 2. Total and  fuel NO, produced by (a)  petroleum oils (/ denotes doped distillate or residual
oils) and (b) all liquid fuels.

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     TABLE I
Detailed fuel analyses






Symbol
Ultimate Analysts:
Orlxin. %
IlytlroKrn, %
Nitrogen. %
SlllftlT. %
Ash. %
Oxyjcrn. t
Ojitfjdion Car-
bun Residue, %
Asph-iltene. %
FL«h Point. »F
Pour Point. *F
API Gravity >t
60°F
Viscosity. SSU, at
140-F
at 210-F
Heat of Combustion:
Cross Rtu/lb
Net Btu/lb
Calcium, ppro
Iron, ppm
Mtiijjnese. ppm
MtiK'wsium, ppm
Nickel, ppm
Sodium, ppm
Vanadium, ppm
m



Alaskan
Diesel
*

86.90
12.07
0.008
0.31
<.001
0.62






33.1

33.0
29.5










D2 m

Cali-
VI; - ti>rni»
Trial' No. 2
Diesel . Oil
A 9

mm HUH
9.7-1 12.52
0.028 0.053
1.88 0.27
<.OOI <.001
0.24 038






18.3 32.6

32.0 30.8
28.8 29.5

19.330.








Rl
,


Kast
Coast
o

H6.54
12.31
0.18
036
0023
0(11

2.1
0.34 :
205
50

24.9

131.2
45

• 19.260
18.140
7.1
16
0.09
3.7
6.7
37
14
R2.



Middle
K*st
b.

80.78
1 1.1)5
0.18
O.B7
0.012
041

6.0
3.24
350
48

19.S

490
I3l.fi

19,070
17.9SO
1.2
2.6
0.02
008
13
0.98
25
R3

Law
Sulfur
No. 8
Oil
*

Hfi.57
12.52
0.22
0.21
' 0.02
0.46
•
44
0.94
325
105

25.1

222.4
69.6

19.110
17.970
9.52
123.6
0.46
2.23
14.10
3.74
3.11
R4


Indo/
Malay-
sian
A

86 .5.1
11.93
0.24
0.22 '
0.036
1.04

3.98
0.74
210
61

21.8. •

199
65
.
• 19.070
17.980 •..
14
16
0.13
3.6 ,
19
15
• 101
R5
Venezu-
elan
Desul. -'
fur-
feed
0

S5.92
12.05
0.24
093
0033
O.K3

' 5.1
2.59
176
48

• 23.3

113.2
50.5

18.400 .
17.300 -•
S.7
6.5 :
0.09
3.6
-
'

R6

Pennsyl-
vania
(Antarada
Mess)
b

14.82
11.21
0.34
2. 26
0.067
1.3

12.4
4.04
275
68

' 15.4

1049
240

18.520
. , 17.500
9.2
13.2
0.10
3.3
32.7 .
-". 64.5
81.5
R7



Gulf
Coast
O

84.62 '
10.77
0.36
2.44
0027
1.78

14.8 :
7.02 •
• 155
40

13.2

835
. 181

18.240
" 17.260
4.4 '
. 19
; 0.13
0.4
. 29
: 3.6 '
45
R8 .



Vene- •
Kuelan
0

8.5.24
10.96
0.40
2.22
0.081
1.10

6.8
8.4 •
210
58

14.1

742
'.96.7

18.240
17.400
9.1
11 -
019
3.8
52
32
226
R9


- . _ •.

•' Alaskan
D

86.04
11.18
0.51
1.63
0.034 "
0.61

12.9
5.6 '
!15
38

15.6

1.071
" 194

18.470 .
. 17.580
6.9
24
0.06
1.4
50
37
67
RIO


-•
Calif-
Fomia
V

85.73
11.83
0.62
1.05
0.038
0.71






19.5

246.1
70.00..





•"
:



                                                                                  2
                                                                                  ec.

                                                                                  i
                                                                                  o

                                                                                  0
                                                                                  [=1
                                                                                  D
                                                                                  r
                                                                                  c

                                                                                  o
                                                                                  z

-------






TABLK
I





(continued) ,







Ultima!? Ana!v
Calcium, ppni
Iron, ppni
Manijalifse. ppni
Magnesium, ppni
Ni. If 1. ppni
Sodium, ppni
Va.tatltum. ppni
Rll



Call-
furi.ia
0

S54
11.44
0.77
1.69
0.043
0.71

fl.72
5. IS
Ck(
3S ''.
15.4

K54
129

IS.470
17.430
21
7.1
O.S
5.1
65
21
44
RI2



Call.
fornia
0

S5.33
11.23
0.79
1.BO
0.0.12
1.02

9.22
S.IS
150
.10
15.1

74S.O
131.0

IS.4SO
17.440
14
53
0.1
3.S
S2
2.6
53
RI3



Cali-
fornia
C2

SB.OK
10.44
O.S«
0.99
0.20
O.h5

15.2
S.62
ISO
42
12.6

720
200

IS.2,10
I7.2HO
U0.6
77.2
O.S7
3 1. 4
ss.o
22.3
66.2
RI4

Cali-
fornia
(Kern
Counts-}
0

S6.61
10.93
O.S3
1.16
0.0.10
0.44

Mi
3.98
225 '
65
1 2.3

46.10
3.52

IS.430
17.4.10
4.4
15
0.15
1.1
6S
.1.4 •
.19
Al


Shall--
l)i-rivt-«t
UKM
f

SK.IS
13(10
0.24
0.51
OIKll
1.07

4.1
0.0.16
IS2
40
33.1

3B.I
30.7

IH.430
1S.240
0.13
6,1
0.06

0.43
0.09
1.1
A2




Synthuil
.

SB.30
7.44
1,16
O.SO
I.56
2,54

2.1.9
IB.55
210
SO
S'l.l-l

IO.S«0
f •**?

IH.-ISO
15.SOO
1 .670
109
«.2
170
2.6
I4S
(15
A3



Crinlr
Shall-
.

S4.6
11,1
2.0S
0.63
.026
1,16

2.»
1.33
250
SO
20.3

97
44.1

IS.290
17,260
1.5
47.9
0.17
5.40
5.00
11.71
<,1
A4



site n
Klrnd
A

S9.91
9.27
0.45
0.065
OOO4
0,111

«. IS
4.10
70
<-72
10.0

40.6
' 32.5

I7.!«0
17.1.10
0,13
3.9
<0,5
0.17
<0,5
0.31
<1.0
A5 A6


Shall-
KI-II-

-------
168
                           COMBUSTION GENERATED POLLUTION
HCN, NO or NH3.010" The intent of staged com-
bustion is to minimize the concentration of total
fixed nitrogen (NH;, + NO + HCN =  TFN) prior
to second stage air addition. Figure 3 presents data
obtained from detailed in-flame measurements  for
a distillate oil (Dl-Alaskan diesel), a typical residual
oil (R9-Alaskan Bunker C), and an alternate liquid
fuel  (A9-SRC-H heavy distillate). These measure-
ments were  made on the centerline of  the furnace
at a  distance of 103 cm (approximately 630 msec)
from the oil nozzle. Detailed radial measurements
indicated that the concentration profile was essen-
tially uniform at this location. These in-flame data
are reported on a  dry, as-measured basis.  Second
stage air was added at 107 cm subsequent  to each
in-flame measurement in these experiments to bring
overall  theoretical  air to  116 percent, and exhaust
NO, measurements, (NO,)K, are also shown (on a
dry,  0 percent O2 basis).
   Decreasing  the  first  stage stoichiometric ratio
reduced NO concentration leaving the first stage.
However, below a  stoichiometric ratio of approxi-
mately  0.8  significant amounts  of  hydrocarbons
(THC) and HCN were measured. Thus, there exists
 a minimum in exhaust NO, concentrations because
 of a competition between decreased first stage NO
 and increased oxidizable  nitrogen species such as
 HCN. It should be noted that HCN concentration
 increased rapidly below SR, = 0.75 and that this
 increase was accompanied by an increase in hydro-
 carbon content of the partially oxidized combus-
 tion products.
   Data for the Alaskan diesel oil (Fig. 3a) also show
 the presence of much smaller but significant con-
 centrations  of HCN and  NHn, although this fuel
 is essentially nitrogen-free. Total conversion of the
• fuel nitrogen would produce 15 ppm TFN  at SR,
 = 0.7.  This confirms previous work'"'" 12  which
 demonstrated that reactions involving hydrocarbon
 fragments and N2 or NO can produce HCN.
   Total fixed nitrogen measured at the exit  of the
 fuel-rich hold-up zone is presented in Fig.  4 as a
 function of stoichiometric ratio for the Alaskan diesel
 oil, three petroleum-derived liquid fuels, three alter-
 nate  liquid fuels, and  methane doped with 0.79
 weight percent nitrogen  as ammonia. All fuels in-
 vestigated showed similar trends. TFN reached a
 minimum concentration at approximately SR, = 0.8,
   240 -
            O.6
                         (o)
                                                           (b)
   Fir.. 3.  NO, HCN,  and NHn production in  the fuel-rich hold-up zone  for (a) Dl-Alaskan diesel oil,
 (b) R9-Alaskan bunker C oil, and (c) A9-SUC-II heavy distillate oil (3% overall excess oxygon).

-------
                  ALTERNATE AND PETROLEUM-DERIVED LIQUID FUELS
                                                                                             169
    1000
     BOO
  g  600
     400
     200
1800


1600


1400


1200


1000


 800
                                                  600-
                                                   400
                                                   200
               0.6
                            0.8
                                         1.0
   0

 SR,
                                                            0.6
                                                                         0.8
                                                                                      I.O
                                (0)
                                                                             (b)
  Fie. 4. The effect of fuel type and stoichiometry on the production of TFN (XXN,) for (a) petroleum
oils, and (b) alternate fuels.
and then increased significantly as the primary zone
became more fuel-rich. The TFN for both the am-
monia-doped methane  and the  fuel oil of similar
nitrogen content (R14)  showed similar characteris-
tics under fuel-lean conditions. However, below SR,
= 0.7 the heavy oil produced significantly less TFN
than the gaseous fuel.
  Figure 5 shows the partition of TFN as a function
of the  first stage  stoichiometric ratio. Data for the
six liquid fuels and the 0.79 weight percent nitrogen
(as NH3) in methane gas are presented as the per-
centage of the original fuel nitrogen existing as HCN,
NH3 or NO at the end of the fuel-rich first' stage.
In each case the missing fuel nitrogen has  either
been converted to Na or still exists in some partially
oxidized fuel fragment. All of the liquid fuels exhib-
ited the same general trends:
• Above approximately SR,  =  0.8,  NO was the
  dominant TFN species.
• Below SR, = 0.75 the major TFN species was
  HCN and under very fuel-rich conditions HCN
  usually accounted  for  more than 50 percent of
  the initial  fuel nitrogen.
• First stage Nil., levels were always low,  generally
  less than 20 percent of the fuel N. Axial profiles
  indicated that near SR, = 0.8, significant amounts
  of NH3 were formed early in the rich zone, but
  decayed rapidly.
  Alternative liquid fuels produced TFN distribu-
tions very similar to those observed with petroleum-
derived liquids. These results are in marked contrast
to similar data obtained with pulverized coal" which
demonstrated that the TFN yield and the preferred
species were both strong functions of coal composi-
tion.
  The fraction of fuel  nitrogen converted to HCN
was somewhat less for the CH4/NH, mixture (JJO
than  for most of the liquid  fuels tested  (Fig.
5a);  however,  conversion  to  Nil,  (Fig.  5b)  was
higher than the  liquids fuels.  The light  (API  =
21.8)  Indonesian/Malaysian residual oil (A)  pro-
duced consistently  higher  conversion  of  fuel
nitrogen  to  HCN, NH., and  NO than the much
heavier (API  = 12.3) Kern County crude oil  (Q)-
Conversely,  conversion to HCN and NIf, for the
+850°F. shale  residuum (II)  was higher than for
the lighter parent crude shale (®); however, conver-
sion to NO  was lower. The  exact  relationship  of

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                           COMBUSTION GENERATED POLLUTION
                                                                                            1.0
                                                   (b)
                                                                                  (e)
            Fie. 5.  The conversion of fuel-bound nitrogen to (a) HCN, (b) NH3, and (c) NO.
simple fuel properties to conversion of fuel nitrogen
to intermediate XN species is not apparent at this
time.

TFN Contersion in Second Sfagc

  Exhaust  NO, emissions  in a  staged combustor
result from conversion of TFN exiting the first stage
and any thermal NO, production during burnout.
Second stage thermal NO, production is not consid-
ered to be significant in this study because changes
in heat extraction  during burnout had almost  no
effect on final  emissions. Figure 6 shows minimum
exhaust NO, and the associated TFN as a function
of total fuel nitrogen content for the seven  liquid
fuels and the CII.,/NH,.  In general, the minimum
exhaust NO, concentration  occurred at  SR,  = 0.78
± 0.02. Under these optimum staged conditions NOt
emissions (and TFN) correlate well with  total fuel
nitrogen content, but the slope is significantly less
than under excess air conditions  (Fig. 2). Only the
SRC-II heavy distillate (ft) exhibited unusually high
emissions,  and this was the direct result of a high
TFN yield (Fig. 6b). NO, NH, and HCN were  all
substantially higher for this fuel than with compara-
ble fuels at the minimum stok-.iiometry (0.78). The
increased TFN may be the  result of basic chemical
bonding differences between the parent coal from
which the SRC-II was derived and petroleum liq-
uids.
  Figure 7 shows the percent of the TFN exiting
the first  siage which  was converted to NO, in the
second stage (based on NO, measured in the furnace
exhaust). Data for all eight  fuels and  first  stage
sloichiomctrics between 0.5 and 0.8 have been  in-
cluded. As the TFN  concentration increased (due
to decreasing  SR,), the percentage conversion de-
creased. This behavior is analogous to that reported
'previously  for poorly mixed excess air  diffusion
flames." The second stage burnout can be consid-
ered an excess air flame with a gaseous hydrocarbon
furl. The general conversion decrease rngy be the
result of a competition between N2 formation reac-
tions which are second order in XN and first  order
NO formation reactions.
  The distillate oil results «^) in Fig. 7 are substan-
tially below all of the residual  petroleum and al-
ternative liquid data and the CH4/NH, results are

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                   ALTERNATE AND PETROLEUM-DERIVED LIQUID FUELS
                                                                                              171
   400
g
8
8 40O
!
   no
         UINIUUU (N0x)f
         I    I   I   I   I    I   I   I   I    I   I   I
                  0.6     1.2    I «     2.0
                  FUEL MTftOOEN (WTXI
                                            2.4
  Fic. 6. The effect of fuel-bound nitrogen content
on exhaust NO. and TFN in the primary zone (£XN,)
(SR, = 0.78. 3%  overall excess Oz).


slightly high. This suggests that TFN conversion
is also dependent on the nitrogen specialion and/or
Che oxidaliv,:. uf the partial products of combustion
at the exit oi" the fuel-rich zone. At the TFN  = 145
ppm point, the first stage  exhaust from the distillate
oil  contained 10,000  ppm hydrocarbons  and the
dominant TFN species was HCN  (SR, = 0.6). In
contrast, the comparable  heavy  oil points  had less
l:han 400 ppm hydrocarbons and NO was the major
TFN species (SR, = 0.78).
  Fic. 7. Conversion of TFN to exhaust NO, (0.5 £
 SH.sO.8).
 Time-Temperature History

  The TFN concentrations shown in Fig. 6 arc in
 excess of equilibrium levels, and Sarofim and co-
 workers" have suggested that increasing the tem-
 perature of the primary zone would prove beneficial.
 The results presented in Figs. 8 and  9 obtained
 with the shale crude  (A3) demonstrate the impact
 of first stage heat loss on the fate of fuel nitrogen.
 The lu)t conditions  refer to the furnace without
 primary zone cooling and with the radiation choke
 (as shown in Fig. 1). To cool the furnace cooling
 coils were added prior  to the second stage choke
 and the  radiation choke was removed.  Figure  8
 shows exhaust NO, and primary zone gas tempera-
 ture as a function of stoichiometric ratio  for the
 two conditions. Minimum NO, emissions were re-
duced  for the hot case, and Ihe optimum stoichi-
ometry was shifted toward  more fuel-rich condi-
tions.
  The  axial profiles presented in Fig. 9 provide an
explanation for this shift in the minimum emission
levels.  Heat extraction in the first stage impacts the
rate of decay of TFN. Under cold conditions both
NO and  HCN essentially freeze,  whereas without
heat extraction the initial rate of decay for all three
species is much, faster,  leading to !ow TFN con-
centrations at the exit of the fuel-rich first  stage.
It should be noted that  heat extraction also affects
the rate of CO oxidation.
                   Discussion

  NO, control via staged combustion involves opti-
mizing the first stage of the combustor with respect
to (1) thermal environment, and (2) sloichiometry.
It appears that heat loss from the first stage should
be  minimized  for  liquid  fuels because  elevated
temperatures accelerate the rate of XN species decay
toward low equilibrium levels. The data presented
in Fig. 8 clearly  indicate that an increase in first
stage temperature results  in a decrease  in NO,
emissions.
  The optimization of first stage stoichiometry  is
more complex. Measurements within  Ihe  fuel-rich
first stage show that at the optimum stoichiomelry
NO, HCN  and Nil, co-exist. TFN exists mainly as
HCN and  Nil, for more fuel-rich  conditions, and
for conditions less fuel-rich than the optimum, NO
is Ihe primary fixed nitrogen species. Three factors
influence Ihe sloichiometry at which Ihe minimum
exhaust NO, emissions  will occur: (1) Ihe amount
of TFN species present, (2) the relative conversion
efficiencies of Ihe TFN species to NO in the second
stage flame, and (3) Ihe influence of other partial
combustion products on TFN conversion.
  Figure lOa shows Ihe percentage conversion of
Ihe first stage TFN for the •: 850°F shale  fraction.

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172
                           COMBUSTION GENERATED POLLUTION
      600
      TOO
   £400
   *
      3OO
      ZOO
      100
                          D HOT PRIMARY

                          O COOL PRIMARY
                   I
                            I
                                                   ISOO
                                                   1200
                                                    1100
                                                    IOOO
                                                                 I
                                                                         J_
                                                                                   I
         0.3      0.6       O.7       0.8      0.9       0.3       O.6      0.7       0.6      0.9

                                                  SRl

          Fie. 8. The influence of fuel-rich hold-up zone temperature profile on exhaust NO,.
                   0.2      O.I       0.6     0.80      O.2       0.4      0.6      O.6

                                            SECONDS

              Fie. 9, CO oxidation and decay of XN species for two temperature profiles.

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   IOO
I80
z- 60
a
8 20
                   ALTERNATE AND PETROLEUM-DERIVED LIQUID FUELS

                                                               100
0.80
                                                     0.5O
           3OO    900  700  IOOO      2000       400O 6000
                       PPM rXN,(ORY. 0%0Z1
                                                                            (b)
  Fie. 10. Influence of first stage exit composition on second stage  NO, formation (A8 — +850°F shale
fraction).
As the  first  stage sloichiometry  is  progressively
reduced from SR, =  1.05, the TFN decreases (due
to decreased first  stage  NO formation) and  the
percent conversion also decreases (due to increased
second stage combustion). These two effects result
in a rapid decrease in exhaust NO,. Below SR, = 0.8,
the TFN begins to rise dramatically because of HCN
and  NH, formation, but  the percent conversion
continues to decrease. Thus, in general, there exist
two first stage stoichiometries with identical TFN
levels (e.g.,  1000 ppm) but with vastly different
conversion efficiencies (77  percent versus 26 per-
cent) and, hence, different exhaust emissions.
  Figure  lOb indicates that  there are two major
differences between  the upper and lower percent
conversion curves.  First, below approximately SR,
= 0.8, the major TFN species shifts  from  NO to
HCN. Second, at first stage stoichiometries less than
0.8, significant amounts of unburncd hydrocarbons
are carried into the second stage flome. Folsom el
al."  have shown that in  a  simple diffusion flame
the conversion of  HCN and NH3 to  NO and the
retention  of NO arc affected by  the  hydrocarbon
content of the  fuel.  NH3 conversion  is low when
hydrocarbons are  absent,  and hydrocarbons  are
necessary for the reduction of NO or HCN to  N2.
Thus, staged combustion requires the minimization
of TFN, as well as the production of an optimum
TFN/fuel mixture for burnout.
                  Conclusions

  Data have been presented showing the impact of
 fuel properties on NO, formation from liquid fuels
 under both excess air and staged conditions. Inves-
                                        tigations with a wide range of fuels indicate that:

                                        1. Fuel NO formation from petroleum-, shale- and
                                          coal-derived liquid fuels can  be  correlated by
                                          the total fuel nitrogen content under excess air
                                          conditions.
                                        2. NO, control for high nitrogen fuels  is  most
                                          effective when a rich primary zone is  held at
                                          an optimum stoichiometry to minimize both the
                                          TFN concentration and the  TFN  conversion to
                                          NO in the second stage flame. This concentration.
                                          can be minimized by increasing the temperature
                                          of the fuel-rich zone and/or reducing the initial
                                          fuel nitrogen content. The second stage  conver-
                                          sion decreases with increasing  hydrocarbon con-
                                          tent.

                                                       Acknowledgments

                                          These investigations were carried out under Unit-
                                        ed States Environmental Protection Agency (EPA)
                                        Contract 68-02-3125 and the authors gratefully ac-
                                        knowledge '.he guidance of the Project Officer, \V.
                                        S. Lanier. The authors also  wish to  acknowledge
                                        the assistance of J. A., Naccarato,  J. G., Llanos and
                                        J. H. Tomlinson in conducting the experiments, and
                                        particularly to \V. C. Rovesti  of Electric Power
                                        Research  Institute, J. E. Haebig of Gulf Research
                                        and Development Company and  L. Lvikens of the
                                        United States Department of Energy  for their help
                                        in obtaining several alternative  fuels.
                                                        REFERENCES

                                         1.  MANSOUH, M. N. AND M. GKKSTKIN, "Correlation
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174
                           COMBUSTION GENERATED POLLUTION
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