EPA-600/2-77-196
September 1977             Environmental Protection Technology Series
                          AT-SEA  INCINERATION
                 OF ORGANOCHLORINE WASTES
                 ONBOARD THE M/T VULCANUS

                            Industrial Environmental Research Laboraton
                                 0«ice of Research and Developrnen
                                ' S .Environmental Protec tion ftgencv
                            Research Tnangle Park, North Carolina 277

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                                      EPA-600/2-77-196
                                        September 1977
      AT-SEA INCINERATION
OF ORGANOCHLORINE WASTES
ONBOARD THE  M/T VULCANUS
                     by
         J.F. Clausen, H.J. Fisher, R.J. Johnson, E.L. Moon,
         C.C. Shih, R.F. Tobias, and C.A. Zee

                   TRW, Inc.
                  One Space Park
              Redondo Beach, California 90278
                Contract No. 68-01-2966
               Program Element No. 1AB604
             EPA Project Officer: Ronald A. Venezia

           Industrial Environmental Research Laboratory
            Office of Energy, Minerals, and Industry
             Research Triangle Park, N.C. 27711
                   Prepared for

           U.S. ENVIRONMENTAL PROTECTION AGENCY
             Office of Research and Development
                Washington, D.C. 20460

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                                ABSTRACT
     This report describes the incineration of 4100 tonnes of organochlorine
wastes by the M/T Vulcanus in an EPA designated burn area in the Gulf of
Mexico under a special permit granted by Region VI of the EPA.  The wastes,
containing 63% chlorine, orginated from manufacturing processes conducted
by the Shell Chemical Co., Deer Park, Texas, and was loaded onto the
Vulcanus at the Shell Deer Park facility.

     The incineration process was monitored by a field sampling team from
TRW, Redondo Beach, Ca.  Waste destruction efficiencies and total combustion
efficiency were determined by five methods, each with separate means of
sampling, analysis, and calculation.  Incinerator efficiencies of at least
99.9% were observed, at an average waste feed rate of 22 tonnes/hr.  The
process was carried out at a flame temperature averaging 1535°C and at
dwell times calculated to be 0.9 seconds.

     An automatic waste shut off system was incorporated into the incinera-
tion process, and was pre-set so as to shut down the flow of waste if the
flame temperature should drop below 1200°C.  The temperature of the process
was monitored directly by an optical pyrometer for flame temperature and
indirectly by thermocouples which measured wall temperature and which were
statistically correlated with the flame temperature.
                                     ii

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                                 PREFACE
     Organochlorine incineration on board the M/T Vulcanus operating
in the Gulf of Mexico was accomplished under provisions cf an Environmental
Protection Agency Special Permit.  Thermal  destruction of such wastes  at
sea is a relatively new disposal method in  the United States.  The purpose
of sampling and monitoring approximately one-third of the total waste
destroyed during this incineration operation was twofold.  First,  there
was a definite need to test the suitability and reliability of a comprehensive
stack gas sampling apparatus and an on-line monitoring instrumentation
system.  And secondly, data was required in support of developing  United
States guidelines and regulations for new incineration ships.  It  was
not the intent of t is work to insure compliance with permit operating
conditions for Gulf of Mexico incineration  activity.

     Successful accomplishment of this effort was due to the assistance
and cooperation of a large number of individuals and their respective
organizations.  Equipment design and development, definition of sampling
requirements and the acquisition of samples and subsequent analysis was
accomplished by personnel from the Applied  Technology Division and the
Environmental Engineering Division of TRW,  Inc., Redondo Beach, California.
Engineering liaison to adapt test equipment on-board the Vulcanus  was
facilitated by the management of Ocean Combustion Services, B.V.,  of
The Netherlands.  Subsequent installation of this equipment as well as the
acquisition of data could only have been accomplished with the complete
cooperation of the ship's officers and crew.

     Technical direction, assistance and planning of the program's
conceptual design and implementation was received from a number of agencies
within the U. S. Government.  These include the U.  S. Environmental
Protection Agency's Oil and Special Materials Control Division  (OSMCD),
Washington, D.C.; Industrial Environmental  Research Laboratory  (IERL),
Research Triangle Park, North Carolina; and the Regional Office, Region IV,
Dallas, Texas.  Guidance in installing equipment on the  Vulcanus to conform
with U. S. maritime regulations was provided by the U. S.  Coast Guard,
Headquarters, Washington, D.C.

      Representatives of the Shell Chemical Company, Deer Park, Texas,
provided waste samples for preliminary analysis prior to the burn as well
as technical details regarding their original sampling and monitoring
work on board the Vulcanus in 1974.  Personnel of Arthur D. Little, Inc.,
Cambridge, Massachusetts, provided consultation regarding sample
preparation and analysis.

      The authors are indebted to the many individuals of all  these
organizations for their contributions and cooperation.

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                                CONTENTS

                                                                   Page

1.  Introduction and Summary	1
2.  Description of the M/T Vulcanus	C
    2.1  Vessel-General Layout  	   G
    2.2  Tanks and Pumps	   6
    2.3  Incinerator System 	   6
    2.4  Recording and Control Equipment  	  11
         2.4.1  Waste Measurements	11
         2.4.2  Wall  Temperature Measurements 	  11
         2.4.3  Emergency Automatic Waste Shut-off  	  11
         2.4.4  Special Equipment 	  12
3.  Test Description	14
    3.1  Operational  Procedures 	  14
         3.1.1  Test  Procedures	14
         3.1.2  Safety Procedures 	  16
         3.1.3  Test  Commentary	16
    3.2  Sampling Methods 	  19
         3.2.1  Probe and Probe Mount	19
         3.2.2  On-Line Gas Monitoring	21
         3.2.3  Acquisition of Combustion Products	25
    3.3  Analytical  Techniques	28
         3.3.1  Extractions and Sample Preparation	28
         3.3.2  Analysis of Concentrated Extracts 	  30
         3.3.3  Analysis of Gas Bag Samples  	  31
    3.4  Problems Encountered  	  31
         3.4.1  Sampling Train Impingers	31
         3.4.2  Sorbent Module	32
         3.4.3  Filter Holder	33
         3.4.4  SASS  Train Control  Unit	33
                                    iv

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                               CONTENTS (Continued)

                                                                     Page

         3.4,5  On-Line Instrumentation	33
         3.4.6  Degradation of Gas Bag Fittings	34
4.  Test Results	35
    4.1  Operational  and Field Data Summary	35
         4.1.1  Waste Feed Rate and Mass Emissions	35
         4.1.2  Temperature and Residence Time	36
         4.1.3  On-Line Gas Composition	40
         4.1.4  Plume Characteristics  	   50
         4.1.5  HCI Measurements on Board	50
    4.2  Analytical Results	52
         4.2.1  Waste Feed Analysis Results	52
         4.2.2  SASS Train Sample Analysis Results 	   57
         4.2.3  Gas Bag Sample Analysis Results	63
         4.2.4  Burner Head Residue Analysis Results 	   6R
5.  References	67
Appendix A - Schedule of Waste Consumption by
             Tank Number and Location	68
Appendix B - Tabulation of Temperatures in Furnaces  	   70
Appendix C - Safety Procedures 	   76
Appendix D - Burner Maintenance Record  	   81
Appendix E - GC/MS Reconstructed Gas Chromatograms 	   84

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                                 FIGURES

2-1.   M/T Vulcanus - incineration vessel	  7
2-2.   Tank layout schematic	  8
2-3.   Incinerator configuration	  8
2-4.   Incineration system- burner and thermocouple  locations	10
3-1.   Sampling port locations	15
3-2.   Probe design diagram	19
3-3.   Diagram of probe mount for the Vulcanus	20
3-4.   Probe mount with probe fully withdrawn	21
3-5.   Sampling port dimensions	22
3-6.   Portable laboratory location aboard the M/T Vulcanus	23
3-7.   Equipment arrangement in the portable laboratory	24
3-8.   Flow diagram of on-line instrument system	25
3-9.   Source assessment sampling system (SASS) schematic	26
4-1.   Controller/flame temperature correlation-starboard
       incinerator	38
4-2.   Controller/flame temperature correlation-port incinerator	39
4-3.   On-line gas composition data - Test IV, March 9	44
4-4.   On-line gas composition data - Test V, March 10	45
4-5.   On-line gas composition data - Test VI, March 11	46
4-6.   Combustion efficiency data - Tests IV, V, and VI
       (March 9, 10, and 11, respectively)	47
4-7.   Combustion efficiency vs. probe position	48
4-8.   C02 concentration vs. probe position	49
4-9.   CO concentration vs. probe position	49
4-10.  HC1 sampling locations
       1) combustion deck 2) bridge 3) main deck 4) stern	53

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                                 TABLES
1-1.    Definition of destruction efficiency terms	  3
1-2.    Summary of calculated destruction  efficiencies	  3
2-1.    Specification of the M/T Vulcanus	  9
3-2.    Description of on-line instruments	24
4-1.    Waste feed rates	36
4-2.    Gas composition data summary	41
4-3.    Test data summary for shipboard incineration test
       series I-VII	43
4-4.    Hydrogen chloride (HC1) in air aboard vessel	51
4-5.    Summary of Vulcanus samples	54
4-6.    Representative waste composition by GC/MS	55
4-7.    Calculated approximate emission rates of inorganic elements...56
4-8.    Effluent gas concentrations from analysis of sorbent
       trap extracts (mg/m3)	58
4-9.   Gravimetric results on organic SASS samples	60
4-10.  LRMS results on organic  SASS  samples	62
4-11.  Analytical recovery for  SASS  samples	62
4-12.  Gas bag  constituents  by  LRMS	63
4-13.  Gas bag  analysis  by Tenax/GC	64
4-14.  Compounds  found  in burner head residue	66
                                   vn

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                      1.   INTRODUCTION  AND  SUMMARY
     Thermal  destruction of chlorinated  hydrocarbon wastes  at  sea  is a
relatively new disposal  technique for wastes  generated  in the  United States.
In late 1974, organochlorine wastes were incinerated  in the Gulf of Mexico
for the first time by the Motor Tanker (M/T)  Vulcanus.   This effort,
monitored by the U.  S. Environmental Protection Agency  (EPA),  provided
an initial technical basis for concluding that at sea incineration was
a viable alternative to other means of disposal using land  based facilities
(Reference 1).

     A second incineration program, again burning organochlorine waste,
was performed on board the M/T Vulcanus during the period  5 through  13 March,
1977.  This second Gulf of Mexico incineration afforded an  opportunity to
employ recent technology for monitoring and assessing the  environmental
effectiveness of this disposal process.   The purpose of this test  work
was to evaluate the adequacy and reliability of the monitoring and comprehensive
sampling system.  Previously, these systems had been utilized  on  land-based
incineration facilities (References 2, 3).  The ability to  make such a
system reliably operate in the more harsh environment encountered  during
at sea incineration remained to be demonstrated.  A second  equally important
objective for the current program was acquisition of sufficiently  comprehensive
data to support developing at sea incineration regulations  and guidelines
for future new incinerator vessels.

     The scope of activities for this work included design  and preparation
of the stack gas sampling and monitoring apparatus, development of a
sampling and analysis protocol, acquiring samples and monitoring waste
effluent during incinerator operation, as well as analysis  of these samples
followed by evaluation of the results.  This report presents results
obtained during the EPA sponsored monitoring and sampling program.

      During the sampling and monitoring operations on board the M/T
 Vulcanus in March,  1977, approximately 4100 tonnes (metric tons)
 of Shell Chemical Company wastes were incinerated.   This was  accomplished
 under Special Permit No. 750D008E granted to the Shell Development
 Company by Region VI of the Environmental Protection Agency
 (Reference 4).  This represented about one-third of the total waste
 destroyed as allowed by the permit conditions.  The site  of the combustion,
 as fixed by the permit, lay in the Gulf of Mexico within  a rectangle

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defined by the following coordinates:


          Latitude                       Longitude

          27° 06' 12" N                  93° 24'  15" W

          26° 32' 24" N                  93° 15'  30" W

          26° 19' 00" N                  93° 56'  00" W

          26° 52' 40" N                  94° 04'  40" W

At its nearest point to land, this site is approximately 130 miles to the
south of Sabine Pass, Texas.

     The wastes burned were produced as by-products in the manufacture of
allyl chloride, epichlorohydrine, dichloroethane and vinyl chloride at
Shell Chemical Company's Deer Park, Texas, plant.  The material  consisted
primarily of low molecular weight chlorinated aliphatics and had a gross
heat content of 3,860 kcal/kg (6,950 Btu/lb).

     Sampling operations utilized a high volume EPA Source Assessment
Sampling System (SASS) with a sampling rate of 0.085 cubic meters per
minute.  This sampling train was used to trap and remove organic vapors
from the stack effluent.  Sample acquisition was by a remotely actuated,
water-cooled stainless steel probe capable of traversing the starboard
incinerator stack diameter of 3.4 meters.  During stack sampling operations,
incineration effluent products were simultaneously monitored for total
hydrocarbons, carbon monoxide and dioxide, nitrogen oxide and dioxide
as well as oxygen concentration.  These parameters were measured in real
time to monitor the overall combustion efficiency of the incinerator.
SASS train components were subsequently analyzed in detail by laboratory
methods.  The purpose of these analyses was to determine how effectively
the incineration process destroyed constituents in the organochlorine
waste feedstock.

     The waste was burned at an average rate of 22 tonnes per hour or
approximately 11 tonnes per hour for each incinerator.  Total elasped
burn time was 186 hours and 45 minutes.  The average flame temperature
was 1535°C as determined by optical pyrometer measurements.  Under these
conditions, a combustion gas residence time in the Incinerator was calculated
to be approximately 0.9 seconds.

     Six waste incineration sampling tests (I through VI) and one background
test (VII) burning fuel oil alone were conducted.  Because sampling tests
were longer and generally more successful for tests IV through VII, these
test data and samples were analyzed more intensively.  Data from the
on-line analyzers were used to calculate combustion efficiency while
sampling operations were in progress.  Analytical results as well as
on-line total hydrocarbon measurements provided the basis for calculating
waste destruction efficiencies.  Five efficiencies were determined, each
with separate means of sampling, analysis and calculation.  These five

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destruction efficiency terms are listed  and  defined  in Table  1-1.  The
resulting destruction efficiency values  are  presented  in Table  1-2 for
tests IV through VII.  The latter was the background or baseline  test
using fuel oil.
         TABLE  1-1.   DEFINITION OF DESTRUCTION EFFICIENCY TERMS
Destruction
Efficiency
Term
DECE
DETHC
DEGGHC
DEsc3ci3

DEGGC3C13
Method of Efficiency Calculation
% C.Oy-%CO
-S-CB-— x 10°
THC fed-THC from on-line monitor
THC Ted x 10°
THC fed-THC in grab gas sample
~ 	 " THC Fed 	 * 10°
C3C13 fed - C3C13 in SASS samples
	 7 n toA x 10°
C3C13 fed
C,C1, fed- C,C1, in grab gas samples
_j j — ?...-i 	 	 	 x inr
C3C13 fed x IOC
Description of Method
Overall comhustu.'. efficiency based on carbon
dioxide and carbon monoxide concentrations. CC^
and CO were measured by continuous on-line
monitors on board the Vulcanus.
Total organic destruction efficiency based on
total hydrocarbons (THC) measured by a continuous
on-line monitor on board the Vulcanus.
Total organic destruction efficiency based on
total hydrocarbons measured in the Tedlar bag
grab gas samples analyzed by GC/F1D.
Waste destruction efficiency based on trichloropro-
pane (major waste constituent) found in SASS train
samples. Trichloropropane was identified and
quantified by GC/MS.
Waste destruction efficiency based on trichloropro-
pane found in grab gas samples by GC after Tenax
concentration.
      TABLE 1-2.  SUMMARY OF CALCULATED DESTRUCTION EFFICIENCIES

DECE
DETHC
DEGGHC
DEsc3ci3
DE6GC3C13
Test Number
IV
WASTE
99.98%
99.991%
99.998%
99.98%
>99.999%a
V
WASTE
99.96%;;
99.996%
99.996%
99.92%
>99.999%b
VI
WASTE
99.97%
99.996%
99.997%
99.98%
>99.999%b
VII
BACKGROUND
99.97%
99.997%
99.999%
-
     a)  Waste constituents not detected
     b)  Based on trace quantity of trichloropropane  found

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       The  results  of  these  tests  indicate that incineration performance
  on  the  M/T  Vulcanus  was consistently greater than 99.9 percent for both
  waste and total organic destruction efficiency.  These results are
  comparable  to  land-based incinerator performance with chlorinated waste
  materials (References 2, 3).  Trace levels of known waste constituents
  such  as trichloropropane (0.1 to 0.6 mg/nr) were found in the effluent
  gases.  Additionally, low  ppm and ppb levels of chlorinated and alkyl
  substituted benzene  compounds were found in some samples.  These materials
  could have  been in the waste feed at levels which were too low to make
  confirmed indentification, or they may have been masked by other
  constituents during  the waste characterization.  This identification
  level was estimated  to be  less than 0.5 percent in the waste.  A specie
  at  0.5 percent, if totally undestroyed in the incinerator, would create
  an  emission level  of approximately 700 ppm which is about 1000 times the
  amount actually found.  Thus, efficient destruction of these compounds
  is  still  indicated if they are indeed waste constituents at a 0.5 percent
  level.  Two other possible sources of these materials may be postulated.
  These compounds may have been by-products of the combustion, having been
  synthesized in the process or the materials may have been the result of
  a chlorination of otherwise non-chlorinated materials within the sampling
  train.

      An interesting and significant result derived from the on-line
 monitoring data was that a fixed position effluent gas sampling probe would
  have sufficed to insure that incinerator combustion efficiency was always
 equal  to  or greater than 99.9 percent.   Potential  wall effects on the
 combustion gas composition were apparently eliminated at distances greater
 than 15 cm from the inside incinerator wall  surface.

       The  Vulcanus  incinerators were effective in destroying  this
organochlorine waste  material.  The sampling (SASS)  train, although
advantageous for acquiring  large volume samples, was of marginal utility
due  to the use of  stainless steel construction in many components.
Corrosion  was a continual problem area due to the high (approximately
6-8  percent) hydrochloric acid (HC1) content in the  combustion products.
An all glass sampling train would eliminate this problem.  The on-line
analyzer system was adequate for the monitoring program.   Frequent
calibration  and maintenance was, however, required to  keep the system
on-line at the desired times.  Most difficulty was experienced with the
CO,  C02 and NO analyzers.  Although these instruments were designed for
process stream measurement  (for instance, utilities, cement kilns, etc.),
it is doubtful that the extremely hostile environment! of at  sea incineration
was  ever considered in their original design specifications.  In particular,
the  shock  and vibration modes encountered at sea are somewhat unique.
Equally significant was the salt air environment and high HC1 concentration
in the combustion gas stream.  The monitoring system employed was adequate
for  this experimental work.  In future applications of this type, more
attention  must be given to the technical details which will reduce
maintenance and increase instrument reliability.  This appears entirely
feasible within current technology.

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      Cooperation and assistance by the ship's  crew was  excellent.
Incinerator controls and instrumentation was sufficient.   Additional
incinerator wall  temperature thermocouples and  readouts  would be  desirable
for purposes of redundancy since existing thermocouples  cannot be replaced
during furnace operations.  Waste feed rates can only be determined  via
tank depletion rates based upon depth soundings.  A remote gaging system
would be advantageous from the standpoint of handling hazardous wastes
especially of a volatile nature.  Similarly, waste flow metering  equipment
would be useful to acquire real time data as opposed to time averaged data
as at present.  This is, however, an admittedly very difficult technical
requirement to implement.

      No significant incidents related to safety were experienced during
sampling and monitoring operations.  In retrospect, adequate scaffolding
should have been installed around the traversing probe.   Replacement of
the probe at sea constituted a safety hazard to the sampling crew.
Subsequent incineration test programs at sea should include development
of a definitive, formal safety plan.  Although oral safety briefings were
conducted, no formal written safety document was employed during this
test.  Because of the unique working environment at sea, a safety plan
is advisable in the future.

      Ship-to-shore radio communications were at best only marginal.
The precise technical reasons for this  situation are unknown.  To facilitate
subsequent test programs, a communications  plan should  be developed  that
establishes pre-arranged  reporting times and format, and  insures equipment
compatibility.

      And finally, an at  sea sampling and monitoring operations  plan
must coordinate with all  interested or  associated  government  organizations
such as U. S.  Customs  and the U. S. Coast  Guard.  Uhen properly briefed,
their assistance is most  helpful.

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                   2.  DESCRIPTION OF THE M/T VULCANUS
2.1  VESSEL - GENERAL LAYOUT

     The M/T Vulcanus, originally a cargo ship, was converted in 1972 to a
chemical tanker fitted with two large incinerators located at the stern of
the vessel.  The vessel meets all applicable requirements of the Inter-
governmental Maritime Consultative Organization (IMCO) concerning transport
of dangerous cargo by tanker.  Figure 2-1 shows a picture of the vessel and
Table 2-1 gives some of the ship's specifications.  Both the picture and
the table were furnished by Ocean Combustion Services, B. V., Rotterdam,
The Netherlands, who manage the vessel.

     Because of her size - an overall length of 102 meters, a beam of
14.4 meters, and a maximum draft of 7.4 meters - the Vulcanus is able to
operate worldwide.  Two diesel engines drive a single propeller to give
cruising speeds of 10 to 13 knots.  Her crew numbers 16; ten to operate the
vessel and six to operate the incinerators.

2.2  TANKS AND PUMPS

     In this double-hull, double-bottom vessel, the waste is carried in
15 tanks which lie within the inner hull (Figure 2-2).  The tanks range in
size from 115 to 574 cubic meters (cu m), with the overall waste capacity
being 3,503 cu m.  Tanks are filled through a manifold on deck using a
dockside loading pump.  During normal operation the waste tanks can be dis-
charged only through the incinerator feed system.  There is, however, pro-
vision for discharging the cargo into the ocean if an emergency arises.
The manner in which the piping system is constructed makes it possible for
any tank to be connected to either incinerator and for cargo to be trans-
ferred from one tank to another.

     The space between the two hulls is used for ballast.  Ballast tanks
may be filled with sea water and emptied independently as required to trim
and balance the ship.  Fuel oil is carried in tanks under and in the
engine room.  The engine room is separated from the cargo tanks by double
bulkheads.   The pump room and generator room are situated between the
engine room and the waste tanks.

2.3  INCINERATOR SYSTEM

     Waste is burned in two identical refractory-lined furnaces located at
the stern of the ship.  Each incinerator combustion chamber consists of
two main sections, a combustion chamber and a stack, through which the
combusting fluids pass sequentially (Figure 2-3).  This dual chamber con-
figuration, which is characteristic of most high intensity combustion

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             Figure 2-1.   M/T Vulcanus  -  incineration  vessel

systems,  uses the first chamber for internal  mixing  and  the  second  for
adequate residence time.   Each furnace  has  the following characteristics:
     Overall  Height
     Combustion Chamber
        O.D.
        I.D.
     Stack (Top)
        O.D.
        I.D.
     Combustion Capacity (Max)
     Combustion Air
     Burners  (Saacke Type)
     Volume
     Residence Time:
10.45 meters (m)

5.5 m
4.8 m

3.8 m
3.4 m
12.5 Tonnes/hour
90,000 cu m/hour  (maximum)
3
120 cu m
0.9 sec at 1200°C (calculated)

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TanX No. 6 BB
              Tank No. 5 BB
                          Tank No. 4 BB
                                       Tank No. 3 BB
                                                    Tank No. 2 BB
                                                                   Port
TanX No. 5 Centre  Tank No. 4 Centre  Tank No. 3 Centrd Tank No. 2 Centre
                                                                 Tank No. 1
Tank No. 6 STB| Tank No. S STJ Tank No. 4 STBl  TanX No. 3 STB
               Tank No. 2 STB
                  Figure 2-2.   Tank layout schematic
                                                                   Starboard
             4.6 M
              1.
 10.45 M
              3.5 M
             0.75 M
3.4M.

 I.D.
                                      4.8M

                                      I.D.
                                                                     > STACK
                                   COMBUSTION
                                     CHAMBER
                   Figure 2-3.   Incinerator configuration

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              TABLE 2-1.   SPECIFICATIONS OF THE M/T VULCANUS
      Length overall

      breadth

      Draft, maximum

      Deadweight

      Speed

      Tank capacity

      Number of tanks


      Tank coating



      Loading equipment


      Hose connection


      Safety equipment




      Waste to be processed
      Incinerators

      Incinerator Capacity
101.95 meters

 14.40 meters

  7.40 meters

 4,768 tonnes

 10-13 knots

 3,503 cubic meters (cu m)

15, ranging in size from
115 cu m to 574 cu m

No coating in tanks, pipes, pumps, etc.
All equipment consists of low carbon
steel

Not available, but can be placed on
board, if required

10.2, 15.2, and 20.3 centimeters
(4, 6, 8 inches) in diameter

Specially designed for this task and
in accordance with latest regulations
of IMCO, Scheepvaart-Inspectie (The
Hague)

Must be liquid and pumpable.  May con-
tain solid substances in pieces up to
5 centimeters in size.  Must not attack
mild steel
 up  to  25  tonnes/hour
     Air for the combustion is supplied by large fixed speed blowers with
a rated maximum capacity of 90,000 cubic meters per hour for each incin-
erator.  Adjustable vanes are incorporated in the combustion air supply
system which when deflected, increase system pressure drop and reduce the
flow rate.  Although no instrumentation is installed to monitor air flow
rate, normal operation is stated by the ship's crew to be between 75,000
and 80,000 cubic meters per hour.

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      Liquid wastes are fed to the combustion system by means  of  electrically
 driven pumps.   Upstream of each burner supply pump is a device  (Gorator)
 for reducing the solids in the waste to a pumpable slurry.  The  Gorator
 also acts as a mixing pump by recirculating the waste through the waste
 tank.   Power for the blowers, pumps and other parts of the  incinerator
 system is supplied by two diesel-generators with a total  capacity of 750  KW
 at  440 volts and 60 Hertz.

     Three burners of the  vortex type  are  located  on  the same level at the
periphery of each furnace  near  its  base.   The  burners  are of a rotating
cup, concentric design, which deliver  waste  or fuel  oil  through a central
tube to an atomization  nozzle,  where it meets  high velocity air delivered
through an annul us.  The burners are directed  as shown in Figure 2-4.
       BURNER 6
 BURNER 5
                                             THERMOCOUPLE INDICATORS
                                             (BLACK-BOX AND CONTROL PANEL)
                                             (STARBOARD FURNACE)

                                             THERMOCOUPLE FOR STARBOARD
                                             FURNACE AUTOMATIC SHUT-OFF
                                      BURNER 4
                                      BURNER 3
         BURNER 1
                                              THERMOCOUPLE FOR PORT
                                              FURNACE AUTOMATIC SHUT-OFF


                                              THERMOCOUPLE INDICATORS
                                              (BLACK BOX AND CONTROL PANEL)
                                              (PORT FURNACE)
BURNER 2
   Figure 2-4.  Incineration system  -  burner and thermocouple locations
                                     10

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     Periodically the burners require cleaning.   The burners  are  normally
cleaned one at a time with the remaining two burners firing waste during
the cleaning.  This is easily accomplished because the burners  are readily
accessible.  Each burner has a vertical  pivot or hinge so that  it can  be
swung out of the furnace.   The opening left by this operation is  temporarily
closed by a cover.  The burners are cleaned by a metal tool which is pushed
through the burner.  Three-way valves are utilized on each burner providing
waste feed, fuel oil feed or a shutoff condition.  Waste and  fuel oil  can-
not be valved into a burner simultaneously; however, alternate  burners could
be operated with fuel and waste to achieve higher combustion  temperatures
if necessary.

2.4  RECORDING AND CONTROL EQUIPMENT

2.4.1  Waste Measurements

     The measurement of waste in the tanks during this burn was accomplished
by sounding the depth of waste in each tank with a tape.  In  order to  comply
with U.S. Coast Guard requirements, a new measuring system which is sealed
to prevent vapors from escaping into the ambient air was installed at  the
completion of the burn.

2.4.2  Wall Temperature Measurements

     Temperatures during operation of the incinerators are measured by two
platinum-platinum/10% rhodium thermocouples in each incinerator.  Each pair
is located in a well opposite one of the burners.  One thermocouple is
located approximately 1.3 centimeters from the inside surface of the
refractory lining.  This thermocouple provides temperature information to
the automatic waste shutoff system and is referred to as the "controller"
thermocouple in the Appendix B data tables.  A second thermocouple approxi-
mately 4 centimeters from the inner surface of the firebrick is referred to
as the "indicator" because it provides temperature information to a panel
located in the incinerator control room and to a panel located on the
bridge.  The Appendix B data table refers to the bridge panel as the  "black
box."  In addition, this control panel indicates the day, month and time,
and has lamps which show the burners and pumps are operating.

     The thermocouples used to feed the automatic waste shut off system and
the recording equipment have been quite reliable and durable, according to
personnel of the M/T Vulcanus.  There were no known failures during the
burn covered in this report.

     The possibility of replacing a thermocouple during  a burn was dis-
cussed.  The opinion expressed by the operating  personnel is that  removal
and replacement of a thermocouple in a furnace  is  not feasible while  operating.

2.4.3  Emergency Automatic Waste Shut-off

     For the March 1977 burns, an automatic waste  cut-off system was  used.
This system, called  the Plastomatic 2000  and  supplied by Withoff-Phillips,
Bremen, W. Germany,  uses a thermocouple  controlled,  spring loaded, solenoid
                                     11

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actuated valve which shuts off waste to the burners when the temperature
of the furnace drops below a pre-set selected temperature.   During these
tests the EPA required the shut off temperature to be set at 1200°C.

     If the temperature in a furnace drops below the pre-selected minimum,
a solenoid is de-activated, allowing a spring loaded valve to close, thus
shutting off the flow of waste to the three burners of that furnace.  The
valve which is thus closed shuts the line in both directions.  The waste
pumps are also stopped at this time by cutting off power.  A power failure
or thermocouple burnout in the Plastomatic system would also shut off the
flow of waste to the burners involved.

     A demonstration of the action of the solenoid-actuated valve was set
up by the Chief Electrician and Chief Engineer of the Vulcanus.  A cutaway
model of the valve was set up, the valve opened, and the solenoid activated
electrically.  The valve remained open.  Upon breaking the electrical con-
tact, the spring closed the valve rapidly and positively, preventing flow
in either direction.  The breaking of the electrical contacts simulated the
action of the Plastomatic system if Its thermocouple should Indicate
temperature lower than the one selected at the control panel.  Similarly,
a loss of power would shut off the waste flow to the furnace, and would
prevent backflow of the waste.

     If the system should function,  i.e.,  shut off the waste flow, the pump
which has  been stopped and the valves which have been closed may be
restarted  after the cause has been identified and corrected and after the
Plastomatic has been reset.   It should be noted that procedures require
restart and reestablishment of the desired temperatures using fuel oil
before waste can be burned again.

     As shown in the Appendix B data tables, the thermocouple providing
wall temperature sensing to the automatic shutoff system ("controller"
thermocouple) may also be utilized to Indicate real time wall temperature
measurements.  This is accomplished by adjusting the controller from the
shutoff temperature setting (in this instance, 1200°C) to increasingly
higher temperature settings.  When the adjusted setting is coincident with
the actual  temperature sensed by this thermocouple, the feed valve relay
clicks.   Observation of the pointer location with respect to the temperature
scale on the dial  provides a temperature reading.  The waste shutoff system
is not immediately activated since a time delay is incorporated 1n the
electrical  circuit.  The pointer 1s then reset to the desired automatic
shutoff temperature before the system can activate.  The ability to record
temperatures in this manner is useful in the event that the "indicator"
wall temperature should fail during operation.

2.4.4  Special Equipment

     Certain equipment, not usually found aboard chemical tankers, has been
installed  on the Vulcanus because of Its particular type of operation.  These
items of equipment are:
                                     12

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     Loran and Decca Navigational  Aids:   This  equipment is  needed  in  Euro-
pean waters (Decca)  and United States waters  (Loran)  in order to assure  pre-
cise location of the ship at all  times.   During  the current trip,  Loran
was used to locate and keep the Vulcanus in the designated burn area.

     Anemometer:  This equipment measures the velocity and force of the
wind.  It is therefore useful in selecting an attitude of the ship during
various wind conditions such that the plume may  be directed away from the
ship and its personnel.

     Radio Communication;  The Vulcanus  is equipped with SSB (single side
band) and DSB (double side band) radio for voice and code communication;
MF (medium frequency) and SF (short wave) telegraphy; Marifoon (VHF) (all
channels) for close in voice communication; and Semafoon (a private tele-
phonic communication system).

     Optical Pyrometer;  A portable optical pyrometer was utilized durinq
the test program to measure incinerator flame temperatures.  These measure-
ments were taken periodically (see Appendix B data tables) using a Leeds
and Northrup Optical Pyrometer operating in the 6500 A range.

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                           3.  TEST DESCRIPTION
     This section presents the manner in which the sampling  tests  were
carried out.  It is divided into the following subsections,  listed in
order of discussion:

        •  Operational procedures.

        t  Sampling methods.
        •  Analysis techniques.

        •  Problems encountered.

     The operational, sampling, and analysis procedures were designed  and
selected with consideration given to the nature of the waste.   A prelimi-
nary survey sample of the waste material was acquired and analyzed prior
to the final planning of the shipboard incineration test program.   The
waste was a low-viscosity, low-ash liquid with a gross heating value of
3,860 kcal/kg (6,950 Btu/lb).  Its elemental composition was 30.01 percent
carbon, 4.17 percent hydrogen, 0.012 percent nitrogen, 0.009 percent
sulfur, 62.6 percent halogens (as chlorine), and 3.2 percent oxygen
(by difference).  6C/MS analysis showed the waste to consist nearly
entirely of low molecular weight (2-3 carbons), chlorinated  alkyl  com-
pounds with trace amounts of oxygenated chloroalkyl compounds.  Samples
of the waste material actually burned were taken on board the ship
during the tests and the results of analyzing those samples  are presented
in Section 4.2.1.

 3.1  OPERATIONAL PROCEDURES

     Detailed operating and safety procedures were reviewed  and approved
prior to arrival of the TRW sampling team on board the M/T Vulcanus.
Procedures and operating conditions were also recorded during the actual
tests.  Following are brief summaries of procedures and a test-by-test
commentary on events that took place on the vessel.

3.1.1  Test Procedures

     Sampling was conducted on the starboard incinerator.  Two sample
ports were available for probe insertion; however, safety considerations
ruled out Port #2 (see Figure 3-1).  Port #1, located above a burner and
pointing toward the center of the incinerator, was used to obtain the
combustion gas samples.  During each test several points along this
diameter were sampled since the probe could traverse the stack.
                                    14

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                          PORT NO. 2 LOCATED
                          90° FROM KEEL
                          CENTER LINE
PORT NO. 1  LOCATED
OVER BURNER AND
POINTING TO CENTER
OF INCINERATOR
                  Figure  3-1.  Sampling port locations


     A total  of seven  sampling tests were conducted.  The last test was
for a background while only fuel oil was burned in the starboard incin-
erator.  The basic procedure  for each  test was:

        •  Verify sampling system ready

           -  Fill  first  two  impingers with caustic solution
           -  Fill  last impinger with  silica gel
           -  Leak check  the  system
           —  Fill  impinger box  with ice

        •  Verify on-line instrumentation ready

        •  Start sampling system
                                   15

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        •  Stabilize flow rates and temperatures in sampling  system

        t  Activate on-line analyzer system

        •  Extended sampling duration

           -  Process data acquisition
           —  Effluent gas composition data acquisition

           -  Effluent gas sampling

        •  Shutdown on-line analyzer

        •  Shutdown sampling system

        •  Recover and store samples

     Each sampling test was scheduled to run from three to five hours.

3.1.2  Safety Procedures

     Safety requirements for handling and operating the sampling trains
and ancillary equipment were established and adhered to, including the
fol1owi ng:

        •  Only authorized personnel were permitted in the sampling
           area during a test.

        •  Visual  observation of the test system was maintained at all
           times during tests.

        •  Entry suits and Scot-Paks were available in the immediate
           area.

        •  Safety belts were used when working on the probe or probe
           mount.

        •  Sampling tests were performed only when weather conditions
           were favorable.

     Safety procedures for operations of the Vulcanus crew are contained
in Appendix C.

3.1.3  Test Commentary

     Six sampling tests were conducted during the incineration of the
organochlorine wastes and one background test with fuel oil.  For con-
venience, the waste tests were conducted before the background test.
Before starting waste combustion, the furnaces were heated to operating
temperature by burning fuel oil.  When the preselected temperature had
been reached, the system was switched over to waste.  Because a "cold"
                                    16

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furnace must be heated slowly in  order  to  avoid  cracking  the  refractory
liner, the burners were turned on and off  intermittently,  in  order  to
provide slower and more uniform heating.   After  preheating to operating
temperature, changeover to waste  was accomplished  by switching each burner
successively to waste.  The effect on the  temperature was  small,  a  lowering
of approximately 10-20QC being observed on the thermocouple dial  on the
control panel in the combustion room.

     General observations of the  incinerator operation were noted.   The
typical flame produced by the burners was  bright,  intense white,  free  of
dark areas and free of sputtering.  No  black particulate  matter was
observed above the stack exit. The daytime appearance was one of heat
convection above the incinerator.  At night the  gases above the incinerate:-
were white against the black sky.  Excursions of flames beyond the in  :iii
erator were not observed while waste was being burned. An occasional
vibration was noted in the furnace. This  condition appeared  to be asso-
ciated with burners which were being pushed to capacity.   Backing off  of
the flow rate to the burner appeared to eliminate the condition.   The
phenomenon did not appear to correlate  with any  other parameters, i.e.,
time of day or night, ship, speed, etc.  A continual inspection of the
incinerator burners was maintained by  the Vulcanus personnel.  Burners
were cleaned periodically, usually yielding a black coke  or tar at the
nozzle.  A sample of this was given to  the TRW team.  Appendix D lists
the burner cleaning history.

     On-line gas monitoring data  was obtained during all  tests.   Some
problems were encountered with the analyzer system.  These were corrected
as they occurred and the system functioned well  under the confined and
harsh shipboard environment encountered at sea.   Sampling system mal-
functions precluded obtaining sufficient samples for organic analysis
during the initial three tests (see Section 3.4 for detailed  discussions
of the problems encountered during the sampling and monitoring activities).
These problems were corrected and three subsequent waste burn sampling
tests were conducted.  The duration of these sampling tests was typically
2-1/2 hours each.  In addition, a background sampling test (with the
incinerator burning fuel oil) was also successfully accomplished.

Test I - First Haste Test:  Problems were encountered at the  initiation of
the test.  The large  impinger designed to hold the caustic scrubbing
solution collapsed and forced the test to be terminated after 35 minutes.
Just before the test was terminated, the quartz liner in the  sampling
probe cracked due to a temporary  thermal overload and a new probe was
installed for Test II.

Test II - Second Waste Test:  This test was terminated after  approximately
20 minutes because the smaller glass impingers  (substituted after  the Test I
problem) that were filled with caustic solution became plugged with a white
carbonate precipitate.  The thermal overload of the  probe, experienced dur-
ing Test I, was avoided during this test by careful  control  of cooling flow
rates.
                                    17

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Test  III -Third Waste Test:  The concentration of caustic solution in the
impingers was reduced for this test to prevent the formation of the car-
bonate precipitate, and the test ran smoothly for slightly more than one
hour.  However, the test then had to be terminated because of a large
quantity of sorbent trap resin had passed through a hole corroded in the
resin support screen.

Test  IV - Fourth Waste Test:  This was the first test from which the
sample acquired was of sufficient quantity for organic analysis.  Sampling
was performed for 2.5 hours.  During this test, the sorbent trap operating
temperature was increased from 25°C to approximately 55°-60°C to reduce
the amount of condensation in the sorbent trap module.  The caustic solu-
tions and silica gel in the impingers were changed midway through the
test.  (See Section 3.4.1).   One of the starboard incinerator burners (#5)
was shut off during the first 20 minutes of the test to repair a valve.

Test  V - Fifth Waste Test;  Sampling was performed for 2.5 hours.  Midway
through the test the caustic solution in the impingers was changed.  The
sorbent module was operated at approximately 70°C.  To further reduce the
amount of condensation, the sorbent module was run at a slightly higher
temperature than the previous test.

Test  VI - Sixth Waste Test;   Strong wind conditions existed during this
test.  There was difficulty in keeping the probe stationary and finally
it was tied down.   About 80 minutes into the test the incinerator was
completely shut down for maintenance purposes.  The reason for this com-
plete shut down is unknown; however, this was the only such instance where
a complete shutdown of one incinerator occurred.  Coincident with the shut-
down, all three burners were cleaned.  During the approximately two-hour
delay, the impinger solutions were changed. Total sampling time was 2.5
hours.  After the test was over the probe was removed and the liner was
solvent washed.

Test VII  - Background Test:   A baseline test was performed with fuel oil
to acquire background data on the performance of the starboard incinerator
while burning only auxiliary fuel.  A new probe was installed and a three
hour sample was procured.   About 30 minutes into the test, it was dis-
covered that the incinerator temperature was only about 950°C instead of
1250°C.   Operating temperatures were increased to the normal operating
temperature by increasing the fuel oil feed rate.  The feed rate may have
increased too fast because approximately 1.5 hours into the test, flames
were observed over the rim of the incinerator.  After the test was com-
pleted it was impossible to remove the probe from the incinerator.  It is
believed that when the flames were shooting over the rim of the incinera-
tor the probe became overheated and was bent.  After this test was
completed the incinerator was shut down.  Several hours later, after the
probe had cooled,  it was possible to withdraw the probe from the incinera-
tor.  The probe was then removed and the quartz liner was washed with
solvent.
                                    18

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3.2  SAMPLING METHODS
     Sampling methods used In the tests  were chosen  to cover  two  basic
areas:

        a)   Continuous,  on-line monitoring of gas  composition  to
             determine and follow steady state conditions.

        b)   Collection and concentration of effluent gas products to
             identify and quantify the trace organic species present.

     Gas samples for both of these systems were extracted by the same
probe.   The gases were drawn from the stack area through heat-traced
Teflon lines and then split.  One portion continued on to the portable
laboratory installed on the ship which contained the on-line monitoring
system.  The other portion passed through an organic collection and
concentration system.

3.2.1  Probe and Probe Mount

     The probe was a stainless steel jacketed, water-cooled probe with a
quartz liner and is shown in Figure 3-2.  The liner provided an inert
surface for the sample gas and the cooled, stainless steel jacket
shielded this gas from extreme combustion temperatures in order to quench
any further reactions of the sample constituents.  Further cooling of the
gas was modulated by aspirating an air/water mixture into the space
between the steel jacket and quartz liner.  The probes were approximately
15 feet in length.
                  AIR/WATER MIXTURE RETURN
                  AIR/WATER MIXTURE IN
                  SEA WATER IN

                  SEA WATER RETURN
SEA WATER OUT

      SEA WATER IN
                                                AIR/WATER
                                                MIXTURE OUT
                        OVEN-
       - QUARTZ LINER

  PROBE CROSS SECTION


   QUARTZ LINER
             ..AIR/WATER
            /MIXTURE IN
                     Figure  3-2.   Probe  design  diagram
                                    19

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     The probe was supported and moved by the system shown  schematically
in Figure 3-3 and pictorially in Figure 3-4.   Design features  for this
probe mount are given below:

        1.   The probe tip was positioned into the effluent gas  stream
             by a pneumatic system.   No adjustment was  possible  for
             azimuth and elevation.

        2.   Insertion positioning accuracy was ±0.5 feet by command
             from the control module which was located  on the  deck
             above the bridge.

        3.   The probe mount was attached to  the incinerator flange as
             shown in Figure 3-5.  The outboard end of  the  mount
             assembly was supported on an A-frame from  the  deck.

        4.   Servicing of the probe required  that personnel climb up
             to the probe mount.

        5.   Installation of the probe and mount was done  in port when
             no burning was occurring.
  PROBE BASE
  AND FILTER
                                     FLANGE ON
                                     INCINERATOR
                       PROBE
                   w
        BALL BRG.
                               PROBE CARRIAGE
                                            CONVEYOR
                                            ROLLER
                               A-FRAME
                               SUPPORT
WALL OF
INCINERATOR
           Figure 3-3.  Diagram of probe mount for the Vulcanus
                                    20

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                  PROBE
      CARRIAGE
      A-FRAME
      SUPPORT
                                                   FILTER
                                                   OVEN
                                                NEUMATIC
                                                 DEVICE
            Figure 3-4.   Probe mount with probe fully withdrawn


       6.    The following connections were  incorporated into the probe
            or probe mount:

            a)  Teflon sample line to connect  the probe to the filter
                housing

            b)  Support flanges  for the filter oven

            c)  Seawater coolant lines  for  the probe

            d)  Air coolant lines for the probe

            e)  Thermocouple leads

            f)  Pneumatic lines  for insertion  control  of  the probe

3.2.2  On-Line Gas Monitoring

     A containerized assembly which could be secured on the ship's deck
was prepared for monitoring  the  test burns.  A standard fiberglass rein-
forced plywood (FRP) shipping container was modified to house the on-line
monitoring instrumentation and to serve as  the portable laboratory for
the sampling team.  The container previously had been  in  freight service
                                    21

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             RIM OF
             INCINERATOR
                      0.9
                     METER
                -
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    Figure 3-6.   Portable laboratory location aboard  the M/T  Vulcanus
timbers were necessary so that the container would clear a Butterworth
hatchcover.   The bottom container was used for storage.

     The arrangement of equipment in the portable laboratory is shown
in Figure 3-7.   The on-line gas analyzers were government furnished  and
are described in Table 3-2.  With the exception of the 02 and CO
analyzers, redundant on-line instruments were furnished by EPA.  As
shown in Figure 3-8, on-line monitoring was performed on the gas sample
stream after processing by the gas conditioner.  In addition, because
the Beckman Model 742 02 analyzer would be disabled by HC1 vapors, a
soda lime scrubber for acid gas was utilized in the oxygen analyzer
sample line as shown.  A TRW furnished gas chromatograph  (Carle Model
No. Ill) was included in the gas analysis system to serve as a primary
back-up for the 02 analyses and as a secondary back-up for C02-  This
instrument was slated for use only in the event of failure of the
primary government furnished analyzers.  The continuous on-line monitor-
ing instruments encountered only minor problems which were corrected as
they occurred, therefore the gas chromatograph was not needed during the
tests.
                                    23

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ILtCr. AND
PLUflBIMS
j-eoxct on
THIS
s/eef
    Figure  3-7.   Equipment arrangement in the portable laboratory
            TABLE 3-2.  DESCRIPTION  OF  ON-LINE INSTRUMENTS
Species Analyzed
Hydrocarbons (HC)
Carbon Monoxide (CO)
Carbon Dioxide
(C02)
Nitrogen Oxide
(NO)
Nitrogen Dioxide
(N02)
Oxygen (02)
Mfg. & Model
Beckman 108 A
Beckman 31 5B
Beckman 3 ISA
Beckman 315A
Beckman 255A
Beckman 742
Analyzer Type
FID
IR
IR
IR
UV
Electro-
chemical
Instrument Range
0 - 90% in 8 ranges
0 - 200 ppm, 0 - 2000
ppm, 0-2%
0 - 4%, 0 - 8%, 0 - 15%
0 - 500 ppm, 0 - 2000
ppm
0 - 200 ppm, 0 - 400
ppm
0 - 5%, 0 - 10%,
0 - 25%

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SHIP'S COMPRESSED
 MR SOURCE
T-rr.--^-""\	
I   jr	— I     !    !^   &	
            s -WAY VALVE]
          BLOW
          BACK
          LINE
VENT
            • .   ^ PURGE AIR
            IS \-—/TV.	
      I


      T CONDITIONER
      PPD
           Figure  3-8.  Flow diagram of on-line instrument  system


 3.2.3  Acquisition  of Combustion Products

      The EPA Source Assessment Sampling System (SASS)  was  used  to trap
 and remove the organic vapors from the effluent emissions.   This high
 volume sampling train is  shown schematically in Figure 3-9.   The filter
 and filter oven associated with the SASS sampling train were mounted on
 the sampling probe  assembly.  A heat-traced Teflon line conveyed the
 sample gases from the filter to the solid sorbent trap module.  The
 sorbent module along with rest of the sampling train was located on the
 deck above the bridge.  This sorbent module, located upstream of the
 impingers, contained a bed of XAD-2 resin to trap the organic constituents.
 The module that houses the sorbent trap is temperature controlled  to
 deliver a gas stream as  low as 20°C to the trap.

      Because the  sorbent  material is known to have poor trapping  efficiency
 for low molecular,  high volatility organic species in the C-j to GS range
 (Reference  5),  it  was necessary to^supplement the organic sorbent trap.
 An integrated, composite  grab gas sample was taken, therefore, utilizing
 28-liter Tedlar gas sample bags.  This composite gas sample was taken at
                                     25

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          INCINERATOR
          WALL
                                 TO ON-LINE
                           FILTER   MONITORING
                           HOLDER  EQUIPMENT
   •—=?:
                                          SOLID
                                          SORBENT
                                          TRAP
                                          MODULE
 QUART'. '
 LINER -
                  XAD-2
                  CARTRIDGE
                               CONDENSATE
                               COLLEaOR
                                                - .. „._.  FINE ADJUSTMENT
                                                GAS METER  »Y PASS VALVE

                                                 '•       ' COARSE
ICE «ATH
                                                          ADJUSTMENT
       VACUUM
       LINE
                                                         •HT
                                                      VACUUM
                                                      PUMP
                                              DRY TEST METER
                                    ORIFICE if
                                    MAGNEHEUC GAGE
     Figure 3-9.   Source assessment sampling  system (SASS) schematic
the Beckman  instrument gas conditioner, which minimized sample  alteration
and facilitated  the sampling operation.

      The sampling train was  operated at a flow rate  of approximately 0.085
 cubic  meters per minute  (cu m/m1n).  Gas volumes were measured to 0.03
 liters, with a leak  rate of less than 0.1 I1ters/m1n.   The following
 samples were obtained from  three waste tests and the  background test:

          •  Particulate  filter:  The filters used  1n Tests I,  II,  III
             and VII were removed from the filter housing with  little
             or no  difficulty.   The filters from  Tests IV, V, and VI,
             however,  were stuck to the perforated  metal filter support
             and broke apart  under the slightest  attempt to remove
             them.  A  metal spatula was used  to scrape adhering filter
             material  off the support, but it was not possible  to
             recover it all.   The filters were placed in petri  dishes
             for storage  and shipment.

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       t  Solvent heated line wash:   A pentane rinse  of  the  heat
          traced line connecting the filter housing and  the  sorbent
          trap module was made after each test.  The  rinsate was
          collected in an amber glass bottle with a Teflon-lined
          lid.

       •  Solid sorbent trap:  The canisters were removed from the
          module and placed in glass jars.

       •  Sorbent module washes:  Departures from the original test
          plan were implemented on board the ship for the sorbent
          module trap washing procedure due to the condition of the
          module after the tests.  The surfaces contacting the
          sample gas were coated with a mixture of what appeared
          to  be metal chloride salts, HC1 and water.   The original
          washing sequence of pentane/methylene chloride, isopropyl
          alcohol and pentane was ineffective  in removing the
          surface coatings.  A field decision was made to use rinse
          solvents in the following order  1) water  (which dissolved
          the salt coating), 2)  isopropyl alcohol, 3) pentane/
          methylene chloride, and 4) pentane.  All washings were
          placed in amber glass  bottles with Teflon-lined lids.
          The sorbent module from Test VII (fuel oil  background) was dis-
          assembled after the test and an attempt was made to clean it.
          It  was coated with a heavy layer of what appeared to be iron
          rust.  These deposits  were not removable with any of the
          available solvents aboard ship.  The entire module assembly
          was packed up and  shipped back to the laboratory for further
          inspection and solvent rinsing.
        • Condensate  solution:   The condensates  from the sorbent  trap
          module were  transferred to  amber glass  bottles  with
          Teflon-lined  caps.

        0 Combined  impinger  solutions:   The caustic  impingers were
          combined  and  stored  in amber glass  bottles with Teflon-lined
          caps.

        • Acidified  split  of combined  liquid  impingers:   An aliquot
          of  each  impinger sample was  transferred to a  Nalgene bottle
          and acidified with nitric acid.

        • Spent  silica!  gel:  The spent silica gel was  stored in
          glass  bottles.

        • Three  grab  gas samples:   The Tedlar bags were packed in
          sturdy fiber drums.

     Solvent washes of the quartz Uner were not performed after each
waste burn test due to the delicate and hazardous nature of the operation.
The probe used for Tests II through VI was rinsed with pentane after 1t
was removed.  A rinse of the Test VII (background) probe was also made.
Pentane was  poured Into the quartz Uner Inlet using a funnel  and was
collected from the outlet 1n an amber glass bottle fitted with a Teflon-
lined cap.  The Inclined probe was rotated to Insure solvent contact with
all interior  surfaces of the quartz Uner.
                                    27

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3.3  ANALYSIS TECHNIQUES

     Samples taken as described in Section 3.2 were analyzed for both
organic and selected inorganic constituents.  The techniques used for
the various sample preparation steps are described below, and the anal-
ysis methods are described in the subsequent section.

3.3.1  Extractions .and Sample Preparation

     Samples were removed from the sampling train, stored and prepared
for analysis as described below by sample type.

Probe Washes:  In the laboratory the probe wash samples were inspected
for suspended solids and, seeing none, they were dried over anhydrous
sodium sulfate.  These samples were then measured for volume, a small
aliquot was taken, and the remainder was concentrated down to 10 ml to
be analyzed for organic materials including waste constituents.

Fi1ters:  The filters were not weighed because the 1) loss of filter
material and 2) substantial amounts of crystalline corrosion products
on the filters, precluded any accurate determination of particulate
weight.  Thus particulate mass loadings could not be determined for
these tests.  The filters were, however, extracted for organics with
pentane for 24 hours.  The pentane extracts were dried over anhydrous
sodium sulfate, diluted to volume and an aliquot was taken for storage.
The remainder was concentrated down to 10 ml.

Heated Line Washes:  During laboratory preparation this rinse was
combined with the pentane extracts of the sorbent trap resin into one
sample.

Sorbent Canisters:  Changes in the procedures for extracting and preparing
the contents of the sorbent canisters for analysis were implemented due
to the extensive coating of the resin with corrosion products.  It was
found that pentane, the planned first solvent for extraction, had no
apparent effect on their removal.  Water was found to have good dissolving
power, and it was decided to extract the resin and rinse the canisters
first with water.  The canisters were soaked in deionlzed water to dissolve
the deposits on them, and the resulting liquid was added to the water used
to make the first resin extraction.  This aqueous Soxhlet extraction of
the resin was carried out for four hours.  The resin samples 1n the thimbles
were drained of as much water as possible, and the water extracts were in
turn extracted with pentane using separatory funnels.

     Pentane was added to the Soxhlet extractors to continue the extrac-
tion after the water extract was removed.  However, the immiscibility

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of the pentane with the remaining  water  in  the  resin would  not permit
wetting of the XAD-2 with the pentane.   In  addition, the  pressure  caused
by the pentane column height was not sufficient to  force  the  water through
the siphon tube and cause the extractor  to  "dump".  To  correct this
situation, 50 milliliters of acetone (nanograde) was added  to each
thimble.  The acetone mixed with the water  and  purged the water  from the
resin.  These acetone/water rinses were  transferred directly  into  the
Soxhlet receiving flask, along with the  pentane required  for  the next
extraction step.  The pentane resin extraction  was  then carried  out for
24 hours.

     The pentane extracts of the resin samples  were combined  with  two
other pentane samples:  1) the pentane rinse of the heated lines,  and
2) the pentane extract of the water used to extract the XAD-2 resin.
The combined solutions were dried over sodium sulfate,  an aliquot  was
taken for archival storage and the remainder was concentrated down to
10 ml for organic analysis.

Sorbent Module Washes:  The laboratory preparation  procedures for  these
samples were as follows:

        a)   The water washings were liquid/liquid extracted with
             pentane using a separatory funnel.  The  pentane layer
             was saved for combination with other washings of the
             module.

        b)   The IPA washings were dried over anhydrous sodium
             sulfate and concentrated down to 10 ml.

        c)   The pentane/methylene chloride and neat pentane rinsings
             were combined with the pentane extract of the module
             water wash  (item a).  This solution was dried over sodium
             sulfate and then concentrated down to 10 ml  for organic
             analysis.

     The uncleaned module from Test VII was photographed and washed
sequentially with  IPA,  50/50 pentane/methylene  chloride  solution,  and
finally pentane.  The  rust coating remained after  the rinsings.  The
rinses of the Test VII  module were treated the  same as the other test
samples.

Sorbent Module  Condensates;   In the  laboratory,  the condensates were
neutralized to  pH  7 with sodium hydroxide, and  then extracted with
pentane  in separatory  funnels.  The  pentane extracts were  dried over
anhydrous sodium  sulfate and  concentrated  to 10 ml.

Impinger  Solutions:  No preparation  or  analyses were performed  on either
the  neat  impinger solutions  or  the acidified splits of these samples.
These samples would normally  be analyzed for inorganic constituents;
however,  inorganic analysis was not  required for this  program.
                                    29

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 Silica Gel:   T.'ie spent  silica  gel was  reweighed in the laboratory to
 determine  the amount  of water  absorbed.  The silica gel was then regener-
 ated  for future  use.

 Grab  Gas Samples;   No preparation was  required for these samples.

 3.3.2  Analysis  of  Concentrated Extracts

      The organic samples,  in the form  of 10 ml concentrates, were analyzed
 by  a  combination of qualitative and quantitative techniques.  The quali-
 tative techniques were  selected to generally characterize the major
 organic components  in the  concentrated samples, and the quantitative
 techniques focused  on the  waste constituents and hazardous potential
 by-products.

 Gravimetry:   Aliquots (1-2 ml) of the  10 ml concentrates were evaporated
 in  small glass bottles  at  ambient conditions to remove the solvent.  The
 residues were weighed on a micro-balance.

 Infrared Spectrometry (IR):  The organic residues obtained in the gravi-
 metric determination  were  examined by  IR on a Perkin Elmer Model 521
 Grating Spectrophotometer. When there was sufficient material,  the  sample
 was run  as a  smear  on a salt window.   Smaller quantities were mixed with
 KBr and  pressed  into  a  pellet for analysis.

 Low Resolution Mass Spectrometry (LRMS):  Microgram quantities of the
 sample residue were transferred to a glass probe tip which was,  in turn,
 placed in the batch inlet  probe of a Hitachi RMU 6 magnetic sector mass
 spectrometer.  The  probe tip was ballistically heated from 50° to over
 400°C  and a mass spectrum  was taken every 50°C.

 Gas Chromatography/Mass Spectrometry (GC/MS):  Two instrument systems
 were used for this portion of the analysis.  System 1 was a Finnigan 9500
 gas chromatograph interfaced via a single stage glass jet separator to a
 Finnigan model 3100D  quadrupole mass spectrometer controlled by a System
 Industries, System 250 computer software package.   System 2 was a
 Finnigan 9610 gas chromatograph interfaced via a glass jet separator to
 a Finnigan model 4000 quadrupole mass  spectrometer.  This system is
 controlled by a Data General Nova 3 computer and a Finnigan-Incos soft-
ware package.  The scan cycles and mass ranges varied somewhat between
 systems, but scan cycles were typically 1.8 to 2.0 sec.  Mass ranges
were typically between 20  and 300, but were expanded out to as much as
650 mass units as required.

     The GC column in System 1, used for all the samples, was 3 percent
OV-17 on 100/120 mesh Chromosorb W AW-DMCS.  The oven was programmed
from 20°C to 200°C at 12°C per minute.   Repeat analysis for confirmation
of original data and more details was performed using GC/MS System 2.
Slightly different column  lengths and program rates were used to achieve
similar retention times  with the two instruments.   A Chromosorb 101
                                    30

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column was subsequently used on a limited  number of samples  where  the
initial data indicated that light volatile materials required  better
separation.  The oven was programmed from  125°C to 225°C at  10°C per
minute.

3.3.3  Analysis of Gas Bag Samples

     Although some degradation of the Tedlar bags' nylon fittinqs  had
been observed (see Section 3.4.6), no damage critical to sample integrity
was noticed upon packing the bags for shipment to TRW's Redondo Beach,
California facility nor when they were inspected after arrival. Soon
after their arrival at TRW, the gas bag contents were analyzed directly
by low resolution mass spectrometry (LRMS).  For improved sensitivity,
a  subsequent analysis was  planned  using a  pre-concentration on Tenax/GC
followed by gas chromatography analysis.  In the interim between the
LRMS analysis and Tenax/GC analysis, however, the fittings cracked and
degraded.  The fitting literally fell to pieces.  The bags were resealed
with tape and a new fitting was installed  in each damaged bag.  The
contents of the bag for each test were transferred to new bags and the
Tenax/GC work started immediately.

     Tenax/GC, a porous polymer GC column packing material, was used to
concentrate the trace organic materials in the bag samples.  Liter
quantities of gas from the bags were passed through columns packed with
Tenax.  The Tenax columns were then thermally desorbed and the desorbed
species analyzed by gas chromatography with flame ionization detection
(FID).

3.4  PROBLEMS ENCOUNTERED

     In spite of detailed  planning and preparation for these field tests,
a  few  incidents occurred that  had  not been anticipated.  The main factors
contributing towards these incidents were  the  initial sampling operations
on a shipboard incineration program by the sampling  team and several
components of the sampling system  which were comparatively  new technical
developments with very little  field experience.   The  problems which
occurred  during  the sampling  and monitoring  activities  on  board the
Vulcanus  are  described in  the following paragraphs.

3.4.1  Sampling Train  Impingers

     Sodium hydroxide was  added  to the  sampling  train impingers to scrub
out  the hydrochloric acid  (HC1)  thereby protecting  the  pumps  and  dry test
meter.  The high volume  sampling  train used  in  these tests  as  well as
the  high  concentration of  HC1  in the  effluent  gases (approximately
6  percent), required a large  amount  of  sodium  hydroxide.   In  order  to
accommodate the  sodium hydroxide the  sampling  train was altered to
include a  two  gallon polypropylene bottle containing sodium hydroxide
which  was  installed in the sampling  system between the sorbent module
and  the  impinger system.   Once the first  test was initiated the vacuum
created  in the sampling  system by the pumps  slowly collapsed the  bottle
                                     31

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thereby forcing the solution into the regular impingers.   This problem
was solved by substituting additional glass impingers for the poly-
propylene bottle.

      Before  the main problem was diagnosed 1n the first test, it was
noted that the sampling flow rate was only 0.03 cu m/min.  As a con-
sequence of  this low flow rate, the sample gas coming out of the probe
couldn't be  maintained above 120°C.  In trying to Increase the temperature
of this gas, inadvertently the probe became overheated and the resulting
deformation  caused the quartz liner to crack.  This necessitated changing
the probe before the second test was initiated.

      Fifteen minutes into the second waste test the sample gas flow rate
dropped off  and finally stopped.   The impingers containing the sodium
hydroxide solution were caked with a thick white precipitate.  The carbon
dioxide in the effluent gases had reacted with the concentrated sodium
hydroxide solution to form insoluble carbonate salts.  The original
concept had  been to use a concentrated sodium hydroxide solution (50 per-
cent) so that the impinger solutions would not have to be changed during
the test.  To minimize the precipitate problem the caustic solutions
were  diluted to 10 percent solutions and were changed during the tests.
When  HC1 vapors were detected in the control  module exhaust  (using litmus
paper), the  sampling train operation was stopped so that the caustic
solutions could be changed.  When the caustic solutions were changed,
the last impinger containing the silica gel was also changed.  The silica
gel was used to protect the pumps and dry test meter by removing the
moisture from the gas stream.

3.4.2  Sorbent Module

     The major problems encountered with the operation of the SASS train
were due to the hostile operating environment.  Because the waste was
highly chlorinated (50-70 wt percent halogen as chlorine), the operating
conditions of the incinerators produced an effluent gas which contained
approximately 6 percent hydrogen chloride (HC1).  It was also noted that
during the sampling tests the relative humidity was high (>50 percent)
thereby adding to the moisture content of the effluent gas.  Any con-
densation of the effluent gas produced a very corrosive environment.
The SASS train, with all its stainless steel  components simply was not
designed to operate under these corrosive conditions.

     The main problem with the sampling system was corrosion in the
sorbent module.  This was first noted in Test III.  When the condensate
was first emptied into the drain bottle, there was an appreciable
amount of liquid of a dark green color.  The problem actually surfaced
about one hour into the test when a large amount of resin was detected
in the drain bottle after one of the periodic emptyings of the condensate
reservoir section.   The resin had ended up in the drain bottle because
the acidic environment had corroded a hole in the stainless steel screen
supporting the resin and a considerable portion of the resin had dropped
into the condensate collection section.  Other observations revealed
                                   32

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that the whole module was heavily coated with corrosion products.
Several solvents were used to try to remove these corrosion  products,
however, distilled water proved most successful.

     Originally the sorbent module was intended to be operated at  20°C,
i.e., the effluent gas entering the XAD-2 resin would be at  this tempera-
ture.  During Test III the module had been operated at 25°C.   This was
the lowest temperature that could be obtained.  Because of the corrosion
caused by the large amount of condensation at that temperature, for the
remainder of the sampling tests it was decided to operate the sorbent
module at a higher temperature (55-70°C) in order to try to  reduce or
minimize condensation in the module.  This seemed to reduce  the amount
of condensate which was collected in the drain bottle; however, the
module was still heavily coated with corrosion salts.  Operating the
module at these higher temperatures allowed the train to be  operated long
enough to collect a sufficient sample for organic analysis.

3.4.3  Filter Holder

     In all the sampling tests which involved waste burning, there was  a
problem in trying to remove the filter from the holder.  The filter was
stuck to the support screen and could not be removed in one piece.  In
several instances the filter had to be scraped off the screen.  There
was also evidence of corrosion on both the screen and filter holder.
This problem was not encountered during the background sampling test
when the incinerator was operated on only fuel oil.

3.4.4  SASS Train Control Unit

     The control unit worked very smoothly until the last day of testing.
During the background test (fuel oil) the thermocouple readings became
very erratic.  A hand-held temperature readout device  (API Instrument. Co.)
was used to check the thermocouples.  The results indicated  that the
thermocouples were functioning properly, therefore, for the  remainder of
the test the API instrument was used to obtain the thermocouple readings.

3.4.5  On-line Instrumentation

     A progressive deterioration of performance, i.e., base-line drift,
was noted with the COa analyzer.  Frequent calibration of the analyzer
was required in order to obtain reliable data.  The instrument tended to
stabilize; i.e., return to levels of prior performance, during the final,
background test when there was no HC1 persent.  The NO analyzer caused
some difficulties, especially when trying to "zero" the instrument, but
that anomaly disappeared after one day.  There appears to have been no
day-to-day effect of HC1 on the oxygen analyzer  (semipermeable membrane)
or the hydrocarbon analyzer (flame ionization detector).  The oxygen
analyzer had a soda lime scrubber to remove HC1 which  was effective.
                                    33

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     After observing the dally operation and performance of the
instruments as the test program progressed, there were indications that
HC1 in the combustion gas may have been the source of drift and noise
problems.  The manufacturers of the non-dispersive infrared analyzers
(CO, CO?, and NO) claim that no significant damage will occur to the
materials of construction if the sample containing the HC1 is moisture
free.  In the initial test, when the quartz liner cracked, a moisture
laden sample reached the on-line monitoring system.  Before any further
tests were performed, the complete on-line analyzer system was thoroughly
cleaned and purged with air.  Before the background test was started, the
analyzer system was again thoroughly cleaned and purged with air.  During
this cleaning, moisture was very much in evidence  throughout the system.


3.4.6  Degradation of Gas Bag Fittings

     During the sampling program at sea, it was noticed that the internal
parts of the nylon fittings were beginning to soften or melt as evidenced
by a loss of definition in sharp corners and machined threads, etc.  It is
believed that HC1  in the combustion gases hydrolytically attached to the
nylon to cause polymer chain scission and physical  failure of the part.
No damage was observed on the gas bags for the fuel oil background run
where HC1 was not present.  The fittings were inspected each day, and
it appeared that the attack seemed to stop before the fitting leaked or
could not function.

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                             4.   TEST  RESULTS


     Six sample tests and one background  test  were  run.  The  test results
described in the following sections  include:

        •  Data taken in the field during the  tests.

        •  Data from analysis of the test samples in  the laboratory.

4.1  OPERATIONAL AND FIELD DATA SUMMARY

     Data acquired on board the ship during the tests covered the subjects
of waste feed rates, temperatures in the incinerators, on-line gas  composi-
tion monitoring, plume characteristics, and ambient HC1 levels on the ship's
decks.  Each of these are discussed iim the following sections.

4.1.1  Waste Feed Rate and Mass Emissions

     Time averaged waste feed rates were recorded during the burn period.
These data are shown in Table 4-1.  The time and tank volume data were provided
by the M/T Vulcanus and are  contained  in Appendix A.  Total  incineration
time for the waste was 186 hours  and 45 minutes  during which  time 4100
tonnes of waste were burned.  The average waste  feed  rate was thus approxi-
mately 22 tonnes/hr.  This rate  is  based on the  time  required to deplete
each tank and  on a depth  sounding at the start and end of drawing waste
from the tank.

      The theoretical emission rates of the major stack gas components from
 each furnace were calculated.  Based on an average waste feed of 11  tonnes/hr,
 the elemental composition of the waste,an average excess air of 90 percent,
 and a relative humidity of 80 percent at 29.4°C (85°F).  The resulting
 values were:
                                       Mole Percent in Stack  Gas
      Species    Emission Rate        Net Basis        Dry Basis

        C02       6,160 Nm3/hr           8.20             8.82

        HC1        4,350 Nm3/hr           5.79             6.23
        H20       5,280 Nm3/hr           7.03

        Q£        6,630 Nm3/hr           8.83             9.49

        N2       52,690 Nm3/hr          70.15            75.45

   tor a total  stack gas  emission rate of  75,110 normal cubic meters (at 0°C)
   p^r hour  (Nm3/hr).   The calculations  were  based on the  assumptions that the
   cMorine  present  in  the waste was  converted to  HC1,  the carbon  was converted
   t« C02,  and the  hydrogen  was  converted  to  HC1 and H20.  These assumptions
   have  been  verified by both thermodynamic equilibrium calculations and
   actual measurements,  which indicated  that  HC1 was the  predominant chlorine
   compound  present  and  that CO  was present only at  ppm levels  in  the stack gas
   9! J5e wa£er ^fapor em1tted with  the stack  gas,  approximately 45 percent
   (2,360 Nnp/hr) was due to the presence  of  moisture 1n  the inlet air.  Also.

                                      35

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                      TABLE 4-1.  WASTE FEED RATES
Tank
Number
2C
5C
1
4C
3C
2P
3P'
4P
5P
Volume
(cu m)
562
415
444
425
398
256
232
300
234
Start
Day Hour
3/5
3/7
3/8
3/9
3/10
3/11
3/11
3/12
3/13
2000
0400
0300
0530
0515
0500
1815
0715
0215
End
Day Hour
3/7
3/8
3/9
3/10
3/11
3/11
3/12
3/13
3/13
0400
0300
0530
0515
0500
1815
0715
0215
1415
Time
(cu m)
32
23
26.5
23.75
23.75
13.25
13
19
12
Volume
Burned
(hrs)
558
382
440
396
406
243
221
300
222
Feed
Rate ,
(T/hr)a
22.5
22.0
21.5
21.5
22
24
22
20.5
24
     T • tonne (1000 kg)
 at  90  percent excess air,  the combustion air feed rate was calculated to be
 75,160 m3/hr (wet basis at 25°C), or about 16.5 percent below the maximum
 combustion air feed rate of 90,000 m3/hr.

 4.1.2  Temperature and Residence Time

     Direct flame temperatures were measured 1n the furnaces using a Leeds
and Northrup Optical  Pyrometer, Catalog No. 8621, Serial No. 1009955.
Calibration of this instrument was furnished in a notarized document from
Leeds and Northrup, Houston, Texas, in February, 1977.  This instrument
operates in the 6500 A region using a 500 A band-pass.  It is probable that
the HC1 in the combustion products would not have a large effect on the
validity of the temperature readings from this instrument because the
principal frequency for HC1 absorption is 6 microns (60,000 A).   Any effects
at the operating frequency of 6500 A would be due to 6th or 7th overtones
which would be relatively very weak.

     The data taken by the Chief Engineer of the Vulcanus, comparing the
flame temperatures with the thermocouple-derived wall temperatures is
contained in Appendix B.   This comparison was performed in order to establish
a statistical relationship between wall and flame temperatures.   The desired
result is a correlation between flame and wall temperature such that auto-
matic shut-off of waste to the burners can be triggered from wall tempera-
ture, using a preset value on the automatic shut-off system.  The controller
minimum temperature setting was 1200°C.  The controller is neither locked
nor sealed and  therefore  it is  possible to alter the temperature setting.
                                    36

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     The statistical  correlations between flame temperature  and  controller
temperature for the starboard and port Incinerators  are presented  1n
Figure 4-1 and 4-2 respectively.   These graphs  also  Indicate the variations
1n flame temperature  to be expected at a given  controller  temperature at
different confidence  levels.   For example, to determine the  starboard con-
troller temperature to Insure that flame temperature will  exceed 1300°C at
a confidence level  of 99.9%,  a line 1s first drawn from 1300°C on  the flame
temperature axis horizontally to  Intersect the  lower 99.9% confidence level
line.  Next, from this intersection, a vertical line is drawn downward to
the controller temperature axis,  where a value  of 1180°C 1s  obtained.
This means that if the controller temperature is 1180°C, there is  a  99.9%
probability that the  flame temperature is 1300°C or  higher.   Conversely,
there would be only 1 chance  1n 1000 that the flame  temperature  would be
less than 1300°C if the controller temperature  was 1180°C.

     Figure 4-2 can be used in a  similar manner to determine the relation-
ship between flame temperature and controller temperature for the  port
Incinerator.  This technique  can  be used both to select a given  set  of
flame/controller temperatures for setting the automatic waste shut-off
system and to estimate the probability of having attained adequate flame
temperatures given the controller set temperature.

     The residence time of combustion gas in the furnace can be  calculated
from the stack gas emission rate (discussed in  Section 4.1.1) and  the furnace
volume.  Since the volume of each furnace is 120 m3, the residence time,  t,
for each furnace can be calculated as:

                        .           120       _„
                          " 75.110 v    ~  sec
                             3,600 x 273.16
where T is  the furnace temperature in °K.  The residence times  calculated
are given below:

               Flame Temperature            Residence Time

                     (°C)                         (sec)

                     1100                         1.14

                     1200                         1.07

                     1300                         1.00

                     1400                         0.94

                     1500                        0.89

                     1600                        0.84

                     1700                        0.80
                                    37

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                                                         % CONFIDENCE
                                                        LEVEL
         STARBOARD INCINERATOR
                         1000      1050        1100

                        CONTROLLER TEMPERATURE - ° C
1150
1200
Figure 4-1.  Controller/flame temperature correlation
                  starboard incinerator.
                                38

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    1600
     1500
     1400
     1300
     1200
O
o
 I
Jtf

i
     1100
     1000
                                                                 % CONFIDENCE
                                                                 LEVEL
      900
      800
             900
 950
 1000       1050       1100


CONTROLLER TEMPERATURE - °C
1150
1200
       Figure 4-2.
Controller/flame  temperature  correlation
        port incinerator.
                                        39

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4.1.3  On-line Gas Composition

     Signal outputs from the on-line instruments were recorded on strip
charts and an EsterHne-Angus data logging device which automatically
 printed  out the  millivolt  signal  from each Instrument at two minute inter-
vals.  Data was  recorded during the duration of the operation of the SASS
train.  The monitoring was interrupted only when 1) the SASS train was
shut down or 2)  Instrument calibration checks were made during a test.


     The results of the gas composition analyses, presented in Table 4-2,
were calculated on a dry basis, I.e., the samples were water free when
analyzed and no correction has been made for removed moisture.  The
oxygen values have been corrected for the volumes of C0£ and HC1 which
were removed from the oxygen analyzer sample feed before analysis.  The
range of levels for each species shows the maximum and minimum levels seen
for all valid data points.   The average value is a numerical average of
all valid points.

     The strip chart recordings of the on-line  Instruments were compared
to  logged sampling and monitoring events occurring during the run.  When
a  transient condition was observed on a recording  (an unusually high or
low short term datum point Inconsistent with surrounding data) which cor-
related in time  with a logged, physically observed occurrence, a review
was made of the  probable association between the events.  Data was only
considered nonrepresentatlve of the Incineration process when It was highly
probable that an unrelated event, such as turning on of the sampling  pump,
etc., caused the apparently spurious result.

     A few transient data points occurred each time the sampling system
was started, since material that had condensed in the probe before sampl-
ing was then vaporized and pulled into the gas composition analyzers.
This particularly affected the hydrocarbon and CO analyzers, which read
ppm levels.   Transient "spikes" of CO and hydrocarbons on the strip chart
during start of sampling were therefore not included as representative
data points.  Erratic data near the end of Test I were also eliminated,
because these points occurred after the probe liner had broken and cooling
water entered the sampling system.  A transient "spike" 1n CO and hydro-
carbon data during Test IV was observed when burner #5 was restarted after
replacement of a valve associated with the #5 burner.  Performance of the
Incinerator was improved after this maintenance was completed, as indicated
by an Increase in C02 and decrease In CO measurements.  Both performance
levels were Included in the Test IV data; however, the transient data
during burner restart was deleted.  The wide range of gas composition data
and combustion performance during Test VII, the background test with fuel
oil, resulted because feed rates were varied during the test to increase
temperatures to levels more comparable to the waste tests.
                                    40

-------
                                  TABLE 4-2.   GAS COMPOSITION  DATA SUMMARY
Test
No.
I
II
III
IV
V
VI
VIIcco>] - m, ,00
      Method 3

^Background test  (fuel oil)

-------
      The combustion efficiency is calculated  from the  C02 and CO concen-
 trations of the effluent gases using the following equation:

                                [co-] - [co]
      % Combustion Efficiency = —	   x   100
                                   [C02J
 Based on the data obtained during the  monitoring of  the M/T Vulcanus, the
 average combustion efficiencies  for each  run  ranged  from 99.96 to 99.98
 (Table 4-3).

      EPA Method  3 was  used to  calculate the excess air in the effluent
 gases.  The following  equation is utilized:

                          [02]  -    0.5 [CO]
      % Excess Air =
                      .264  [N2]  -  ([02]-0.5[CO])


The excess air ranged from 60 to 150% and, as seen from Table 4-2, the
average oxygen concentration ranged from 7.4 to 11.7%.

     A summary for etch of the gases measured during the test series is
provided in Table 4-3,  The data entries are based on the two minute
readings for each gas over the entire test series.  This provides the
highest and lowest valid two minute reading observed during any of the
tests, the average reading, the standard deviation and the number of
valid 2 minute readings used.  The'tolerance band provides the range in
2 minute readings which will include 99% of the data with a confidence of
90%.  That is, if all conditions were exactly the same for the incinerator,
feed, etc., in further tests, 99% of the valid data acquired would be
found to lie within the range in 90% of the tests made.  The tolerance
band is based on an assumption of normal population of data.

     The data acquired during Tests IV, V, and VI provide a large sample
for study of Incinerator effluent characteristics.  These three tests
provided data for different days of operation, different tanks of waste,
and several different probe positions.  The tests were sampled extensively
through the water-cooled probe/on-Hne Instrument system, providing data at
two minute Intervals for all 5 gases (Og, C02, CO, NO, volatile hydrocarbons),
The data obtained at the two minute sampling rate was recorded on printed
paper tape.  This tape was corrected before use in the statistical studies.
The correction was made by comparison with the continuous reading strip
chart recorders for each instrument, and log books, to remove the data
transients identified on the strip charts as occurring after Instrument
start-ups or probe adjustments.   The corrected tape thus provides a data
base for a statistical study of probe position effects and time-oriented
furnace performance changes.  A summary of the data base 1s provided for
each of the gases In Figures 4-3,-4, and-5, for the three tests.  Figure
4-6 is a plot of the combustion efficiency versus time for the three tests.


                                    42

-------
             TABLE  4-3.  TEST  DATA SUMMARY  FOR SHIPBOARD INCINERATION TEST SERIES  I-VII
-P.
CO

Minimum
Maximum
Mean
Standard Deviation
Sample Size
Tolerance Band*

Minimum
.Maximum
Mean
Standard Deviation
Sample Size
Tolerance Band3
X CO
.0002634
.006826
.0025470
.001347
220
.0025470
+.0037

.33 x 10"4
.00758
.00278
.00269
55
.00278
+ .008
Test Series
% co2
5.179
12.032
9.223
2.164
158
9.223
+6.033
Test VII
4.946
14.927
9.180
2.422
54
9.180
+7.208
I-VI (Waste Tests)
% 02 % HC
4.027
15.838
10.074
2.117
237
10.074
+5.812
(Fuel Oil
1.799
13.373
7.390
4.032
58
7.390
+11.950
0
.007396
.001467
.001469
192
.001467
+.004056
Control )
0
.007589
.0007475
.001544
60
.0007475
+.004562
% NO
.0007597
.053295
.009913
.009024
229
.009913
+.0248

.0007597
.10764
.03065
.03358
60
.03065
+.09923
% Combustion
Efficiency
99.916
99.997
99.972
.015
158
99.972
+ .042

99.906
99.999
99.974
.025
54
99.974
+ .074
      There  1s  90% confidence that 99% of the 2 minute test readings will  be
      within  this  range.   (A normal distribution 1s assumed).

-------
   o
   L.3
   in.
  o
  o
             o
             03
     PERCENT VOLUME  VS TIME TEST IV
  o
  o
  o
  o
  LNJ..
  O

  O
CM'

O

CJ


 «.o

CMC?

Oo_


Li.
III
..-o
o
  o
  o
  CO
  o
  o
 o
 O


 ID
 o
 o
           C3
            y.oo
il'.SO      10.00
    TIME
11.00
1! .50
12.00
                                                                                   12.5Q
           Figure 4-3.  On-line  gas  composition data -  Test IV, March 9


                                         44

-------
o
o
iyj_.
                           PERCENT VOLUME VS TIME TESTJf
\f>
          "9.00
                         TIMlf
11.50
12.00
         Figure 4-4.   On-Hne gas composition data - Test V, March 10
                                      45

-------
li.
O
O
(-J
                               V.QLUME VS TIME-TEST VI
                         ib.oo    10.'jo
                             TIME
          Figure 4-5.  On-Hne gas composition data  -  Test VI,  March 11


                                        46

-------
  o
  C3
o
  CD
  CD
   •

  CD-
  0)
  oo
  en
  CD_
  en
  r-
  o>
  O)
  (O
O^-i
-»CD
U_CD-




 •

t—

COJ£



CQo>_

ST'

O
  CO

  O)
  O).
  cn
  CM
  CD
  CD.

  CD
  cn
  cn_
  CD
  o
  cn
              COMBUSTION EFFICIENCY MS TIME TESTS IV,  V,  VI
                                                    1*1 .50
12.50
^9.00      9.50       10.00

               TIME
10.50
                                              .00
12.00
        Figure  4-6.
                    Combustion efficiency data - Tests  IV, V, and VI
                    (March 9, 10, and  11, respectively)
                                       47

-------
     The data for combustion efficiency (Figure 4-.6) were next examined for
effects of varying probe position.  To do this, an average combustion ef-
ficiency was computed from the series of readings taken each 2 minutes
while the probe remained at a single position.  This provided a series of
combustion efficiency averages versus probe position for Tests IV, V and VI,
as shown in Figure 4-7.  The numbers adjacent to each point on the graph
indicate the number of 2 minute readings averaged and included in that
particular point.  Figure 4-7 indicates that combustion efficiency was
99.96% or greater except when the probe was less than 40 cm (16 in) from
the incinerator wall.  The 99.92% combustion efficiency calculated at 15 cm
(6 in) from the wall may have been affected by ambient air leakage through
the sampling port around the probe.
yy.w
99.98
OO O7
#
b
LLI
0
U.
ui OO O*\
O
P
i/> OO QA
CO
o
O oo 01

77.92
•
•
A



i
1
1
1
/i
/ •
• TESTV
TEST V
TEST l\

10
• J
/
/
/
t


\ 	
1 — —

S
s




i^^B

y*






^*
r






j!^
,o~*






j-
-*"22<
,-^
4
^••A





	 	
!— ••*"






7*
' 	 13

^2





	 —

<.
\




i































           25    50    75   100   125   150   175   200   225   250   275  300  325   30

                                 SAMPLE PROBE DEPTH, CM


          Figure 4-7.  Combustion efficiency vs. probe position.
     Since the combustion efficiencies plotted in Figure 4-7 were calculated
from the COg and CO measurements at each probe position, the C02 and  CO con-
centrations versus probe position were then evaluated  (Figures 4-8 and 4-9,
respectively).  These data indicate that both C02 and  CO concentrations
varied more from test to test than as a function of probe position, except
for the CO data at 15 cm from the incinerator wall.  CO increased signifi-
cantly when the probe was close to the wall during Test V, as shown 1n
Figure 4-7.  These data suggest that incinerator combustion efficiency
could have been measured with a fixed position probe which extended some
distance greater than 15 cm into the furnace.  All CO/COp measurements
beyond this point yielded efficiency calculations equal to or greater
than 99.9 percent.
                                   43

-------
 12
  11
#
uT
Q
s
6
       • TEST IV'
       • TEST V -
       A TEST VI •
                        JO.
                              i;
                                        28
                                                      12
                                                    13
            1Q
   0     25    50    75    100    125   150    175   200   225    250   275   300    325   350
                                 SAMPLE PROBE DEPTH, CM


           Figure 4-8.   CC^  concentration  vs. probe position
  80


  70


  60


  50


  40



  30


  20


  10
1

ILI
O

§
       • TEST IV

       • TESTV	

       A TEST VI 	
                         A
                         28
            10
          25    50    75
                         100   125    150    175   200   225   250   275    300   325   350
                                  SAMPLE PROBE DEPTH, CM
             Figure  4-9.  CO concentration vs.  probe  position.

                                          49

-------
 4.1.4  Plume Characteristics

      The plume from the Vulcanus was typical of the combustion of an
 organochloride.  Under conditions of high humidity and a fairly strong
 breeze (>6 meters/second), the plume was observed to "touch down"
 100-200 meters downwind of the ship.  This behavior was observed to be
 general over a range of 999 to 1009 millibars (mb), 75-96% relative
 humidity (RH), and 5-17 m/sec wind velocity.

      When the wind velocity decreased below 5 m/sec and the RH fell below
 75-80%, the plume became diffuse, stayed aloft,  and often become Invisible
 At this time the addition of ammonia gas through a standpipe between the
 stacks and at the plane of the stack outlets produced  a visible plume of
 ammonium chloride.   The plume could thus be traced when conditions  pre-
 vented droplet condensation involving HC1  gas.   When the humidity was high
 (I.e., above 75-802) and the wind velocity was low, the plume was voluminous
 white and dense and remained aloft.  Under these conditions, touch  down was '
 not observed for an estimated 5-10 miles.

      The threshold conditions for aerosol  formation for HC1-water vapor
 systems have been studied (Reference 6).  In general,  the requirements for
 visible HC1 droplet formation and growth,  i.e.,  a visible plume, are 78%
 RH minimum, nuclei  of NaCl  or MtyCl of approximately 0.02 y  diameter to
 provide condensation localities,  and HC1 in the  vapor  around the condensing
 droplets.   When water condensation occurs,  a mist will  form  regardless of
 the HC1  concentration in the vapor.  Conversely,  if no condensation of water
 occurs,  no  mist will  form,  even if HC1  is  present in large amounts.   Personnel
 of the M/T  Vulcanus stated  that a visible  plume was always obtained when
 burning  a  European  waste in the North Sea,  as  opposed  to the diffuse
 plume discussed above.   The reasons for this difference are  not obvious
 at this  time.   Analyses  of  the two wastes  showed  the European waste to contain
 5.4%  hydrogen and 40% chlorine, while the Shell'waste  contained 4.2%
 hydrogen and 63% chlorine.   Thus  the  Shell waste would  be  expected  to
 yield combustion products lower in water content  and higher  in  HC1  content
 than  the European wastes.   However, this difference does not necessarily
 completely  explain  the  lack of a  plume in  the Gulf of  Mexico.

 4.1.5  HC1 Measurements on  Board

     Some combinations of wind  velocity, wind direction  and  ship  attitude
 resulted in contact of the  plume with the decks of  the  ship.  Even when
 the plume was not evident,  it was occasionally possible  to detect the
 presence of HC1, both by  its odor and by direct measurements  for  HC1 with
Drager detection tubes.  This behavior  lead  to consideration of atmospheric
conditions and ship-wind combinations which must be  avoided  if  contact of
the plume with the ship is to be minimized.  Table 4-4  lists  these condi-
tions.  The wind forces listed in this table of from 6-17 meters/second
correspond to velocities of 12-34 knots  (1 knot - 1/2 m/s).  Matching  the
ship's speed to a vectored velocity of the wind in the ship's direction
produced a plume which remained aloft and which results  in HC1  values on
the ship of zero.
                                   50

-------
                                  TABLE 4-4.   HYDROGEN CHLORIDE  (HC1)  IN AIR ABOARD VESSEL
en
Date
3/9/77



3/10/77












3/11/77








Time
(see
Moire
1800



0845



1400



1700




1030



1745*




Location
4-n
Main Deck
Combustion
Deck
Stern
Bridge
Combustion
Deck
Main Deck
Bridge
Combustion
Deck
Main Deck
Bridge
Combustion
Deck
Main Deck
Stern
Bridge
Combustion
Deck
Stern
Bridge
Combustion
Deck
Main Deck
Stem
Relative
Humidity
(X)
66X

m
N
821

M
N
86X

H
H
96X

N
H
H
861

H
N
87X

H
II
H
Ship
attitude
055°

M
M
258°

II
H
245°

•
*
235°

M
•
H
080°

H
H
320»*

«
•
H
Wind
Direction-Force
150°-6 m/s

M
H
140°-11 m/s

M
H
150°-10 m/s

H
M
130°-9 m/s

*
•
H
140°-17 m/s

H
N
140**-! 2 m/s

M
H
H
Barometer
(mbl
1012

It
N
1007

N
M
1004

M
H
1002

M
II
H
999

M
H
999

H
H

Cone.
HC1
(Dmri
1.5

1
1
0

4
2
0

2
1
2

6
1.5
0
0

2
4
0

0
0
0
                Captain oriented ship so as to match speed to plume vector 1n ship's direction
                plume high aloft - no HC1 on board

-------
      The various locations where the Drager HC1 samples were taken are
 marked on the plan of the M/T Vulcanus shown in Figure 4-10.  The downwind
 (lee) side of the ship showed HCl-positive data.  No HC1 was detected on
 the windward side.

 4.2  ANALYTICAL RESULTS

      Of the six waste incineration sampling tests, sampling train malfunc-
 tions in the first three tests limited the sampling duration to less  than
 one hour.  Consequently, waste incineration Tests IV, V, and VI, with
 sampling durations in excess of two hours, were selected for the detailed
 laboratory analyses.  In addition, samples acquired from Tests  VII,  the
 background run burning fuel oil alone, were also analyzed as a  baseline
 test for comparison to the waste incineration  tests.   A test and sample
 summary is presented in Table 4-5, and the results from analyzing these
 tabulated samples  are presented and discussed  in this section.

 4.2.1   Waste Feed Analysis Results

      This section presents the results of  the  organic and elemental
 characterization of the representative waste feed samples taken during
 each test.

 4.2.1.1   Organic Constituents

      Neat samples of the blended waste feed (BWF) from each test were
 analyzed  on  a  gas chromatograph equipped with  a flame ionlzation detector
 (FID)  and an OV-17  column (see Section 3.3 for details of the procedure).
 The  chromatograms were  examined and  there  was  a  peak-for-peak,  shoulder-
 for-shoulder match  for  each  sample.  Therefore,  a careful  analysis of
 any  one of the BWF  samples was  applied to  all  of the  representative waste
 feed samples.  The  representative  sample from  Run IV  was  chosen  for the
 detailed  analysis.

     The  composition  of  the  waste  is presented  in Table  4-6.  Qualitative
 identification of the waste  constituents was accomplished  by GC/MS while
quantification was made on the basis of the GC analyses using the flame
ionization detector (FID).  The percentages have been adjusted slightly to
 reflect the fact that trichloropropane was present at 20 percent on the
basis of direct calibration for that compound.    (Trichloropropane is used
as the basis for one of the waste destruction efficiency calculations.
This is discussed in Section 1.)


 4.2.1.2   Elemental  Characterization  and Estimated Emission  Rates

     In order to estimate  the  hourly elemental  emission  from the waste
 incineration, duplicate samples of the Shell waste were  surveyed  for
elemental content.  The waste  samples  from each  day of  testing were first
 blended;  then two aliquots of  this blend were  combusted  over nitric acid
 in a Parr bomb.  The  resulting  solutions were  analyzed  by  spark  source
mass spectrometry (SSMS) which  is a semi-quantative survey  techique.
The major inorganic constituents  (approximately  equal  to  or greater than
500 ppm) were calcium, chlorine, magnesium, phosphorus,  and sodium.
 Other trace elements  found are  reported 1n Table 4-8.   The  average detection
 limit for those elements  not discovered in these waste  samples was 0.5 ppm.
                                     52

-------
Figure 4-10.  HC1  sampling locations
             1) combustion deck 2) bridge 3)  main deck 4)  stern
                                53

-------
TABLE 4-5.  SUMMARY OF VULCANUS SAMPLES
Test Number
Date of Test
Length of Sampling Time (min.)
Volume of Gas Sampled (dry std. m )
Moisture in Gas Sample (vol. %)
SASS Samples Collected
Quartz Probe Liner Wash (PW)
Particulate Filter (PF)
Heat- traced Sample Line
Wash (HLW)
XAD-2 Sorberrt Trap (ST)
Module Trap Hashes
Water (MTW-H^)
Isopropyl alcohol (MTW-1PA)
Pentane (MTW-P)
Pentane/methylene chloride
(MTW-PM)
Module Trap Condensate (Cond)
Contained Liquid Impinders
(01)
Acidified split (CLI-A)
Basic split (CLI-B)
Silica Gel (L4)
Blended Waste Feed (BWF)
Tedlar Bag Samples (GG)
IV
3/9/77
150
12.5
15.2

-
X
X
X

X
X
X
X
X
X
X
X
X
X
X
V
3/10/77
160
13.4
15.4

-
X
X
X

X
X
X
X
X
*
X
X
X
X
X
VI
3/11/77
150
12.1
20.0

X
X
X
X

X
X
X
X
X
X
x ;
X
X
X
X
VII
3/13/77
180
15.8
9.3

X
X
" >
X
X

-
X
X
X
X
X
X
X
X
X
X
                  54

-------
       TABLE 4-6.  REPRESENTATIVE WASTE COMPOSITION BY GC/MS
          Compound
Hole %
1,1-01chloroethane
B1s(D1chloromethyl)ether
l,2-D1chloroethane
1,2-D1chloropropane
1,2-D1chloropropene
Tetrachloroethy1ene
1,1,2-Tr1chloroethane
1,2,3-Tr1chloropropane
2,3-D1chloro-l-propanol
2-Chloroethy1chloroformate
1,2-Bromochlorocyclobutane
1,2,3,4-Tetrachlorobutane
Contains 4 Cl, possibly 1,2,3,3-Tetrachloropropene
Possible 2,3-D1chloro-2-methylprop1onaldehyde
Halogenated, unknown, MM at least 141
2-Bromo-l,2-dlchloropropane
Halogenated, MU at least 189
 4
 7
14
27
11
0.3
 6
19
 3
0.7
0.9
 2
0.5
0.3
0.5
 1
  2
                                 55

-------
                    TABLE 4-7.  CALCULATED APPROXIMATE EMISSION RATES OF INORGANIC ELEMENTS
Element
Lead
Ban' urn
Iodine
Silver
Molybdenum
Zi rconi urn
Strontium
Rubidium
Bromine
Sel eni urn
Arsenic
Gallium
Zinc
Copper
Concentration
in Waste
(ppm)
5-20
10-20
2-4
1-8
10-20
1-5
5-30
0.5-1
5-10
1-5
1-5
0.5-2
10-30
10-30
Calculated
Emission
Rate (kg/hr)
0.1-0.4
0.2-0.4
0.04-0.09
0.02-0.2
0.2-0.4
0.02-0.1
0.1-0.7
0.01-0.02
0.1-0.2
0.02-0.1
0.02-0.1
0.01-0.04
0.2-0.7
0.2-0.7
Element
Nickel
Cobal t
Iron
Manganese
Chromium
Titanium
Scandium
Potassium
Sulfur
Silicon
Aluminum
Fluorine
Boron
Lithium
Concentration
in Waste
(ppm)
10-100
1-5
30-400
1-5
5-200
10-20
0.1-1
-300
30-60
90-100
10-50
10-50
1-10
0.5-2
Calculated
Emission
Rate (kg/hr)
0.2-2
0.02-0.1
0.7-9
0.02-0.1
0.1-4
0.2-0.4
0.002-0.02
~7
0.7-1
~2
0.2-1
0.2-1
0.02-0.2
0.01-0.04
en
01

-------
      Approximate mass emission rates  were  calculated  by multiplying mg/kg
 (ppm) concentrations  by the  average feed rate  of  the  waste  (22,000 kg/hr).
 Thus a metal  present  at 10 ppm in  the waste would be  emitted at approxi-
 mately 0.22 kg/hr.  These calculated  emission  r*ates are also included  in
 Table 4-8.   Emission  rates for the major Inorganic constituents (Ca, Cl,
 Mg, P, and  Na) were ^10 kg/hr.  Total emissions can be estimated by
 multiplying the above rate by the  duration of  the burn.

 4.2.2  SASS Train Sample Analysis  Results

      This section describes  the results of the analysis performed on the
 samples removed from  the SASS train.  Table 4-6 summarizes  the samples
 and their sources.  Direct analysis for known  and expected  waste constitu-
 ents was made by combined gas chromatography/mass spectrometry (GC/MS).
 Additionally, a survey analysis was made wherein  an aliquot of each sample
 extract was evaporated, the  residue weighed, and  qualitative analyses
 made on the residue using infrared (IR) and low resolution  mass spectrom-
 etry (LRMS).   These methods  are described  in Section  3.3.2.

 4.2.2.1   GC/MS Analysis

      Combined gas chromatography/mass spectrometry (GC/MS) was used for
 the direct  analysis of  the appropriate samples for known waste constituents.
 The samples were  the  solvent extracts and/or concentrates of the SASS Train
 components  such as probe  rinses, filters,  line rinses, module rinses and
 sorbent traps.  Two column systems were used:

      a)   Three percent  OV-17  on  Chromosorb W was  used for all samples.

      b)   Chromosorb 101 was  used for more  effective separation of the
          more volatile  species when they were detected using the OV-
          17 column.

      The  results of these analyses showed  that only the samples from the
 sorbent  trap  and the  trap module wastes contained  chlorinated species.
 The  amounts in  the trap module washes were so very much lower compared to
 levels found  in the resin extract that in  summing  these, the final  levels
 for  the module  samples  reported  in Table 4-8 did not change in the one
 significant figure reported.  All four of  the sorbent trap  (ST) samples
 contained chlorinated organics.  This includes the trap extract from the
 background test but the number of chlorinated compounds and their levels
were  very much  less.  Two reasons why the  background trap extract con-
 tained chlorinated species are postulated, 1) contamination during sampling
 and  analysis,  2) residual chlorinated material in  the tanks and lines which
 contained the fuel oil  used  in the background test.   No special efforts
were  made to  identify the source of the chlorinated species found in the
 MV-VII background resin extract.

      The  list of reported compounds include some  that were  not found in the
original waste analysis.  The  source of these materials may be, 1) low
 level waste constituents not  positively Identified in the waste analysis
 (probably less than 0.5% in the waste); 2) unexpected by-products of the
 incineration  process;  or 3) products from  unknown  reactions going on in the
sorbent trap  resin.  No further work was performed to identify the source
of these materials as  it was  considered outside the scope of the analysis
task.
                                    57

-------
TABLE 4-8.  EFFLUENT GAS  CONCENTRATIONS  FROM ANALYSIS OF  SORBENT TRAP
              EXTRACTS
Spectrum
No.a
18
35
41
52
73
89
153
164
184
196

200

213
224

239

247
253
258
266
271
279
295
298
330
345
352
360-362
368

Assignment
C8H18
Dichloropropane
C8H18
C9H20
C10H22
Trichloroethane
Tetrachloroethane b
Trichloropropane
Dichloropropanol
C* Substituted Benzene (e.g.,
di ethyl benzene)
Alkyl, Oxygenated Aromatic MW 164
(e.g. , Butyl Cresol )
03 Substituted Styrene
Unsaturated Chlorinated Hydrocarbon b
MW 2162, Possibly Tetrachlorobutene
C6 Substituted Benzene (e.g.,
Triethylbenzene)
Tetrahydronaphthalene
Cl4 Hydrocarbon MW >258b
Chlorinated Aromatic MW >166b
Naphthalene (or Azulene)
C* Substituted Benzene Mixture
Chlorinated Aromatic b
Chlorinated Aromatic*5
Chlorinated Aromaticb
Chlorinated Aromatic MW >200+b
Dichloro, C4 Substituted Benzeneb
Uichloro, C4 Substituted Benzene b
Dichloro, C5 Substituted Benzenesb
Tetrachloro Cy Substituted Benzeneb
(MW >246)
378 j Trichloro, Alkyl Substituted Benzeneb
, (MW >236)
390 ' Trichloro, Alkyl Substituted Benzeneb

416

1
L_ 1
(MW >236)
Hexachlorobenzene b
Total Chlorinated Organics, mg/m
Total Organics, mg/m
IV
-
-
-
-
-
-
0.09
0.1
0.04
0.6

0.3

0.2
0.1

0.1

0.05
-
0.07
0.8
-
0.02
0.2
0.3
0.2
0.8
0.4
0.1
0.2

0.1

0.2

0.04
3
5
i
V
0.02
0.04
0.04
0.02
0.04
0.06
0.09
0.6
0.04
0.6

0.3

0.3
0.5

0.1

0.04'
0.1
0.1
0.7
-
0.04
0.2
0.4
0.2
0.8
0.5
0.5
0.2

0.2

0.3

0.04
5
10
VI
-
-
-
-
-
_
0.06
0.2
0.04
0.6

0.3

0.2
0.1

0.1

0.04
0.02
0.05
0.8
-
-
0.2
0.3
0.3
1.0
0.5
0.2
0.2

0.3

0.3

0.05
4
6
1
VII
-
-
-
-
-
-
-
-
-
0.2

0.1

0.2
_

0.2

-
-
-
0.5
0.1
-
0.1
0.4
0.05
0.1
0.1
-
-

^

»

-
1
2

             a'Spectrum numbers refer to GC/MS run for MV-V-ST which is shown
              in Appendix E.

              ^Chlorinated compounds not confirmed as being present in the
              waste.
                                        58

-------
     Table 4-8 also presents the summation of chlorinated organics  and
total organics (Including the chlorinated organics)  found in the3resin
extract (ST) samples.  The range of these totals is  1  to 10 mg/m and cor-
responds to destruction efficiencies greater than 99.99%.  These destruction
efficiencies were not reported 1n the summary of this  report since  additional
material may be present in the sample and may not have eluted from  the
chromatographlc column.  This would have lead to erroneously high destruc-
tion efficiency values.

     Table 4-8 contains several compounds which were only partially identified
Into a general class of compound.  There are many reasons why partial identi-
fications can only be made.  Several of the most important are:

     1)  too little component to create a usable spectrum

     2)  unstable molecular ion which provides no molecular weight  information

     3)  similar compounds and isomers which produce virtually identical  spectra

     4)  time and budget limitations on the interpretation of the data


     The lower limit of detectabllity for this analysis was established
using trichloropropane standards.  It was determined that trichloropropane
can confidently be reported when 10 ng are injected  in a 10 microliter
solution volume.  Within the current error limits, this detectabi1ity is
presumed to be valid for all the chlorinated species found in the waste.
All samples were concentrated to 10 ml; therefore, the detection limit is
approximately 0.01 mg for the waste feed constituents.  Even though the
chromatogram for the sorbent trap (ST) extract from the background  test VII
1s not as similar as the other ST samples from waste burns, there still is
enough similarity between them to suggest that similar compounds were
recovered from the sorbent trap regardless of whether the fuel was  waste
or No. 2 oil.  This similarity is shown in gas chromatograms reconstructed
from the 6C/MS data (see Appendix E).  The source of the commonality in
extract composition likely lies in the sorbent resin and/or the manner in
which,it is extracted and prepared for analysis.  No work was performed to
Investigate this situation as 1t was considered outside the scope of the
program.  In like manner, the source of the chlorinated compounds found in
the sorbent resin from Test VII (background) is difficult to explain con-
sidering that fuel oil (typically with low ppm concentrations of chlorine)
was the burner feed.  It is also unlikely that this represents cross-
contamination from the test equipment since a new probe was used and the
sample lines had been flushed with pentane.

      The levels of waste constituent material  found in the sorbent trap
 module washes (MTW) was very much lower than the levels found In the
 sorbent traps.   In fact, the levels do not exceed 0.006 mg/m3 (1 part
 per billion).  These amounts are only about 1 to 2  percent of the  amount
 found in the sorbent traps.   Considering the overall  accuracy of the
 analysis and the number of significant figures 1n the results 1n Table
 4-8  the trace  amounts found 1n the module washes were not tabulated.
 They also do not affect the calculated waste destruction efficiencies.
 GC/MS analysis  of the probe rinse samples found no  waste constituents
 or other chlorinated organics.

                                     59

-------
 4.2.2.2  Gravimetric Analysis

      The gravimetric results,  listed  in Table 4-9  show the distribution
 of nonvolatile organic materials  through  the SASS train.  The majority of
 the material  appeared in  the IPA  module rinse, the first solvent used in
 the series  of rinses.   However, due to the polarity of this solvent, a
 question arose as  to the  possible presence of inorganics in these IPA
 samples. Thus thermal  gravimetric analysis (TGA) were performed which
 showed  20 to  40 percent residues  remaining at 900°C.  On the basis of the
 TGA results,  the IPA samples were assumed to be -70 percent organic on the
 average, and  the values in Table  4-9  were adjusted on that basis.

          TABLE 4-9.    GRAVIMETRIC RESULTS ON ORGANIC SASS SAMPLES
Sample Description
Filter extract, mg
Heat-traced line rinse plus XAD-2
resin extract, mg
Condensate extract, mg
Water module rinse extract, mg
Pentane module rinse plus pentane/
methylene chloride module rinse, mg
Isopropyl alcohol module rinse, mg
Total, mg
Test IV
0.00
320
0.00
0.00
0.00
130b
450
Test V
0.70
110
0.00
0.00
1.4
51 Ob
620
Test VI
0.00
97
1.1
0.00
0.92
480b
580
Test VII
0.00
17
0.01
_a
48
490b
560
a)
  'No sample taken.
  'Values are 70 percent of numbers obtained by gravimetry.  Adjustment
  was made on the basis of TGA data showing the IPA rinses to be
  60 to 80 percent inorganic materials.

     The only other significant source of nonvolatile organics from the
SASS train was the combined XAD-2 resin extracts and heat-traced line
rinses.  In particular, no significant amount of organics were collected
in the filters, water module rinses, or module condensates.   The rinse of
the probe used for the waste tests contained only 6 mg of nonvolatile
organics and the rinse of the background test probe contained no non-
volatile ortanics. The 6  mq  of non-volatile organics  is  especially
insignificant when one considers the volume of gas that passed through
that probe (>50 m3).

4.2.2.3  Infrared Analysis

     The infrared analysis qualitatively identified chlorinated hydro-
carbins in the following  samples:  the sorbent trap module IPA wash  from
Test VI, and the XAD-2 resin extracts  (combined with heat-traced sample
line washes) from Tests IV, V, and VI.  Also present in  the sorbent  trap

                                    60

-------
module IPA wash samples from Tests  V and  VII were  an  inorganic acid and a
hydrocarbon.  The pentane/methylene chloride sorbent  trap module washes
from Tests VI and VII contained a secondary alcohol  (glycol).

4.2.2*4  Low Resolution Mass Spectrometry Analysis

     Samples for LRMS analysis were selected on  the basis of the gravimetric
results.  In general, any sample from Tests IV,  V, VI,  or VII with a
residue weight of 100 n9 or more was analyzed.   The analysis was performed
using the direct Inlet or solids probe technique.  The  analytical details
are found in Section 3.4.2.  The objective of  this kind of  qualitative
analysis 1s to determine 1f there 1s anything  present 1n the samples which,
because of Its functional group composition or compound class, might be
considered hazardous (e.g., chlorinated compounds, polynuclear aromatics,
etc.) and require further examination using more sophisticated methods.

     All compounds discussed in this section were  identified from their
spectral patterns, which must be extracted from  the  other spectral informa-
tion caused by other compounds in the sample.   It  is  therefore possible
that these compound 1ndent1f1cations are not entirely correct  1n every
case.  For example, chlorinated compounds are  usually easy  to  detect due
to the Isotopic pattern of the chlorine atom;  however,  exact compound
Identification can be elusive.

     To summarize the LRMS results, nearly all of the samples  contained
HC1 and H20.  Most of the samples contained a  group  of  materials  that  have
been found as artifacts in the majority of samples from previous  incinera-
tor sampling work.  These ubiquitous materials consist  of phthalic add
esters, hydrocarbon oils, fatty add compounds (soap),  and  glycols.  These
easily identified substances are of little significance 1n  the assessment
of the process performance.  There  were some  aromatic and halogenated
species detected and these are listed in Table 4-10.   Although they were
found mainlv in the sorbent trap extracts, some were also observed  in  the
heated line washings and the module trap washings.  The majority of these
compounds would also be seen and more properly identified  in the GC/MS
analysis of the same unevaporated samples, with  the  exception  of  the benzole
add and the CSQ phenyl compounds.


4.2.2.5  Analytical Recovery for SASS Train  Samples

     Two samples were prepared to determine  the analytical  recovery.   One
milligram of the waste feed was added to an  unused sorbent trap canister.
A water sample doped with  Img of waste feed was also prepared to which HC1
and iron, nickel and chromium salts were added.  This simulated both the
condensate solution and the aqueous sorbent trap module washes.   This
aqueous sample was split and one part was neutralized to pH7 with sodium
hydroxide to simulate the manner 1n which the aqueous samples were treated
In the analysis.  Of the compounds  present 1n the waste, only trichloro-
propane was found in these doped samples by GC/MS analysis.  This is not
                                     61

-------
             TABLE 4-10.  LRMS RESULTS ON ORGANIC SASS SAMPLES
      Sorbent Trap
   Heated Line Wash
  Sorbent Module Wash
   Chlorotoluene

   Dichloro isopro-
   pyltoluene
   Benzoyl chloride

   Benzoic acid

   Butyl  aniline

   C3Q phenyl  compound

   Dimethyl  allene
   phosphom'c  acid

   Mixed  benzoates

   Ethyl  benzaldehyde
Chlorotoluene

A highly fluorinated
chlorobutane (possibly
tetrachlorohexaf1uoro-
butane)
2296
    or Cly compound,
Chlorotoluene

A highly fluorinated
chlorobutane (possibly
techtrachlorohexaf1uoro-
butane)
    or Cly compound
 surprising at  the  levels at which  the control samples were doped. Trichlo-
 ropropane is one of  the major waste constituents, and many of the lesser
 species did not exceed our estimated detection threshold.  Recoveries
 based on trichloropropane are reported  in Table 4-11.


             TABLE 4-11.  ANALYTICAL RECOVERY FOR SASS SAMPLES

Sorbent Trap
Sorbent Module Condensate
Sorbent Module Condensate
Neutralized
Trichloropropane
Added (pg)
200
100
100
Trichloropropane
Found (yg)
220
60
40
Recovery
(Percent)
110
60
40
     Another source of sample loss is that constituents may be lost in
the concentration steps.  These samples were concentrated up to one
hundredfold using the fractional distillation process of a Kuderna-
Danish evaporator.  Any waste constituents which have a higher vapor
pressure than the pentane, acetone or isopropanol solvents will be
preferentially lost.  Moreover, some of the less volatile compounds may
                                     62

-------
be partially lost due to the Incomplete effectiveness  of the  fractional
distillation column.  Any or all  of the sources  of Incomplete sample
recovery may affect any of the samples which were treated.

     The data reported for the sorbent trap extracts In Table 4-8,  were
not corrected for analytical recovery because the sorbent trap recovery
sample yielded more than 100 percent; therefore  no correction was required.
The sorbent trap module wash samples were corrected for 40 percent
analytical recovery, but they still resulted in  the trace levels reported.
It Is stressed that these tables  reflect analytical  recovery  changes  only.
Trapping efficiency for the sorbent traps was derived  from the graphs 1n
Reference 5.

4.2.3  Gas Bag Sample Analysis Results

     Two analytical procedures were used to characterize these samples.

        •  Low Resolution Mass Spectrometry (LRMS) of the neat, as
           received, bag sample.

        t  Concentration of trace constituents using absorption on Tenax,
           followed by desorption and GC analysis.

4.2.3.1  LRMS Analysis

     A portion of a Tedlar bag sample from each of Tests IV through VII
was analyzed by low resolution mass spectrometry for:

        a)   Semi-quantitative composition of the major constituents,
             e.g., 02, N2, C02, HC1, etc.

        b)   Qualitative determination of levels of the chlorinated
             organics known to be present in the waste feed.

     The major constituents are presented in Table 4-12.  Comparison of
the data with that from the on-line analyzers shows fair agreement with
02* C02> and ^.  Though attack and degradation of nylon valves on the

                TABLE 4-T2.  GAS BAG CONSTITUENTS BY LRMS

Test Number
IV
V
VI
VII
Concentration, Mole Percent
H2
<0.001
0.01
0.006
<0.001
H20
0.02
0.03
0.1
0.03
N2/CO
79.3
79.2
79.6
79.7
°2
15.6
15.4
10.8
14.3
Ar
1.1
1.1
1.1
1.1
co2
3.9
4.3
8.4
4.8
HC1
N/D
N/D
N/D
N/D
   N/D = Not  detected.   Limit  of detection was  200 ppm.

                                    63

-------
  Tedlar bags  had  occurred,  this  demonstrates  that  the gas  1n the bag was
  not  ambient  air  resulting  from  leakage or other sample  loss and that the
  bag  sample integrity was adequate  for analysis of residual trace
  chlorinated  organics in the  effluent stream.  The low levels of HC1
  reported  in  the  LRMS data  can be explained by the fact  that the nylon
  fittings  on  the  Tedlar bags  were found to have undergone  hydrolytic
  attack by the HC1.

      A search of the same  data was made for all chlorinated compounds and
  specifically known waste constituents.  However the technique was not
  sensitive enough  to yield  adequate detection limits.  This led to the use
  of the  technique  discusssed  in the following section.

  4.2.3.2  Tenax/GC Analysis

      The results of the Tenax concentration and GC/FID analysis are shown
  in Table 4-13.  Calibration for the waste constituents was performed
  using trichloropropane.  This major constituent of the waste was used as
  a tracer for all  waste constituents.  Waste destruction efficiencies were
 calculated on the basis of trichloropropane analysis results.

      Also presented in the table is a measure of the total organics which
 were detected by the FID.   The levels were calculated from total GC peak
 area integration data.   Response was determined from injections of known
 amounts of organic material.   The ppm values  are reported as methane for
 ease in comparing data  with the on-line hydrocarbon  analyzer data.  These
 levels  should not be considered to  be more accurate  than ±100 percent.
 The destruction  efficiencies  calculated from  the trichloropropane and
 total organic data are  discussed further in Section  1.

                  TABLE  4-13.   GAS BAG ANALYSIS BY  TENAX/GC
Test
IV
V
VI
VII
Trichloropropane
mg/rn3 (ppb)
<0.06 (<9)
0.12 (21)
0.12 (21)

Waste
Destruction
Efficiency3
(DEGGC3C13)
>99.999
>99.999
>99.999

Total Organic
Material
mg/m3
(ppm as Methane)
9 (12)
186 (27)
12 (18)

Total Organic
Destruction
Efficiency
(DEQGHC)
Percent
99.993
99.991
99.991
99.996
a'Based upon trichloropropane as a typical  waste constituent and present
  in the waste at 20 percent (W/W).
                                     64

-------
4.2.4  Burner Head Residue Analysis  Results

     The requirement for routine cleaning of the burner heads  was  frequent
during the incineration of the waste.   There was interest in characteriz-
ing the burner head residue for hazardous constituents  since the residue
Is a potential disposal problem.  A  sample of the residue weighing
51.7 grams was broken up into 10-12  mesh size and extracted  with pentane.

     Several analyses were performed on this sample and the  results
are as follows:

        •  A 1ml aliquot of the concentrate  was evaporated down just to
           dryness and weighed.  The residue amounted to 3.6 weight
           percent of the original burner head sample.

        t  An IR spectrum was obtained of a  smear of the residue and the
           spectrum indicated the presence of hydrocarbons and possibly
           some glycols.  No trace of the waste constituents was found.

        •  The low resolution mass spectrometer (LRMS)  data  indicated
           HC1, trichloropropane, bromodichloropropane and hydrocarbon
           oil.

        •  The burner head extract was also  analyzed by GC/MS.  The
           results show that most of the compounds in the waste feed
           (as seen in the representative waste sample) were also  present
           in this extract.  The GC separated the mixture of the earner
           eluting compounds very effectively, and most of the waste
           constituents were identified.  The second portion of the
           chromatogram consisted largely of incompletely resolved peaks
           constituting a major portion of the total response  seen in the
           chromatogram.  The general character of the compounds in  this
           higher boiling portion of the mixture shown by their spectra
           was  that of aromatic compounds, some of which were  chlorinated.
           Intensive effort to completely separate and identify each
           compound in the mixture was not carried out due to  budget and
           schedule considerations.   Complete quantification is not
           achievable  for an additional  reason, which is that  much of the
           material in the weighed residue discussed above is  likely to be
           polymeric "tars", an unknown portion of which is  not likely
           to elute from a gas chromatograph.  The identified  compounds
           and their calculated concentration  (wt/wt) in the burner head
           scrapings are presented in Table 4-H,  The reconstructed
           chromatogram of this sample is shown in Appendix  E.
                                    65

-------
     TABLE  4-14.   COMPOUNDS  FOUND  IN  BURNER HEAD RESIDUE
       Compound
  Concentration in
Burner Residue mg/kg
Dichloroethane
Dichloropropane
Dichloropropene
Trichloroethane
Trichloropropane
Dichloropropanol
bis(2-chloroethyl)ether
Tetrachlorobutane
         15
         70
         50
         85
        120
        115
         80
         80
                            66

-------
                             5.   REFERENCES
1.  Wastler, T. A., et al.f "Disposal  of Organochlorlne Wastes by
    Incineration at Sea," EPA-430/9/75-014, July 1975.

2.  TRW Report on "Destroying Chemical Wastes in Commercial  Scale
    Incinerators", Contract No.  68-01-2966, Facility Report  No.  1,
    The Marquardt Co., October 1976.

3.  TRW Report on "Destroying Chemical Wastes in Commercial  Scale
    Incinerators", Contract No.  68-01-2966, Facility Report  No.  6,
    Rollins Environmental Services, April  1977.

4.  Federal Register, June 28, 1976,  Part III.   Environmental  Protection
    Agency - Ocean Dumping - Proposed  Revision  of Regulations  and
    Criteria.

5.  Levins, P., et al, "Selection and  Evaluation of Sorbent  Resins
    for the Collection of Organic Compounds," EPA-600/7-77-044,
    April 1977.

6.  Fenton,  D. L., and Renade, M.  B.,  "Aerosol  Formation Threshold for
    HC1-Water  Vapor Systems," Environmental Science and Technology,
    10:1160-62,  1976.
                                   67

-------
                     APPENDIX A



SCHEDULE OF WASTE CONSUMPTION BY TANK NUMBER AND LOCATION
                         68

-------
VO
Tank No. 6 BB
CBM - 112
HT



Tank No. 5 BB
CBM - 117
11 5m Vl 07m5
start 3-13 021=
stop 3-13 1*15
12hrs-24tA
with SB. Tank
Tank No. 5 Centre
CBM - 415
382 m5
start 3-7 04OO
stop 5-8 OJOO
23hrs.-22t/h
Tank No. 6 STI
CBM - 112

Gasoel

Tank No. 4 BB
CBM- 150
142m5+158m5
start 3-12 0715
stop 3-13 0215
19hrs-20.5t/h
•;ith SB.Tank
Tank No. 4 Centx
CBM =• 425
396m5
start 3-9 0530
stop 3-10 0515
ca.24hrs=21,5tA
Tank No. 5 STI
CBM - 117



Tank No. 3 BB
iWiiW
start 3-11 181;
stop 3-12 071;
1.3nrs=22t/h
with SB.Tank
e Tank No. 3 Centre
CBM -398
406m5
start 3-10 0515
stop 3-11 0500
ca.24hrs-22tA
Tank No. 4 STI
CBM =150



Tank No. 2 BB
CBM,= 128,
119mVl24.ni5
start 3-11 0500
stop 3-11 1815
ja.13hrs.524tA
*ith SB.Tank
Tank No. 2 Centre
CBM = 5$2
55Bm5
start 3-5 2000
stop 3-7 0400
32hrs-22,5tA
Tank No. 3 STI
CBM - 116



Tank No. 2 STB
CBM - 128



MTS "VULCANUS "
Vulcanus Shipping Co. P
S INGAPORE

start Heat ins up 3-5- 0800
start Waste Combustion 3-5
stop Waste Combustion 5-13
Tank No. 1 ^v^
CBM •," 444 ^Vj
440m5
start 3-8 0300
stop 3-9 0530
26,5hrs.-21,5t/h ^^

Waste Combust ion-186hrs 45M!
ca.22t/h


Ship
per



TOT
r^RM
i




2 BB




2 CTR




2 ST!




3BB



3CTR



3 ST




4BB



4CT



4ST1




5BB



5CTR



5STB




6BB



6STB




T01AL CBM
5l63m'-ca 4100t.


-,

-------
               APPENDIX B
TABULATION OF TEMPERATURES IN FURNACES BY
a)  Optical Pyrometer (Flame Temperature)
b)  Wall Thermocouples
                    70

-------
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3/5
3/5
3/5
3/5
3/6
3/6
3/r
3/5
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3/5
3/6
3/6
3/6
j zero
i 2100
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I 	 	
i 23CO
! 2400
J01CO
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f> W



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1560
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J! 1120 |1130 | 1200
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;; 1160 11160 ! 1200
jjj 1150 jH5oy 1200




	




	
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   APPENDIX C
SAFETY PROCEDURES
        76

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VULCOS SHIPPIH6 CO. PTL LTD.
            TELEPHONEi «MU
       CABLES : VULCASHIP TCLCX RS 11KO
  VULCANUS SHIPPING CO. PTC. LTD.. SINGAPORE. 1.
                                           «9. ROBINSON MOAD. JRO FLOOM.
                                           •INOAPOME I.
                                     77

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   Before loading!
 1.clean portholes on trunks
 2.check deventing valves and gaugindvalves
 3.check overflow valve XK± manually and plug overflowrtank
 4.inspect pressure/vacuum valve
 5.have emergency firefighting pump tried out with two (2) hoses
 6.check and tr£ out emergency shower next to galley
 7.check if all manifold,charge and discharge valves are closed
 B.chetic if loadingjfilters are clean
 9.operate fireflaps of pumproom,ventilator room and generaterfcoom
10.check on properties of cargo
11.have international shore connection r eady
                                       \^
   At loading place;
 1.check international ship/shore safety check list with shore representative
 2.rig up gangway with net and buoy
 3.rig up firewarps fore and aft
 4.red flag/red light
 5.close scuppers
 6.try out emergency shut-off valve
 7.if required: dip tanks with shore representative
 B.connect two(2) Sr4iighting hoses to the line
 9.put three (3) fire extinguishers near manifold
10.have two (2) safety suits on deck
11.have two (2) safety belts and lines on deck
12.have two (2) self contained breathing apparatus on deck
13.one bucket with lid,containing salted water on deck
14.one eye-washing bottle with distilled water on deck
15.one first aid satchel on deck
16.have enough safety and protective clothing (cleaned) standing by
1?.pressure on emergency shower
18.check if all sharft trunks and butterworth-holes are tightly shut
19.have ship BONDED before connecting
20.connection to be made with at least four (4) bolts.Check.
21.have dripping-pan put under connection
22.check high-level alarm and on
23.have sufficient gasmasks/facenasks with brown fliters(Drager) ready
   Loading;
 1.Contact engine department for OK loading
 2.open "(emergency shut-off valve
 3.open manifold valves
       one
 4.open/,tankvalve and check if cargo is running in the intended tank,then open seer
                                       73

-------
 Durin,? loading;
1.Check tanktevel regularly and maintain xfcnxM connunication with loading-station
2.check high-level alarm regularly

If necessary a gas return line can be connected.

All personnel involved in cargo handling must wear protective clothing,boots,
gloves,helmet and goggles.
As the vessel crust be able to move under its own power,all repairs on the main
engines must be authorized by the Master,Chief Engineer,Port/captain and LoadingBas
General rules on safety will be found in:
Tanker Safety Guide
Petroleum Tankahip Safety.
Both publications are tc be/found in the meeting-room and must not be removed from
                                                                          there.
                                                      The Master,
                                                         i.J.Haverda
                                         79

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l.In order to vent the incineratodroom properly,all ventilators must run


  for at least twenty (20) minutes before starting the incinerators.


  During this time all burners,pumps etc.are blocked by a time relais.


2.If during incineration (gasoil or chemicals) the output of a ventilatun:


  drops (insufficient air flow), a optical and accoustical alarm is given.


  Automatic airpressure controllers are installed on each ventilator.


3.When the flame of a burner goes out,a photo-cell shuts the magnetic valv ;


  before the burner and the flow of the medium is cut.


4.Should during the incineration of chemicals the temperature drop XK&KX belov


  the required level,all pumps will stop and the magnetic valves before the
            y,-,.:•-•'

  burners close..In that case the installation must be preheated again to the


  required temperature by gasoil.


5.In case of emergencies (line failure or similar) the installation can be


  stopped by emergency-switches.These are located:


  on the suLirh  contel desk in the incineration room


  on the bridge


  near both of the two entrances to the incineratorroom on the main deck


  in the crew's accomodation.


  There are five (5) switches in total.


6.There is an alarm system fitted in the bilges of the pumproom.In case of


  line failure in the pumproom,the main discharge valves can be closed from


  the main deck.


7.In case of spillage in the incinerationroom the personnel must immediately


  don gasmasks (drager filter brown).The same applies to entering the pumproce


8.For protection against chemicals protective clothing,gloves and boots


  must be worn.An eye washingshower is situated in the incineration room.


9.The watches change every four hours and are kept by an engineer and an


  aseistent-engineer.The pumproom and the ventilatorroom are checked hourly.


  The incineratorroom ia constantly occupied.3etween this room telephone


  connections exist with the bridge,engineroom,mess-room,pumproom and cabins


  of the engineers.
                                    80

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       APPENDIX D



BURNER MAINTENANCE RECORD
            81

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 3-5   Start with  heating  up  0800  (Gasoel)
       2000 start  with  Waste  combustion.

 3-6   0300-0343 stop Burner  Nr.5.
       0300-0324 clean  Burner Nr.4-5-6.
       0409-0433 clean  Burner Nr.1-2-3-4-5-6.
       1610-1630 clean  Burner Nr.1-2-3-4-5-6.
       2115 Stop Gorator 2 and start Gorator 3.

 3-7   0400-0420 clean  Burner Nr.1-2-3-4-5-6.
       0900-1010 stop PS.Oven rep.Air-Fan.

 3-8   0315-0325 clean  Burner Nr.1-2-3.
       0608-0622 clean  Burner Nr.4-5-6.
       0624-0635 clean  Burner Nr.1-2-3.
       1500-1510 clean  Burner Nr.4-5-6.
       1600-1610 clean  Burner Nr.1-2-3.

 3-9   0202-0213 clean  Burner Nr.4-5-6.
       0638-0650 clean  Burner Nr.1-2-3.
       0718-0731 clean  Burner Nr.4-5-6.
       0950-1020 stop Burner  Nr.5 rep.E.-Valve.
       1747-1757 clean  Burner Nr.4-5-6.

 3-10   0000-0010 clean  Burner  Nr.4-5-6.
       0700-0714 clean  Burner  Nr.4-5-6.
       0714-0739 clean  Burner  Nr.1-2-3.
       1350-1425 stop Burner  Nr.5 change E.-Valve.
       1633-1647 clean  Burner Nr.4-5-6.
       1650-1702 clean  Burner Nr.1-2-3.
       2357-2400 clean  Burner  Nr.4-5-6.
3-11  0000-0010 clean Burner Nr4.4-5-6.
      0010-0021 clean Burner Nr.1-2-3.
      0350-0355 clean Burner Nr.5.
      0615-0628 clean Burner Nr.4-5-6.
      0800-0925 stop Burner Nr.4 rep.Elect.
      1120-1127 clean Burner Nr.4-5-6.
      1345-1355 clean Burner Nr.1-2-3.
      1500-1505 clean Burner Nr.5.
      1720-1725 clean Burner Nr.2.

3-12  0205-0230 clean Burner 4-5-6.
      0230-0246 clean Burner 1-2-3.
      1025-1035 Burner 5 with Gasoel.
      1055-1108 clean Burner 4-5-6.
      1500-1510 clean Burner 4-5-6.
      1730-1742 clean Burner 1-2-3.
      2130-2135 Burner 5 with Gasoel.

-------
3-13  0250-0255 clean Burner 5.
      0609-0620 clean Burner 4-5-6.
      0620-0632 clean Burner 1-2-3.
      0828-1412 SB.Oven with Gasoel  for the Test.  (15t  Gasoel)
      1425 stop PS.Oven.
      1415 stop Waste Combustion.
                                     83

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              APPENDIX E





GC/MS RECONSTRUCTED GAS CHROMATOGRAMS
                 84

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                  21/».I«-1VST  s-»  Dv-17  29-ZBOC I2C M1N 8BBI3
               a    10   a  •»  «   a  0  TB   »   IB  tag  >w  129 iao  i«  iso  i«o iig  i«e
C?'
en

-------
                            IB   m  »   188  118  12B  138  1«  IB  1GB  I1B  198  198  288 218  228  238  »8 288  «8  ZTB
                                                                                                                                 238  3BB a»  328 308  MB
Wat- NMni-er s~» ov-n
                                           108 118  12B  138  l«  ISO  10  170  188  130  288  218
  10   20   30
 a-ETOUl NLMER

-------
                1O1. K*M EXT  S'» CH-n
09
                 IS  2B   3D  K)  SB
                 SPECTTU1 IOBEH

-------
                                TECHNICAL REPORT DATA
                         (Please read Instructions on tlic reverse before completing)
1. REPORT NO.
 EPA-600/2-77-196
                           2.
                                                      3. RECIPIENT'S ACCESSION NO.
4. TITLE AND SUBTITLE
 At-Sea Incineration of Organochlorine Wastes
   Onboard the M/T Vulcanus
                                |5. REPORT DATE
                                 September 1977
                                 i. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
J.F. Clausen, H.J.  Fisher,  R.J. Johnson, E. L.
C.C.  Shih,  R.F. Tobias, and C. A.  Zee	
                          Moon,
                                                      8. PERFORMING ORGANIZATION REPORT NO.
9. f ERFORMING ORGANIZATION NAME AND ADDRESS
 TRW, Inc.
 One Space Park
 Redondo Beach, California  90278
                                10. PROGRAM ELEMENT NO.
                                1AB604
                                11. CONTRACT/GRANT NO.

                                68-01-2966
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: 11/75-12/76
                                14. SPONSORING AGENCY CODE
                                  EPA/600/13
is. SUPPLEMENTARY NOTES IERL-RTP project officer for this report is Ronald A. Venezia,
 Mail Drop 62, 919/541-2547.
16. ABSTRACT
               report describes the incineration of 4100 tonnes of organochlorine
 wastes by the M/T Vulcanus in an EPA-designated burn area in the Gulf of Mexico
 under a special permit granted by EPA Region VI.  The wastes , containing 63%
 chlorine, originated from manufacturing processes.  The incineration process was
 monitored by an industrial field sampling team.   Waste destruction efficiencies
 and total  combustion efficiencies were determined by five methods , each with inde-
 pendent means of sampling, analysis,  and calculation. Incinerator efficiencies of at
 least 99. 9% were observed at waste feed rates of 22 tonnes /hour.  The process was
 carried out at a flame temperature averaging 1535 C and at dwell times calculated
 to be 0. 9 seconds.  An automatic waste shutoff system, incorporated into the incin-
 eration process , was preset to shut down the waste flow if the flame temperature
 dropped below 1200 C.  The temperature of the process was monitoried directly by an
 optical pyrometer for flame temperature , and indirectly by thermocouples which
 measured wall temperature and which were statistically correlated with the flame
 temperature.
17.
                             KEY WORDS AND DOCUMENT ANALYSIS
                DESCRIPTORS
 Air Pollution
 Incinerators
 Ships
 Sea Water
 Chlorine Organic
    Compounds
Waste Disposal
Organic Wastes
Chlorine
Industrial Pro-
  cesses
                                          b.lDENTIFIERS/OPEN ENDED TERMS
Air Pollution Control
At-Sea Incineration
Organochlorine
                                               COSATI Held/Group
13B

13J
08J

07C
07B

13H
13. DISTRIBUTION STATEMENT

 Unlimited
                     19. SECURITY CLASS (This Report}
                     Unclassified
                                                                   21. NO. OF PAGES
                     20. SECURITY CLASS (This page)
                     Unclassified
                                              22. PRICE
EPA Form 2220-1 (9-73)
                                         G8

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