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                  RESEARCH REPORTING SERIES


Research reports of the Office of Research and Development. U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination  of  traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:

    1. Environmental Health Effects Research

   2. Environmental Protection Technology

   3. Ecological Research

   4. Environmental Monitoring

   5. Socioeconomic Environmental Studies

   6. Scientific and Technical Assessment Reports (STAR)

   7. Interagency Energy-Environment Research and Development

   8. "Special" Reports

   9. Miscellaneous Reports

This report has been assigned to the INTERAGENCY ENERGY-ENVIRONMENT
RESEARCH AND  DEVELOPMENT series. Reports in this series result from the
effort funded  under the 17-agency Federal Energy/Environment Research and
Development Program. These studies relate to EPA's mission to protect the public
health and welfare from adverse effects of pollutants associated with energy sys-
tems. The goal of the Program is to assure the rapid development of domestic
energy supplies in an environmentally-compatible manner by providing the nec-
essary environmental data and control technology. Investigations include analy-
ses of the transport of energy-related pollutants and their health and ecological
effects;  assessments of, and  development of, control technologies for energy
systems; and integrated assessments of a wide range of energy-related environ-
mental issues.
                       EPA REVIEW NOTICE
This report has been reviewed by the participating Federal Agencies, and approved
for  publication. Approval does not signify that the contents necessarily reflect
the views and policies of the Government, nor does mention of trade names or
commercial products constitute endorsement or recommendation for use.

This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.

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                                   EPA-600/7-84-074a
                                   July 1984
 ENVIRONMENTAL ASSESSMENT OF A
CRUDE-OIL HEATER USING STAGED AIR
      LANCES FOR NOX REDUCTION
                     Volume I
                 Technical Results
                         By
                      R. DeRosier
                    Acurex Corporation
                Energy & Environmental Division
                    555 Clyde Avenue
                     P.O. Box 7555
                Mountain View, California 94039

                  EPA Contract 68-02-3188
              EPA Project Officer: Robert E. Hall
           Industrial Environmental Research Laboratory
           Research Triangle Park. North Carolina 27711
                        for
          U.S. ENVIRONMENTAL PROTECTION AGENCY
              Office of Research and Development
                  Washington, DC 20460

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                              ACKNOWLEDGMENTS

       This test was performed in cooperation with TOSCO Corporation at their
refinery located in Bakersfield, California.  Appreciation is gratefully
extended to J. Caufield, C. Mulkey, J. McCaskill, and D. Walker of TOSCO
Corporation for their help and cooperation in arranging and conducting this
test.  Recognition is extended to R. Tidona, A. Frohoff, and J. Pionessa  of
KVB, Inc. for operating the continuous monitors and staged air lances.
Special recognition and thanks are extended to the Acurex field test crew of
M. Chips, J. Holm, J. Sniffen, and J. Steiner, under the supervision of
B. DaRos.

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                              TABLE OF CONTENTS


Section                                                                  Page

   1    INTRODUCTION	   1-1

   2    SOURCE DESCRIPTION AND OPERATION  	  .  	   2-1

   3    EMISSION RESULTS  	   3-1

        3.1    CRITERIA AND OTHER GAS PHASE  SPECIES EMISSION
               RESULTS	   3-1
        3.2    TRACE  ELEMENT EMISSION RESULTS   	   3-8
        3.3    ORGANIC EMISSION RESULTS   	   3-16

        3.3.1  GI-CS  Hydrocarbon, TCO, and Gravimetric Analyses   .  .  .   3-17
        3.3.2  IR Spectra of Total Extracts	   3-20
        3.3.3  Low Resolution Mass Spectrometry  (LtfMS) of Total
               Extracts	   3-20
        3.3.4  Gas Chromatography/Mass Spectrometry Analysis  of  XAD-2
               Extracts	   3-24

        3.4    RADIONUCLIDE EMISSION RESULTS 	   3-27

   4    ENVIRONMENTAL ASSESSMENT  	   4-1

        4.1    EMISSIONS  ASSESSMENT   	   4-1
        4.2    BIOASSAY ANALYSIS  	   4-2
        4.3    CONCLUSIONS	   4-2

        APPENDIX A ~ TEST EQUIPMENT AND  PROCEDURES	   A-l

        APPENDIX B — TRACE ELEMENT CONCENTRATIONS AND MASS
                      BALANCES	   B-l
                                     111

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                            LIST OF  ILLUSTRATIONS
Figure                                                                   Page
 2-1   Schematic of the Crude-Oil Heater Tested  	     2-2
 2-2   Flow Schematic of Staged Combustion Air System  for  a  Natural
       Draft Process Heater	     2-5
 3-1   Refinery Crude Heater Sampling Locations  	     3-3
                                      IV

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                                LIST OF TABLES
Table                                                                    page
 1-1    Completed Tests During the Current Program ..........   1-4
 2-1    Heater Operating Conditions  .................   2-3
 3-1    Flue Gas Measurements  ....................   3-2
 3-2    Gaseous Emissions   ......................   3-4
 3-3    Fuel Analyses  ........................   3-6
 3-4    Sulfur Balance   ...... .  ................   3-7
 3-5    Flue Gas Trace Element Emissions  ..... .- ..........   3-9
 3-6    Relative Trace Element Concentrations Between the Baseline and
        Low-N0x Tests  ........................   3-11
 3-7    Baseline Test Trace Element Mass  Balance  ...........   3-12
 3-8    Low NOX Test Trace  Element Mass Balance   ...........   3-14
 3-9    Summary of Total Organic Emissions  ..............   3-18
 3-10   XAD-2 Extract TCO Results  ..................   3-19
 3-11   Summary of IR Analyses of SASS  Sample Total Extracts  .....   3-21
 3-12   Summary of LRMS Analyses of XAD-2 Extracts ..........   3-22
 3-13   Compound Classes and Characteristic Fragment Ions Sought by
        Direct- Insert ion Probe LRMS  ......... .  ........   3-23
 3-14   Compounds Sought in the GC/MS Analysis and Their Detection
        Limits . ...........................   3-25
 3-15   Results of the GC/MS Analyses   ................   3-26
 3-16   Particulate Radioactivity  ..................   3-27
 4-1    Flue Gas Species Emitted at Levels Exceeding 0.1 of an
        Occupational Exposure Limit  .................   4-3
 4-2    Bioassay Results  .............. .  ........   4~3

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                                   SECTION 1
                                 INTRODUCTION

       This  report  describes and presents results of environmental  assessment
tests  performed  for the Industrial  Environmental  Research Laboratory/Research
Triangle  Park  (IERL/RTP)  of the Environmental  Protection Agency (EPA) under
the Combustion Modification Environmental Assessment (CMEA) program, EPA
Contract  No. 68-02-3188.   The CMEA started in  1976 with a 3-year study (NOX
EA), EPA  Contract  No.  68-02-2160, having the following four objectives:
       •   Determine multimedia environmental  effects from stationary
           combustion  sources and combustion modification technology
       •   Develop  and document control  application guidelines to minimize
           these effects
       •   Identify stationary source and combustion modification R&D
           priorities
       •   Disseminate program results to intended users
       During the  first year of the NOX  EA, data  and methodologies  for the
environmental assessment  were compiled.   Furthermore, priorities for the
schedule  and level  of  effort for the various source/fuel/control  combinations
were identified.  This effort revealed major data gaps,  particularly for
noncriteria pollutants (organic emissions and  trace elements)  for virtually
all combinations of stationary combustion sources and combustion modification
techniques.  Consequently,  seven environmental  field test programs  were
                                      1-1

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undertaken to fill these data gaps. The  results  of  these  tests  are  documented
In seven individual reports  (references  1-1  through 1-7)  and  in the final
NOX EA report summarizing the entire 3-year  effort  (reference 1-8).
       The current CMEA program has as its major  objective  the  continuation
of multimedia environmental  field tests  initiated in  the  original NOX  EA
program.  These tests, using standardized Level  1 sampling  and  analytical
procedures (reference 1-9) are aimed at  filling  the remaining data  gaps  and
addressing the following priority needs:
           Advanced NOX controls
           Alternate fuels
           Secondary sources
           EPA program data  needs
           —  Residential oil combustion
           ~  Wood firing in residential, commercial,  and  industrial  sources
           —  High interest emissions determination  (organics, radionucl ides,
               candidate hazardous air pollutant  species, etc.)
           Nonsteady-state operations
       Advanced forms of combustion modifications have  been developed  in
recent years as a means of reducing NOX  emissions without adverse
consequences, such as capacity loss caused by derating  the  unit.  Staged
combustion using air injection lances is one form of  combustion modification
that is relatively easy to retrofit to industrial-sized combustion  equipment
since it requires only minor hardware modification.
       A refinery crude oil  heater, using staged  combustion by  means of  air
injection lances (reference  1-10), was selected  for environmental tests  under
the CMEA program.  The objective of the  tests was to  quantify air emissions
from the heater operating in its normal  state and compare these with emissions
                                      1-2

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from the heater in the low-NOx configuration while  using  the air lances. The
data presented in this report quantify  stack emissions  and  identify  pollutants
of concern using results  from standard  sampling  and analytical  procedures.
       Table 1-1 lists all  tests  performed  to  date  in  the CMEA  effort  and
outlines the source, fuel,  combustion modifications,  and  level  of  sampling  and
analysis in each case.  Results of  these  test  programs  are  discussed in
separate reports available  through  EPA.
                                      1-3

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                              Table  1-1.   Completed Tests During the Current  Program
       Source
       Description
      Test Points
     Unit Operation
      Sampling Protocol
Test Collaborator
Spark ignited natural
gas-fired reciprocating
internal  combustion
engine
Large bore, 6-cylinder,
opposed piston, 186 kW
(250 Bhp)/cyl. 900 rpm,
Model 38TDS8-1/8
   Baseline (pre-NSPS)
   Increased air-fuel
   ratio aimed at
   meeting proposed
   NSPS of 700 ppm
   corrected to IS
   percent 02 and
   standard atmospheric
   conditions
Engine exhaust:
  — SASS
  — Method 5
  -- Gas sample  (Cj - Cg HC)
  -- Continuous  NO, NOX, CO,
     C02, 02, CH4, TUHC
Fuel
Lube oil
Fairbanks Morse
Division of Colt
Industries
Compression ignition
diesel-fired
reciprocating internal
combustion engine
Large bore, 6-cyUnder
opposed piston, 261-kU
(350 Bhp)/cyl, 900-rpm,
Model 38TDD8-1/8
   Baseline (pre-NSPS)
   Fuel injection retard
   aimed at meeting pro-
   posed NSPS of 600 ppm
   corrected to IS per-
   cent 0? and standard
   atmospheric conditions
Engine exhaust:
  -- SASS
  — Method 8
  -- Method 5
  — Gas saipple  (Cj -  Cf, HC)
  — Continuous  NO, NOX, CO,
     COZ, 02. CH4, TUHC
Fuel
Lube oil
Fairbanks Morse
Division of Colt
Industries
Low-N0x residential
condensing heating
system furnished by
Karl sons Blueburner
Systems Ltd. of Canada
Residential hot water
heater equipped with
M.A.N. low-NOx burner,
0.55 ml/s (0.5 gal/hr)
firing capacity, con-
densing flue gas
Low-N0x burner design
by M.A.N.
Furnace exhaust:
  -- SASS
  -- Method 8
  — Method 5
  -- Gas sample (Cj - Cg HC)
  -- Continuous NO, NO,, CO,
     C02, 02, CH4, TUHC
Fuel
Waste water
New test
Rocketdyne/EPA
1ow-NOx residential
forced warm air furnace
Residential warm air
furnace with modified
high pressure burner and
firebox. 0.83 ml/s
(0.7S gal/hr) firing
capaci ty
Low-N0x burner design
and Integrated furnace
system
Furnace exhaust:
  - SASS
  — Method 8
  — Controlled condensation
  — Method 5
  -- Gas sample (Cj - Cg HC)
  — Continuous NO. NOX, CO.
     C02, 02, CH4. TUHC
Fuel
New test

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Table 1-1.  Continued

Source
Pulverized coal-fired
utility boiler,
ConesviUe station







Nova Scotia Technical
College industrial
boiler






Adelphi University
industrial boiler







Pittsburgh Energy
Technology Center (PETC)
Industrial boiler






Description
400-MU tangent 1 ally
fired; new NSPS
design aimed at
meeting 301 ng/J
NOX limit





1.14 kg/s steam
(9,000 Ib/hr) ftretube
fired with a mixture
of coal-oll-water (COW)





1.89 kg/s steam
(15,000 Ib/hr)
hot water
fire tube fired with a
mixture of coal-oll-
water (COM)



3.03 kg/s steam
(24.000 Ib/hr) watertube
fired with a mixture of
coal-oil (COM)




Test Points
Unit Operation
ESP inlet and outlet,
one test








- Baseline (COW)
-- Controlled SO?
emissions wttn
limestone injection





-- Baseline (COW)
-- Controlled S02
emissions with
Na2COj injection





-- Baseline test only
with COM







Sampling Protocol
ESP inlet and outlet:
— SASS
— Method 5
— Controlled condensation
-- Gas sample (Ct - C6 HC)
-- Continuous NO, NOX, CO,
C02. 02
Coal
Bottom ash
ESP ash
Boiler outlet:
-- SASS
— Method 5
— Method 6
— Controlled condensation
-- Gas sample (Cj - C6 HC)
-- Continuous 02, C02,
CO. NO
Fuel
Boiler outlet:
-- SASS-
-- Method 5
-- Method 8
-- Controlled condensation
-- Gas Sample (q - C6 HC)
-- Continuous 02, C02, NO,
CO
Fuel
Uoiler outlet:
-- SASS
-- Method 6
-- Controlled condensation
-- Continuous 02> C02, NO.
TUIIC, CO
-- N^O ijrdb sainplu
Fuel

Test Collaborator
Exxon Research and
Engineering (ER&E)
conducting cor-
rosion tests






Envirocon per-
formed part icu late
and sulfur
emission tests





Adelphi University








PETC and lienural
Electric (ill)







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                                                     Table 1-1.   Continued
       Source
       Description
      Test Points
     Unit Operation
      Sampling Protocol
Test Collaborator
TOSCO Refinery vertical
crude oil heater
2.54 Ml /day
(16,000 bbl/day) natural
draft process heater
burning oil/refinery gas
   Baseline
   Staged combustion
   using air Injection
   lances
Heater outlet:
  -- SASS
  -- Method 5
  -- Controlled condensation
  — Gas sample (C( - C6 ItC)
  -- Continuous 0?. NO, CO,
     CO?, HC
  — N?0, grab sample
Fuel otl
Refinery gas
KVB coordinating
the staged com-
bustion operation
and continuous
emission monitoring
Mohawk-Getty Oil
industrial boiler
8.21 kg/s steam
(65.000 Ib/hr)
watertube burning
mixture of refinery gas
and residual oil
   Baseline
   Ammonia injection
   using the noncatalytic
   Thermal DeNOx
   process
Economizer outlet:
  — SASS
  -- Method 5, 17
  -- Controlled condensation
  •- Gas Sample (Ci - C6 HC)
  — Ammonia emissions
  — N?0 grab sample
  -- Continuous 02, NO,
     CO, C02
Fuels (refinery gas and
  residual oil)
New test
Industrial boiler
2.52 kg/s steam
(20,000 Ib/hr) watentube
burning woodwaste
   Basel1ne (dry wood)
   Green wood
Boiler outlet:
  -- SASS
  -- Method 5
  -- Controlled condensation
  -- Gas sample (Cj - C6 HC)
  — Continuous 02. NO, CO
Fuel
Flyash
North Carolina
Department of
Natural Resources,
EPA 1ERL-RTP
Industrial  boiler
3.16 kg/s steam
(29,000 Ib/hr)
firetube with refractory
firebox burning woodwaste
-- Baseline (dry wood)
Outlet of cyclone participate
collector:
  -- SASS
  -- Method 5
  -- Controlled condensation
  -- Gas sample (Ct - Ce HC)
  -- Continuous 02, NOX, CO
Fuel
Bottom ash
North Carolina
Department of
Natural Resources,
EPA 1ERL-RTP

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                                                     Table  1-1.   Continued
       Source
       Description
      Test Points
     Unit Operation
      Sampling Protocol
                                 Test Collaborator
Enhanced oil  recovery
steam generator
15 MW (SO million Btu/hr)
steam generator burning
crude oil equipped with
MHI low-NOx burner
-- Performance mapping
— Low NOX operation
Steamer outlet:
  — SASS
  -- Method 5
  — Method 8
  — Gas sample (Cj - C6 IIC)
     Continuous Oy, NOX, CO,
     CO?
     NoO grab sample
Fuel
                                 Getty Oil  Company,
                                 CE-Natco
Pittsburgh Energy
Technology Center
(PETC) Industrial
boiler
3.03 kg/s steam
(24,000 Ib/hr) watertube
fired with a mixture of
coal-water (CUM)
   Baseline test only
   with CUM
Boiler outlet:
  -- SASS
  — Method 5
  — Method 8
  -- Gas sample (Cj - C6 HC)
     Continuous ,0?. NOX. CO,
     COp, TUIIC
     NoO grab sample
Fuel
Bottom ash
Collector hopper ash
                                 PETC and General
                                 Electric

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                                                   Table 1-1.  Concluded
Source
Internal combustion
engine — nonselective
NOX catalyst
Industrial boiler
Industrial boiler
Description
BIB HP Waukesha engine
equipped with OuPont USER
catalyst
180 kg/hr steam
(400 Ib/hr) stoker fired
with a mixture of coal
and waste plastic
7.6 kg/s steam
(60,000 Ib/hr) watertube
retrofit for CHM firing
Test Points
Unit Operation
— Baseline
— Baseline (coal)
— Coal and plastic
— Baseline (CUM)
Sampling Protocol
Catalyst inlet and outlet
-- SASS
-- NH3
-- HCN
— Grab sample NgO
-- Continuous 0?, CO?, NOX
TUHC fuel
Boiler outlet
~ SASS
— VOST
— Method 5/8
-- HC1
— Continuous 02. NOX, CO,
CO?, 1UHC
— N?0 grab sample
Fuel
Flyash
Bottom ash
Cyclone ash
Boiler outlet
-- SASS
-- VOST
— Method 5/8
— Grab sample (Ci-Cg HC)
— Grab sample ^0
— Continuous NOX. CO, CO?,
02. TUHC, S02
Fuel
Test Callaborator
Southern California
Gas
Vermont Agency of
Environmental
Conservation
EPRI, E. 1. OuPont
I
CO

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                         REFERENCES FOR SECTION 1
1-1.   Larkin, R., and E. B. Higginbotham, "Combustion Modification Controls
       for Stationary Gas Turbines:  Volume II.  Utility Unit Field Test,"
       EPA-600/7-81-122b, NTIS PB 82-226473, July 1981.

1-2.   Higginbotham, E. B., "Combustion Modification Controls for Residential
       and Commercial Heating Systems:  Volume II.  Oil-fired Residential
       Furnace Field Test," EPA-600/7-81-123b, NTIS PB 82-2311756, July 1981.

1-3.   Higginbotham, E. B., and P. M. Goldberg, "Combustion Modification NOX
       Controls for Utility Boilers:  Volume I.  Tangential Coal-fired Unit
       Field Test," EPA-600/7-81-124a, NTIS PB 82-227265, July 1981.

1-4.   Sawyer, J. W., and E. B. Higginbotham, "Combustion Modification NOX
       Controls for Utility Boilers:  Volume II.  Pulverized-Coal Wall-fired
       Unit Field Test," EPA-600/7-81-124b, NTIS PB 62-227273, July 1981.

1-5.   Sawyer, J. W., and E. B. Higginbotham, "Combustion Modification NOX
       Controls for Utility Boilers:  Volume III.  Residual-Oil Wall-Fired
       Unit Field Test," EPA-600/7-81-124c, NTIS PB 82-227281, July 1981.

1-6.   Goldberg, P. M,, and E. B. Higginbotham, "Industrial Boiler Combustion
       Modification NOX Controls:  Volume  II.  Stoker Coal-Fired Boiler Field
       Test — Site A,ft  EPA-600/7-81-126b, NTIS PB 82-231085, July 1981.

1-7.   Lips, H. I., and E. B. Higginbotham,  "Industrial Boiler Combustion
       Modification NOX Control:  Volume  III.  Stoker Coal-Fired Boiler Field
       Test — Site B,fl EPA-600/7-81-126c, NTIS PB 82-231093, July 1981.

1-8.   Waterland, L. R., et al., "Environmental Assessment of Stationary
       Source NOX Control Technologies —  Final Report," EPA-600/7-82-034,
       NTIS PB 82-249350, May 1982.

1-9.   Lentzen, D. E., et al., "IERL-RTP  Procedures Manual: Level 1
       Environmental Assessment  (Second Edition},'1 EPA-600/7-78-201,
       NTIS PB 293795, October 1978.

1-10.  Tidona, R. J., et al., "Refinery Process Heater NOX Reductions Using
       Staged Combustion Air Lances," EPA-600/7-83-022, NTIS PB 83-193946,
       March 1983.
                                     1-9

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                                   SECTION 2
                        SOURCE DESCRIPTION AND OPERATION

        The  tests  were  performed on a natural  draft, crude-oil  process heater
located at  the  TOSCO oil  refinery in Bakersfield, California.   The heater has
a rated maximum firing rate of 16 MW (55 million Btu/hr) heat input.  The
heater  is fired by  six John Zink D8A-22 natural  draft burners, which are
combination oil/gas burners with a turndown ratio of 3:1.  Testing was
performed with  the  unit firing approximately a 64/36 (heat input basis)
refinery gas/oil  mixture.   All  six burners were firing reabsorber gas from the
plant.   However only four  were cofiring oil  during the tests due to plugged
oil guns in the other  two  burners which could not be cleaned in time for the
tests.   This unit normally fires exclusively reabsorber gas during the summer
(when tests were  performed) since it is in plentiful  supply as a result of
normal  refinery operations at this time of year.
        Figure 2-1 is a schematic diagram of the process heater.  The sampling
ports were  located  approximately 6 stack diameters from the damper which is
not enough  to establish a  uniform velocity profile.  This is supported by
preliminary traverse data  which indicated that the flow was predominately on
one side of the stack  (reference 2-1).   Table 2-1 summarizes the boiler
operating data  for  both tests.   As noted, the heater  was firing about
64 percent  reabsorber  gas  and 36 percent oil  (by heat input for both tests).
The fuel flowrates  remained essentially constant throughout the tests.   There
                                      2-1

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   Cl

   o =
  o E
   -CM
                                           •Stack 4  ft, 6 in.
                                            outside  diameter
                                            (1.4m)
   c

   LO
c

CM =
 Lft   _

 o  ^

  " CM
 4->
 •*-  1
 CO  f
           u
                            ra;
                                            Convection
                                            section
                                            'Jot 'to  Scale

                                            Radiant section
                                            16 ft, 9.5 in.
                                            outside diameter
                                            (5.1m)
                                            15 ft, 9.5 in.
                                            inside diameter
                                            (4.8m)
                                          Air plenum and
                                          sound suppression
                                          box
Figure 2-1.   Schematic  of  the Crude-Oil Heater Tested
                         2-2

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Table 2-1.  Heater Operating Conditions

Process rate, 1/s (bbl/day)
Reabsorber gas
Flowrate m3/min (scfm)
Heat input MW (million Btu/hr)
Fuel oil
Flowrate kg/mi n (Ib/min)
Heat input MW (million Btu/hr)_

Temperatures, °C (°F)
Crude in
Crude out (east)
Crude out (west)
Tube 13, pass A
Tube 13, pass B
Tube 15, pass A
Tube 15, pass B
Tube 20, pass A
Tube 20, pass B
Tube 25, pass A
Tube 25, pass B
Pressures, kPa, (psig)
Crude in (east)
Crude in (west)
Crude out
Burner - oil3
Burner - steam3
Burner - gasb
Gas pressure to heater
Excess air (percent)0
Baseline
21.5 (11,640)

7.1 (251)
8.35 (28.5)

6.59 (14.5)
4.77 (16.3)
c

196 (384)
338 (641)
336 (637)
403 (758)
407 (764)
391 (735)
373 (704)
397 (746)
411 (772)
411 (771)
416 (780)

960 (140)
896 (130)
227 (33)
324 (47)
537 (78)
30 (4.4)
234 (34)
22
Low NOX
21.5 (11,640)

7.1 (251)
8.13 (27.7)

6.55 (14.4)
4.75 (16.2)


196 (384)
339 (642)
339 (642)
405 (761)
395 (743)
387 (728)
373 (704)
395 (743)
395 (743)
406 (762)
408 (766)

960 (140)
896 (130)
234 (34)
324 (47)
537 (78)
30 (4.3)
241 (35)
17
3Average of four burners using oil
^Average of all six burners
Calculated from fuel analyses and flue gas
                              measurements
                  2-3

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were no significant changes in the operating conditions  of  the  heater which
would affect the crude oil flowing through it.
       The-low NOX test used a system of air injection lances to effect  staged
combustion for NOX control.  Figure 2-2 presents a schematic of the  system
which consists of a fan to supply air to the lances, a manifold and  associated
tubing, and 24 (4 per burner) variable-height lances (reference 2-2).  The
lances consist of vertical tubes of 316 stainless steel, having a 3.18-cm
(1.25-in.) outer diameter with a 45° elbow near the end.  The elbow  provides
better mixing across the flame.  Although the air lances are capable of
delivering half of the stoichiometric combustion air, they delivered 44
percent during the test.  The rest of the combustion air is delivered through
secondary air registers located at the base of the heater.  Air flow through
the heater is controlled by the stack damper located above the convection
section.
                                     2-4

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r\j
i
en
                                         Heater
                        L_	J
                                                                            Staged air system
                                              Flexible  tubing


                                                             Butterfly valve
                See  detail  A  and  B
                                                                               r3-in. PVC    VIO-in. x 8-in.
                                                                               I ball valve   \reducer
                                                                              X
8-in. cap
                                                                 7
                                                                ''a-'
                                                                                                 -™- outlet
                  8-in.  x 4-in.  saddle fFVC)  td> connect 8-in.  PVC to 4-in. x 3-in. bushing
90° PVC
                          ,
                             -in.  PVC-T
            3-in.  PVC-1
                              1.75-in.  ID
                              flexible  tube
                                3-in. x 1.25-in.
                                reducer
                                Pi tot tube

                               3-in. ball valve
       Detail A
       Side view
       typical
                                                                                  )=O=(
                                                                                            -3-in. x 1.25-in.
                                                                                            reducer
                                                                                           3-in. PVC
                                                                                               8-in. PVC
                                                                                   Detail  B
                                                                                   Top  view
                                                                                   typical
            Figure  2-2.
                                           Flow Schematic of Staged Combustion Air System
                                           for a Natural Draft Process Heater
                                                                                                                  cv
                                                                                                                   i
                                                                                                                  X

-------
                        REFERENCES FOR SECTION 2
2-1.  R. DeRosier and B.  OaRos,  "Environmental  Assessment of a Crude-Oil
      Heater Using Staged Air Lances for NOX Reduction,"  Vol II:   Data
      Supplement, Acurex  Technical  Report,  TR-82-94/EE,  November  1983.

2-2.  Tidona,  R.  0.,  et al,  "Refinery Process Heater NOX  Reductions Using
      Staged Combustion Air  Lances," EPA-600/7-83-022, NTIS  PB 83-193946,
      March 1983.
                                    2-6

-------
                                  SECTION 3
                              EMISSION RESULTS

        The  objective  of this  test program was to measure flue gas emissions
from a  crude-oil  heater in  an "as-found" (baseline) configuration and using
staged  combustion  for NOX control  via air injection lances.  Table 3-1
summarizes  the  flue gas emissions measurements made' by Acurex and the test
collaborator  KVB,  Inc.  Figure 3-1 shows the sampling locations.  Succeeding
discussion  of the  measurement results has been arranged by pollutant grouping.
Criteria and  other gas  phase  emissions are discussed in section 3.1, inorganic
trace elements  in  section 3.2,  organic species in section 3.3, and
radionuclides in  section 3.4.  Section 4 presents an environmental assessment
of the  emissions  and  the results  of biological testing of the organic sample
extracts.
3.1     CRITERIA AND OTHER GAS PHASE SPECIES EMISSION RESULTS
        Table  3-2  summarizes gaseous and particulate emissions measured during
both the baseline  and staged  combustion tests.  Continuous monitors (described
in appendix A) were used to measure Og, CO?,  CO, NOX, and S02 emissions.   The
only significant changes in these measurements between the two tests were
decreases in  03 and NOX. Emissions of other  species remained relatively
unchanged.  The average Og level  in the low-NOx test was 3.3 percent compared
to a baseline level of  4.0 percent.  The NOX  reduction for this test was  31
percent, a decrease to  118 ppm  from a baseline level  of 172 ppm (at 3 percent
°2» dry)'   In previous  tests, KVB  has achieved 64 percent NOX reductions
                                      3-1

-------
                     Table 3-1.  Flue Gas Measurements
          Pollutant
         Measurement Technique3
   NOX, 02, C02, CO, S02
   Particulate matter
   S02/S03
   C1"C6 hydrocarbons
   Volatile and condensable
   organic species, trace
   elements
Continuous monitors^
EPA Method 5
Controlled condensation
Gas chromatography
Source Assessment Sampling System (SASS)
Measurement and analysis techniques are discussed in detail in appendix A
Performed by KVB
                                    3-2

-------
                  ULU
UJU
                 Method 5
                 SASS
                 C,-Cg grab samples
                                            N90 grab samples
                                             '
                                            Controlled
                                             condensation
                                                              ,
                                            Heated sampling
                                            line to continuous
                                            monitors
                                            02, C02', CO, S02, NO,
                                            Oil and readsorber gas

                                                  JFuel samples
Figure 3-1.  Refinery Crude  Heater  Sampling Locations (Sketch not  to Scale)
                                   3-3

-------
                            Table  3-2.  Gaseous Emissions

As Measured
0?, percent (dry)
C02, percent (dry)
CO, ppm (dry)
NOX, ppm (dry)
SO?, ppm
Continuous monitor (wet)
Controlled condensation (dry)
S03
Controlled condensation, ppm (dry)
Water, percent
N20, ppm (wet)
Vapor phase organics (Ci-C$) ng/dscm
Sennvolati le organics (TCO), rag/rtscm
Nonvolatile organics (Gravimetric),
mg/dscm
Corrected
CO
NOX (as N02)
N?0
Continuous monitor
Controlled condensation
S03
Controlled condensation

Paniculate ~ Method 5
Solid
Condensable
inarticulate -- SASS
Vapor phase organics (Ci-Cs)
rcu
Gravimetric
Baseline
Range
3.3 to 4.3
10.5 to 13.6
0 to 10
152 to 174

120 to 170
	 a

—
•-
~
.-
—
—

ppmb
4.0
172
59
190
103

2.5
mg/dscm

31.1
9.4
8.7
16.3
0.4
0.4
ng/J
1.19
83
27
128
69

2.1


8.35
2.52
2.34
4.4
0.11
0.11
Average
4.0
12.1
3.8
162

151
97

2.4
15.9
47.1
16.3
0.4
0.4b

lb/106 Btu
0.0028
0.19
0.064
0.30
0.16

0.0049


0.019
0.0059
0.0054
0.010
0.00019
0.00026
Low NOX
Range
3.1 to 4.2
11.3 to 12.4
0 to 10
108 to 125

125 to 170
—

—
--
—
—
~
—

PP."
3.5
118
33
180
117

1.8
pig/dscm

20.0
3.2
8.1
2.8
0.09
0.5
ng/J
- 0.99
56
15
118
77

1.5


5.0
0.80
2.0
0.72
0.022
0.13
Average
3.3
11.7
3.4
116

148
115

1.8
16.5
27.15
2.8
0.08
0.5

lh/106 Btu
0.0023
0.13
0.0315
0.27
0.18

0.0035


0.012
0.0019
0.0046
0.0017
0.000023
0.00030
Extractive sample
bAt  3 percent Og, flry
                                        3-4

-------
although these were with  100  percent  refinery  gas  firing  (references  3-1
and 3-2).
       Since the nitrogen  content  of  the  oil was  the  same for  the  two tests
(0.83 percent measured  for the  baseline and  0.85  percent  measured  for the  low
NOX as shown in table 3-3),  the reduction in NOX  can  be essentially  attributed
to the staging provided by the  air lances.   Similar to the NOX trend, ^0
emissions decreased from  59  to  33  ppm (at 3  percent 02, dry)  from  the baseline
to low-NOx tests.  CO levels  dropped  slightly, from 4.0 to 3.5 ppm (at
3 percent 02, dry).
       Sulfur species emissions were  measured  by  continuous monitors  (S02),  a
controlled condensation train (S02 and $03), and  SASS (particulate sulfur).
As shown in table  3-2,  S02 emissions, as  measured by  continuous monitors
decreased from 190 ppm  (at 3  percent  02,  dry)  in  the  baseline  test to 180  ppm
(at 3 percent Og,  dry)  in  the low-NOx test.  The  controlled condensation train
measurements showed an  increase from  103  ppm to 117 ppm  (both  at 3 percent 02,
dry) between the baseline  and low-NOx tests.   However, the relative  magnitude
of change for each method  is  small  enough that a  conclusion that S02 emissions
were unchanged is warranted.  The  fact that  the sulfur content of  the fuel oil
was measured to be 0.94 percent for the baseline  and  0.90 percent  for the
low-NOx test, supports  this conclusion. S03  emissions, as measured by the
controlled condensation train,  decreased  from  2.5 ppm to  1.8 ppm (at  3 percent
°2» dnO although, again,  the magnitude of this change is insignificant.
Particulate sulfur emissions  for both tests were  reported as greater  than
0.56 yg/dscm because the sulfur concentration  in  the  SASS filter catch
exceeded the upper measurement  limit  of the spark  source  mass  spectrometry
(SSMS) analysis methodology.  Based on the above  information,  table  3-4
presents a sulfur mass  balance  for the two tests.   In both tests,
                                     3-5

-------
Table 3-3.  Fuel Analyses

Fuel gas (percent by volume)
Hydrogen
Nitrogen
Carbon monoxide
Methane
Ethane
Ethyl ene
Propane
Propylene
Isobutane
n-butane
Total butenes
Isopentane
n-pentane
CQ plus
Heating value, MJ/m3
(Btu/ft3)
Oil (percent by weight)
Carbon
Hydrogen
Oxygen (by difference)
Nitrogen
Sulfur
Heating value, MJ/kg
(Btu/lb)
Baseline

8.7
1.1
0.4
22.7
16.7
3.8
29.2
3.3
11.1
1.7
0.5
0.2
0.1
0.5
70.56
1,892

87.37
10.47
0.39
0.83
0.94
43.44
18,720
Low NOX

9,3
0.8
0.5
24.5
16.5
4.0
28.5
3.6
9.5
1.3
0.7
0.2
0.1
0.5
68.71
1,842.6

86.66
10.98
0.61
0.85
0.90
43.54
18,760
            3-6

-------
          Table 3-4.  Sulfur Balance (g/s as Sulfur)
Fuel
Flue gas
S02a
S03b
Parti cul ate
Totals
Balance
(out/In)
Baseline
In
1.03




1.03
Out


0.84
0.01
>2 x 10-6
0.85
82 percent
Low NOX
In
0.98


t

0.98
Out


0.77
0.01
>2 x 10-6
0.78
80 percent
aFrom continuous monitor
      controlled condensation
                             3-7

-------
approximately 80 percent of the sulfur is accounted  for.   The  imbalance  is
probably attributable to inaccuracies in estimation  of  the fuel  flowrates,
rather than the particulate sulfur measurements  (the balance increases  to only
93 percent in the baseline test if it is assumed  that all  the  solid
particulate collected in the Method 5 train were  sulfur,  an unlikely
possibility).
       Because of the small amount of particulate expected from  burning  oil
and gas, no particulate size fractionation was done  in  the SASS  train.
However, particulate emissions, as measured by both  SASS  and Method 5,  showed
a decrease for the low-NOx test.  SASS particulate dropped from  8.7 to
8.1 mg/dscm (at 3 percent 03), while the solid particulate measured by
Method 5 dropped from 31.1 to 20.0 mg/dscm (at 3  percent  03} and condensable
particulate decreased from 9.4 to 3.2 mg/dscm (at 3  percent 02).  The
significant discrepancy between the SASS and the  Method 5 results is most
likely due to the proximity of the sampling location  to a flow disturbance.
For this reason the multipoint Method 5 result is more  reliable  than the
single-point SASS result.
3.2    TRACE ELEMENT EMISSION RESULTS
       The SASS train samples from the heater outlet were analyzed for
73 trace elements using Spark Source Mass Spectrometry  (SSMS)  and Atomic
Absorption Spectroscopy (AAS).  Once the trace element  concentrations were
determined by laboratory analysis, trace element  flowrates for the flue  gas
vapor and condensed phases could be computed.  Appendix B presents trace
element concentrations in the SASS components and in  the  gas stream as well as
flowrates on a mass per time and mass per heat input basis.
       Table 3-5 summarizes the trace element concentrations which exceeded
the lower detectability limits in either test.  The  elements calcium,
                                     3-8

-------
                Table 3-5.  Flue Gas Trace  Element  Emissions^
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Bismuth
Boron
Bromine
Cadmium
Calcium
Cerium
Ces i urn
Chlorine
Chromium
Cobalt
Copper
Dysprosium
Erbium
Europium
Fluorine
Gadolinium
Gallium
Germanium
Gold
Hafnium
Hoi mi urn
Iodine
Iridium
Iron
Lanthanum
Lead
Lithium
Lutetium
Magnesium
Manganese
Mercury
Molybdenum
Emissions
Basel ine
(ug/dscm)
__b
<0.97
<0.97
6.6
<0.004

>1.8
6.6
0.0004
—
__
0.18
100
4.2
0.039
7.4



180

0.18
__
__
__

0.27

28
--
0.0093
0.038

0.89
1.3
<0.71
0.015
Low NOX
(ug/dscm)
80
<0.96
<0.96
15
<0.0004

--
22
0.47
380
1.2
<0.47
66
28
0.079
52



0.47

0.0016
0.00040
__
__

0.94

190
2.7
1.2
0.0060

9.4
11
<0.32
3.0
Element
Neodymium
Nickel
Niobium
Osmium
Palladium
Phosphorus t
Platinum
Potassium
Praseodymium
Rhenium
Rhodium
Rubidium
Ruthenium
Samarium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tantalum
Tellurium
Terbium
Thallium
Thorium
Thul ium
Tin
Titanium
Tungsten
Uranium
Vanadium
Ytterbium
Yttrium
Zinc
Zirconium

Emissions
Baseline
{ug/dscm)

>30
0.35


0.012
...
110
--


0.18


__
<0.71
750
0.0036
>910
14
>880

0.0004


—

<0.0004
5.3

—
0.81
—

12
0.94

Low NOX
(ug/dscm)

29
2.7


33
--
1,100
--


<2.5


<0.13
0.0016
770
6.8
>690
2.3
>1,600

<0.54


0.0012

0.0004
5.4

0.0012
1.7

0.27
f\C
95
8.5

aBlanks indicate concentration below the detection limit of the sampling and
 analysis protocol
^Measured concentration less than concentration  in blank
                                     3-9

-------
chlorine, fluorine, iron, potassium, silicon, sodium, and sulfur were detected
at concentrations exceeding 0.1 mg/dscm in at least one of the tests.  Of
these eight elements, two (sodium and sulfur) could not be quantified because
the concentration in the sample exceeded the upper quantification  limit of  the
SSMS technique.
       Table 3-6 summarizes the changes in trace element concentrations
measured in each test.  This information identifies those trace elements whose
concentration differed by more than a factor of three (the accuracy of Level 1
analysis) between the two tests.  Of the 48 trace elements detected at greater
than the limit of the analysis method, emission levels of nine were within  a
factor of three between the two tests, six were higher in the baseline test,
25 were higher in the low-NOx test, and the changes in eight were
indeterminate.  Roughly half of the trace element concentrations which
differed by more than a factor of three between the two tests, differed by  a
factor of 10 or more (four out of six of those higher in the baseline and
12 out of 25 of those higher in the low-NOx).
       Table 3-7 presents the trace element mass balance for the baseline
test, based upon the SSMS analysis of the fuel oil and the SASS components.
From the table, it is apparent that for only three elements do the inlet and
outlet balance within a factor of three, which is the limit of Level 1
accuracy.  The oil analysis results are probably high for chromium, nickel,
and iron, due to potential contamination from the Parr bomb ashing of the oil
for SSMS analysis.  However, the mass balance does indicate six elements which
were detected in the fuel but not in the outlet, and 15 elements which were
detected at the outlet, but not in the fuel.
       Table 3-8 presents the trace element mass balance for the low-NOx test.
For this test, only two elements are detected in the fuel but not  the exhaust,
                                     3-10

-------
Table 3-6.  Relative Trace Element Concentrations Between the Baseline and
            Low-N0x Tests
Unable to
Determine
Cs
Ni
Rb
Se
Na
S
Te
Sn

















Higher in Baseline
By a Factor of >3a
Be*
B*
F*
Ga*
Li
Sr



















Within Factor
of 3 Between
Tests5
Sb
As
Cl
Co
Hg
Mo
Si
Ti
V
















Higher in Low NOX
By a Factor of >3a
Al
Ba
Br
Cd*
Ca*
Ce*
Cr
Cu
Ge*
I
Fe
La*
Pb*
Mg*
Mn
Nb
P*
K*
Sc*
Ag*
Th
U*
Y
Zn
Zr
aAn asterisk  indicates  where  the  concentration  differed  by a factor
 of greater than  10
^Changes  in concentration  within  a factor of 3  indicated that the
 concentrations are  equal  within  the  accuracy of the analysis
                                    3-11

-------
  Table 3-7.  Baseline  Test  Trace  Element Mass Balance
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Bromine
Cadmium
Calcium
Cesium
Chlorine
Chromium
Cobalt
Copper
Fluorine
Gallium
Germanium
Iodine
Iron
Lead
Lithium
Magnesium
Manganese
Mercury
Molybdenum
Nickel
Niobium
Phosphorus
Platinum
Potassium
Rubidium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Tellurium
Thorium
Tin
Titanium
Oil
(wg/s)
1,600


220

11
55

3,300

220
66
<11
770
22
33

11
1,400
22
98
1,100
77
Na

880

990
220
8,700

<11

4,900

<11
11
>35,000

<44

660
Heater Outlet
(wg/s)
0.1
<3.4
<3.4
23
<0.014
>630
2.3
0.0014

0.62 to 2.3
360
15
0.14
26
620
0.63

0.94
99
0.33
0.13
3.1
4.5
<2.5
0.054
>110
1.2
0.043

400
0.62 to 2.3

• <2.5
2,650
0.013
>3,200
50
>3,100
0.0014

<0.0014
19
Mass Balance
(Out/In)
0.000062
*b
*
0..10
*
>5.7
0.43
*
0
*
1.6
0.22
>0.012
0.034
28
0.019
*
0.86
0.070
0.015
0.0014
0.0028
0.058
*
*
>0.12
*
0.000043
0
0.045
*
0
*
0.54
*
>290
4.6
*
*
0
*
0.028
j*Not determined
°Unable to determine
                             3-12

-------
Table 3-7.  Concluded

Element
Uranium
Vanadium
Yttrium
Zinc
Zirconium
Oil
(ug/s)
<55
220
22
980
88
Heater Outlet
(ng/s)

2.8

43
3.3
Mass Balance
(Out/In)
0
0.013
0
0.044
0.038
          3-13

-------
 Table 3-8.  Low NOX Test Trace Element Mass Balance3
Element
Aluminum
Antimony
Arsenic
Barium
Beryllium
Boron
Bromine
Cadmium
Calcium
Cerium
Cesium
Chlorine
Chromium
Cobalt
Copper
Fluorine
Gallium
Germanium
Iodine
Iron
Lanthanum
Lead
Lithium
Magnesium
Manganese
Mercury
Molybdenum
Nickel
Niobium
Phosphorus
P 1 at i num
Potassium
Rubidium
Scandium
Selenium
Silicon
Silver
Sodium
Strontium
Sulfur
Oil
(u9/s)
1,420


190

110


1,750


550
110
<22
660
44
11


2,800

98
220
1,310
55
Nb

870

550
1,200
7,210



1,750

660
56
3,600
Heater Outlet
(ug/s)
260
<3.2
<3.1
49
<0.0013

68 to 77
1.5
-1,260
4.0
<1.5
2,200
91
0.26
170
1.5
0.0053
0.0013
3.1
630
8.9
4.1
0.02
31
37
<1.05
9.8
96
8.9
110

3,630
<8.2
<0.44
0.0053 to 8.9
2,550
22
>2,300
7.6
>5,300
Mass Balance
(Out/In)
0.19
*c
*
0.45
*
0
*
*
0.72
*
*
4.0
0.83
0.012
0.26
0.035
0.00048
*
*
0.22
*
0.041
0.000091
0.0023
0.68
*
*
0.11
*
0.20
0
0.50
*
*
*
1.5
*
>3.5
0.14
>1.5
aBlanks indicate elements below the detection limit;
 trace elements not listed were not detected in either
 the inlet or outlet
bNot analyzed
cUnable to determine
                          3-14

-------
Table 3-8.  Concluded
Element
Tellurium
Thorium
Tin
Titanium
Uranium
Vanadium
Yttrium
Zinc
Zirconium
Oil
(yg/s)

<98

1,100
<88
87

330

Heater Outlet
(yg/s)
<1.8
0.0040
0.0013
18
0.0040
5.5
0.89
310
28
Mass Balance
(Out/In)
*
0.000040
*
0.016
0.000045
0.063
*
0.95
*
          3-15

-------
while 19 are detected in the exhaust but not the  fuel.  However,  eight  trace
elements (Ba, Zn, Mn, Cr, Ca, K, Cl and Si) balanced within  a  factor  of  three.
The same potential contamination problem with  iron, nickel,  and  chromium in
the oil  sample still exists, so those results  should be treated  with
suspicion.
       For both sets of data, some of the concentrations were  indeterminate
because the sample and blank concentrations were  both reported as  larger than
the upper quantisation limit of the SSMS methodology.
3.3  ORGANIC EMISSION RESULTS
       Organic analyses were performed on selected SASS samples  according to
EPA Level 1 protocol (reference 3-3), as outlined in appendix  A.   Volatile
organic species having boiling points nominally in the  CI~CQ range  of  -106°  to
32°C (-160° to 90°F) were determined by onsite gas chromatographic  analyses  of
grab samples.  SASS samples were extracted with methylene chloride  in  a
soxhlet apparatus.  Semi volatile organic matter with boiling points nominally
in the Cy-Cjs range of 32° to 300°C (90° to 572°F) were determined  in  the
laboratory by total chromatographable organic  (TCO) analysis of  the organic
module sorbent (XAO-2) and condensate sample extracts.  Nonvolatile organic
species having boiling points nominally in the greater  than  Cj/  range  of
>300°C (>572°F) were measured by gravimetric analysis of SASS  sample  extracts
including filter  catches.
       Infrared spectrometry (IR) was also performed on the  gravimetric
residue filter catch and organic module sorbent extracts to  identify  organic
functional groups  present.   If certain TCO and gravimetric criteria were met,
further analysis  by low  resolution mass spectrometry  (LRMS)  was  performed.  In
addition, specific  polynuclear aromatic and selected other organic species
                                      3-16

-------
were identified by gas chromatography/mass  spectrometry  (GC/MS)  analysis  of
total sample extracts.  A  discussion  of  the analytical  results  follows.
3.3.1  C]-_C_g Hydrocarbon,  TCP,  and  Gravimetric  Analyses
       As indicated  in table  3-9,  vapor-phase  hydrocarbon  (C^-Cs)  emissions
decreased from  16.3  mg/dscm  under  baseline  conditions to 2.8 mg/dscm under
low-NOx conditions.   In the  baseline  test,  they were somewhat evenly divided
among the €3, €3, and €4 boiling  point  ranges  while the low-NOx test produced
only nominal C2 hydrocarbons.   Total  organic emissions in  both  tests were
dominated by the Cj-Cs fraction;  these  accounted for 95 percent in the
baseline and 73 percent in the  low-NOx  test.
       Table 3-9 also summarizes  organic emission results  from the TCO and
gravimetric analyses.  The TCO  results  have been compromised somewhat in these
tests due to the use of XAD-2 resin which had  been inadvertantly contaminated
by acetone  between  resin preparation  and eventual use.  Thus, several acetone
solvent contaminants and acetone  dimerization  products, all  of low-molecular
weight and  in the TCO boiling point range,  were introduced into the resin.
This resulted in a  high TCO  blank  for the XAD-2 resin for both tests.
Table 3-10  shows the sample  extract and  field  blank TCO values from both
tests, and  indicates the high,  contaminated blank.
       In an attempt to correct for the  high blank, GC/MS analyses of the
extracts were performed to identify and  quantitate specific  contaminant
species in  both the  blank  and sample  extracts.   Subtracting  the amount of
these contaminant species  found in  both  sample and blank extracts  from the TCO
levels of each, allowed defining  a  corrected TCO value for both samples and
the blank.  These corrected  levels  are  also shown in table 3-10.  TCO values
listed in table 3-9  reflect  these  corrected values.  It should be  noted that
                                      3-17

-------
Table 3-9.  Summary of Total  Organic  Emissions
Organic Emissions
Volatile organic gases analyzed in
the field by gas chromatography:
n
P
C5
C6
Total Cj-Cg
Volatile organic material analyzed
by TCO:
XAD-2
Organic module condensate
Total Cj-C-[Q
Nonvolatile organic material
analyzed by gravimetric procedure:
Filter
XAD-2
Organic module condensate
Total Ci6+
Total organics
Baseline
(mg/dscm)

0
3.6
4.8
6.4
1.5
0
16.3

0.36
<0.001
0.36

<0.2
0.4
0.4
17.1
Low NOX
(mg/dscm)

0
2.8
0
0
0
0
2.8

0.06
0.02
0.08

<0.3
0.3
0.2
0.5
3.4
                        3-18

-------
   Table 3-10.  XAD-2 Extract TCO Results
                 Baseline TCO
                     (n>g)
           Low-N0x TCO
             (mg)
Uncorrected
Sample extract
Blank
Sampl e
Corrected
Sample extract
Blank
Sample
39
30
11
 0.5
10.5
25
30
<5
 2.3
 0.5
 1.8
                    3-19

-------
all contamination consisted of TCO boiling range compounds so gravimetric
results should be unaffected.
       The data shown in table 3-9 suggest that emissions of C;+ organics  are
unchanged with firing mode.  Again, these data are compromised  to  some  degree
because of the resin contamination.  However, given the GC/MS corrective
procedure employed, the data are defensible.
       In order to evaluate the overall reliability of the organic extraction
and analysis procedure, a sample of clean (and uncontaminated)  XAD-2 was
spiked with 1.0 mg of TCO material.  Extraction, concentration, and TCO
analysis of this spiked sample gave 0.74 mg implying a 74 percent  recovery
by the procedure.
       No liquid chromatography (LC) fractionation of extracts  was performed
for these tests, since the TCO + gravimetric organic content of no extract
sample exceeded the LC fractionation criterion of 15 mg.
3.3.2  IR Spectra of Total  Extracts
       IR spectrometry was used to identify organic functional  groups present
in SASS samples.  Table 3-11 summarizes the results of these analyses for  the
filter, XAD-2, and the organic module condensate extracts for both tests.
Only the XAD-2 extract from the baseline test showed measurable absorbances.
These were characteristic of aliphatic hydrocarbons.
3.3.3  Low Resolution Mass Spectrometry (LRMS) of Total Extracts
       Table 3-12 presents the results of direct-insertion probe LRMS of the
total XAD extracts from both tests.  Table 3-13 lists the compound classes and
fragment ions used to identify compound categories present.  In the baseline
test, ethers, heterocyclic sulfur compounds, and carboxylic acids  are major
components indicated, while halogenated aliphatics, aromatic hydrocarbons,
nitriles, alcohols, and heterocyclic nitrogen compounds are minor  categories
                                     3-20

-------
Table 3-11.  Summary  of  IR  Analyses  of SASS Sample Total  Extracts
Baseline
SASS Component
Filter
XAD-2

OMC
Frequency
(cm-1)
—
2,920
2,840
—
Assignment
No Peaks
CH Alkane
CH Alkane
No Peaks
Low NOX
SASS Component
Filter
XAD-2
OMC
Frequency
—
—
--
Assignment
No Peaks
No Peaks
No Peaks
                                3-21

-------
Table 3-12.  Summary of LRMS Analyses of  XAD-2  Extracts
Species Category
Baseline: TCO + Grav = 0.76 mg/dscm
Ethers
Carboxylic acids
Heterocyclic sulfur
compounds
Alkyl ha 1 Ides
Alcohols
Nitriles
Aromatic hydrocarbons
Heterocyllc nitrogen
compounds
Total
Low NOX: TCO + Grav =0.35 mg/dscm
Alyphatic hydrocarbons
Amines
Carboxylic acids
Aromatic hydrocarbons
Total
Intensity
100
100
100
10
10
10
10
10
350
100
100
10
10
220
Estimated Flue
Gas Concentration
(mg/dscm)
0.22
0.22
0.22
0.02
0.02
0.02
0.02
0.02
0.76
0.16
0.16
0.02
0.02
0.36
                           3-22

-------
Table 3-13.  Compound Classes and Characteristic Fragment Ions Sought by
             Direct-Insertion Probe LRMS
         Compound Class
        Fragment  Ions  (m/e")
Polycyclic aromatic hydrocarbons
Aliphatic hydrocarbons
Halogenated aliphatics
Aromatic hydrocarbons
Ethers
Alcohols
Phenols
Nitriles
Phthalate esters
Amines
Ketones
N-Heterocyclics
Mercaptans, sulfides
Benzothiophenes
Carboxylic acids
Amides
 178,  202,  216, 228, 252, 276
 57,  71
 79,  81,  93,  95,  107,  109, 49, 63
 50,  51,  77,  78,  79, 91
•45,  59,  73
 45,  59,  61,'  73,  75
 51,  77,  94
 54,  68,  82
 61,  59,  71,  87
 44,  58
 51,  71
 117, 167,  129,  179
 47,  61,  75
 57,  58,  59,  69,  70, 85,  97,  111,  125
 60,  73,  149
 58,  72,  86,  100
                                   3-23

-------
indicated.  In the 1ow-NOx test, aliphatic hydrocarbons  and  amines  are
indicated as major components while aromatic hydrocarbons  and  carboxylic  acids
are indicated as minor components.  The estimated emission level  for  each
compound category detected, shown in table 3-12, was calculated  by
proportioning the total €7+ organic emission levels shown  in table  3-9  among
the intensities noted in table 3-12.
3.3.4  Gas Chromatography/Mass Spectrometry Analysis of  XAD-2  Extracts
       GC/MS analyses of the organic module extracts from  the  SASS  train  were
performed to detect and quantify specific polycyclic organic materials  (POM)
and selected other organic compounds.  The POM and other compounds  sought in
the analysis are listed in table 3-14 along with their detection  limits in  the
GC/MS analyses.  The results of the GC/MS analyses are summarized in
table 3-15.  Duplicate analyses of the low-NOx XAD-2 extract were performed to
assess the precision of the analyses.  Table 3-15 shows  that these  agreed
quite well.  The average of these two analysis runs are  used in  the following
comparison between baseline and low-NOx emissions.
       Eleven specific compounds were identified in concentrations  ranging
from <0.04 to 1.4 ug/dscm.  In general, emissions of these species  were lower
in the low-NOx test than the baseline.  The general decrease in  these
semivolatile organic priority pollutant species emissions  from a  total  of
4.1 ug/dscm to 1.9 ug/dscm is consistent with the decrease in  total organic
emissions noted previously.
       Analysis of XAD-2 resin spiked with naphthalene,  phenanthrene, and
pyrene yielded recoveries of 33 percent, 38 percent, and <1  percent,
respectively.  This suggests that the uncertainty in the data  presented in
table 3-14 is approximately a factor of three, at least  for  the  more  volatile
species analyzed for.
                                     3-24

-------
Table 3-14.
Compounds Sought in the GC/MS Analysis and Their Detection Limits
(ng/yl Injected)
                                Acid Compounds
  2,4,6-trichlorophenol
  p-chloro-m-cresol
  2-chTorophenol
  2,4-di chlorophenol
  2,4-dimethylphenol
                       5       2-nitrophenol
                       5       4-nitrophenol
                       5       2,4-dinitrophenol
                       5       4,6-dinitro-o-cresol
                       5       pentachlorophenol
                               phenol
 5
20
20
20
 5
 1
                            Base  Neutral  Compounds
  1,2,4-trichlorobenzene             1
  1,2-dichlorobenzene                1
  1,2-diphenylhydrazine              1
    (as azobenzene)
  1,3-dichlorobenzene                1
  1,4-dichlorobenzene                1
  2,4-dinitrotoluene                 1
  2,6-dinitrotoluene                 1
  2-chloronaphthalene                1
  3,3'-dichlorobenzidine             5
  3-methyl cholanthrene             40
  4-bromophenyl  phenyl ether         1
  4-chlorophenyl  phenyl ether        1
  7,12-dimethyl  benz(a)anthracene   40
  N-nitrosodi-n-propylamine          5
  N-nltrosodimethylamine            NA
  N-nitrosodiphenylami ne             1
  acenaphthene                       1
  acenaphthylene                    1
  anthracene                         1
  benzo(ghi)perylene                 5
  benzidine                         20
  benzo(b)fluoranthene               1
  benzo(k)fluoranthene               1
  benzo(a)anthracene                 1
  benzo(a)pyrene                    1
                               benzo(c)phenanthrene          40
                               bis{2-chloroethoxy)methane     1
                               bis(2-chloroethyl)ether        1
                               bis(2-chloroisopropyl)ether    1
                               bis(2-ethylhexy!)phthalate     1
                               butyl benzyl phthalate         1
                               chrysene                       1
                               di-n-butyl  phthalate           1
                               di-n-octyl  phthalate           1
                               dibenzo(a,h)anthracene         5
                               dibenzo(c,g)carbazole         40
                               diethyl phthalate             1
                               dimethyl  phthalate             1
                               fluoranthene                   1
                               fluorene                       1
                               hexachlorobenzene             1
                               hexachlorobutadiene            1
                               hexachlorocyclopentadiene      1
                               hexachloroethane               1
                               indeno(l,2,3-cd}pyrene         5
                               isophorone                     1
                               naphthalene                   1
                               nitrobenzene                   1
                               perylene                      40
                               phenanthrene                   1
                               pyrene                         1
                                      3-25

-------
Table 3-15.  Results of the GC/MS Analyses
Species
Phenol
Naphthalene
1,3-dichlorobenzene
1,4-dlchlorobenzene
1 ,2-dichl orobenzene
Nitrobenzene
2-n1trophenol
Diphenylamine
1,2-diphenylhydrazlne
(as azobenzene)
Phenanthrene
2,6-dinitrotoluene
Other polynuclears
Baseline
(ug/dscm)
1.0
<0.04
0_.08
0.04
0.1
0.2
<0.2
0.1
1.4
1.2
<0.04
<0.04
Low NOX
(yg/dscm)
Run 1
0.20
0.40
<0.04
0.04
<0.04
0.04
0.43
0.08
<0.04
0.10
0.10
<0.04
Run 2
0.55
0.78
<0.04
O.Q8
<0.04
0.08
0.39
0.08
0.04
0.20
<0.04
<0.04
Average
0.4
0.6
<0.04
0.06
<0.04
0.06
0.41
0.08
0.04
0.15
0.07
<0.04
                    3-26

-------
3.4    RADIONUCLIDE EMISSION RESULTS
       Portions of the SASS filters were analyzed  for  alpha,  beta, and gamma
activity.  In both cases, the filter activities were less  than or equal to  the
activity of the blank, as shown  in table 3-16.  Thus,  there are  no significant
participate radionuclide emissions from this  source.

                   Table 3-16.   Particulate Radioactivity



Basel ine
Low NOX
Blank
'Activity pCi/filter*
(*
Gross Al pha
1 18
15 ± 12
1 19
Gross Beta
60.6 + 7.8
75.0 ^ 11.3
99.6 +_ 13.5
Gross Gamma
5 143
£ 143
< 142
     aThe + values are the  2 sigma  Poisson  standard  deviation  of  the
      counfing error.
                                     3-27

-------
                         REFERENCES FOR SECTION 3
3-1.  Tidona, R. J., et al., "Refinery Process Heater NOX Reductions Using
      Staged Combustion Air Lances," EPA-600/7-83-022, NTIS PB 83-193946,
      March 1983.

3-2.  Hunter, S. C., W. A. Carter, and R. J. Tidona, "Control  of NOX
      Emissions from Petroleum Process Heaters Using Staged Air Lances,"
      presented at the West Coast Section meeting of the Air Pollution
      Control Association, Palm Springs, CA, October 1981.

3-3.  Lentzen, D. E., et al.,  "IERL-RTP Procedures Manual:  Level  I
      Environmental  Assessment (Second Edition)," EPA-600/7-78-201, NTIS
      PB 293795, October 1978.
                                    3-28

-------
                                   SECTION 4

                            ENVIRONMENTAL ASSESSMENT



       This  section  discusses  the potential  environmental  significance of the

refinery  heater  testing  including bioassay testing.  As a  means  to rank
                                                 f
species discharged for possible further consideration, flue gas  stream species

concentrations are compared to occupational  exposure guidelines.  Bioassay

analyses  were conducted  as  a more direct measure of the potential  health

effects of the effluent  streams.   Both of these analyses are aimed at

identifying  potential problem  areas  and providing  the basis for  ranking

pollutant species and discharge streams for further consideration.

4.1    EMISSIONS ASSESSMENT

       To obtain a measure  of  the potential  significance of the  pollutant

levels in the flue gas analyzed in this test program, flue gas concentrations

were compared to an  available  set of health-effects-related indicies.  The

indices used for comparison were  occupational  exposure guidelines,

specifically the time-weighted-average Threshold Limit Values  (TLV's) defined

by the American Conference  of  Governmental  Industrial Hygienists (ACGIH)

(reference 4-1).

       The comparisons of the  flue gas stream  species concentrations  to these

indices should only  be performed  to  rank  species emission  levels for  further

testing and analyses.  Table 4-1  lists those pollutant species emitted  at

levels greater than  10 percent  of their occupational  exposure guidelines.
                                     4-1

-------
4.2    BIOASSAY RESULTS
       Bioassay tests were performed on the organic sorbent  (XAD-2) extracts.
The bioassay tests performed were health effects tests only  (reference 4-2).
These were:
       •   Ames assay, based on the property of Salmonella typhimurium mutants
           to revert due to exposure to various classes of mutagens
       •   Cytotoxicity assay (CHO) with mammalian cells in culture to measure
           cellular metabolic impairment and death resulting from exposure to
           soluble toxicants
A detailed description of the biological analyses performed- is presented in
Volume II (Data Supplement) of this report.
       Table 4-2 summarizes the results from the Ames and CHO assays.  The
XAD-2 extract showed moderate toxicity and moderate to high mutagenicity.
4.3    CONCLUSIONS
       The use of staged air lances resulted in a decrease in NOX emissions,
with no significant adverse impacts.  Particulate and organic emissions
exhibited slight decreases while trace element emissions exhibited an apparent
increase which may be only partially attributable to increases in the trace
element concentrations in the fuel.  Bioassay results of XAD-2 extracts
indicated that the extracts were of moderate toxicity for both tests although
the mutagenicity of the extracts increased from moderate for the baseline test
to high for the low-NOx test.
                                     4-2

-------
      Table 4-1.   Flue Gas Species Emitted at Levels Exceeding 0.1  of an
                  Occupational Exposure Limit


Species
S02
NCL (as N02)
Silver, Ag
Potassium, Kb
Sodium, Nab
Phosphorus, P
Nickel, Ni
Copper, Cu
Iron, Fe
Calcium, Cab
Flue Gas Concentration (yg/dscm)

Baseline
480,000
200,000
0.0036
110
>910
0.012
>3.0
7.4
28
<0.004

Low NOX
470,000
140,000
6.8
1,100
>690
33
29
52 '
190
380b

Occupational Exposure
Guideline (ug/m^)a
5,000
6,000
10
2,000
2,000
100
100
200
1,000
2,000
threshold Limit Value {reference 4-1)
bTrue value probably higher; at least one component of the SASS train showed a
 sample and blank concentration higher than the upper quantification limit
                         Table 4-2.  Bioassay Results

Test
XAO-2 extract:
Baseline
Low NOX
Bioassay
Amesa

M
H
CHOb

M
M
               aM - Moderate mutagenicity, H - High mutagenicity
               bM - Moderate toxicity
                                     4-3

-------
                           REFERENCES FOR SECTION 4
4-1.  "Threshold Limit Values for Chemical  Substances and Physical  Agents in
      the Work Environment with Intended Changes for 1982," American
      Conference of Governmental  Industrial  Hygienists, Cincinnati, Ohio,
      1982.

4-2.  Brusick, D. J., and R.  R. Young,  "IERL-RTP Procedures Manual:  Level 1
      Environmental Assessment, Biological  Tests," EPA-600/8-81-024, NTIS
      PB 228766, October 1981.
                                     4.4

-------
                                  APPENDIX A
                         TEST EQUIPMENT AND PROCEDURES

A.I     CONTINUOUS  MONITORING SYSTEM
        KVB,  Inc. provided continuous" vapor phase species emissions monitoring
                                               f
for  this  test  program  using a rack-mounted monitor and recorders located in a
mobile  emission laboratory.  A flow schematic of this flue gas sampling and
analyzing  system is  shown in figure A-l.  The sampling system uses one of
three double-headed  positive-displacement diaphragm pumps to continuously draw
flue gas  from  the  stack  into the laboratory.  The sample pumps pull  from up to
six unheated sample  lines.   Selector valves allow composites of up to six
points  to  be sampled at  one time.   The probes are connected to the sample
pumps with 0.95-cm (3/8-in.)  or 0.64-cm (1/4-in.) nylon line.  The
positive-displacement  diaphragm sample pumps provide unheated sample gas to
the refrigerated condenser  (to reduce the dew point to 1.7°C (35°F)), to a
rotameter  with flow  control  valve,  and to the 02, NOX, CO, and COg
instrumentation.   Flow to the individual  analyzers is measured and controlled
with rotameters and  flow  control valves.   Excess sample is vented  to the
atmosphere.
        To obtain a representative sample  for the analysis of N02,  S02,  and
hydrocarbons, the  sample  must be kept above its  dew point, since both water
and heavy hydrocarbons may  be condensable,  and  S02 and N02 are quite soluble
in water.  For this  reason, a separate electrically heated sample  line  is  used
                                     A-l

-------
ro
                                                                  Heated Lin*
                                                                      Mao I fold
                                                             Vacuum
                                                                                                   Hot
                                                                                                 fianpl*       Dry Ba»pl«l Lln««
                                                                                                  Lina    (Typical 6«t-Up Si* Lln«a|.
                                                                                                                     Banpl*
                                                                                                                      Puap*
                                                                                                                       U)
                                                                                                                                CondaitMr

                                                                                                                                Not/Cold
                                                                                                                                 Switch
                                                                                                 Rafriteration CondeniBr

                                                                                                 a*pla Praaiura
                                                                                                             .         A
                                                                                                            ^ )Span   li iSpan
                                                                                                            CO
                                                                                                                     CO,
                             Figure A-l.   Flue  Gas  Sampling and Analyzing  System  (Reference A-l)

-------
to bring  the  sample  into  the laboratory for analysis.  The sample line is
0.95-cm  (3/8-in.)  Teflon  line,  electrically traced and thermally insulated
to maintain a sample temperature of up to 204°C (400°F).  A heated diaphragm
pump  provides hot  sample  gas to the hydrocarbon, S02 and NOX analyzers and
cold, dried gas  to the  other continuous analyzers via the condenser previously
described.
       The laboratory trailer is equipped with the analytical  instruments
shown in  table A-l to continuously measure concentrations of NO, N02,  CO,  C02,
03, S02,  and  hydrocarbons.   All  of the continuous monitoring instruments and
                                                 t
sample handling  system  are  mounted in the self-contained mobile laboratory.
The instruments  themselves  are  shock mounted on a metal  console panel.
       Due to the  failure of the electronic datalogger just prior to the start
of these  tests,  the  gaseous emission measurements were determined by manually
interpreting  the stripchart recordings and recording 15-min averages.
A-2.   PARTICULATE TESTS
       Particulate mass emission tests were performed each day in accordance
with EPA  Methods 1 through  5.   The sampling train used is illustrated  in
figure A-2.   Both  solid particulate matter collected in  the filter ahead of
               Table  A-l.   Emission  Measurement  Instrumentation

Species
Carbon monoxide
Oxygen
Carbon dioxide
Nitrogen oxides
Sulfur dioxide

Measurement Method
IR spectrometer
Polarographic
IR spectrometer
Chemi 1 unri nescent
UV spectrometer

Manufacturer
Beckman Instruments
Tel edyne
Beckman Instruments
Thermo Electron Co.
DuPont Instruments
Model
No.
865
326A
864
10A
400
                                     A-3

-------
                                                               •Smith-Greenberq  impinger
  Stack temperature T.C.
  Probe temperature T.C.
      >\\\\\\\\\\\v\
 "S"  type
 pi tot  tube
Pi tot AP
magnehelic
pressure gages
           AH orifice plate
     Orifice AH
     magnehelic gage
                                                                         Modified  Smith-Greenberg
                                                                         impingers
                                      meter  ^00ml (each)   Empty ALice bath

                                                           Fine adjustment
                                                           by pass valve
                           Silica gel
                           •dessicant
         Dry test meter


Figure A-2.  Particulate Sampling Train
           Vacuum
           Gauge
       'Coarse
       adjustment
       valve

Air tight
vacuum
pump
                                                                                   Vacuum
                                                                                   line

-------
the impinger section and condensable  particulate  collected  in  the  impingers
were measured, as  indicated  in  figure A-3.
A.3    SULFUR EMISSIONS
       Sulfur emissions  (SO? and  $03) were  measured  using the  controlled
condensation system  illustrated in  figure A-4.  This  sampling  system,  designed
primarily to measure vapor  phase  concentrations of  $63  as HjSO^ consists  of  a
heated Vycor probe,  a  condenser (condensation  coil),  impingers,  a  pump,  and a
dry gas test meter-  By  using the condenser,  the  gas  is cooled to  the  dew
point where 503 condenses  as HgSO^  S02 interference is prevented by
                                                t
maintaining the temperature  of the  gas above  the  water  dew  point.   Sulfur
dioxide is collected in  a  3 percent hydrogen  peroxide solution.  Both  SOg  and
503 (as H2$04) are measured  by titration with  a  0.02 N  NaOH solution  using
barium thorin as the indicator.  A more detailed  discussion of the sampling
and analytical techniques  for the controlled  condensation  system is given  in
reference A-2.
A.4    TRACE ELEMENTS  AND  ORGANIC EMISSIONS
       Emissions of  inorganic trace elements  and  organic compounds were
sampled with a Source  Assessment  Sampling  System  (SASS). The  SASS train was
designed and built for EPA's Industrial Environmental Research Laboratory,
Research Triangle  Park,  for  Level  1 environmental assessment (reference  A-3).
It collects large  quantities of gaseous and solid samples  required for
subsequent analyses  of inorganic  and  organic  emissions  as well as  particle
size measurements.
       The SASS system,  illustrated in figure  A-5,  is generally  similar  to the
system utilized for  total  particulate mass  emission  tests,  with  the exception
of:
                                      A-5

-------
       FILTER
   DESICCATE AND
      WEIGH TO
  CONSTANT WEIGHT
 PROBE. NOZZLE
AND FILTER WASH
                                                           EVAPORATE AT
                                                         ROOM TEMPERATURE
                                                           AND PRESSURE
  EVAPORATE AT
ROOM TEMPERATURE
  AND PRESSURE
MEASURE VOLUME
    TO -1 ml
                        DESICCATE AND
                          WEIGH TO
                       CONSTANT WEIGHT
                                                           EXTRACT WITH
                                                             3 i 25 ml
                                                            ETHYL ETHER
                       EXTRACT WITH
                         3 I 25 ml
                       ETHYL ETHER
                                                                      EXTRACT WITH
                                                                        3 > 25 ml
                                                                      CHLOROFORM
                                                                                              FILTER THROUOH
                                                                                                i? mm TYPE A
                                                                                                GLASS FILTER
                                                                                               EVAPORATE AT
                                                                                             ROOM TEMPERATURE
                                                                                               AND PRESSURE
                                                                                              DESICCATE AND
                                                                                                WEIGH TO
                                                                                             CONSTANT WEIGHT
                                   EVAPORATE ON
                                    STEAM BATH
                                   AND WEIGH TO
                                  CONSTANT WEIGHT
                               FILTER THROUOH
                               A 4T mm TYPE A
                                 GLASS FILTER
                                                     ROOM TEMPERATURE
                                                     CONSTANT WEIGHT
NOTES.
11 ALL WEIGHTS ARE TO NEAREST OOlQ
2) DESICCATE ALL SAMPLES FOR 24 HOURS PRIOR TO WEIGHING
      Figure A-3.    Sample  Analysis  Scheme  for  Particulate  Sampling  Train
                                                    A-6

-------
-1/b"  quartz nozzle

   316 stainless steel  union
-High temperature
  heating mantle
                       Goksoyr/Ross
                        condenser
            Quartz filter holder
                       Probe T.C
         5/8" quartz probe
                                                            Heavy wal I
                                                            1/4" 1.0.
                                                           Latex tubing
                                             Submersible water
                                             circulation pump
I                                                                            Stainless
                                                                             condenser heat
           Coarse adjustment
              valve
     Orifice AP
  magnehelfc gauge
                          Dry test nieter
 Air tight  vacuum pump
       _Sm!th-Greenberg
     implnyer (100 nt  Jt (1,0


      [nipty modified  Smlth-
                Impninei


~Slli(d <|t>l (il'SUdllt tl cl|)
                         Control nioiJule
                Figure  A-4.    Controlled  Condensation  System

-------
                                               iluatcd oven -
CO
                   Stainless
                     steel
                    sample
                    nozzle
Stack
velocity
Magnehelic
gauges
                                                                                           !/<"' fi
                                                                                              11 if
                                                                                           I -.(> lotion
                                                                                          ball  voIvu
                               Organic module
                              Stainless steel
                               probe assembly
                              Gas temperature T.C.

                                 1/2" Teflon line
                                                                        Oven

                                                           Sorbent  cartridge

                                                        Heater  controller
                                                                           W'Tefbnli
                                                                         Condcnsate
                                                                    _lcol lector vessejl
                                                                                     Imp/cooler trace
                                                                                  element collector
                                                                                         Coarse adjustment
                   Fine adjustment
                     valve
                                       Orifice 6H
                                       Magnehelic
                                       gauge
   Vacuum pumps
I
1(10 ft3/min  each)
                                                                                                                               Inipinger
                                                                                                                                 T.C.
                                                  Ice bath
                                                  600 grams
                                                  Silica  gel
                                                   desiccant
                                                  500 ml
                                                   0.2 M AgNOi
                                                   0.2 M (NH4)2  S208
                                                  SOO ml
                                                   30% H202
                                                                                                  Heavy wal 1
                                                                                                  vacuum line
                                                    Figure  A-5.   Schematic of SASS  Train

-------
        o    Particulate  cyclones (not used in these tests) heated in the oven
            with  the  filter to 230°C (450°F)
        •    The addition of a gas  cooler and  organic sampling module
        *    The addition of necessary vacuum  pumps
        Schematics  outlining the sampling and analytical  procedures used with
the  SASS equipment are  presented  in figures  A-6 and A-7.
        Inorganic analyses  of solid and liquid samples from the SASS train were
performed with spark source mass  spectroscopy (SSMS) for most of the trace
elements.   Atomic  absorption spectrffscopy (AAS) was used for analyses of
                                              <•
mercury (Hg), antimony  (Sb) and arsenic (As).
        Quantitative  information on total organic emissions was obtained by gas
chromatography for total chromatographable organics (TCO) and by gravimetry
(6RAV)  of methylene  chloride extracts of solid samples and samples collected
in the  sorbent module (XAO-2) and condensate trap.  Infrared spectroscopy (IR)
and  GC/MS were used  for identification of organic functional groups and
polycyclic  organic matter  (POM) and other organic species in solid and liquid
extract SASS samples.   Liquid chromatography of extract samples was not
performed in this  test  program because the samples contained less than 15 mg
of total organics.   Direct insertion probe low resolution mass spectroscopy
(LRMS)  of the XAD-2  resin  extracts was performed to identify and semiquantify
organic categories present in extract samples.   Figure A-8 illustrates the
organic analysis methodology used.
        Passivation of the  SASS train with 15 percent by volume HN03 solution
was  performed prior  to  equipment  preparation and sampling to produce
biologically inert surfaces.   Detailed descriptions of equipment preparation,
sampling procedures, and sample recovery are discussed in reference A-3 and
will  not be repeated here.
                                      A-9

-------
SAMPLE






SORSENT CARTRIDGE —
AaulOUSCONDENSATE
FIRST IMP1NGER
SECOND ANO THIRD
IMOIMRCOC rnupiwcn
« 0 a x *
1 SI g 2 2 S
5 «a s £ * 2
1 IIs- i > i i a
£ *o> x «OT *S
2 000 S OH" J H



*Sv» ^/ *
>— «C SPLIT
f^ ^ • •
•^ ^ - -^
^ -i ^X ' • • •

._ *


SPtlT X A A
S GRAMS * *
COMBINE
^ AQUEOUS PORTION
\ ORGANIC EXTRACT * • • N


u
3 1
a i
z <


•i

• •
  TOTALS
5   2   5
                                                                                                    8   1
* If r*amr«d. umoi* ifiould tit Mt •••<• »oc biological irulyin it th« point.

Thit u»o • r«qu,r«d to d««in« th« ton) "»» of o»rtieul»t« 
-------
Figure A-7.  Exhaust Gas Analysis Protocol

-------
                                Organic Extract
                                      or
                              Neat Organic Liquid
1
I
TCO
Analysis
                                  Concentrate
                                    Extract
      1
GC/MS Analysis,
POM, and other
organic species
1
                                       I
I
LRMS

Infrared
Analysis
                                                                                
-------
A.5    Cx-C6  HYDROCARBON SAMPLING  AND  ANALYSIS
       Samples of flue gas  for Cj-Cg  hydrocarbon  analysis  were  collected  using
a grab sampling procedure.   Flue  gas  was  extracted  from  the  stack  at  an
average velocity point that  corresponded  with  the average  velocity point
selected for SASS sampling.  Samples  for hydrocarbon analysis were  collected
using the apparatus diagramed  in  figure A-9.   The equipment  consisted of  a
nonheated 0.63 cm (0.25-in.) (o.d.),  stainless-steel  probe fitted  with an
0.7 urn-sintered, stainless-steel  filter attached  to the  probe inlet.   The
outlet of the sampling probe was  directly attached  to the  inlet of a  Thomas,
                                                i
Teflon-lined, diaphragm  vacuum pump.   A 500-cm3,  stainless-steel,  heated
sampling cylinder placed on  the  outlet  of the  pump  was used  to  collect this
sample under pressure.
       Sampling cylinder construction consisted of  specially wrapping each
assembly with a 1.8m  (6-ft), heavily  insulated, 576-watt,  heat  tape powered  by
a percentage voltage  controller.  A type K (Alumel/Chrome!)  thermocouple
implanted on the metal surface of the sampling cylinder was  used to monitor
the cylinder temperature during  operation.  To ensure even and  efficient
heating of the sample cylinder each unit  was  covered with  approximately
1.9-cm (0.75-in.) of  ceramic fiber  insulation. Figure A-10  presents  a
schematic of the sampling cylinder  construction details.
       Prior to flue  gas sampling,  the sampling cylinders  were  preconditioned
by heating each unit  to  approximately 150°C (300°F) and  purging with  zero air
(grade 0.1) for 10 min.  To  extract a flue gas sample the  assembled apparatus
was positioned and allowed  to  preheat to the  desired sampling temperature of
120° to 150°C (250° to 300°F).   Once  up to temperature the diaphragm  pump was
started and the sampling cylinder was alternately pressurized and  vented  with
flue gas to purge the system.  Usually 8 to 10  purge cycles were performed with
                                      A-13

-------
  sintered stainless-steel filter
l/4-1n.  stainless-steel
  probe
                                            Teflon diaphragm pump

                                              Pressure gauge


                                                   Inlet valve
                                                                                            500-cm  stainless-steel
                                                                                               sample cylinder
I
t—•
-p.
                                                  • •iAlllllllllllBlllI
                                    Cleramic  insulation
                                      and heat tape
                                                                                           Outlet
                                                                                              valve
                                                                                   Thermocouple
                                             Figure  A-9.
                                     Hydrocarbon  Sampling  System

-------
01
                                    Ceramic  fiber insulation
                                       Heat  tape


                        Stainless-steel sample valve
                                                                                                              Stainless-steel
                                                                                                              sample valve
                               Figure A-10.  Schematic  of  Sampling  Cylinder Construction

-------
the last one being retained for analysis.  Final  pressure  in  the  sampling
cylinder was typically 207 to 345 kPa  (30 to  50  psia).
       Sample analysis was conducted onsite using  a Varian, Model  3700,  gas
chromatograph.  This unit is equipped  with a  flame ionization  detector  (FID)
automatic injection loop, and automatic linear temperature programming.
Table A-2 details the instrument specifications.   The gas  chromatograph  output
was recorded using a Hewlett-Packard Model 3390A  reporting integrator.
       All  samples and calibration standards  were  analyzed using  repeated
injections via the automatic 2-cm3 heated sampling loop.   Separation  of  CI-GS
hydrocarbon components was done on a 1.8m x 0.32  cm x 0.63 cm
(6 ft x 1/8 in. x 1/4 in.) (o.d.) silanized stainless-steel column  packed with
60/80 mesh Poropak Q (Super 0) using an isothermal program at  120°C.  Table
A-3 presents a summary of the GC operating condition used  for  the field
analysis.
       A summary of Cj-Cg hydrocarbon  analysis conducted on selected  samples,
sample blanks, and calibration standards may  be  found in volume  II  of this
report.  Calibration standards consisting of  a mixture  of  C^-Cg  parafinic
hydrocarbons (15 ppm each) in nitrogen were analyzed at the beginning and end
of each sample day.  Blank samples of  zero air were also analyzed in  order to
quantify any sample apparatus equipment interference.
A.6    NeO EMISSIONS
       The stack gas grab samples were extracted  into stainless  steel
cylinders for laboratory analysis for  ^0.  For  analysis each  sample  cylinder
was externally heated to 120°C (250°F), then  a 1-ml sample was withdrawn with
a gas-tight syringe for injection into a gas  chromatograph.   The analytical
equipment consisted of a Varian 3700 gas chromatograph  equippped with a  63Ni
electron capture detector and a 3.65-m (12-ft) stainless-steel column packed
                                      A-16

-------
with Poropak Super Q, 80/100 mesh.   The  injector temperature was  kept  at
the detector at  350°C,  and  the  column  temperature at  33°C.   Elution time  for
    was approximately 5 min, with  a flowrate of 20 ml/min of nitrogen.
                                      A-17

-------
          Table A-2.  Gas Chromatograph Specifications
Van an Model 3700 Gas Chromatograph
    Sensitivity
    Zero range

    Noise (inputs capped)
    Time constant

    Gas required
1 x 10-12 A/mV at attenuation  1 and
range 10-12 A/mV
-lO"1! to 10"9 A (reversible with
internal switch)
5 x 10-15 A; 0.5 uV peak to peak
220 ms on all ranges  (approximate  Is
response to 99 percent of peak)
Carrier gas (helium), combustion air,
fuel gas (hydrogen)
           Table A-3.  Summary of GC Operating Conditions
       Injector temperature
       Column temperature
       Detector temperature
       Temperature program
       Carrier gas
       Fuel gas

       Combustion air
   120°C
   120°C
   250°C
   Isothermal  (120°C.)
   Helium  (grade 5.0)
   Hydrogen  (grade 5)  276  kPa
  .(40 psi)
   Zero air  (grade 0.1) 414  kPa
   (60 psi)
                                A-18

-------
                         REFERENCES FOR APPENDIX A
A-l.   Tidona, R. J., "NOX Emissions Assessment:  Gaseous  Emissions From a
       Refinery Process Heater  in Baseline  and  Low  NOX  Configurations," KVB,
       Inc., Irvine, CA, KVB11  47800-1284,  prepared  for Acurex Corporation,
       July 1981.

A-2.   Maddalone,  R. and N. Gainer, "Process Measurement  Procedures:
       Emissions," EPA-600/7-79-156, NTIS PB 80-115959, July  1979.

A-3.   Lentzen,  D. E., et al.,  "IERL-RTP Procedures  Manual:  Level 1
       Environmental Assessment  (Second  Edition),"  EPA-600/7-78-201,
       NTIS PB 293795, October  1978.
                                     A-l 9

-------
                                 APPENDIX B
               TRACE ELEMENT CONCENTRATIONS AND MASS BALANCES

       Symbols appearing in the tables:
           DSCM    Dry standard cubic meter at 1 atm and 20°C
           MCS     Microgram
           PPM     Part per million by weight
           SEC     Second
           ng/J    Nanogram per Joule
           <       Less than
           >       Greater than
           N       Element not analyzed
           U       Unable to determine
       Trace elements having concentrations less than the detectable  limit
or having a blank value greater than the sample value were given  an
arbitrary concentration of zero.  Values in the form A < x < B were
determined by letting elements reported as less than some concentration  be
represented by a concentration of zero for the low value and the  reported
concentration as the high value.
                                  B-l

-------
       Detectability limits for the various samples were the following:

       •   Filter                 — <0.1 yg/g

       t   XAD-2                  — <0.1 ug/g

       •   Impinger and organic

           module concentrate     — <0.001

       t   Fuel Oil               — <0.1 pg/g
                                   Baseline           Low NOX
  FUEL IN

     Gas
        m3/s
        MW

     Oil
        9/s
        MW

  EXHAUST GAS OUT

     DSCM collected by SASS         27.568            27.702
     DSCM/s                          3.519             3.288
     Molecular weight dry           30.01              30.01
     Moisture, percent              15.9              16.5
     02, percent dry                 4.0               3.3


Standard conditions:   20°C (68°F)  and 1  atm.   One molecular  weight of

an ideal gas occupies 24.04£ at standard conditions;
0.118
8.32
109
4.74
OJ18
8.10
109
4.75
                                   B-2

-------
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MCG/SEC
HEA1ER MASS BALANCE ....
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                                 TECHNICAL REPORT DATA
                          (Please read /nunictwns on the reverse before t ample ting)
 1. REPORT NO.
 EPA-600/7-84-074a
        2,
                                   3 RECIPIENT S ACCESSION NO.
4. TITLE AND SUBTITLE
 Environmental Assessment of a Crude-Oil Heater
  Using Staged Air Lances for NO  Reduction; Volume
  I. Technical Results
                                   5. REPORT DATE
                                   July 1984
                                   6. PERFORMING ORGANIZATION CODE
7, AUTHOfl(S)
                                                       8. PERFORMING ORGANIZATION REPORT NO
 R. DeRosier
                                    TR-82-94/EE
9. PERFORMING ORGANIZATION NAME AND ADDRESS
 A cur ex Corporation
 P.O. Box 7555
 Mountain View,  California 94039
                                   10. PROGRAM ELEMENT NO.
                                   11. CONTRACT/GRANT NO
                                    68-02-3188
 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
                                    Final; 6/81 - 11/83
                                   14. SPONSORING AGENCY CODE
                                     EPA/600/13
15. SUPPLEMENTARY NOTES iERL-RTP project officer is Robert E.  Hall, Mail Drop 65; 919 /
 541-2477.  Volume II is a Data Supplement.
 16. ABSTRACT
          This volume of the report gives emission results from field tests of a
 crude-oil process heater burning a combination of oil and refinery gas.  The heater
 had been modified by adding a system for injecting secondary air to reduce NOx
 emissions.  One test was conducted with the staged air system (low NOx), and the
 other, without (baseline).  Tests included  continuous monitoring of flue gas  emissions
 and source  assessment sampling system (SASS) sampling of the flue gas with subse-
 quent laboratory analysis  of the samples utilizing gas chromatography (GC),  infra-
 red spectrometry (IR), gas chromatography/mass spectroscopy (GC/MS), and low
 resolution mass  spectrometry (SSMS) for trace metals. Flue gas concentrations of
 NOx were reduced 30 percent (from 83  to 56 ng/J) with the staged air system. Total
 organic emissions dropped from 17.1 to 3.4 mg/dscm from the baseline  to the low-
 NOx test (due primarily to a reduction in  the C sub 1 to C sub 6 boiling point range
 compounds  which constituted most of the organic emissions).  GC/MS analysis iden-
 tified 11 semivolatile priority pollutant compounds  in both tests, most of them pre-
 sent in higher concentrations during the baseline test.  LRMS analysis suggested the
 presence of eight compound categories  in the organic emissions during the  baseline
 test and four in the  low-NOx test.
 7.
                             KEY WORDS AND DOCUMENT ANALYSIS
                 DESCRIPTORS
                                           b.IDENTIFIERS/OPEN ENDED TERMS
                                               C.  COSATI I ICId/CfOUp
 Pollution
 Nitrogen Oxides
 Crude Oil
 Gases
 Heating Equipment
 Lances
 Flue Gases
Assessments
Pollution Control
Stationary Sources
Staged Combustion
Refinery Gas
Air Lances
Environmental Assess-
 ment	
13 B
07B
UH, 08G
07D
13A
131
21B
14B
13. DISTRIBUTION STATEMENT

 Release to Public
                       19. SECURITY CLASS (This Report/
                       Unclassified
                        21. NO. OF PAGES
                           102
                       2O. SECURITY CLASS (This page)
                       Unclassified
                                               22. PRICE
EPA Form 2220-1 (9-73)
                     B-31

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