&EPA
United States
Environmental Protection
Agency
Municipal Environmental Research EPA-600/2-78-108
Laboratory May 1978
Cincinnati OH 45268
Research and Development
Kepone
Incineration
Test Program
-------
RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environmental
Protection Agency, have been grouped into nine series. These nine broad cate-
gories were established to facilitate further development and application of en-
vironmental technology. Elimination of traditional grouping was consciously
planned to foster technology transfer and a maximum interface in related fields.
The nine series are:
1. Environmental Health Effects Research
2. Environmental Protection Technology
3. Ecological Research
4. Environmental Monitoring
5. Socioeconomic Environmental Studies
6. Scientific and Technical Assessment Reports (STAR)
7. Interagency Energy-Environment Research and Development
8. "Special" Reports
9. Miscellaneous Reports
This report has been assigned to the ENVIRONMENTAL PROTECTION TECH-
NOLOGY series. This series describes research performed to develop and dem-
onstrate instrumentation, equipment, and methodology to repair or prevent en-
vironmental degradation from point and non-point sources of pollution. This work
provides the new or improved technology required for the control and treatment
of pollution sources to meet environmental quality standards.
This document is available to the public through the National Technical Informa-
tion Service, Springfield, Virginia 22161.
-------
EPA-600/2-78-108
May 1978
KEPONE INCINERATION TEST PROGRAM
by
Bruce A. Bell
Design Partnership
Richmond, Virginia 23226
Frank C. Whitmore
Versar Inc.
Springfield, Virginia 22151
Grant No. R-805112
Project Officer
Richard A. Carnes
Solid and Hazardous Waste Research Division
Municipal Environmental Research Laboratory
Cincinnati, Ohio 45268
This study was conducted
in cooperation with
Commonwealth of Virginia
Department of Health
Richmond, Virginia 23219
MUNICIPAL ENVIRONMENTAL RESEARCH LABORATORY
OFFICE OF RESEARCH AND DEVELOPMENT
U.S. ENVIRONMENTAL PROTECTION AGENCY
CINCINNATI, OHIO 45268
-------
DISCLAIMER
This report has been reveiwed by the Municipal Environmental Research
Laboratory, U.S. Environmental Protection Agency, and approved for publica-
tion. Approval does not signify that the contents necessarily reflect the
views and policies of the U.S. Environmental Protection Agency, nor does
mention of trade names or commercial products constitute endorsement or
recommendation for use.
-------
FOREWORD
The Environmental Protection Agency was created because of increasing
public and government concern about the dangers of pollution to the health
and welfare of the American people. Noxious air, foul water, and spoiled
land are tragic testimony to the deterioration of our natural environment.
The complexity of that environment and the interplay between its components
require a concentrated and integrated attack on the problem.
Research and development is that necessary first step in problem solu-
tion, and it involves defining the problem, measuring its impact, and
searching for solutions. The Municipal Environmental Research Laboratory
develops new and improved technology and systems to prevent, treat, and
manage wastewater and solid and hazardous waste pollutant discharges from
municipal and community sources, to preserve and treat public drinking water
supplies, and to minimize the adverse economic, social, health, and aesthetic
effects of pollution. This publication is one of the products of that re-
search, a most vital communications link between the researcher and the user
community.
The aftermath of the release of large quantities of Kepone to the envir-
onment in Hopewell, Virginia, has resulted in the collection of Kepone and
Kepone-contaminated materials for which a safe, economical, and environ-
mentally acceptable method of destruction is required. The study reported
here presents the results of a pilot-scale study of incineration of Kepone.
Francis T. Mayo, Director
Municipal Environmental Research
Laboratory
iii
-------
SUMMARY
One result of Kepone production operations by the Life Sciences Corpora-
tion in Hopewell, Virginia, has been an accumulation of large amounts of
Kepone and Kepone-contaminated materials that must be disposed of. Work by '
Design Partnership of Richmond, Virginia, under contract to the Commonwealth
of Virginia, has indicated that thermal destruction is the safest and most
convenient way to dispose of these materials. In addition, Rubey and Duvall (1)
have shown that Kepone is thermally destroyed at temperatures on the order of
350° to 400°C but that several thermal degradation products are stable to
temperatures of 900°C.
The Kepone Incineration Test (KIT) program was undertaken to evaluate
incineration as a method of destroying Kepone and Kepone-containing materials
and to determine the range of operating variables required for complete de-
struction. The program, undertaken at the Surface Combustion Division of
Midland-Ross Corporation in Toledo., Ohio, was divided into two phases:
(a) experiments involving the direct injection of low BTU solutions of Kepone
into the afterburner, and (b) experiments involving the co-incineration of
sewage sludge and various amounts of Kepone injected into a rotary kiln.
Each phase was designed so that succeeding experiments involved larger amounts
of Kepone and/or alterations in afterburner temperature and residence time.
The management structure of the KIT program worked well and contributed
much to completion of the program. A committee of representatives from the
federal, state, and local agencies whose responsibilities include air and
water quality was organized and designated the Burn Authority. This group,
which had at least one member on the site at all times during the tests, had
final authority to allow the experiments to continue, to cease, or to be
modified in order to meet the pre-assigned standard that under no circum-
stances would Kepone emission of 1 microgram per cubic meter be reached.
The Burn Authority was aided by the Experimental Management Group, which was
made up of one senior member from each participating contractor. This latter
group had the additional responsibility of conducting the experiments and re-
porting the results to the Burn Authority. The Health and Safety Group saw
that the facility was properly prepared to isolate the contaminated areas and
was responsible both for training all personnel in the use of safety equip-
ment and for monitoring the use of safety equipment. \ The Public Information
Group had the responsibility for keeping the press and the interested public
completely informed as to the program.
The experimental procedures are outlined in Section 5 of this report and
fully treated in Appendix D. The Burn Authority and the Experimental Manage-
ment Group altered procedures when it became apparent that the high-level in-
iv
-------
jection experiments could result in emissions approaching the preset allow-
able limit.
The pertinent experimental results obtained in the KIT program follow.
RESULT OF KEPONE INCINERATION EXPERIMENTS
Experiments
Kepone feed
rate
Total » Stack
feed Total Kepone emission
time fed concentration
(g/min) (min)
(g)
(g/m3)
After-
Total stack burner
output temp.
(g) (°C)
Injection
runs
1
2
3
4
5
Sludge
runs
6+
7
8
- 9
10
11
Totals
Acetic acid
only
1.67 x 10-5
1.67 x 10~5
1.67 x 10~2
1.50
Background
Toledo sludge
only
5.68
, 5.68
5.68
24.2
—
130
135
100
115
120
120
315
240
220
165
—
2.16 x 10~3 ND
2.25 x 10- 3 ND
1.67
172.5
—
— '
1789
1354
1241
3995
8553
ND*
5.35 x ID'8
2.96 x 10~7
ND
1.7 x 10~8
2.4 x 10-8
2.55 x 10-8
2.95 x 10~8
—
1260
ND 1260
ND 1093
ND* 1093
1.76 x 10-4 1093
7.1 x 10~4 1093
ND 1093
1.85 x 10~4 1149
1.85 x 10~4 1093
1.53 x 10~4 1038
1.67 x 10~4 10931
1.58 x 10-3 —
* There was an apparent Kepone peak on the extract from the filter—a peak
that disappeared on base partitioning of the extract.
+ Experiment 6 was run with a contaminated scrubber (25 ppb) in an attempt
to determine the cause of the high emission in the previous experiment.
For each experiment the efficiency of destruction exceeded 99.9999 percent.
Health and safety procedures were adequate in that no individual was exposed
to detectable levels of Kepone, as indicated by before and after blood tests,
and no escape of Kepone into the ambient air was detected by air samplers on
the premises.
The recommendations that derive from these experiments may be summarized
as follows:
(1) The incinerator system should consist of a fume incinerator capable
of sustained operation at about 1000°C and with sufficient volume
v
-------
to allow residence times of about 2 seconds, a pyrolyzer capable
of substained operation at about 450°C to vaporize and (probably)
to decompose the Kepone partially, a strongly basic (pH above 9.0)
scrubber system, and a suitable pollution control system. The
entire system must be designed to operate at a significantly nega-
tive pressure and should be fitted with sensors that detect and
warn when these conditions are not met.
(2) Provision should be made to Jeed solid materials directly into
sludge because the use of acetic acid seems to introduce complica-
tions for large-scale operations. The direct feed of low-BTU
solutions into the. incinerator without the mediation of the pyro-
lyzer should be possible even though the particular combination of
conditions at the experimental site seems to indicate that this is
not a useful approach.
(3) The facility should have a full-time safety engineering group on
its staff. The experience at Midland-Ross suggests that even
though the personnel have been carefully trained in the need for
and the proper use of protective equipment, they need to be re-
minded to use such equipment properly. In addition, the acetic
acid spill that occurred during the KIT program points out the need
for prompt action in the event of an accident—action that can be
properly initiated only by a professional safety engineer.
(4) The incineration system used for the large-scale destruction of
Kepone and Kepone-bearing materials should be separated into areas
that could be heavily contaminated and those areas that could not.
The introduction of protective gear could thus be controlled to
minimize both the equipment needed and the time and efficiency
penalties exacted by its use.
(5) The facility should provide for the retention of all liquid and
solid effluent streams until analysis shows they are not contamina-
ted. In this context, there should be a well designed sampling
arrangement built into the plant and a suitably designed sampling
program. This sampling program should be fully supported by on-
site analytical capability suitable for trace analysis.
(6) For successful operation, a public information program should be
an integral part of the provisions for final disposal.
(7) The KIT program did not include the determination of parameters
for materials used, the precise geometry of a suitable incinerator
system, or even the possible performance penalties exacted by the
use of safety equipment. Such matters were left for later design
studies and should be evaluated.
VI
-------
CONTENTS
Foreword ill
Summary iv
Figures., viii
Tables ix
Acknowledgment x
1. Introduction 1
2. Conclusions 5
3. Recommendations 6
4. Facilities 8
5. Experimental Program and Results 21
References 50
Appendices
A. Kepone fact sheet 51
B. Wipe test protocol and results 54
C. Laboratory equipment and supplies on site 63
D. Experimental procedures 64
E. Furnace and incinerator system data 82
F. Typical chromatograms 122
G. Log of events 130
H. ERA(RTP) confirmatory analysis results and
blood test results 134
vii
-------
FIGURES
Number
Page
1 Program Management Structure 2
2 Kepone Incineration System Schematic 8
3 Experimental Area - Isolation Plan 10
4 Injection Feed Head 13
5 Pneumatic Diagram of Kepone Injection System 14
6 Electrical Network, Feed System Control 15
7 Mix Room 16
8 Calculated Scrubber Load of Kepone as a Function of
Time 11.2 gm/rain. Kepone Feed; AB Temp. 1149°C
(2100°F) 34
9 Calculated Scrubber Load of Kepone as a Function of
Time 5.64 gm./min. Kepone Feed; AB Temp. 1093°C
(2000°F) 35
10 Calculated Scrubber Load of Kepone as a Function of
Time 5.64 gm./min. Kepone Feed; AB Temp. 1038°C
(1900°F) 36
11 Calculated Scrubber Load of Kepone as a Function of
Time 24.2 gm./min. Kepone Feed; AB Temp. 1093°C
(2000°F) 37
12 Kiln Exit Temperature as a Function of Time 11.2
gm. /min. ; AB 1149°C Coincineration 41
13 Kiln Exit Temperature as a Function of Time Feed
5.6 gm./min.; AB 1093°C Coincineration 42
14 Kiln Exit Temperature as a Function of Time Feed
5.6 gm./min.; AB 1038°C Coincineration 43
15 Kiln Exit Temperature as a Function of Time Feed
24.2 gm./min.; AB 1093°C Coincineration 44
viii
-------
TABLES
Number Page
1-1 Results of Kepone Incineration Experiments v
1 Summary of Kepone Incineration Experiments 24
*
2 Summary of Stack Sampling Data 25
3 Summary of Stack Velocity Data 26
4 Stack Kepone Concentration Data for Injection
Experiments 27
5 Stack Kepone Concentration Data for Coincineration
Experiments 28
6 Scrubber Sample Data i 30
7 Combustion Efficiency for Kepone Injection 31
8 Coincineration Efficiency for Kepone with Sewage
Sludge 32
9 Tabulation of Kepone Input and Loss Rates (Scrubber) 38
10 Incinerator Efficiency as Derived from Scrubber Data 40
IX
-------
ACKNOWLEDGMENT
The Kepone Incineration Program could not have been successfully carried
to completion without the full and complete cooperation of the members of the
Burn Authority and the agencies they represent:
E.H. Bartsch, Director, Bureau of Sanitary Engineering,
Department of Health, Virginia
R.A. Carnes, Environmental Scientist, Solid and Hazardous
Waste Research Division, MERL, USEPA
D. Krygielski, Engineer, Toledo Pollution Control Agency
K.J. Klepitsch, Jr., Chief, Solid Waste Branch, USEPA,
Region V
Julius Foris, Chief, Division of Technical Support Operations,
Office of Air Pollution Control, Ohio EPA
We would like to express our appreciation to Richard A. Carnes, USEPA
Project Officer, for his assistance and cooperation throughout this project.
In addition, special thanks are extended to the public officials and the
people of the City of Toledo for their patience and understanding: most
particularly Paul Finlay, Director, Toledo Pollution Control Agency.
x
-------
SECTION 1
INTRODUCTION
The serious environmental contamination produced by the Kepone manufac-
turing operations of Life Sciences Corp., of Hopewell, Virginia, has resulted
in the necessity for the disposal of large quantities of Kepone and Kepone
contaminated water, soil, sewage sludge, and a variety of other materials.
A strong concensus of opinion, supported by a study conducted by Design
Partnership of Richmond, Virginia, has developed that the safest, most econ-
omical and most convenient method of disposal of these materials is by
thermal destruction. This decision is strongly supported by the laboratory
studies of Duvall and Rubey(l) which have shown that Kepone is thermally
unstable at temperatures above 350°C and that even the most thermally stable
of its breakdown or thermal rearrangement products (hexachlorobenzene) is
unstable at temperatures on the order of 900°C.
The general difficulties inherent in the extrapolation of laboratory
scale data to large scale operations made it imperative that an intermediate
(pilot) scale test series be carried out. This pilot scale series would
serve the dual purpose of extending and confirming the Rubey and Duvall^l)
findings, while at the same time define the necessary range of operating
parameters for the safe and complete destruction of Kepone and its products.
The desirable physical arrangement of equipment for these pilot scale tests
would consist of a rotary kiln for volatilization in conjunction with an
afterburner capable of operating at temperatures of the order of 1100°C with
residence times of the order of several seconds. In addition, the installa-
tion should possess adequate air pollution control equipment. A search re-
vealed that such an installation was not available within the Commonwealth,
but that the facility at Midland-Ross, Surface Combustion Division in Toledo,
Ohio was available.
In the course of negotiations with Surface Combustion, it became obvious
that the wide publicity that had been accorded the disastrous effects that
resulted from the exposure of the employees of the Life Sciences Co. had
generated a situation which made it very difficult for the officials of the
City of Toledo and the State of Ohio to grant the necessary permission for
the tests to take place. The result of this concern was an extended series
of meetingswith representatives of the responsible governmental bodies. From
these meetings a detailed plan of operations was evolved that all parties
agreed would allow the necessary tests to be carried out under conditions
that would guarantee the safety of the surrounding community as well as that
of the operating personnel. Specifically, the result of these deliberations
was the generation of a unique management structure which provided the re-
sponsible governmental officials with a strong measure of control of the day-
to-day operations. In addition, a very detailed protocol for the
-------
experimental program was constructed.
PROGRAM MANAGEMENT
After much discussion, the program management structure as outlined in
Figure 1 was evolved as offering the strongest possible control over the
program by both the responsible governmental bodies and by the technical
staff that would be assigned to the program. Briefly, the plan was for the
detailed experiments to be carried out under the direction of the Experimen-
tal Management Group under stringent safety procedures established by and
monitored by the Health and Safety Group. The results of each experiment
were then presented to the Burn Authority along with any necessary additonal
information. The latter group was then empowered to make the decision as to
whether the program should proceed on the basis of the protocol, or should be
modified. The results of each experiment and the resulting Burn Authority
decision were then to be transmitted to the interested public through the
medium of the Public Information Group.
The Burn Authority
The Burn Authority consisted of the following individuals:
E.H. Bartsch, Director, Bureau of Sanitary Engineering,
Department of Health, Virginia
R.A. Carnes, Environmental Scientist, Solid and Hazardous
Waste Research Division, MERL, USEPA
D. Krygielski, Engineer, Toledo Pollution Control Agency
K.J. Klepitsch, Jr., Chief, Solid Waste Branch, USEPA,
Region V
J. Foris, Chief, Division Technical Services, Ohio EPA
In order that the Burn Authority could properly fulfill its responsi-
bilities with respect to the Kepone incineration test (KIT) program while
at the same .time to allow the members to meet their individual agency
responsibilities, it was arranged that at least one member of the Authority
would be in residence at all times. In addition, daily telephone communi-
cation between members of the Authority would be maintained. In those
situations which might suggest that a significant alteration of the protocol
was required, the entire Burn Authority was to be assembled.
Health and Safety Group
The responsibility of the Health and Safety Group began with assistance
in the design of the facilities at Surface Combustion so as to provide maxi-
mum isolation of the facility. Further, this group was to provide for the
personnel safety requirements during operations and the daily monitoring of
personnel and facility to assure that proper hygiene was maintained and that
the required protective measures were, in fact, employed. A further dis-
cussion of the health and safety measures that were undertaken and enforced
is presented in Section 4 of this report. The effectiveness of these
measures is treated in Section 5 and in Appendix B.
-------
u>
HEALTH
AND
SAFETY
BURN
AUTHORITY
EXPERIMENTAL
MANAGEMENT
EXPERIMENTS
PUBLIC
INFO-
FIGURE I PROGRAM MANAGEMENT STRUCTURE
-------
Public Information
The activities of the Public Information Group were primarily directed
to explaining to the interested press and the public the facts of the pro-
gram so as to allay any fears of even a small chance for contamination
resulting from these experiments. During the actual experimental program,
the Public Information Group took the responsibility of releasing a daily
bulletin which outlined the results of that day's experiment and indicated
the nature of the next step in the program. The nature of the general infor-
mation that was made public may be seen by examination of the "Kepone Fact
Sheet" that is included as Appendix A to this report.
Experimental ?-!anagement Group
The responsibilities of the Experimental Management Group, which was
made up of a senior individual from each of the three contractors that par-
ticipated in the program, was charged with the detailed conduct of the exper-
imental program and with the responsibility of keeping the Burn Authority
completely informed of the daily progress. Further, this body was required
to assist the Burn Authority in its deliberations as to the significance of
the results of each specific experiment and as to the propriety of continuing
as scheduled.
GENERAL OBSERVATIONS ON THE OPERATION OF THIS STRUCTURE
In spite of the obvious complexity of the management structure outlined
above, the result was, in practice, highly successful. The dedication of
the members of the Burn Authority in their responsibilities to the public and
their sympathy for the goals of the program, were in no small way responsible
for the successful outcome. The only point at which the management structure
was not particularly successful was in the area of the Experimental Manage-
ment Group. The precise reasons for this problem are not clear, but it would
seem that a troika of technical managers is not the most appropriate way to
manage an experimental program; there should have been one individual
charged with the responsibility subject to inputs from the individual field
managers, and whose final decisions are subject to review by the Burn
Authority.
-------
SECTION 2
CONCLUSIONS
The results and conclusions derived from the KIT program may be summar-
ized as follows:
(1) Coincineration of Kepone with sewage sludge is a safe and environ-
mentally acceptable method of disposal of Kepone. The results of
these experiments indicate that the destruction efficiency of
Kepone is in excess of 99.9999 percent in a system consisting of a
pyrolyzer, fume incinerator operating in the order of 1000°C with
residence times in the order of two (2) seconds and a caustic
quench/scrubber system. In no case was a detectable/Kepone level
found in the pyrolyzer ash.
(2) Periodic deviations from negative pressure in the kiln permitted
the escape of small quantities of Kepone to the air in the kiln
room.
(3) Direct injection of low BTU solutions of Kepone would appear from
these experiments not to be a useful process. This conclusion is
not as firmly based as one would hope as is discussed in Section
5. Although acetic acid appears to be the best and safest
available choice as a Kepone solvent, the addition of acetic
acid to sludge resulted in foaming problems.
(4) Adequate safety instruction coupled with constant monitoring to
assure the proper use of safety equipment is necessary to prevent
the exposure of operatingopersonnel.
(5) The planning of the facility and its isolation structures were such
as to prevent the escape of Kepone into the surroundings while at
the same time making it very easy to clean up the facility after
the completion of the tests.
(6) Real time analyses of Kepone on the site of such a procedure is
highly satisfactory and of great assistance in the decision making
process.
(7) The concept of a Burn Authority made up of representatives of the
responsible agencies is highly satisfactory in the control of an
experiment such as the KIT program.
(8) Only a completely informed public can be cooperative at least in
terms of an experiment such as the KIT program.
-------
SECTION 3
RECOMMENDATIONS
As a result of the KIT program several recommendations may be made that
will be applicable to the operations of a full scale installation for the de-
struction of Kepone and Kepone containing materials.
(1) The incinerator system should consist of a fume incinerator that is
capable of sustained operation at temperatures of the order of
1000°C and with sufficient volume as to allow residence times of
the order of two seconds; a pyrolyzer capable of sustained opera-
tion at temperatures of the order of 450°C which serves to vapor-
ize (and probably to partially decompose) the Kepone; a strongly
basic (pH above 9.0) scrubber system and a suitable air pollution
control system. The entire system must be designed to operate at
a significantly negative pressure and should be fitted with sensors
that detect and warn when these conditions are not met.
(2) Provision should be made to allow feed of solid materials directly
into sludge since the use of acetic acid, which for experimental
purposes was an excellent choice, seems to introduce additional
complications for large scale operations. The direct feed of low
BTU solutions into the incinerator without the mediation of the
pyrolyzer should be possible even though the particular combin-
ation of conditions at the experimental site seems to indicate
that this is not a useful approach.
(3) The facility should have a full-time safety engineering group on
its staff. The experience at Midland-Ross suggests that even
though the personnel have been carefully trained in the need for
and the proper use of protective equipment, they are in constant
need to be reminded to use such equipment properly. In addition,
the acetic acid spill that occurred during the KIT program points
out the need for prompt action in the event of an accident - action
that can only be properly initiated by a professional safety
engineer.
(4) The incineration system that is used for the large scale destruc-
tion of Kepone and Kepone bearing materials should be separated
into areas that are potentially heavily contaminated and those
areas that are not subject to potential contamination. By this
type of separation, the introduction of protective gear can be
controlled so as to minimize the equipment needed. By such a pro-
cedure, it should be possible to minimize the time and efficiency
penalties that are exacted by the use of protective equipment.
-------
(5) The facility should provide for the retention of all liquid and
solid effluent streams until analysis shows that they are not con-
taminated. In this context there should be a well designed
sampling arrangement built into the plant which should be accom-
panied by a suitably designed sampling program. This sampling pro-
gram should be supported by on-site analytical capability suitable
for trace analysis of all samples derived from the system.
(6) A fully informed public is a requirement for the successful oper-
ation of a program of this type. Therefore, a public information
program should be an integral part of the final Kepone disposal
program.
(7) The KIT program was designed to determine the feasibility of incin-
eration for the disposal of Kepone and the range of conditions that
are required to affect this disposal in a safe manner. There was
no serious attempt to determine the proper range of such parameters
as materials that should be used, the precise geometry for a
suitable incinerator system or even the performance penalties that
would be exacted by the use of personnel safety equipment. Such
matters were deemed to be appropriate subjects for the design
studies that would follow the demonstration that Kepone could be
thermally destroyed in a safe manner under thermal conditions that
were reasonable.
-------
SECTION 4
FACILITIES
It Is appropriate to discuss the facilities that were involved in this
program in several categories: (a) the Surface Combustion incineration fac-
ility; (b) the temporary installations that were added to the Surface Com-
bustion facility to provide isolation of the facility and to provide for
personnel safety and hygiene; (c) the facilities that were provided for the
handling of Kepone and Kepone solutions; and (d) the facilities that were
provided for sampling and for real time analysis of the sampled material.
SURFACE COMBUSTION EXPERIMENTAL INCINERATOR
A schematic of the layout of the experimental incinerator at Surface
Combustion is shown in Figure 2. The individual components and their char-
acteristics are discussed in the following section.
Rotary Kiln Pyrolyzer
The rotary kiln pyrolyzer was 1.52 m in diameter and 3.0 m in length
fitted with rotary seal charge and discharge connections so as to minimize
the leakage of gases into or out of the kiln. It was heated directly by the
hot gases from a 0.923 J/sec burner to maintain a nominal temperature of
500°C. Normally this kiln was batch fed through cover doors on the side, but
for the purposes of the coincineration experiments the sludge feed was
accomplished through a water cooled feed line which entered the kiln through
the discharge pipe. The maximum feed rate was a nominal 45 kg/hr (100 lb/
hr). Cake build-up within the kiln was prevented by ten rows of link
chain within the kiln.
Fume Incinerator - Afterburner
The fume incinerator, with a residence chamber volume of 2.4m-^, was
fired by two 0.147 J/sec capacity throat mix burners and an auxiliary gas
supply. The incinerator was equipped with a temperature controller and a
high limit safety shutoff instrument. In this configuration, the maximum
temperature that could be sustained was 1260°C with residence times of the
order of several seconds.
Quench
The hot gases from the incinerator were cooled by evaporative cooling
of the quench water that was injected at the bottom of the incinerator. The
quench system, as well as the emergency cooling spray system, used water de-
rived from the brine tank to compensate for evaporative losses with the
8
-------
STACK
KEPONE
INJECTION
(INJECTION RUNS ONLY)
STACK
SAMPLE
SLUDGE
FROM
FEED
SYSTEM
(SLUDGE
RUNS
ONLY)
KILN
AFTERBURNER
SCRUBBER
SCRUBBER SLOWDOWN
TO CONTAMINATED
STORAGE
FIGURE 2 KEPONE INCINERATION SYSTEM SCHEMATIC
-------
Scrubber
The scrubber, a 76 cm diameter tower, was packed to a depth of 1.83 m
with 5 mm Intalox plastic saddle packing. A liquid distributor at the top
of the packed bed caused the liquid to be evenly distributed across the
packed bed. The mist eliminator consisted of a 15 cm bed of saddles placed
above the liquid distributor. The motive force for gas flow through the en-
tire system was an induced draft fan with capacity of 0.94 m^/sec. mounted
at the top of the scrubber. A recirculation tank at the bottom of the scrub-
ber was interconnected with the quench tank so that they together served as a
single reservoir for recirculating fluids. The pH of the recirculating water
was periodically measured and subsequently adjusted to lie between 9 and 10
by the addition of a 12 percent caustic solution from a separate caustic
solution reservoir.
Sludge Feed System
Kepone contaminated sludge was simulated by the mechanical mixing of
appropriate amounts of Kepone solution in acetic acid into Toledo sludge in
the feed tank. The latter was a cylindrical vessel, 86 cm in diameter and
60 cm high fitted with a pneumatic stirrer. The 10 cm outlet port in the
conical bottom of the feed tank was fitted with a screen and connected to a
two stage, size 3 variable speed Moyno pump. The discharge line was fitted
with a pressure relief valve and with provision to either inject sludge from
the feed tank or water from the mains. The feed line, which entered the kiln
within the kiln discharge line, was water jacketed to prevent caking within
the feed line. At the end of a run, the feed line was flushed with water.
Stack
During the initial injection experiments, there seemed to be a serious
problem with excess water in the stack, so that a new alloy stack was in-
stalled. There was also added a stack reheater which effectively reduced
stack condensation.
HEALTH AND SAFETY FACILITIES
The contributions of the Health and Safety Group to the facilities
consisted largely in the design of the protective enclosure that isolated
the facility and that provided for the protection of the operating person-
nel. The general features of the facility that was provided are shown in
Figure 3.
Operations and Control Area
The Operations and Control Area, which included the incinerator, the
scrubber, the furnace operational equipment and the brine and caustic
storage tanks, was enclosed by a wooded framework lined on the inside with
heavy plastic material. This area was accessible only to specifically
authorized personnel through the normally locked doors and was considered
to be minimally contaminated. Personnel that worked within this area were
required to wear disposable coveralls, rubber boots and rubber gloves. On
10
-------
OBSERVATION
WINDOWS
AMBIENT
^CONTAMINATED V!
V////7///////
OPERATIONS
AND
CONTROL
MINIMAL
CONTAMINATION
yCJ
SHOWER
LOCKER
CLEAN
y
ENTRANCE ONLY
B SERVAT 1 ON
WINDOWS
FIBERGLASS FILTERS
FOR AIR MOVEMENT
AMBIENT
ENTRANCE ONLY
CLEAN
CONTAMINATED
MINIMAL CONTAMINATION
OFFICE
AND
STORAGE
LABORATORY
FIGURE 3'- EXPERIMENTAL AREA-
y
ISOLATION PLAN
y
-------
leaving, it was necessary to remove the protective clothing and wash face and
hands at the sink that was provided at the egress.
Kiln and Mixing Areas
Since it was anticipated that Kepone and Kepone solutions would be
exposed within this area, this was designated as a hazardous area. Per-
sonnel that worked in these areas were required to wear full protective
equipment including respirator. Further, when the operator was handling
glacial acetic acid, he was required, in addition, to wear a face mask. The
only entrance to this area was through the Change/Shower area; the doors
shown to the outside (Figure 3) from the mixing room were emergency doors.
Change/Shower Area
The Change/Shower Area was provided to afford proper isolation of the
facility by maintaining contaminated clothing within the change area and by
making persons exiting from the Mixing/Kiln Area shower before dressing in
street clothes. In addition, all personnel that had been in the Operations
Room were required to shower at the end of the day.
All waste waters from the facility, including from the shower, were im-
pounded in underground tanks fro the duration of the program. Only after
these impounded waters were shown to have undetectable Kepone levels could
they be released into the normal sewage system. In the event that there were
detectable traces of Kepone, these waters were to be placed in drums for
return to Hopewell.
General Features
The walls and the floors of the facility were specially prepared so as
to allow a rapid and safe cleanup at the completion of the program. After
wipe tests were shown to indicate no residual Kepone contamination, the
plastic wall coverings were removed and destroyed. In addition, during the
course of the program, frequent wipe tests were conducted to assure the ab-
sence of Kepone contamination within the various areas if the facility. The
protocol for these wipe tests is discussed in Appendix B. There is also a
summary of the results of the wipe tests included in Appendix B.
FEED SYSTEMS
The experiments that made up the KIT Program were of two general forms,
direct injection of glacial acetic acid solutions of Kepone into the incin-
erator and coincineration of Kepone 'doped1 Toledo sludge injected into the
kiln. The feed equipment used for each is discussed below.
Direct Injection System
The direct injection experiments were designed to study the feasibility
of direct injection of Kepone containing low BTU fluids into the incinerator
without the necessity of the intermediate route through the kiln. The
equipment that was designed for this purpose consisted of a set of two (2)
12
-------
injection nozzles and the facility necessary to mix, store and feed solutions
of Kepone in glacial acetic acid.
It was decided that the injection nozzles should be placed as near to
the input port of the incinerator as was physically possible in order to ob-
viate the possibility of deposition of Kepone on the cool walls of the duct
from the kiln to the incinerator. The thermal conditions that were thought
to exist at the point within the duct at which the injection heads were to
be introduced suggested that the small openings in a conventional spray in-
jection head would soon be clogged. For this reason a less conventional de-
sign, shown in Figure 4, was adopted for these heads. The Kepone solution
was fed through a 5mm diameter stainless tube to the head. The thermal
conditions that were computed to exist within the head were such that vapori-
zation should have occurred within the enlarged portion of the head. The
heads, spaced some 30 cm apart, were directed upstream so as to increase the
exposure time to assure the elimination of droplets.
The feed system that was used for the mixing, storage and feed of the
glacial acetic acid solutions of Kepone is shown in the schematic diagram
Figure 5 with the electrical control system diagram shown in Figure 6. It
will be noted from Figure 5 that the motive force that was used for the
transfer of solutions throughout the system was dry nitrogen gas. The elec-
trical system is somewhat complex, a complexity necessitated by the require-
ment of interlocking the various operations so as to obviate a possible mis-
management of the highly corrosive acetic acid. The corrosive nature of the
solvent also required that all the fittings in the feed system be either of
aluminum, teflon or stainless steel. The physical layout of the feed system
and its associated electrical control system are shown in Figure 7 which also
shows the nature of the portective equipment that was required within the
mixing room.
Sludge Feed System
As is indicated in Section 4 it was decided that the sludge exper-
iments would best be conducted by 'doping' Toledo sludge with Kepone so as
to generate a series of concentrations with a fixed sludge feed rate (45kg/hr)
which was dictated by the kiln characteristics. It was further decided that
personnel protection during the mixing and feed operations could best be
obtained by mixing solutions of Kepone in glacial acetic acid into the sludge
rather than by adding the dry Kepone to the sludge. There is no basis for
concluding that a dry mixing system could not be used in a facility better
equipped. The only significant problem that developed during these mixing
operations was connected with the rather vigorous reaction of the acetic acid
with the sludge, a reaction that caused some foaming to occur.
SAMPLING AND ANALYTICAL PROCEDURES
Sampling Methods
The stack gas stream was sampled at the output of the scrubber using
the EPA Standard Method 5 (2) with an RAG Stacksampler (R) along two perpendi-
cular traverses at four sampling points per traverse. The heated probe was
introduced through each 7.8 cm diameter port in turn and maintained at each
13
-------
SECTION A
RIGHT END VIEW
L- 3.0 _
2.O
WELD
..
r-
WELD
_
IM
^
3.0
.WELD
1.5
-^
*r
>.
^WELO ^^
.50
3.0O
-WELD
-WELD
.266 DIA.EIGHT HOLES EQUALLY
SPACED ON 9.000 01A 8C
I.OO DIA TUBE WELDED IN 1.02
OIA HOLE — SEE NOTE I
.38 DIA TUBE -SEE NOTE I
NOTES:
I. MATERIAL OF 1.00 DIA. TUBE AND
.38 DIA. TUBE -TYPE 304 STEEL
2. TOLERANCES:
3 DEC PLACE TOL * .005
2 DEC PLACE TOL - .010
I DEC PLACE TOL - .10
FIGURE 4 INJECTION FEED HEAD
-------
• TO KILN
CHARCOAL
FIGURE 5 PNEUMATIC DIAGRAM OF
KEPONE INJECTION SYSTEM
-------
FIGURE 6 ELECTRICAL NETWORK, FEED SYSTEM CONTROL
-------
-------
sampling point for approximately five (5) minutes. The collected sample
was passed through a 0.45 micron filter prior to its introduction into the
impinger train. The first two impinger tubes of the sample train contained
100 ml of spectrograde isoctane. The entire assembly of impingers was
maintained at near OoC by use of ice and salt.
Isokinetic sampling was accomplished by first calibrating the S pitot
tube against a calibrated Dwyer pitot tube using a slant gauge manometer.
Minor adjustments were continuously made in the pumping speed as needed to
compensate for variations in air stream velocity during a sampling run or
when the probe was moved to a new sampling point.
On completion of a sampling run, the filter-cyclone assembly was
removed from the heated probe box, transferred to a container and removed to
the laboratory where the sample was recovered. An identical procedure was
followed *-ith th first ind -ecund imp'ng r t be th entire assembly was
removed from the sampling box, transferred to a carrying box and removed to
the laboratory. This procedure was adopted to decrease the possibility of
contamination but was also found to markedly increase the efficiency of
handling the collected samples.
At the end of each stack sampling run, a one (1) liter sample of the
scrubber water was taken. During the high level coincineration runs, further
scrubber samples were taken so as to derive a profile of the changes in
scrubber concentration as a function of time. Ash samples were taken at the
end of each coincineration run.
Analytical Methods
The laboratory that was set up on site and the detailed equipment list
are discussed in Appendix C. Suffice it to say here that the primary instru-
mentation that was used was a Hewlett-Packard Model 5700 series gas chroma-
tograph with a Ni63 electron capture detector. The column that was normally
used was a pyrex column 180 cm by 0.4 cm packed with 5% OV-210 on Gas
Chrom Q, operating with the injection port at 200°C, the column temperature
at 1950C and the detector port temperature at 250°C. The carrier gas used
was a mixture of argon and methane (95% argon) at a flow rate of 45-50 ml/min.
Quantification was made using peak area as determined by a Hewlett-Packard
Model 3380 recorder-integrator. Since the identity of the Kepone was based
on the retention time, numerous authentic samples were injected to assure
proper identity of the Kepone peak.
G.C. retention time was found to "wander" to a greater extent than is
normally observed in the laboratory. It was apparent that the extreme weather
conditions that occurred during these experiments, coupled with the absence
of temperature control in the laboratory (personnel frequently had to work
in the laboratory fully clothed in overcoats, mufflers and gloves), caused
variations in operating conditions of the gas chromatograph. The only ef-
fective control measure that could be taken was the introduction of frequent
authentic samples.
Calibration
As suggested above, the extreme weather conditions at the site during
18
-------
these experiments made it necessary that authentic and known concentration
samples of Kepone be injected on a schedule far more frequently than is nor-
mally the case. In addition, it was found necessary to check the volumetric
calibration of measuring glassware by preparing spiked samples - this also
made necessary because of the abnormal temperatures in the laboratory. As
indicated above, the laboratory was well equipped with primary standards as
well as with secondary working standards of Kepone solutions. The primary
observed variation in the GC records for Kepone was a wandering of the re-
tention time, there was no discernable effect on quantitation of the amount
of Kepone present.
Quality Control Measures
Deliberate duplicates and spiked samples were introduced ad lib as part
of the internal quality control program. In addition, a random number of
method blanks were used with distilled water as the sample. Further, spiked
filters provided by the EPA and spiked water samples provided by the Virginia
Consolidated Laboratory were analyzed. Many of the ambient air filters and
the high volume air monitor filters were split and sent to EPA (RTF) for
confirmatory analysis. Results of these EPA (RTP) confirmatory analysis are
presented in Appendix H.
Laboratory Monitoring and Interferences
As is usual, the laboratory was constantly monitored by an ambient air
monitor on a continuous basis. Further, routine wipe samples were taken at
weekly intervals from the floor, ceiling and laboratory benches. In ad-
dition, at frequent but irregular intervals "clean glassware" was rinsed
in pesticide grade benzene, the washings concentrated and the concentrate
injected into the GC, in order to determine the adequacy of the glassware
washing procedures. No glassware contamination was observed by these tests.
All reagents used in this program were similarily checked for possible Kepone
contamination and for the presence of interferences. At no time during the
experimental program was Kepone detected either in the ambient air filter or
as a contaminant in clean glassware or in reagents.
Sample Handling
Because of the considerable variety of sample types that were treated in
the course of this program, it is appropriate to discuss the initial sample
preparation for each of the following classes of samples:
Filters and Paper Samples
In this category are included stack sample filters, ambient air filters,
high volume air filters and wipe samples (made from a piece of Whatman filter
paper). In the case of the first two, filters were delivered to the labora-
tory in a sealed holder; the wipe samples and the high volume filters were
delivered in sealed envelopes. Each filter was routinely checked for mois-
ture, color, physical change and particle deposition before being handled,
without noteworthy observation. After inspection, each filter was folded
into a cylindrical shape, using clean tweezers, and placed into a 30 ml
19
-------
glass-stoppered graduated centrifuge tube. Measured amounts of benzene (10
ml for stack gas filter and ambient air filter, 50 ml for the others) was
then added to the tube, the hole stoppered and allowed to soak for 10-15
minutes. A 3 microliter aliquot of the extract was injected into the gas
chromatograph. A second sample served as a check on the first.
Scrubber Samples
The one (1) liter scrubber samples were transported to the laboratory
and cooled to room temperature by immersion in cold water. A homogeneous
200 ml sample was then transferred to a 500 ml erlenmeyer flask wherein the
sample was acidified by the addition of 50% l^SO^ dropwise while stirring.
The resulting solution was then transferred to a separatory funnel and ex-
tracted with three successive portion (20 ml each) of benzene. The extracts
were then combined and concentrated by evaporation to 5 ml. A3 microliter
aliquot was injected into the GC for measurement.
Cyclone and Impinger Samples
After the volume of the condensed fluids in the cyclone was measured
and the pH determined, the cyclone assembly was washed with several succes-
sive acetone washings. The combined washings and the collected fluids were
then acidified with 6N HC1 and extracted with benzene. The benzene extract,
after concentration to 5 ml, was injected into the GC in the form of a 3
microliter aliquot for analysis.
The procedure followed for the impinger bottles paralleled that for the
cyclone assembly, the contents of the first and second impinger being com-
bined to form the sample.
Kiln Ash Samples
At the end of each of the coincineration experiments, a sample of the
collected ash was taken for residual Kepone analysis. After the sample was
thoroughly mixed, a 1.00 gram portion was weighed out. This sample was ex-
tracted with 50 ml benzene and the resulting suspension filtered through a
Whatman filter. The filtrate was then concentrated to 5 ml, from which a 3
microliter aliquot was injected into the GC. If there was an indication that
the sample contained Kepone the original material was then extracted on
a soxhlet extractor and again chromatographed.
Additional Sample Cleanup
In some cases, particularly during the coincineration experiments, the
benzene extracts were found to exhibit a large number of chromatographic
peaks, thus making accurate identification of the Kepone peak difficult. In
these cases an additional cleanup step was instituted. The benzene extract
was dried under a gentle stream of nitrogen in a 45 C water bath. The resi-
due was dissolved in 10 ml of 1 N NaOH followed by three successive extrac-
tions with 10 ml portions of hexane. The combined hexane extracts were con-
centrated to 5 ml and analyzed for degradation products of Kepone. The
residual basic solution was acidified with 50% H-SO and extracted with ben-
zene. The benzene extract was then chromatographed for Kepone. On spiked
samples, this method of base-partitioning has shown Kepone recoveries of
better than 90%.
20
-------
SECTION 5
EXPERIMENTAL PROGRAM AND RESULTS
EXPERIMENTAL PROGRAM
The toxicity of Kepone and the nature of the publicity associated with
the aftermath of the Hopewell incident made it essential that every safe-
guard be taken to prevent any exposure of the people of Toledo to unburned
Kepone. The measures taken in this regard may be summarized here as follows:
1. The absolute imposition of an upper limit on the allowed emission,
established as one microgram per cubic meter at stack conditions.
2. The careful sampling of the stack during all periods of Kepone
injection into the furnace system.
3. Use of high-volume air samplers at various locations on the Midland-
Ross property; these samplers to be in use during the entire experi*
ment.
4. The entrapment and entrainment of all waters generated within the
facility so that no discharge of Kepone to the environment could
occur through this route.
5. Provision of essentially real time analysis of all stack samples so
as to assure .that the stack levels did not exceed the 1.0 ygm/mr
limit.
6. The use of an experimental protocol designed as a series of experi-
ments with stepwise increases in the injection rate of Kepone such
that any significant approach toward the emission limit would cause
the experiments to be terminated.
7. The placing of control of continuation into the next experiment in
the hands of a committee of officials directly concerned with
environmental protection who could, after review of each completed
experiment, decide to proceed or to alter the course of the program.
To proceed in an orderly manner, a detailed protocol, discussed
earlier, was designed before the beginning of the experiments.
EXPERIMENTAL PROTOCOL
In order to establish a standard procedure for progressive increases in
the Kepone injection rate, a definite series of experimental steps was es-
tablished prior to the beginning of the test program. It was provided that
the Burn Authority would have the absolute authority to determine continua-
tion or cessation of the experimental program, and, further, it was deemed
appropriate for the Burn Authority to utilize the technical staff for assis-
21
-------
tance in the decision making process, especially if it were predicted that to
continue along the pre-arranged steps would lead to the emission of unaccep-
table levels of Kepone. The protocol outlined below was established as a
guideline for an experimental program, subject to change as dictated by ex-
perimental findings as the program advanced.
Initial Program
It was considered appropriate to carry out the experimental program in
two phases; (a) Direct injection of Kepone solutions into the duct leading
to the afterburner so as to simulate processes associated with the destruc-
tion of technical grades of Kepone, and (b) Coincineration of Kepone in
sewage sludge to simulate processes expected to be involved in the incinera-
tion of the sludge from the Hopewell Lagoon. In this spirit, the following
set of experiments were planned (for completeness, the final pre-program
protocol is appended as Appendix D):
Phase 1. Direct injection Experiments
1. Kepone feed at 1.5 x 10~5 gm/min., 1260° C (2300°F),
2 second residence times.*
2. Kepone feed at 1.5 x 10 ~5 gm/min., 1093°C (2000°F),
2 second residence time.
3. Kepone feed at 1.5 x 10 ~2 gm/min., 1093°C (2000°F),
2 second residence time.
4. Kepone feed at 15 gm/min., 1093°C (2000°F),
2 second residence time.
5. Kepone feed at 15 gm/min, 1093°C (2000°F),
1 second residence time.
o o
6. Kepone feed at 15 gm/min. 1038 C (1900 F),
1 second residence time.
Phase 2. Coincineration Experiments
1. Toledo sludge blank, 1093°C (2000°F),
2 second residence time.
**
2. Hopewell sludge at same conditions as above.
3. James River sediments at same conditions as above.**
In all cases, the stated residence time is a nominal figure used as a
lower bound on an acceptable residence time.
Because the James River was completely frozen over, this experiment was
dropped from the protocol.
22
-------
4. Toledo sludge doped at 25 percent (on dry basis) with
Kepone, same conditions as above.
5. Toledo sludge doped at 50 percent (on dry basis) with
Kepone, same conditions as above.
Modified Program
As the direct injection experiments proceeded during the program, it
became obvious from stack gas analyses that the higher injection rates
planned would seriously challenge the afterburner so as to allow the stack
emissions to approach or exceed the limit of 1 microgram per cubic meter, and
that some alteration of the protocol was required. It was then determined
that, in the interests of completing the experiments without exceeding the
emission limits, it was desirable to omit the high level injection experi-
ments and proceed to the coincineration studies.
As a result of such decisions based on the completed experiments, the
actual series of experiments that were carried out consisted of the following:
Phase 1. Direct Injection Experiments
1. Acetic acid alone
2. Acetic acid solution of kepone; 1.67 x 10 gm/min.,
1260°C (2300°F), with 2 second residence time.*
3. Acetic acid solution of kepone; 1.67 x 10 gm/min.,-
1093°C (2000°F), with 2 second residence time.
_2
4. Acetic acid solution of kepone; 1.67 x 10 gm/min.,
1093 C (2000°F), with 2 second residence time.
Phase 2. Coincineration Experiments
1. Toledo sludge, 1093°C (2000°F), 2 second residence time.
2. Toledo slydge with kepone, 5.68 gm/min. of kepone,
1149 C (2100°F),with 2 second residence time.
3. Toledo sludge with kepone, 5.68 gm/min. of kepone,
1093°C (2000°F),with 2 second residence time.
4. Toledo sludge with kepone, 5.68 gm/min. of kepone,
1038°C (1900°F), with 2 second residence time.
5. Toledo sludge with kepone, 24.2 gm/min. of kepone,
1093°C (2000 F), with 2 second residence time.
* As before, the cited residence times are to be considered as nominal
values to be used as a lower bound on the actual (calculated) residence time.
23
-------
EXPERIMENTAL RESULTS
The chief results of these experiments are displayed in Table 1 which
summarizes the primary data derived from these tests. The detailed data on
the furnace operations are presented in full in Appendix E, whereas the
data derived from the stack and scrubber Kepone concentration measurements
are displayed in the sections which immediately follow. In order to further
simplify the following presentation, examples of typical chromatograms of
authentic standards and of typical samples are displayed in Appendix F. In
addition, a detailed log of the day by day events that characterized this
program is presented in Appendix G.
Before proceeding with the presentation of the detailed data it is
appropriate to indicate several results of a general nature that derive from
these experiments. First, the interaction of the Burn Authority with the
Experimental Management Group was continuous and of great benefit to the
overall program. Evidently, this form of program management is a viable and
useful tool to be exploited in all such experiments with hazardous materials.
There has been some question raised about the effect of the personnel
safety measures on the productivity of the operating personnel. Although
this was not considered to be an experimental variable, the reduction in
productivity did have a major impact on the program costs. Specifically, the
day-by-day wearing of protective equipment in the Operations Room and the
personal hygiene regimen imposed on those workers, appears to have resulted
in a 15 to 20 percent increase in costs of these day-by-day operations. It
would also appear that the necessity of the full protection, including the
respirator, resulted in a 50 percent decrease in productivity (this is only
an estimate). Further, the expenditure of some 10 hours per person in the
lecture portion of the safety program, had a significant impact on the total
manpower hours that were expended, especially in terms of a program limited
to some eight weeks.
Stack Sampling Data
The stack samples were collected in accordance with EPA Method Five
using the RAC Staksampler (R). The data for the twenty eight (28) separate
stack sampling runs are summarized in Table 2 and 3 which follow. The de-
rived quantities were calculated in accordance with the procedures outlined
in ASTM Method D2929- The corresponding Kepone concentrations found for
these stack runs are tabulated in Tables 4 and 5. It will be noted that at
no time did the stack emission rate exceed the pre-established level of
1 x 10 gm/m at stack conditions.
Scrubber Data
The scrubber samples were, in the earlier experiments, taken at the end
of each stack sample run. Unfortunately, it was discovered that the position
from which such samples were taken was the reservoir for the scrubber system
and thus the concentration measurements were of little significance. In
addition, it was found that the average level of water in the scrubber system
24
-------
TABLE 1: SUMMARY OF KEPONE INCINERATION EXPERIMENTS
Experiments
Kepone Feed
Rate
(gms/min)
Total
Feed
Time
(min)
Total
Kepone
Fed
(gms)
Stack
Emission
Concentration
o
(gm/m )
Total
Stack
Output
(gms)
After- After- Key for Key for
burner burner Scrubber Stack
Temp Temp Samples Scans
Injection Runs
1
2
3
4
5
Acetic Acid Only
1.67x10"
1.67x10"'
1.67x10
1.50
,-5
,-2
130
135
100
115
2.16 xlO"3
2.25 x10"3
1.67
172.5
ND
ND
ND*
5.3Sx10"8
ND
ND
ND*
1.76 x 10"*
1260
1260
1093
1093
1093
2300
2300
2000
2000
2000
1
2,3
4-6
7,8
9-11
1
2^3
4,5,6
7,8
9,10,11
Ul
Sludge Runs
6*»
7
8
9
10
11
Background
Toledo Sludge Only
5.68
5.68
5.68
24.2
120
120
315
240
220
165
-
-
1789
1354
1241
3995
,-7
2.96x10
ND
1.7 x 10"8
2.4 x10"8
2.55 x 10~8
2.95 x 10~8
7.1 x 10"^
ND
1.85X10"4
1.85 xW4
1.53 x 10"4
1.67x 10"4
1093
1093
1149
1093
1038
1093
2000
2000
2100
2000
1900
2000
12
13,14
16-22
23-31
32-40
41-46
12
13,14
16-19
20-22
23-25
26-28
Totals
8553 gms
1.58x 10~Jgms
Apparent kepone peak on chromatogram of filter collected. The kepone peak did not appear after base
partitioning of original extract.
Experiment 6 was run with a highly contaminated scrubber water (25 ppb of kepone) in an attempt to find the causes
of the high emission in the previous experiment.
See Tables 4, 5, & 6
See Tables 2 & 3
-------
TABLE 2 Summary of Stack Sampling Data
Run Pmeter Impinger Sample Water Total Percent Sample Water
No. Temp. Volume Collected Sample Water Time Loss
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20
21
22
23
24
25
26
27
28
(mm Hg)
678
579
599
617
597
478
511
538
544
627
572
645
533
(°K) (m3)
300
300
303
290.5
291.6
301
298
306
300
296
306
300
263
1.
1.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
138
169
537
993
933
663
780
477
662
681
637
817
741
(ml)
100
100
145
105
100
460
429
400
412
91
380
170
444
Aborted
572
544
551
480
478
572
658
470
467
460
584
587
634
305
298
301
310
313
314
305
311
305
301
301
297
302
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
0.
676
713
706
665
648
630
447
648
545
651
688
655
527
349
377
226
202
215
246
165
185
170
260
143
156
163
(tn3)
1.
1.
0.
1.
1.
1.
1.
1.
1.
0.
1.
1.
1.
1.
1.
1.
1.
1.
1.
0.
1.
0.
1.
0.
0.
0.
267
316
768
171
113
645
619
188
418
798
290
102
580
277
376
111
060
070
029
688
015
897
170
954
921
774
15
17
36
41
18
62
55
64
57
21
56
27
56
—
52
54
41
46
49
49
41
47
46
52
29
32
37
(min . )
48
45
31
48
48
42
42
40
40
41
35
39
39
—
34
32
32
32
32
29
25
32
29
30
32
30
26
(gm/sec)
32
31
84
38
13
125
119
117
105
36
119
70
135
123
126
94
90
88
102
98
87
85
107
72
78
102
.8
.5
.5
.5
.2
26
-------
TABLE 3 Summary of Stack Velocity Data
Sp. Gr. __
% Stack Tg fVK) v Q
Run No. Water Gas . ave ave
T = Stack Temperature ( K)
s
h = Velocity Pressure (nrniH^o)
v = Stack Gas Velocity (m/sec)
3
Q = Stack Gas Flow Rate (Standard m /hour)
27
(°K) (m/sec) (SCMH x 10 3)
2
3
4
5
6
7
8
9
10
11
12
13
14
1 C
13
16
17
18
19
20
21
22
23
24
25
26
27
28
15
17
36
41
18
62
55
65
57
21
56
27
56
~~
52
54
41
46
49
49
41
47
46
52
29
32
37
0.815
0.794
0.869
0.852
0.932
0.780
0.803
0.773
0.797
0.921
0.800
0.900
0.800
0.814
0.809
0.852
0.835
0.825
0.825
0.852
0.831
0.836
0.816
0.894
0.883
0.866
362
361
361
352
358
355
355
355
355
355
351
386
390
A r\ f\*V*^* Q n
ADOirtEQ
405
408
408
405
411
411
422
405
405
405
405
405
405
0.397
0.383
0.438
0.430
0.358
0.410
0.417
0.318
0.335
0.314
0.374
0.465
0.468
0.449
0.461
0.473
0.478
0.446
0.432
0.424
0.484
0.450
0.484
0.503
0.477
0.496
8.43
8.23
8.99
8.82
7.07
8.83
8.84
6.89
7.13
6.22
7.89
9.70
10.42
___«
10.09
10.44
10.43
10.61
10.03
9.71
9.51
10.77
9-99
10.87
10.80
10.30
10.81
1.52
1.48
1.62
1.62
1.30
1.61
1.61
1.26
1.31
1.14
1.46
1.63
1.73
— ___
1.62
1.66
1.66
1.70
1.59
1.54
1.46
1.72
1.60
1.74
1.73
1.65
1.73
-------
TABLE 4 Stack Kepone Concentration Data
for Injection Experiments
Sample
2
3
4
5
6
7
8
9
10
11
12
13
14
15
Kepone Detected
(gms)
ND
ND
ND
ND
ND
ND*
ND
ND
90 x 10 g
17 x 10
296 x 10 ~9
ND
ND
ABORTED
Sample Vol.
(SCM)**
1.267
1.316
0.768
1.171
1.113
1.645
1.619
1.188
1.418
0.798
1.290
1.102
1.580
Kepone Cone.
(gm/M3)
0
0
0
0
0
0
0
0 _9
63 x 10 n
21 x 10
229 x 10 y
0
0
Kepone Emmission
Rate
(gm/minQ _
0
0
0
0
0
0
0
13.8 x IQ-
4.0 x 10~
55.
7 x 10
0
0
~7
*A peak appeared in the original extract of the cyclone sample which
disappeared after base partitioning of the extract.
**SCM = Standard Cubic Meters at 21.1QC (70°F) and 760 mm Hg pressure.
28
-------
TABLE 5 Stack Keoone Concentration Data
for Colncineration Experiments
Sample Run
16
17
18
19
20
21
22
23
24
25
26
27
28
Kenone
Detected
(gms)
ND
ND
10 x 10
43.9 x 1Q~9
40 x 10
30 x 10~9
28 x 10 n
Q
37 x 10 „
Q
22 x 10 f
34 x 10
31.2 x 10 9
31.3 x 10 9
27 x 10 y
Sample
Volume
(SCM)**
1.11
1.06
1.07
1.03
0.688
1.015
0.897
1.17
0.954
0.021
0.774
Kepone
Cone
(gm/M3)
—
9 x 10~9
41.4 X 10~g
37.4 x 10
29 x 10~9
40.7 x 10~9
36 x 10~9
24.5 x 10~9
29.1 x 10 y
32.7 x 10~9
34.0 x 10 9
34.9 x 10
Kepone Emission
Rate
(gm/min)
—
2.5 x 10~7
11.7 x 10~ 7
7.4 x 10
9.9 x 10~7
10 x 10~7
6.5 x 10~7
_ /
8.4 x 10 '
9.4 x 10~7
9.4 x 10~7
10 x 10~7
*SCM = Standard Cubic Meters at 21.1°C (70°F) and 760 mm He pressure.
29
-------
was not recorded during the earlier runs so that there was no way to deter-
mine the total level of Kepone within the scrubber system. These defic-
iencies were corrected so that scrubber samples 16 through 46 were taken at
the appropriate site within the scrubber system and the level of water within
the system was recorded so that total quantities of Kepone within the scrub-
ber/quench system could be determined. The results of the analyses of the
scrubber concentrations are tabulated in Table 6.
The data that are presented in Column 5 of Table 6 were derived under
the assumption that when the scrubber reservoir had a level of 1.57 m the
total volume of the scrubber/quench system was 1325 1 and that a 2.54 cm
change in this level corresponded to a 16.7 1 change in volume. With this
basis it was possible to convert the measured concentrations of Kepone within
the scrubber (Column 2 - Table 6) into total scrubber kepone loads.
ANALYSIS OF EXPERIMENTAL RESULTS
Efficiency of Combustion
The results from the direct injection experiments are displayed in
Table 7 and those for the coincineration experiments in Table 8. The re-
ported efficiencies all of which exceed 99.99 percent which are based on the
stack emission rate divided by the Kepone input rate, strongly support the
conclusion that incineration is a viable and safe method of disposal of
Kepone and of Kepone contaminated sludges at least under the conditions that
the afterburner temperature is not less that 1038°C (1900°F) and the res-
idence time is of the order of two (2) seconds.
The relatively high levels of Kepone detected in the stack during the
1.5 gm/min. injection run suggested that further tests with even higher in-
jection rates could lead to unacceptable Kepone emission rates; as a result,
such experiments were discontinued in favor of the coincineration studies.
The results of the highest level injection run were complicated by the ab-
sence of any useful method of determining whether passage of Kepone through
the afterburner was due to inadequate vaporization within the injection
nozzle (which was of unconventional design), or to some transient change in
afterburner conditions, or did, in fact, represent an accurate measure of the
capabilities of the afterburner. The internal consistence of the discussion
presented in Section 7.3 does, however, suggest that the measured efficiency
from the injection experiments are entirely consistent with those from the
coincineration experiments.
The high Kepone emission rates that were observed during runs 12-14,
which occurred with no Kepone feed into the system but with relatively
heavily contaminated scrubber water (25 ppb), cannot be readily explained,
especially in view of the fact that during the last of the coincineration
experiments the scrubber concentration rose to even higher levels. It is
perhaps relevant to point out that the measured stack water content was also
30
-------
TABLE 6 Scrubber Sample Data
Measured
Kepone
Time Scrubber Scrubber Kepone
Sample No.# Concentration Taken Volume** Kepone Load Feed
16
17
18
19
20
21
22
23
24
25
26
27
28
29
30
31
32
33
34
35
36
37
38
39
40
41
42
43
44
45
46
#
(ppb)
0
0.74
3.0
3.1
3.1
6.6
5.2
8.3
6.7
5.5
5.2
4.8
4.8
5.19
13.7
11.8
9.6
11.9
15.0
10.9
14.1
13.7
17.2
15.1
13.3
29
31.7
27
32.4
25.9
18.1
(min)*
(Background)
105
155
185
230
260
290
(Background)
30
60
90
125
150
180
210
240
(Background)
10
40
70
100
130
160
180
205
(Background)
18
48
78
108
138
Scrubber sampling during the
AB Temp.
(M3) (gms) (gms/min) (°C)
o .
1.14 8.4 x 10~4 5.68
1.108 3.33 x 10~3
1.242 3.80 x 10
1.292 4.00 x 10~3
1.058 6.99 x 10~3
1.225 6.37 x 10~3
n
1.175 7.87 x 10":: 5.68
1.004 5.52 x 10
0.842 4.38 x 10~3
1.067 5.12 x 10
0.900 4.32 x 10~|
1.125 5.84 x 10
0.933 1.28 x 10~2
1.241 1.47 x 10 2
f\
1.183 1.41 x 10~2 5.68
0.996 1.45 x 10~2
1.376* 1.50 x 10 ,
1.125* 1.59 x 10 j
1.283 1.76 x 10~2
1.067 1.84 x 10
1.195 1.80 x 10
1.050 1.40 x 10~2
f\
1.083 3.43 x 10"^ 24.
0.879 2.37 x 10~2
— /
1.100 3.56 x 10
0.908 2.35 x 10 2
1.133 2.05 x 10
1149
(2100°F)
1093
(2000°F)
1038
(1900°F)
1093
2 (2000°F)
first set of experiments was deemed to
be of no value since there was no measure available for
of the (closed)
data for samples
scrubber system at the time of sampling
1-15 are not
included in this summary.
the volume
. Thus the
* Measured from onset of Kepone feed.
** Calculated from scrubber water level data, based on average filled
scrubber volume of 1325 L (350 gal).
31
-------
TABLE 7 Combustion Efficiency for Kepone Injection
After-
burner Efficiency of
Kepone Feed Rate Temp Stack Kepone Loss Combustion
Stack Sample (gm/min) (°C) (gm/min) %
2 1.67 x IQ~5 1260 0 100*
3 1.67 x 10~^ 1260 0 100
4 1.67 x 10~^ 1093 0 100
5 1.67 x IQ~1 1093 0 100
6 1.67 x 10 ;> 1093 0 100
7 1.67 x 10~2 1093 0 100
8 1.67 x 10"2 1093 0 100
9 1.50 1093 0 100
10 1.50 1093 0 100
11 1.50 1093 13.8 x 10"' 99.99991
12 0 1093 4.0 x 10 •' **
13 0 1093 55.7 x 10"' **
14 0 1093 0
15 0 1093 0
* To speak of 100 percent combustion efficiency is somewhat unrealistic
but is a natural consequence of the definition for efficiency of
combustion in those situations for which there is so small a stack
load of Kepone that it was undetectable. Further, the expression of
the combustion efficiency in terms of 6 or 7 decimal places is just-
ified since even if both the input rate and the emission rate were
in error by as much as 25 percent, the extremes would only affect the
combustion efficiency in the sixth decimal place — again a conse-
quence of the definition of the combustion efficiency and the very
small emission rates that were found.
** Stack samples 12, 13 and 14 were taken during experiments 6 and 7
(see Table 1-1 for details). The scrubber was contaminated so that
even in the absence of Kepone feed there was detectable Kepone in
the stack.
32
-------
TABLE 8 Coincineration Efficiency for Kepone
with Sewage Sludge
Stack Sample
16
17
18
19
20
21
22
23
24
25
26
27
28
After-
burner
Kepone Feed Rate Temp
(gm/min)
Stack Kepone Loss
(gm/min)
Efficiency of
Destruction *
5.
5.
5.
5.
5.
5.
5.
5.
5.
5.
24.
24.
24.
68
68
68
68
68
68
68
68
68
68
2
2
2
1149
1149
1149
1149
1093
1093
1093
1038
1038
1038
1093
1093
1093
0
0
2.
11.
9.
7.
9.
10
6.
8.
9.
9.
10
5
7
9
4
9
5
4
4
4
X
X
X
X
X
X
X
X
X
X
X
10
10
10
10
10
10
10
10
10
10
10
-7
-7
-7
-7
-7
-7
-7
-7
-7
-7
100
100
99.
99.
99995
99998
99-99998
99.
99-
99.
99.
99.
99.
99.
99.
99998
99998
99998
99999
99998
999996
999996
999996
* See footnote Table 7.
33
-------
highly variable during this run and also that the pH of the water collected
in the stack sample also varied from neutral to highly basic (the larger
the collected volume the more likely it was to be basic). Further, the
ambient weather conditions that prevailed during the early set of measure-
ments (runs 1 through 14) when the average temperature was well below 0°C,
had the effect of causing the stack plume to appear to arise from well within
the stack itself. In the interval between the first set of runs and the last
series which involved coincineration (16-28), a new stack and a stack re-
heater were installed. The modified stack coupled with the considerable
amelioration in the weather probably affected the observed results.
Scrubber Kepone Concentration and Kepone Load
During the coincineration experiments it was decided that frequent
scrubber samples should be taken in order to understand better the effects
that the scrubber had on the apparent Kepone destruction ratio of the total
system. The scrubber Kepone load at any instant was found by multiplying the
concentration at that moment by the instantaneous volume of the scrubber
using the conversion factors that are discussed in Section 6.2. The results
of such measurements and calculations are displayed in Table 6 (Column 5)
and more graphically in Figures 8 through 11.
A study of the Figures 8 through 11 indicates that the time rate of
change of the total scrubber Kepone load is quite different in each case and
further, that there are very striking differences in the nature of the ob-
served changes. The data in each plot are summarized by the least squares fit
to an equation of the form
m(t) - m(0) + b(t) (7.1)
where m(t) is the total Kepone mass in the scrubber at time t
m(0) is the initial Kepone mass in the scrubber at time t=0
b is a constant that characterizes each set of conditions
t is the elapsed time
[note also that the constant b is the slope of the plot of m (t) vs. t]
In order to attempt an understanding of the significance of the curves
presented in Figure 8 through 11, it is useful to summarize the data on
stack emission rates from Table 5, with the slopes of the curves in Figures
8 through 11,in Table 9. It is first of all important to note that the-
stack emmission rates (Column 2, Table 9) are, in all cases, on the order of
one percent of the rate o change of the scrubber JKepone load (Column 3,
Table 9). With this observation, we may assume that the rate of loss of
from the scrubber due to evaporative losses up the stack is only a
small effect and thus may be neglected in what follows.
Now, the rate of change of Kepone mass within the scrubber is neces-
sarily the result of the interaction of several phenomena; that is to say,
was injected into the scrubber from the unburned material that
traversed the incinerator. One would expect, in view of the smallness of
the rate of stack emission, that the slopes of the curves in Figure 8 through
34
-------
LEAST SQUARES FIT
M(t) = [-9.7X10-4 + 2.63XIO-5t](gms)
u>
CM
O
E
cr>
Q
<
O
O
Q.
ca
UJ
OQ
00
•=>
on
O
0.8 ••
0*5 ..
0,3 ••
0.1 •-
FIGURE 8 :
100
200 300
TIME OF FEED(min.)
400
CALCULATED SCRUBBER LOAD OF KEPONE AS A FUNCTION
OF TIME (.5.64gm/min. KEPONE FEED-,ABTEMP. II49°C(2IOO°F)
-------
1.5 T
LEAST SQUARES FIT
M(t) = [9.41 x 10-3~5.82 x
M(t) = [1.24 x 10-2+ll.13x
10-5t]gms (0 <;± <,
10-H]gms (I00*t)
ICOminj
CM
g
x
10
E
o>
i.O -•
to
3
UJ
z
o
Q_
111
Q
UJ
O
<
-------
LEAST SQUARES FIT
M(t) = [1.35 x l(T2+2.75xlO-5t]gms
CM
O
X
in
E
o>
I.9T
1.8'
CO
--J
LU
O
a.
LU
1.7-
1.6 • •
cr
LU
CD
CD
Z)
IT
O
1.5- •
1.4-
I.3--
4-
50
100 150
TIME OF FEED(min.)
2OO
FIGURE I0 '
CALCULATED SCRUBBER LOAD OF KEPONE AS A FUNCTION
OF TIME 5.64 gm/min. KEPONE FEED; ABTEMP. I038°C(I900°F)
-------
3.5 X
LEAST SQUARES FIT
m(t)° [3.47X10-2 - 9.27 XIQ-StJ gms
OJ
oo
CM
O
X
V)
E
Q
<
O
Ul
z
O
Q.
LU
a:
UJ
CD
CD
3
cc
O
2.5"
2.0"
50
100
TIME OF FEED(minJ
150
200
FIGURE _LL
CALCULATED SCRUBBER LOAD OF KEPONE AS A FUNCTION
OF TIME 24.2gm/min. KEPONE FEED;ABTEMP.I093°C(2000°F)
-------
TABLE 9 Tabulation of Kepone Input and Loss Rates (Scrubber)
Stack Sample
16
17
18
19
20
21
22
23
24
25
26
27
28
Stack
Kepone Loss
(gm/min.)
2.5
11.7
9.9
7.4
9.9
10
6.5
8.4
9.4
9.4
10
0
0
X
X
X
X
X
X
X
X
X
X
X
10-7
_7
X V* —1
— /
10 '
ID'7
^
10 '
io:
10 7
10_7
10 '
io-7
Slope of
Scrubber Load
(gm/min.)
2.
2.
2.
2.
-5.
9-
9.
2.
2.
2.
-9.
-9.
_Q
63
63
63
63
82
64
64
75
75
75
27
27
27
X
X
X
X
X
X
X
X
X
X
X
X
X
10
10
10
10
10
10
10
10
10
10
10
10
10
-5
_5
^J
-5
_S
_/
-5
-5
-5
~wf
-5
~5
Scrubber
Kepone Input
Rate
(gm/min. )
11.
11.
11.
11.
12.
12.
12.
18.
18.
18.
9
9
9
9
0
0
0
9
9
9
X
X
X
X
X
X
X
X
X
X
0
0
0
10"^
10-5
10 *
10
^n- ^
10
1°1
10 ^
10 J
10 5
39
-------
11 would all be positive; that is one would expect the scrubber load to con-
tinually increase with time. That is clearly not the case, as for example in
Figure 11. It then becomes necessary to assume that there are processes that
operate within the scrubber to decrease the amount of Kepone that is present;
that is to say, there must be processes that are operative within the scrub-
ber that can destroy Kepone. *
In general, the amount of kepone that passes through the incinerator for
a given rate of input to the kiln must necessarily depend on the Kepone feed
rate and on the thermal conditions that occur within the afterburner and in
the kiln. Suppose that, for the sake of argument, it is assumed that the
particular conditions that existed during the run from which the data dis-
played in Figure 11 were obtained, were such as to reduce the rate of Kepone
injection into the scrubber to zero. Under these circumstances, the behavior
of the scrubber during that experiment was governed only by those destructive
processes particular to the scrubber itself. From this observation, we may
estimate that those processes operate to destroy kepone at the rate
dm/dt = 9-27 x 10~5 gm/min (7.2)
as obtained from the slope of Figure 11.
If it is now assumed that these processes are always operative indepen-
dent of the conditions that occur within the kiln or the afterburner, then
the results shown in Equation (7.2 ) may be used in conjunction with the
observed slopes in Figures 8 through 10, to compute the rate at which Kepone
must have been injected into the scrubber in those experiments. The results
of these calculations are displayed in Column 4 of Table 9.
With the data that are displayed in Table 9 and those in Table 1 (for
the Kepone injection rate from Column 2 of Table 1) it is possible to com-
pute the effective efficiency of the incinerator - kiln plus afterburner -
independently of the scrubber effects. The results of this calculation are
displayed in Table 10.
To carry this discussion one step further, it will be recalled that
during the 1.5 gm/min injection experiment, the scrubber Kepone concentra-
tion changed such that, after a total feed of 178 gm of Kepone, the scrubber
load was 3.3 x 10~ gins (corrected for the assumed scrubber loss mechanisms).
If it is now asserted that this result was a consequence of the direct chal-
lenge to the afterburner, then the efficiency of the afterburner for Kepone
*"The discussion regarding the disappearance of Kepone from the scrubber
solution was particularly interesting. I believe, however, that the dis-
appearance of the Kepone is caused by its chemical destruction in the hot
caustic solution of scrubber. Our data at this laboratory show that Kepone
can be completely converted to NaCl and Na2C03 by exposure to caustic solu-
tion at 350°C under pressure with excess oxygen with a residence time of 5
minutes. I think that a similar process is occurring in the caustic solu-
tion of the scrubber in contact with the hot gases at a somewhat slower
rate. By A.J. Frank in response to technical review solicitation,
Corporate Director, Environmental Planning.
40
-------
combustion was 99.981 at a temperature of 1093°C and with a residence time of
the order of two (2) seconds.
To return to the coincineration experiments which involve the kiln as
well as the afterburner, it is appropriate to indicate the kiln exit, temper-
ature as functions of time. The data are presented in Figures 12 through
15. It is immediately noted from Figures 12 through 14, that during these
experiments, the kiln temperature was below 350°C. According to the results
of Rubey and Duvali /Kepone is unstable at temperatures above 350°C so that
it is reasonable to assume that during the experiments described by Figures
TABLE 10 Incinerator* Efficiency as Derived from Scrubber Data
Afterburner Kepone Feed Kepone Input Efficiency of
Temperature Rate to Kiln to Scrubber Incinerator
(°C) (gm/min) (gm/min) (percent)
1149 11.2 1.19 x 10~4 99-9989
-4
1093 -- -- - 5.64 1.2 x 10 99.99789
1093 24.2
1038 5.64 1.89 x lo"4 99-9966
* Incinerator includes both kiln and afterburner but excludes
possible effects due to scrubber.
41
-------
o
o
W
500 T
450 • •
400 • •
£ 350
2
UJ
*, 30°
250 '
0
30 60 90 120 150
FEED TIME (MIN.)
180
2IO
240
270
FIGURE J2_
KILN EXIT TEMPERATURE AS A FUNCTION OF TIME
5.6gm/min., AB I 149°c CO INCINERATION
-------
to
400 T
350 •
3OO -•
o
LU
CE
13
o:
UJ
0.
5
HI
H
X 250
UJ
200 -•
150
FIGURE -11-
l
30 60 90 120 150
FEED TIME (MIN.)
180
210
240
KILN EXIT TEMPERATURE AS A FUNCTION OF TIME
FEED 5.6 g/min., AB I093°C.COINCINERATION
-------
o
o
LU
cc
LU
0.
5
UJ
450
400
350
300
2 25°
200
0
FIGURE J±.
30
O ,
60
90
120 150
FEED TIME
180
210
240
KILN EXIT TEMPERATURE AS A FUNCTION OF TIME
FEED 5.6 gm/min.,AB I038°C COINCINERATION
-------
500
O
o
LLl
•e'-
en
cr
in
a.
5
UJ
400 ••
X
LU
300 ••
30 60 90 120 150
FEED TIME (WIN.)
ISO
210
FIGURE
KILN EXIT TEMPERATURE ASA FUNCTION OFTIME
FEED24.2 gm/min.,AB I093°C COINCINERATION
-------
12 through 14, some of the input Kepone to the kiln escaped to enter the
afterburner.
At this point it should be possible to unravel the separate effects due
to the kiln from those due to the afterburner. Unfortunately, this possi-
bility was not recognized in the initial phases of the experimental study so
that no provisions were made to allow sampling of the (rather lengthy) duct
from the kiln output to the afterburner input. Thus any serious attempt to
discover the separate effects would be almost entirely speculative. There
are several remarks that can be made. If we examine the kiln output
temperature as shown in Figure 15, it is clear that in this case, the exit
temperature never fell below 400°C and this particular experiment exhibited
the behavior shown in Figure 11 wherein the scrubber Kepone load decreased
throughout the entire experiment. Presumably, this behavior arose because
little or perhaps no Kepone was able to escape destruction within the kiln.
Thus it would certainly seem that the function of the kiln in this particular
application is something more than a simple pyrolyzer to vaporize the Kepone
from the sludge.
The Scrubber Effect
Several features of these experiments indicate that there are processes
that occur within the scrubber that have not been illuminated by the nature
of the available data. For example, the apparent association of Kepone with
sodium hydroxide within the escaping stack gases is difficult to account for.
In all cases in which Kepone was found in the stack sample, the fluids that
were collected showed a basic pH. Further, the rate at which Kepone was
"evaporated" from the scrubber as compared to the rate at which water was
evaporated seemed to indicate that the kepone concentration in the stack
water was quite comparable to that in the scrubber as a whole.
The nature of the Kepone destruction process(es) that are postulated to
occur within the scrubber are difficult to visualize, although it should be
noted that the process whereby the hot stream of gases from the afterburner
is quenched should be a rather violent process. It is possible that the
exposure of Kepone to these hot gases in the moment of explosive evaporation
of the quench water might be sufficient to disrupt the molecule. It is even
conceivable that the solution so rapidly evaporated in the quench process
would contribute to the stack load of Kepone. Unfortunately, the scope of
this program was such as to make it impractical to carry out the additional
measurements that would be required to unravel these questions.
It should be stressed that the overall destruction efficiency for Kepone
of the incinerator system including the scrubber was found to be higher than
the kiln-incinerator system without the scrubber.
Observations of the Utility of a Field Laboratory
The climate in which these experiments were conducted was such that it
was imperative that every effort be made to prevent the exposure of either
the operations personnel or the general community to Kepone. It was also
46
-------
deemed essential that there be provided an on-site analytical capability to
perform, on essentially a real-time basis, Kepone analyses of quality com-
parable to those of a standard laboratory. As indicated in Appendix C, a
considerable stock of equipment and reagents was brought to the site in order
to allow these analyses to be carried out. It is gratifying that the only
materials that required local purchase was a supply of distilled and de-
ionized water and ice.
In spite of the somewhat makeshift nature of the physical facilities and
the rigors of the weather, it was found that trace Kepone analyses could be
completed in approximately 15 minutes for aqueous samples and about 30 min-
utes for filters and similar materials. Such promptness allowed almost real-
time results to be made available to the Burn Authority and thus greatly
facilitated important decisions on program changes and continuation.
In the course of some 38 days of laboratory operation nearly 1000 indi-
vidual analyses were performed by a staff of one analytical chemist and one
technical assistant - this is truly remarkable.
The experience that has been gained by this activity suggests that such
a portable facility can be used for many such trace organic analyses. How-
ever, the specific characteristics of Kepone, that is the relative ease with
which Kepone can be separated from other chlorinated organics by base parti-
tioning, were of importance in the speed with which sample cleanup and sub-
sequent analysis could be accomplished. Analyses of compounds such as PCBs
could be expected to be somewhat more time consuming because of the elaborate
cleanup procedures that would normally be required.
Observations on the Adequacy of the Health and Safety Program
The Health and Safety Program was conceived as an integral part of the
KIT program and was found to be entirely adequate. Prior to the onset of
the program, all operating personnel were required to have a blood sample
taken to be compared with a similar sample at the completion of the program.
This test is a very sensitive measure of the magnitude of exposure that was
received. In all cases there was no observed change found in the blood pic-
ture of the operating personnel.* From these data it can be asserted that
no individual was exposed to measurable amounts of Kepone.
In addition, the rather extensive wipe sample program that was under-
taken (as described in Appendix B) showed that the method of isolation that
was employed within the facility was also entirely adequate. At no time was
there detected significant evidence of contamination on the walls or floor of
the operations room. On the other hand, even the contamination found within
the kiln and mixing rooms was of such a nature that relatively little surface
cleaning was required prior to the disassembly of the facility.
The success of the approach used in the KIT program suggests that simi-
lar methods could be of great utility in any installation that is involved
*See Appendix H
47
-------
in the handling of toxic materials.
An interesting side light on the need for training is the need for and
the use of protective equipment was brought out by the acetic acid spill
which occurred during the coldest weather in Toledo. The freezing point of
glacial acetic acid is some 16.6°C so that it was frozen when the 55 gallon
containers were brought into the mixing room. Valiant attempts to thaw the
material finally led to the use of a heating belt on the can. Unfortunately,
the can overheated and caused the plastic liner to be ruptured. By a strange
series of circumstances, this particular container had a small opening near
the bottom of the can, so that with the integrity of the liner breached,
acetic acid began to leak onto the floor. In the excitement of the moment,
the container was turned on its side with the result that a significant
amount of the acid was allowed to spill onto the floor. In any event, the
entire incident was cleaned up with only one very small skin burn resulting -
this in spite of the very corrosive nature of glacial acetic acid.
Seme General Observations
The Surface Combustion facility was not constructed specifically for the
KIT program. This fact introduced several factors into the program that
merit further discussion.
The kiln, which was designed for batch operations, was not new and thus
suffered a number of breakdowns that served to delay the program. The sludge
feed, which was to be continuous, was accomplished by the makeshift intro-
duction of a water cooled line through the hot exit gas duct into the kiln.
This procedure apparently resulted in the flash evaporation of Kepone without
allowing it to remain for a time in contact with the drying sludge. It was
probably fortunate that Kepone is degraded at temperatures of the order of
350-400 C, since otherwise a great deal more of the material would have been
presented to the afterburner. In addition, sludge was noted to fall from the
walls of the kiln onto the cooled water line with the result that there was
a considerable buildup of partially combusted material on the line. At the
end of the run this deposited material was found to be admixed with the ash
so that ash concentration measurements were not particularly meaningful.
Because of the particular arrangement of the components of the system,
there was an excessively long duct run from the kiln to the afterburner. In
spite of the frequently expressed fears that Kepone deposition on the walls
of this duct would vitiate the results of the experiment, there was no evi-
dence of such a deposition when the experiments were finished. Nevertheless,
the use of such a long duct run certainly decreased the thermal efficiency of
the system.
A number of unexplained phenomena plagued the injection runs. The suc-
cessive stack sampling runs were almost impossible to explain in terms of the
measured water content, which was found to fluctuate wildly. After a new
stack fitted with a reheater was installed, there were no such variations
noted. A possible explanation of these results might lie in the extreme
48
-------
weather that occurred during the earlier experiments: it was cold enough that
the plume was actually formed within the stack such that variations in the
actual level at which it formed would account for the variations in the ob-
served results. On the other hand, some of the stack water samples that were
collected showed rather high pH, of the order of 9 to 10, and only when there
was a high pH was there Kepone found in the stack. In the experiments that
involved the coincineration (with the newly installed stack and reheater) no
such high pH waters were collected even though traces of Kepone were detected
in the higher level experiments.
The obvious failure of the Injection head-afterburner combination in
Experiment 5 does not lend itself to a ready explanation. The injection head
design was not conventional, as is discussed in Section 4.3.1, and could not
be directly tested for its ability to entirely vaporize the acetic acid solu-
tion under the conditions that occur within the feed duct. On the other
hand, the flame out detector within the afterburner was not sufficiently
rapid in response to preclude a momentary flameout with the result that con-
siderable gas could pass through without the normal residence time. In the
analysis of the scrubber effect in Section 7.2, it could with justification,
be assumed that the observed Kepone feedthrough in Experiment 5 was in fact
due to the lack of thermal capacity of the afterburner and thus these results
do represent the efficiency of the afterburner. If this is assumed to be
true, then it seems that the primary destruction of Kepone occurred within
the pyrolyzer.
The Surface Combustion incinerator system depended on the fan located on
top of the scrubber to provide the motive force for gas transport through the
entire system. In particular, the ambient pressure within the kiln was main-
tained at slightly below atmospheric by the combined effect of this fan and
the gases generated by the flame input to the kiln as well as from the evap-
orating water and combustion fumes from the sludge. During the period where-
in the coincineration experiments were being conducted, there is evidence
that the kiln experienced excursions of positive pressure. Part of the evi-
dence for this statement arises from visual observation of steam rising from
the ports on the kiln, from the observation of smoke during the period after
the sight glass fell out but more strongly from the observation of Kepone
losses from the kiln. The latter information derives from the observation
that the high volume sampler that was located on the roof of the Mixing Room
so as to sample the exhaust fan from the kiln room. During the period 18
February through 25 February, this sampler picked up Kepone emissions.
During this same time, the level of .Kepone found in the stack was very much
below that detected by the high volume sampler. Fortunately, other high vol-
ume samplers located down wind from the offender showed that dilution effects
had reduced the observed levels to well below the action level.
The discussion on the Scrubber Effect in Section 7.2 indicated that
there was actually no provision for the determination of the actual volume of
the scrubber at any particular time. This necessitated that one assume a
volume and calculate the level effects. Had the system been designed for
research, such provisions would surely have been made.
49
-------
REFERENCES
1. Duvall, D. S., and Rubey, W. A., Laboratory Evaluation ofHigh-Tempera-
ture Destruction and Pesticides, EPA/2-76-299, December, 1976.
2. "Standard of Performance for New Stationary Sources," Federal Register
36 (247): 24876-24895 (23 December 1971).
50
-------
APPENDICES
APPENDIX A. FACT SHEET - KEPONE BURN
1. Data from Duvall and Rubey at UDRI have shown that Kepone is com-
pletely destroyed at temperatures in excess of 500°C (932°F) (Figure
21, their report). These results were obtained in dry air without
flame and with 1 sec residence time.
2. Data from Duvall and Rubey at UDRI also show that DDT (p-p'-DDT) under
similar conditions is completely destroyed at 450°C (842°F) .
3. Work by Versar (Contract 68-01-1587) demonstrated a destruction ratio
of over 99.99% for DDT during co incineration with sewage sludge at 650°C
(1200°F) nominal temperature and afterburner residence times on the
order of 0.1 sec.
•
4. The inference from the above is that the conditions within the surface
combustion furnace/afterburner (1426°C - 2600°F with residence time of
2 sec) is more than adequate for complete destruction of Kepone.
5. The experimental protocol is designed as follows:
Exp. 1. Injection of Kepone solution at the rate of 2.5 x 10 gm/min
for a total injection time of 4 hr for a total injection of 6 mg
(0.0002 oz) of Kepone.
The stack sampling and subsequent analysis is capable of detecting a
quantity of Kepone that is less than 1 millionth of the hourly injection
rate. Thus, in this primary experiment, even if the afterburner had no
effect on the Kepone, the airborne concentration at the ground 100 ft
from the stack would not exceed 2.8 x 10~8 gm/m^ = 2.5 x 10~ H gm/liter.
Assume that a 145-lb human has a lung tidal rate on the order of 5 11-
ters/min and he is exposed to Kepone-laden air at a level of 2.5 x
10"11 x5x60x4=3x 10~8 gm.
Published data(2) suggest LDcQ~1.32 x 10~1 gm/kg body weight for Ke-
pone in rats. Assume that the same LD5Q obtained for humans; then
145 Ib = 66 kg
.7 gm
Hence total exposure ~3 _ of LD^Q dose.
100,000,000
51
-------
Needless to say, no such exposure Is reasonable to expect, and the evi-
dence for complete combustion of the Kepone is persuasive.
6. The total amounts of Kepone to be used in the preliminary experiments
are as follows:
(1) 6 x 10-3 ^
(2) 0.60 gm
(3) 60 gm
(4) 6000 gm
(5) 0.60 gm
(6) 0.60 gm
TOTAL 6.062 x 103 gm = 13.4 Ib
7. Safety Arrangements:
(a) General Public
In view of the computation in Section 5, a level of Kepone emission
(measured at the stack) of less than 1 x 10~^ gm/m3 is sufficiently
stringent to assure public protection. The analytical/sampling
techniques involved are capable of detecting 5 x 10~12 gm Kepone,
which for aim3 sample (^28 ft3) represents an emission level
100,000 times below the safe level.
On the completion of an experiment, the analytical data will be
examined by a committee of senior environmentalists representing
the community, the state, and the Federal EPA. This group will
have the final say as to whether it is safe and prudent to go to
the next step of the experiment. In all cases, an emission that
approaches the limit of 1 x 10~6 gm/m3 will preclude proceeding
further.
(b) Laboratory Personnel and Observer
(1) All Kepone used in this experiment will be in the form of
solutions in sodium hydroxide/water and will be maintained in
sealed containers. Feed of these solutions will be through
tygon tubing directly into the furnace. At no time will
Kepone feed solutions be exposed to the laboratory air.
(2) All safety and health precautions will be directed and over-
seen by the Safety Group made up of recognized representatives
of local and state health departments.
(3) All personnel entering the laboratory will receive blood tests
before and after possible exposure.
8. Pilot-Scale Experiments
52
-------
With the successful completion of the direct injection experiments (#1
through 6), additional experiments will be conducted with sewage sludge
and soil samples, as follows:
(7) Uncontaminated sludge
(8) Hopewell sludge
(9) Kepone-injected sludge
(10) Kepone-containing sediments
(a) Kepone quantities
The Hopewell sludge contains ^ I ppm Kepone,
thus: 1000 Ib sludge - 0.5 gm Kepone
injected sludge I - 2 x 10^ gm Kepone
injected sludge II- 4 x 10 gm Kepone
sediments - 2.5 gm Kepone
The injection process will require that Kepone solution be injected
into the sludge just before the admission of the combined Kepone
sludge into the furnace. The entire experiment, if completed, will
involve at most approximately 150 Ib Kepone. Actually, a total
of 150 gal of Kepone solution is involved at most.
It is planned to initially ship 15 gal of Kepone solution to the
test site. This is sufficient to complete the first six experi-
ments. Only after these experiments have been successfully run
will the additional material be shipped.
(b) Sampling/Analysis
In the pilot-scale experiments, sampling and analysis will be ex-
tended to scrubber water (which will be impounded until it is
determined that there is no Kepone therein) and to the furnace
residuals; these in addition to the stack sampling.
9. Waste and contaminated materials:
(a) Experimental Program is Completed as Proposed - Case I
At the completion of the experiment, all contaminated equipment,
supplies, and residues will be incinerated, with the usual test and
analytical procedures being used. This will be effective since the
fact that the experiments have been allowed to go to completion
53
-------
infers that the incineration does indeed completely remove Kepone.
(b) Experimental Program Terminated Before Completion of Proposed Work-
Case II
Early termination of the experiment will result from the failure of
incineration to completely destroy Kepone. In this event, all con-
taminated materials, supplies, and equipment will be dismantled and
returned to Hopewell in sealed containers.
APPENDIX B. WIPE TEST PROCEDURE
Open the Wipe Test Packet. Remove the gloves from the packet and put
them on without bringing the outside of the gloves into contact with anything
other than the gloves or the inside of the glove package.
Remove the sampling paper envelope and the sampling scale. Take the
15-cm Whatman #4 paper in the right hand. Place the 30-cm sampling scale
against surface to be wiped with the left hand. Wipe the surface the length
of the sample scale.
Move the sampling scale to a new location.
Wipe five separate areas for each sample.
Replace the filter in the envelope, seal it, and record the location, date,
time, and initials of sampler.
54
-------
TABLE B-l KEPONE WIPE SAMPLES 1/12/77
Sampled Description Wipe Sample Level of
f micrograms 'N Contamination
V 1125cm2 / (microgms/sq.ft.)
1 blank .003 .002
2 walls & floor of lab .01 .008
3 walls of lab ND ND
4 floor-kiln rra. ND ND
5 walls-kiln rm. ND ND
6 floor-mixing rm. ND ND
7 walls-mixing rm. ND ND
8 floor-all rooms shower trailer ND ND
9 walls-all rooms shower trailer ND ND
10 control rm. floor ND ND
11 control walls & equipment ND ND
12 sampling platform floor ND ND
13 sampling platform walls & equipment ND ND
*ND = No Kepone detected in sample.
55
-------
TABLE B-2 KEPONE WIPE SAMPLES 1/24/77
Sample// Description Wipe Sample Level of
/micrograms \ Contamination
\ 1125cm2) (microgms/sq.ft.)
14 mixing rm. walls before 2.53 2.08
opening Kepone
15 mixing room floor before 0.15 0.12
opening Kepone
16 mixing room floor after 0.35 0.29
opening Kepone
17 mixing room walls after -*
opening Kepone
18 kiln room floor after opening Kepone - -
19 kiln room walls after opening Kepone ND ND
20 lab floor ND ND
21 lab walls ND ND
22 locker rm. floor ND ND
23 locker rm walls ND ND
24 shower rm. walls ND ND
25 shower rm. floor 0.0197 0.0163
26 sampling platform floor 0.014 0.011
27 sampling platform walls ND ND
28 operations & control rm. floor
29 operations & control rm. walls 0.028 0.023
30 change room floor ND ND
31 change room walls ND ND
laboratory accident, sample lost.
56
-------
TABLE B-3 KEPONE WIPE SAMPLES 1/31/77
Sample// Description
32 change rm. floor
33 hallway floor
34 blank
35 mixing rm. floor
36 mixing rm. walls
37 kiln room floor
38 left in change rm.
39 left in change rm.
Wipe Sample Level of
(micrograms \ Contamination
HZScm^) (microgms/sq.ft.)
<.0.02
<0.0112
<0.02
<0.02
«3.02
<0.02
<0.02
<0.092
<0.02
<0.02
<0.02
<0.02
57
-------
TABLE B-4 KEPONE WIPE SAMPLES 2/22/77
Sample// Description
43 kiln rm. walls
44 kiln rm. floors
45 mixing rm. floor
46 *
47
48 mixing rm. walls
49 mixing rm. floor in area of spill
50 hall floor
51 change rm. floor
52 sampling platform floor
53 sampling platform walls
54 operation & control room floor
55 operation & control room walls
56 laboratory floor
57 laboratory walls
58 locker room floor
59 locker room floor CLEAN
Wipe Sample Level of
/micrograms \
\ 1125cmz /
^» ~
0.0015
0.0024
1.56
ND
ND
0.36
L 1.8
0.78
0.0134
0.186
ND
ND
ND
ND
ND
ND
0.3
Contamination
(microgms/sq . f t .
0.0012
0.0020
1.29
ND
ND
0.30
1.5
0.64
0.0110
0.153
ND
ND
ND
ND
ND
ND
0.2
*Sample identification lost in transit.
58
-------
TABLE B-5 KEPONE WIPE SAMPLES 2/25/77
Sample// Description ,Wlpe Samplex
, / micrograms
60
61
62
63
64
65
66
67
68
69
70
71
72
73
74
75
76
77
78
kiln rm. walls
change rm.
change rm.
hall walls
mixing rm.
mixing rm .
floor
walls
walls
floor
kiln rm. floor
locker rm.
locker rm.
shower rm.
laboratory
laboratory
shower rm.
control rm
samp, plat
samp, plat
control rm
floor
walls
floor
walls
floor
walls
. floor
. floor
. walls
. walls
Level of
Contaminat ion
1125cm2 / (microgms/sq.ft.
* •** ~"
0.17
0.17
0.00008
0.4
0.00008
0.00048
0.00252
0.00004
0.02
ND
0.00005
ND
ND
0.00005
0.00002
ND
ND
ND
ND
0.14
0.14
0.00007
0.3
0.00007
0.00040
0.00208
0.00003
0.02
ND
0.00004
ND
ND
0.00004
0.00002
ND
ND
ND
ND
59
-------
TABLE B-6 KEPONE WIPE SAMPLES 3/1/77
Sample// Description Wipe Sample Level of
/ micrograms \ Contamination
\ il25cm^ / (microgms/ sq.ft.
79
80
81
82
83
84
85
86
' 87
88
89
90
91
92
93
94
95
96
97
samp. plat, floor 0.08
control rm. walls
locker rm. floor
locker rm. walls
shower rm. floor
shower rm. walls
samp . plat . walls
control rm. floor
lab floor & counter (northside)
lab trailer Southside (office)
change rm. floor
change rm. walls
VOID
hall floor
hall walls
mixing rm. floor
mixing rm. walls
kiln rm. floor
kiln rm. walls
0.05
0.13
0.13
0.26
0.40
0.06
0.08
0.13
0.26
12.4
0.52
-
43.3
1.6
36.6
3.66
3.0
1.4
0.07
0.04
0.11
0.11
0,21
0.33
0.05
0.07
0.11
0.21
10.1
0.43
-
35.8
1.3
30.1
3.01
2.5
1.2
60
-------
TABLE B-7 KEPONE WIPE SAMPLES 3/3/77
Sample// Description Wipe Sample Level of
/ micrograms \ Contamination
^ 1125cm2 I (microgms/sq.ft.)
99 change rm. floor ND ND
100 hall floor 1.89 1.56
101 hall walls 0.04 0.03
102 mixing rm. floor 3.3 2.7
103 mixing rm. walls 0.2 0.2
104 kiln rm. floor 0.3 0.2
105 kiln rm. walls 0.05 0.04
61
-------
TABLE B-8 KEPONE WIPE SAMPLES 3/7/77
Sample// Description Wipe Sample Level of
/micrograms\ Contamination
{ 1125cm2 ) (microgms/sq.ft.)
106 hall floor <0.01 <0.01
107 mixing rm. floor -*0.01 <0.01
62
-------
APPENDIX C. LABORATORY EQUIPMENT AND SUPPLIES ON SITE
Laboratory Equipment
The laboratory equipment that was transported to the site consisted
of the following items:
Gas Chromatograph - Hewlett Packard Model 5700 series equipped with
a Ni*>3 electron capture detector and a Hewlett Packard Model 3380A Inte-
grator for both peak area determinations and for the preparation of a hard
copy of the chromatogram.
Gas chromatographic columns of pyrex glass (180 cm long x 4 mm ID)
packed with:
a. 5% OV-210 on gas chrom Q (100-120 mesh)
b. 1.5% OV-17 + 1.95% QF-1 on gas chrom Q (100-120 mesh)
c. 3% OV-210 on gas chrom Q (100-120 mesh)
d. 10% OV-1 on chromosorb-W (AW).
Concentrator - An elevated (45°C) evaporator using a gentle (5-10 ml/
min) stream of dry nitrogen gas.
Assorted Glassware -
a. Graduated cylinders, 10, 50, 250 ml - one dozen each
b. Erlenmeyer flasks with ground glass stoppers: 25, 50, 10&, 250,
500 and 1000 ml - one dozen each
c. Separatory funnels with teflon stop cocks: 50, 125, 500, 1000
and 2000 ml - six of each
d. Pipets - Pasteur, glass disposable, 1, 2, 5, 10 ml - 6 dozen of
each
e. Evaporative flasks and test tubes - graduated 15, 50 and 250 ml -
two dozen of each
f. Microsyringe, 10 yl - six dozen
g. Tweezers, spatulas, etc., teflon coated
h. Glass columns with fritted discs and reservoirs.
Reagents, Solvents and Standards
a. Benzene, methanol, hexane, isoctane, petroleum ether, diethyl
63
-------
ether (all pesticide grade, glass distilled)
b. Sodium sulfate Fisher Certified, granular, anhydrous
c. Florisil, activated
d. Sulfuric and hydrochloric acid, Fisher Certified (ACS)
extracted with benzene
e. Sodium hydroxide l.ON (ACS) pre-extracted with benzene
f . Triple distilled water
g. Reference Materials:
1. Kepone, hexachlorobenzene, hexachlorocyclopentadiene}
mono and dihydro Kepone, reference grade all provided
by U.S. EPA
2. Stock standard Kepone solutions - 200 yg/ml in 98%
benzene + 2% methanol (EPA)
3. 1 yg/yl in benzene from anhydrous Kepone used as
secondary reference
h. Working standard solutions of Kepone and possible degradation
products
*
5
10 pg/yl
30 pg/yl all in 99% benzene + 1% methanol
50 pg/yl
100 pg/yl
* pg = 1 x 10~12 gm.
APPENDIX D. PRE-BURN EXPERIMENTAL PROTOCOL
Incineration Test Program Objective
The proposed incineration test program will establish procedures for
the incineration of the Kepone contaminated sewage sludge at the lagoon in
Hopewell, Virginia. It will also help establish public confidence in pro-
grams for the incineration of Kepone and Kepone contaminated substances.
The following information regarding the incineration of Kepone and Kepone
contaminated substances will be studied by this program.*
The effectiveness of incineration to destroy Kepone (and its hazardous by-
products) at various time-temperature combinations and Kepone concentrations.
64
-------
The effectiveness of Incineration to produce a residue free from Kepone
(and its hazardous degradation products) which can be safely disposed
of by normal means.
Parameters for sludge decontamination and incineration.
Parameters for equipment design.
Background Technology
General - The following summary of information applicable to this in-
cineration test provides the background for the technology to be employed
in this incineration test.
Laboratory Evaluation of High Temperature Destruction of Kepone and Re-
lated Pesticides —
University of Dayton Research Institute
D. S. Duvall arid W. A. Rubey
May 1976
Abstract — The serious problems concerning the Kepone Manufacturing opera-
tions in the Hopewell, Virginia area have been widely publicized. Disposal
problems and environmental cleanup associated with Kepone being found in
soil, water, sewage sludge, etc., have been substantial. Thermal disposal
was considered to be a primary means for solving this disposal problem.
However, basic high-temperature data on Kepone were lacking; accordingly,
the objectives of this study were directed to provide necessary information.
This study was concerned with thermal destruction testing conducted with
three pesticides: Kepone, Mirex, and DDT. A specialized laboratory tech-
nique incorporating a two-stage quartz system (vaporization first, then
high-temperature exposure) was developed. It is important to note that in
this system the pesticide was first converted to the gas phase, then ex-
posed to the high-temperature destruction conditions. Critical parameters
of temperature and residence time were accurately measured. Both the Ke-
pone and DDT molecules, at a residence time of 1 sec, were essentially de-
stroyed at 500°C; however, Mirex, at the same residence time, required
700°C for destruction.
EPA's Chemical Waste Incineration Program by John Schaum and Alfred Lindsey,
1975.
Engineering Feasibility Report - Destruction of Kepone Contaminated Waste
in the Lagoon located at the Hopewell Sewage Treatment Plant by Design
Partnership, May 20, 1976 0
Conference - Toledo, Ohio, 23 June 1976 - This meeting between representatives
from EPA, the State of Ohio, the City of Toledo, D. P. Versar, Inc., and
Surface Division, Midland-Ross dealt with the activities related to the
incineration test of Kepone in Toledo and public reaction c
65
-------
Conference - Washington, DC, 8 July 1976 - This meeting held at EPA was
attended by representatives of EPA, the Commonwealth of Virginia, the
State of Maryland, University of Dayton Research Institute, Allied Chemical,
and D. P. Versar, Inc.. The purpose of the discussion was to share tech-
nology concerning the thermal destruction of Kepone.
Project - 437 - 1973 - Research of Pesticide Disposal by Sewage Sludge
Incinerators by Versar, Inc.
Project - 465 - 1975 - PBC Incineration by Versar, Inc.
Project - 454 - 1974 - Microeconomic Analysis for Selected Toxic Substances
by Versar, Inc.
Project - 474 - 1974 - Microeconomic Study of Various Toxic Substances by
Versar, Inc.
Project - 461 - 1975 - Gas Stream Sampling by Versar, Inc.
Project-464 - 1975 - Water and Waste Water Analysis by Versar, Inc.
Determination of Incinerator Operating Conditions Necessary for Safe Disposal
of Pesticides by Thomas L. Furguson, Fred J. Bergman, Gary R. Cooper, Ray-
mond T. Li and Frank I. Honea - EPA-600/2-75-041
Summation of Conditions and Investigations for the Complete Combustion of
Organic Pesticides by Boyd T. Riley, Jr. EPA-600/2-75-044
Authority, Participants, and Observers
The incineration test is being done for the Kepone Task Force of Vir-
ginia. Due to the nature of the chemical involved and the concern with
public and environmental safety, the incineration test program will be under
the direction of the Test Burn Authority.
Incineration Test Authority — The Incineration Test Authority will be made
up of officials from the Commonwealth of Virginia, EPA/MERL,
Toledo Pollution Control Agency, EPA Region V and Ohio EPA.
The Authority will have the following responsibilities:
Direct the test program and authorize decisions required during the
test progression.
• Interface with regulatory agencies.
• Prepare and authorize all press releases.
Transport and dispose of residues.
• Assure the public safety.
66
-------
The Incineration Test Management Group — The Incineration Test activities
are under the direction of Design Partnership, Inc., consultants to the
Kepone Task Force. The consultants have arranged for Surface Division,
Midland-Ross to provide the incineration test facilities and Versar, Inc.,
to provide testing and laboratory services. Representatives of these firms
will form the Incineration Test Management Group with the following structure:
• The Project Manager will be from Design Partnership and will be in
overall control of the project.
• The Operations Manager will be from Surface Division, Midland-Ross
and will be in charge of incineration operations.
• The Sampling and Testing Manager will be from Versar, Inc., and be
responsible for all sampling and laboratory work.
• Industrial Hygienist
The Incineration Test Management Group will have the responsibility and
authority for the following aspects of the project:
• Safety and Hygiene on the incineration test site.
• Burn procedure.
Documentation.
Observers — Other people, agencies, and organizations interested in the
incineration test will be considered visitors and observers and will be
admitted only by invitation of the Incineration Test Authority.
Description of Facilities
The Incineration test will be done at the Research Laboratory of Sur-
face Division, Midland-Ross in Toledo, Ohio.
Incineration Equipment — The following equipment is available in the Re-
search and Development Laboratory:
Rotary kiln pyrolyzer — The Rotary Kiln Pyrolyzer is five feet in diameter
and 10 ft long. It rotates at 1 rpm and has capability for continuous load-
ing and unloading as well as two hatches for batch loading and unloading.
It is heated directly by hot gases and from a 1 MM BTU/hr capacity burner.
Charge and discharge connections for the hot gases have rotary seals to
prevent leakage of gases into or out of the kiln. The kiln can be operated
at about 1000°F.
Fume incinerator (high temperature afterburner) — The Fume Incinerator to be
used for the pilot tests is equipped with two 500,000 BTU/hr capacity throat
mix burners. The residence chamber volume is about 30 ft^. The incinerator
is furnished with temperature controller and high limit safety shut-off
67
-------
instrumentation.
Quench — Quench is used to cool the gases from the incinerator by evapora-
tive cooling. It is equipped with recirculation tank, pumping system, and
spray nozzles. Emergency cooling water spray nozzle is also provided.
Scrubber — Scrubber is a 30-in. diameter tower packed with 2-in. intalox
saddle plastic packings. The packed bed height is about 6 ft. Scrubbing
is done by 18% caustic solution flowing counter current to gas stream. The
scrubber is equipped with I.D. fan and recirculation tank. Scrubbing fluid
pH is controlled by adding caustic solution. Liquid level in the recircu-
lation tank is maintained by adding make-up water. A controlled quantity
of liquid is purged from scrubber to a brine retention tank continuously.
Sampling and Analysis Equipment —
The following equipment is either available at the Research and Develop-
ment Laboratory, or will be brought to the site by Versar, Inc.:
1. 02, CO, C02, and Hydrocarbon Analyzers (available)
2. The gas chromatograph and its related equipment which includes a
Hewlett Packard Model 5710A gas chromatography system and a Fisher
Model 5000 integrating recorder. The gas chromatograph is equipped
with an electron capture detector (Ni^3). TWO types of columns
are used: A nonpolar 3% OV-1 on 100-200 mesh gas chrom Q.
Moderately polar, i.e., 1.5% OV-17 + 1.95% OF-1 on 100-200 mesh
gas chrom Q.
These columns have been tested with analytical standards of Kepone and
HCB standards and have been found to be heat stable, efficient and to have
good resolving power.
3. RAC Staksampler, control unit, sampling box with stainless steel
sampling probe and pitot assembly and all the assorted glassware.
4. The feed assembly including pump, feed lines and injection probe.
Facilities —-
The facilities on location will include the incineration test facility,
a sample testing laboratory, a conference room, and a temporary office for
the use of the Incineration Test Authority and the Incineration Test Manage-
ment Group.
Sample Transportation
Pure Kepone — Pure Kepone will be transported to Toledo, Ohio, in double
sealed containers.
68
-------
Keoone Contaminated Sludge —
Kepone contaminated sludge will be supplied by the Kepone Task Force of
Virginia. The sludge will be loaded in sealed drums at the lagoon in Hope-
well, Virginia and transported to Toledo, Ohio. The sample will be two 55-
gal drums (30 - 65% solids, 0-57 ppm Kepone).
Blank Sludge —
Blank sludge will be obtained from a sewage treatment plant in the Toledo
area and transported to the site.
Incineration Test Program
The critical aspect of the proposed program lies in the cumulative toxic
nature of Kepone which imposes the necessity of absolute assurance that there
is no loss of this material to the environment as a result of these tests.
The absolute sensitivity of the analytical methods available are very high:
Specifically, the gas-chromatograph electron capture detector (G.C.E.C.) is
capable of unambiguous detection of 2 - 3 x 10"^ gm of Kepone. Thus, by
suitable selection of the size of the samples that are taken from the
emergent streams from the incinerator, highly sensitive observation of all
residual matter may be made.
The stack exhaust stream is the only uncontrollable output stream from
the incinerator and hence represents the critical path to the environment.
In the absence of a published emission standard, it is proposed to adopt the
criterion of safety as being an emission (at stack temperature) not to exceed
1 x 10~" gm/m-*. This factor is such that, on dispersion and dilution in
the atmosphere, the resulting ambient air concentration would be less than
2.5 x 10~° gm/nr (this latter concentration has been taken to be the interim
permissible limit to be used until promulgation of a suitable standard) when
account is taken of the dilution factor of 40 or more.
*The hot polluted stream from the stack ejected into the surrounding air
creates considerable turbulence, which with the natural mixing due to air
currents, causes rapid dilution and mixing of the emergent plume. Under
these circumstances, according to Smith^^, the concentration of any given
pollutant appears, at least initially, to decrease exponentially with the
distance from the point of emission, according to the empirical equation
C(x) = C(o)K x-p
where x is the (downwind) distance, K is a parameter that describes the source
and the nature of the specific pollutant, and p is a parameter varying be-
tween 1.5 and 2. Since the values of K can vary between 0.1 and 10, it is
seen that the concentration at a point 100 ft downwind would be of the order
of 1 percent of that at the stack. More complex descriptions have been given,
but the general result is much the same as that from Smith. See also Cadle(2).
(1) Smith, M.E., "Chemical Reactions in the Atmosphere."
Interscience, New York, 1961.
(2) Cadle, R.D., "Particle Size." Reinhold. New York, 1965, pp. 267 ff.
69
-------
Initial Program --
The initial phase of the program is designed to determine the efficiency
of combustion of Kepone under conditions that guarantee complete safety. This
phase consists of conducting a series of tests with the injection of Kepone
solutions directly into the duct leading from the kiln to the fume incinera-
tor.
Initial test — The initial test will involve the injection, upstream of the
fume incinerator, of Kepone solutions at a rate of 2.5 x 10~5 gm/min which is
sufficiently low that, even in the absence of any combustion, the emergent
stack stream concentration would not exceed the criterion emission level.
Sampling of the stack stream will be carried out such that levels of less
than 1 percent of the criterion emission level will be detectable. After
suitable assurance that combustion is complete, additional direct injection
tests will be conducted at increasing concentrations until it is clear that
conditions existing with the fume incinerator are such as to completely com-
bust the Kepone. On the completion of these preliminary low level tests the
program will proceed to larger scale studies with sewage sludge.
Kepone solution will be injected into the duct at a rate that will in-
sure that, even in the absence of combustion, the emergent (stack) level
will not exceed the criterion level of 1 x 10~6 gm/m^. During this test the
fume incinerator will operate at 2300°F while samples of particulate and
gaseous matter are conducted.
Follow-up tests — Upon the successful completion of the initial test(by
successful, it is meant that the emergent Kepone level is less than 1 per-
cent of the permissible level) additional tests will be conducted at in-
creasing Kepone levels as follows:
Test Temp. (°F) Time (sec) Rate (gm/min)
1 2300 2 2.5 x 10~5
2 2000 2 2.5 x 10~5
3 2000 2 2.5 x 10~2
4 2000 2 25
5 2000 1 25
6 1900 1 25
In each case, triplicate stack samples, taken in sufficient volume
to allow detection of 1 percent of criterion emission rate, will be analyzed
before the next test is conducted.
In all cases following the initial test, samples of all aqueous streams
will also be taken for analysis.
70
-------
Consultation — At the completion of the analyses for each test, a decision
by the Incineration Test Authority will be made as to the safety in pro-
gressing to the next test.
Kepone injection — As indicated in Section 5 the Kepone solutions will
be injected into the hot gases from the kiln at some convenient point before
entry into the fume incinerator. A stainless steel nozzle assembly will be
fabricated and will project through the wall into the duct. The assembly will
be provided with leak-tight seals at the point of entry. Kepone solutions
will be introduced through a metered peristaltic pump from a closed reservoir
at rates as indicated below:
Test 1-10 ml/min of solution containing
2.5 x 10~3 gm/liter of Kepone
Test 2-10 ml/min of solution containing
2.5 x 10~3 gm/liter of Kepone
Test 3-10 ml/min of solution containing
25 gm/liter of Kepone
Test 4 - 200 ml/min of solution containing 125 gm/liter of Kepone
5 Same as 4
6 Same as 4
The above tests will require a total of 80 liters of solution made up
at 125 gm/liter of Kepone in NaOH solution (approximately 22 gal).
The feed line external to the furnace injection line will be of tygon
which will be incinerated at the completion of tests.
Pilot Scale Test —
On the successful completion of the preliminary test, attention will
turn to practical scale tests. In each case all emergent streams will be
sampled during the1 run and advancement to the next step would be conditional
upon satisfactory completion of the previous step. In all cases, the emission
will be the controlling factor.
The specific practical scale program will be as follows:
* Sludge blank - some 1,000 Ib wet weight (18% solids) of sludge ob-
tained locally will be incinerated.
• Hopewell sludge - some 500 Ib wet weight (18% solids) of Hopewell
sludge containing up to 500 ppm (dry weight) will be incinerated.
• Doped sludge - 1,000 Ib wet weight; (18% solids) sludge obtained
locally will be doped to the level of 25% dry weight Kepone and
will be incinerated.
71
-------
Doped sludge - 1,000 Ib wet weight (18% solids) of sludge obtained
locally will be doped to the level of 50% dry weight Kepone and incinerated.
In each case the sludge will be injected by Moyno pump at a rate of 100
Ib/hr of sludge. Each run will be of sufficient duration as to allow tripli-
cate (quadruplicate for the sludge containing Kepone) stack gas sampling. In
addition, periodic samples of the scrubber liquor and the scrubber water will
be taken.
Sampling and Analysis
As in the case in all situations wherein it is necessary to sample
streams of gases of liquids, the size of the sample and the method whereby
it is taken are established by the dual requirements of allowable levels of
the particular contaminant and the ultimate sensitivity of the analytical
method.
In the case of Kepone, the final detection and quantitation step ex-
hibits an ultimate detectivity of 2 to 3 x iO~^ gm. If provision is made
for analytic recovery during the extraction and concentration phases, the
practical ultimate detectivity is taken to be 5 x 10~12 gm. This latter,
practical detection limit, will be used in what follows.
Air Stream Analyses —
It is proposed that the primary monitoring point in the incineration
system be the emergent stack. Air stream analysis will be accomplished with
a full EPA Method Five sampling procedure. The (heated) sampler probe will
be operated along two mutually perpendicular traverses with full provision
for isokinetic sampling. The impinger train will utilize a glass cyclone
and .045 micron glass fiber filter assembly followed by the conventional four-
bottle impinger train. The non-particulate impinger solution (confined to
the first two impingers) will be 1.0N NaOH in deionized distilled water.
Drying of the gas stream before metering will be accomplished by indicator
DrieriteW. The metering equipment will be the RAG stacksampler assembly.
As an additional safety feature, in order to produce essentially real
time analyses, the first of the triplicate gas stream samples will be taken
with the RAG impinger train modified so as to introduce a small cartridge
packed with 10 to 20 gm of uncoated, washed and heat activated Chromosorb
101 absorbent interposed between the 0.45-micron filter and the first impinger
bottle. Although this method does not have the force of extensive use, it
does offer the great convenience that subsequent to sampling, the cartridge
may be removed, the adsorbed chloro carbons removed by hexane washing and
immediately analyzed by chromatography. This method has been shown to be
applicable for chlorinated hydrocarbons to levels of the order of 15 ppt(*)
*Mann, J. B., Enos, H. F., Gonzales, J., and Thompson,
J. F. Environ. Sci. and Techno., 8, 584 (1974).
72
-------
(2 x 10~8 gm/m3) and will be used to get a quick check of the levels of Kepone
and also of the principal chlorinated hydrocarbons (hexachlorobenzene, for
example)** in the exhaust stream.
If the observed levels are acceptable, then the test will be continued
for sufficient time to allow two additional samples to be collected by the
more traditional NaOH impinger train.
Air stream sample volume — As suggested above, the criterion advanced for the
distribution between a successful and an unsuccessful test is a Kepone level
of not more than 1 x 10~6 gm/m3 (at stack temperature). The analytical method
used for Kepone (see Section 7 ') is found to have an absolute detection
limit ^ 5 x 10~12 gm of Kepone. Since the sample extraction procedure re-
sults in a final concentrated sample volume of 0.5 cm3 and the normal injec-
tion volume is 10 A (10-2 Cm3)t it is then necessary to collect a total of
2.5 x 10" gm Kepone from the sampled gas stream Thus, processing aim3
gas sample (^ 0.8 m3 at box temperature) should yield a total Kepone sample
of the order of 40,000 times the detection limit if the level in the gas
stream were at the criterion level of 1 x 10-6 gm/m3. To put this in a
slightly different way, the detection limit is 0.0025 percent of the crite-
rion level.
Other Emergent Stream Samples —
In addition to the primary samples (the stack gases) it will be appro-
priate to also sample the following on a routine basis:
— The emergent quench water
— The emergent scrubber water
— The ash from the kiln
Additional samples — It will be necessary to sample all charges to the kiln
before the pyrolysis of those samples. In addition, background analyses will
be made of the feed water and of any other material admitted to the furnace
system. Further, environmental samples from within the prototype facility
will be analyzed on the completion of the experimental program - this to aid
in any clean up that may be required.
Analytical Method —
Initial sample preparation — Non-aqueous samples, if they are organic
in nature, are first macerated with an equal weight of isopropanol and then
with benzene and anhydrous sodium sulfate. After being allowed to equilibrate
for 12 hr, the filtered extract is evaporated to dryness by impinging a
stream of purified air on the surface of the liquid. The resulting residue
is treated in a manner similar to inorganic specimens.
The dried residue or inorganic matter is transferred to a separatory
**Duvall, D. S., and Rubey, W. A. Private Communication.
73
-------
funnel with small volumes of N-hexane to make a total volume of 100 ml to
which is added 25 ml 1:1 oleum mixture. Shake vigorously, allow layers to
separate and discard the lower layer. Repeat the process several times,
finally washing hexane layer with 10 ml concentrated sulfuric acid, followed
by 5 ml water. Discard all washings.
Extract the dried hexane layer with 100 ml 0.1 M sodium hydroxide three
times, combining the aqueous sodium hydroxide extracts in a 500 ml separatory
funnel .
Analysis of NaOH solution of Kepone — Add few drops of phenolphthalein
solution to the aqueous extracts in the 500 ml separatory funnel. Add 9M
sulfuric acid until the end point (colorless) is reached. Add a few ml of
9M sulfuric acid to insure an acidic solution. Extract this acidified
solution with 150 ml of benzene. After the phases have equilibrated, draw
off the lower (aqueous) phase and discard.
Filter the benzene through a bed of anhydrous, granular ^2864 into a
300 ml flask. Wash both the funnel and the filter bed with benzene and
washings added to the flask. Evaporate the extract on a steam bath under a
stream of nitrogen until fumes remain. After cooling, and the vapors con-
dense, wash the walls of the flask with ethyl ether. Transfer quantitatively
to a graduated cylinder with small portions of ether. Evaporate the solvent
on a steam bath under a stream of nitrogen to approximately 0.3 ml. Determine
the exact volume. Transfer the concentrate to a small stoppered vial and
freeze until analysis.
The final step involves the injection of a 5 to 10 y aliquot of the con-
centrate into an Electron Capture G.C. System with the following charac-
teristics:
Electron Capture detector using
Column of either
10% DC-200 + 15% QF-1 or
1.5% OV-17 + 1.95% QF-1 on 100/120 GCQ
Carrier gas: 95% Argon + 5% methane
Gas flow: 4-55 ml/run
Injection port: 200?C
Oven temp (isothermal) : 220°C
Detector temp: 250 C
A typical chromatogram derived in our laboratories of Kepone indicates
a retention time of the order of 10.6 min and an ultimate detectivity on
the order of 2.5 x 10~12 gm.
Kepone combustion products — Although the full spectrum of possible inter
mediate combustion productions of Kepone has not been determined, it is
known that hexachlorobenzene is one of the principal products.
74
-------
Operating Variables —
In addition to Kepone and chlorinated hydrocarbon analysis of the discharge
streams from the incinerator, it will also be necessary to collect the
following parametric data:
Sludge feed rate
Kepone feed rate
Kiln temperature
Air and gas flow to the kiln burner
Flow of gases from the kiln
Analysis of gases from the kiln
Pressure in the kiln
Temperature in incinerator
Air and gas flows to incinerator burners
Auxiliary gas flow to the incinerator
Effluent gas flow from the incinerator
Quench liquid flows
Make-up water flow to quench
Temperature of stack gases
Scrubbing liquid flow
Caustic addition flow
Purge brine flow from scrubber
Temperature of gases from quench
Pressure of gases from quench
Flow of gases in the stack
Temperature of scrubbing liquid
Proposed Schedule
In the interest of efficiency and to minimize furnace operation times,
it is proposed that the study be carried out on an essentially two-shift
basis: the daytime devoted to the actual combustion runs and the necessary
sampling and the night shift devoted to analysis. The field operations will
take the following form:
Week 1
Mon./Tues. 1st injection run; sampling/analyses
Wed./Thurs. 2nd injection run; sampling/analyses
Fri./Sat. 3rd injection run; sampling/analyses
Week 2
Tues./Wed. 4th injection run; sampling/analyses
Thurs./Fri. 5th injection run; sampling/analyses
Week 3
Monday 6th injection run; sampling/analyses
75
-------
Tuesday Sludge blank run; Sampling/analyses
Wednesday Hopewell contaminated sludge sampling/analyses
Thursday Hopewell contaminated sludge sampling/analyses
Friday Toledo sludge @ 25% Kepone
Week 4
Monday Toledo sludge @ 25% Kepone
Tuesday Toledo sludge @ 50% Kepone
Wednesday Toledo sludge @ 50% Kepone
Thursday River sediments
Friday Recap meeting
Week 5
Monday/Friday Clean up
Residual Disposal
Except, of course, for emissions to the air any material at the end of
the test that cannot be disposed of locally due to public health considera-
tions will be transported to Hopewell, Virginia, for disposal.
Emissions to the Air —
As described previously all air emissions will be constantly monitored.
The test program is designed to ensure that the level of Kepone if emitted
will not reach the maximum level of 1 x 10~6 gm/m^ at stack temperature.
Solids and Liquids —
Ashes and scrubber liquor will result during all incineration tests of
sludge. When pure Kepone is incinerated, there will be no ashes.
All liquid and solid residues resulting from the incineration tests will
be either re-incinerated or repackaged and transported to Virginia for dis-
posal.
Laboratory Residuals —
Same procedures as Solids and Liquids
Spillage and Clean-Up—
Minor spills should they occur will be mopped up. Liquid will be trans-
ferred to the liquid retention tank and rags, etc., will be stored in a
Contaminated-Material Container (CMC). Major spills should they occur will
be absorbed in dry compound. The sweepings will again be placed in the CMC.
All disposable gloves, etc., will be placed in the CMC.
76
-------
Testing program will include incineration of the CMC as part of the
clean-up after incineration tests.
Equipment Clean-Up —
After the incineration test program is complete all equipment and resi-
duals contaminated during the process will be either incinerated or cleaned
with NaOH (which will put Kepone in a solution) for ultimate disposal.
The equipment to be cleaned includes the following:
Moyno pump (stator and rotor) used to pump the sludge
Feed pipe and mixing tank for the sludge
Rotary kiln
Duct between the rotary kiln and the afterburner
Scrubber tower and piping
Quench and pumps
Brine retention tanks
Safety equipment (gloves, respirators, clothing, etc.)
Safety and Hygiene
The prime consideration during the incineration test will be to protect
the personnel, the environment, and the public from being exposed to this
compound. To ensure safety the measures included in this section will be
followed in addition to those normally used.
Incineration Test —
The personnel at the testing facility are experienced with the handling
and burning of toxic and other dangerous chemicals. Such work has been
done and safety procedures are already established.
In order to inform the operating and management personnel about Kepone
and recommend handling procedures a medical briefing will be conducted by
personnel from the Commonwealth of Virginia, Department of Health at the site
prior to the incineration test program.
Only operating and management personnel directly involved with the
incineration test operation will be allowed in either the incineration test
or laboratory areas. Before and after the incineration test they will be
subjected to blood tests to determine if any residual Kepone exists.
Isolation will be accomplished by organizing the incineration test area
and physical facilities such that only those persons whose duties necessitate
their presence are in areas where hazardous materials are handled. Prepara-
tion for incineration tests and equipment readiness will be accomplished
prior to handling of Kepone or Kepone bearing materials or their introduction
into the incineration system.
77
-------
Kepone and Kepone bearing materials will be handled only in closed
systems or in the isolated area designated for mixing, feeding and storage.
The only normal entrance and egress to this area will be through a shower
area with a change of clothes required upon entry and a shower and change of
clothes required prior to leaving the area.
There will be an emergency exit for life safety from this area and a
viewing port to allow observation during the handling procedures.
The control and operation of the incineration and pollution control
equipment will take place in the designated area separated from the mixing,
feeding and kiln areas by barriers preventing air and other materials move-
ment.
Equipment and surfaces in the incineration test area shall be covered
with strippable coverings or plastic film wherever practical. All floors
in the incineration test area will be sealed with either paint or resin
sealants to facilitate cleaning.
Areas within the incineration test area subject to spillage shall be
curbed to contain any foreseeable leakage.
All personnel who have entered the incineration test area for any pur-
pose will shower before leaving the premises and will leave their clothing
including socks and underwear which was worn within the incineration test
area in designated lockers within the contaminated change room. At the end
of the incineration test period this clothing will be incinerated. Street
clothing will be stored in the clean locker room.
Personnel protective equipment worn will be that which is deemed suit-
able for the job and conditions at hand by the Industrial Hygienists assigned
to the incineration test. A list of suitable equipment is attached as Table
D-l.
78
-------
TABLE D-l PERSONAL PROTECTIVE EQUIPMENT
Safety glasses with side shields
Goggles - Sellstrom 882 Fog-free lens
Respirators - Comfo II GMP Type, Part No. 448848, MSA
Cartridges (pesticide) GMP Type No. 448847, MSA
High gauntlet gloves, MSA, Python Neoprene 37994
Paper suits, Edmont-Wilson 55-510
Rain gear, Edmont-Wilson, Coat & Hood 65-110, Bib Overalls 65-120
Boots-Servus, Neoprene 11901, steel toe
Disposable boots (plastic)
Paper boots (paper)
Paper headcover
Disposable towels - obtain locally
Plastic bags (large) - obtain locally
Bag rack - obtain locally
Utility gloves, MSA, 37643 flexible plastic gloves
The above are. examples of equipment needed and does not constitute
an endorsement of the products. Substitution can be made on an equivalent
basis.
The actual number of pieces and sizes of equipment will be determined by
Surface Combustion and will be reviewed at the meeting on September 21, 1976,
in Cincinnati, Ohio.
79
-------
Pure Kepone Transport and Handling —
Since all the Kepone on the incineration test site will be in a liquid
solution, Kepone in the atmosphere (as with dust in the pure powder form)
will be minimized if not eliminated. This means that the exposure to the
operating personnel will be the absolute minimum.
The Kepone will be packaged and transported as previously described.
Kepone containers will be opened by authorized personnel wearing protective
clothing including respirator and goggles. Containers will only be opened in
the incineration test area or the laboratory.
Kepone spills are not anticipated. If there are any, they will be
handled carefully and the clean up material disposed by the procedures des-
cribed in the section on residuals.
Air Sampling and Laboratory Personnel —
Air sampling personnel and laboratory personnel will attend the medical
briefing and will undergo blood tests before and after the incineration test
program. During all times of operation, personnel will wear protective
clothing, goggles and hard hats. Whenever Kepone is handled, respirators
will be used.
Visitors —
No visitors will be allowed in the incineration test area and laboratory
areas.
During the incineration test, visitors will be able to observe the in-
cineration test operation via closed circuit TV from a monitor in the confer-
ence room. A register will be kept of all visitors entering and leaving the
conference room.
Publicity and Communication
Publicity and communication with regard to the incineration test will
be controlled by the Incineration Test Authority (ITA). Under the direction
of the ITA, the Incineration Test Management Group will perform the following
activities:
Escort visitors and inform them of the incineration test and sampling
operation.
Interface with regulatory agencies.
Coordinate the documentation effort.
Press Release —
Press releases will be authorized by the Incineration Test Authority
and cleared through the Toledo Public Information Director.
Prior to the incineration test, Surface Division, Midland-Ross is
80
-------
planning the following pre-incineration test news releases through the Toledo
PID:
30 days prior to test - general newspaper article, science oriented, on
Surface Division work in hazardous waste disposal.
15 days before test - general newspaper article, business oriented,
on Surface Division's new business venture in hazardous waste disposal.
After Kepone contract award and prior to incineration test - newspaper
article to announce R & D program to demonstrate controlled incineration
technology for Kepone disposal.
During and after the incineration test, Surface Division is planning
the following news releases with the approval of the Incineration Test
Authority:
In process - announcement that Surface Division engineers are working
with small quantities of Kepone.
30 days after incineration test - Kepone incineration success story:
1977 - articles in technical journals.
Documentation
The Incineration Test Management Group will be in charge of documentation
of the incineration test program and results.
The Operations Manager will report on the technical aspects of the in-
cineration test, the equipment used, and the residuals.
The Sampling and Testing Manager will report on the test results, on
the air samples, residuals and Kepone inventory.
The Project Manager will write a summary report (including other
aspects, such as transportation, safety and visitors).
During the incineration test, daily oral reports will be made to the
Incineration Test Authority. All day-to-day decisions will be based on
these reports. Distribution of the data will be controlled by the
Incineration Test Authority.
The Project Manager will prepare the final report for submission to the
Incineration Test Authority for submission ultimately to the Virginia Kepone
Task Force.
81
-------
APPENDIX E. FURNACE AND INCINERATOR SYSTEM DATA
oo
N2
KEPONE
SOLUTION
INJECTION
TANK
SAMPLING
PORTS
FIGURE E -I' KEPONE INCINERATION SYSTEM SCHEMATIC
-------
Sat. Temp 184 Deg. F
JKS
3-7-77
00
3230-3730 SCFH Air
340-400 SCFH Fuel
6 - 6.5 GPH Water
Sludge
Kepone 0.9 mg/l
Acetic Acid (9 lit/hr) or 125 SCFH Gas
•n
Si
3)
00
C
3D
(2300 Deg.
F)
27,300 SCFH
Air (20,000 SCFH)
Fuel (1860-1910)
Methane
8
30
5
CD
m
33
49,450
SCFH
Fuel Air
Caustic 7.5 GPM
Water 1.99 GPM
Res. Lime 2.15 sec.
(a) Water in Kiln 1130 SCFH
(b) Water from Fuel 4620 SCFH
(c) Water in Scrubber 2_2,100SCFH
TOTAL 27,850 SCFH (Maximum)
Dry Gas (without leakage) = 21,600 SCFH
FIGURE E-2 FLOW SCHEMATIC-KIT RUN NO. 1
-------
Sat. Temp. 181 Deg. F
JKS
3-7-77
Kepone 0.9 mg/hr
Acetic Acid 9 lit/hr (125 SCFH)
oo
3930-4835 SCFH Air
325-370 Fuel
5.5 - 6 GPH Water
or
960-1040 SCFH
>
•n
3D
CD
c
3D
z
m
3D
27,710 SCFH
Air (20,000 - 20,300 SCFH)
Fuel (1355-1640)
Methane 46,970 SCFH
CO
o
CD
CD
m
3D
Sludge
Res. Time 2.38 sec.
(a) Water in Kiln 1040 SCFH
(b) Water from Fuel 4020 SCFH
(c) Water in Scrubber 19260SCFH
TOTAL 24320 SCFH
Dry Gas (without leakage) = 22,650 SCFH
Fuel Air
Caustic 5.6 GPH
Water 104.9 GPH
FIGURE E-3 FLOW SCHEMATIC - KIT RUN NO. 2
-------
Sat. Terrp. 180 Deg. F
JKS
3-7-77
oo
Ul
(3615-4515) Air
(155-175) Fuel
6-6.7 GPH Water
or
(1040-1170 SCFH)
I Kepone 0.9 gms/hr
I Acetic Acid 9 lit/hr (125 SCFH)
•33
00
c
3D
m
3D
Air (19,700-20.000)
Fuel (570 - 690)
Propane
46,680 SCFH
CO
o
w
CO
Fuel Air
Caustic 6.0 gph
Water 103.8 gph
Sludge
Res. Time 2.37 sec.
(a) Water In Kiln 1170 SCFH
(b) Water from Fuel 3460 SCFH
(c) Water in Scrubber 19140SCF_H
TOTAL 23770 SCFH
Dry Gas (without leakage) = 32,910 SCFH
FIGURE E-4 FLOW SCHEMATIC-KIT RUN NO. 3
-------
Sat. Temp. 180 Deg. F
JKS
3-7-77
00
(42104420) Air SCFH
(175-180) Fuel
6.5 - 7.5 gph Water
I Kepone 90 gms/hr
t Acetic Acid 9 lit/hr (125 SCFH)
m
3J
w
c
30
Z
m
3)
(2000 Deg. F)
26,975 SCFH
Air (19,500 SCFH)
Fuel (520-630) SCFK
Propane 145,725 SCFH
8
ID
CO
m
3J
1
Fuel Air
- Caustic 4.0 gph
•Water 103.5 gph
Sludge
or
(1130-1310 SCFH)
Res. Time 2.44 sec.
(a) Water in Kiln 1310 SCFH
(b) Water from Fuel 3240 SCFH
(c) Water in Scrubber 18750_SCF_H_
TOTAL 23300 SCFH
Dry Gas (without leakage) = 22,425
FIGURE E-5 FLOW SCHEMATIC - KIT RUN NO. 4
-------
Sat. Temp. 179 Deg. F
JKS
3-7-77
Kepone 0 gms/hr
Acetic Acid 0 lit/hr
00
4330 SCFH Air
178SCFHFuel
5.7 gph Water (990 SCFH)
m
•Si
m
c
30
m
(2000 Deg. F)
27,630 SCFH
Air (20,000 - 20,800) SCFH
Fuel 575 SCFH
Propane 46,830 SCFH
CO
O
3)
C
CD
CD
Sludge
Res. Time 2.39 sec.
(a) Water in Kiln 990 SCFH
(b) Water from Fuel 3010 SCFH
(c) Water in Scrubber 1920p_SCjFH_
TOTAL 23200 SCFH
Dry Gas (without leakage) = 23,630 SCFH
Fuel Air
Caustic 0 gph
Water 110.1 gph
FIGURE E-6 FLOW SCHEMATIC-KIT RUN NO. 5
-------
61,520
JKS
3-7-77
Kepone
Acetic Acid
00
00
(4140 - 7640) Air SCFH
<212-345) SCFH Fuel
5.9 - 9 gph Water
(1030-1570) SCFH
m
•x
CD
c
30
(2000 Deg. F)
32,080 SCFH
Res. Time 2.06 sec.
Sludge
0.16gpm
79 Ibs/hr water (1660 SCFH)
J^ Ibs/hr solids
76 Ibs/hr sludge (18% solids)
Air (19,200 SCFH)
Fuel (630-660) SCFH.
Propane
54,370 SCFH
Sat. Temp.
183 Deg. F
U)
o
30
03
CD
m
30
Fuel Air
27 SCFH 6960-7100 SCFH
Caustic 5.25 gph
Water 122.6 gph
(a) Water in Kiln 3230 SCFH
(b) Water from Fuel 4020 SCFH
(c) Water in Scrubber 2227(>_SQF_H_
TOTAL 29540 SCFH
Dry Gas (no leakage) = 24,830 SCFH
out of Scrubber
Ibs of H2O/lb of dry gas = 0.76
FIGURE E-7 FLOW SCHEMATIC - KIT RUN NO. 6
-------
57,400 SCFH
JKS
3-7-77
Kepone - 0
Acetic Acid •
00
(6510-7265) SCFH Air
(295-330) Fuel SCFH
0 Water
m
•33
CO
c
30
m
3)
(2100 Deg. F)
29,070 SCFH
(Maximum)
Air 18,500 SCFH
Fuel (600-640) SCF
Propane
50,380 SCFH
Sat. Tertp.
182 Deg. F
8
30
CD
CD
m
o
Fuel Air
36 SCFH (6750 SCFH)
Caustic 5 gph
Water 117.2 gph (maximum)
Res. Time 2.18 sec.
Sludge (0.145GPM)
1.05 Ibs Kepone/hr
14.60 Ibs Solids/hr
62.45 Ibs Water/hr
_8190Jbs Ac. Acid/hr
87.00 Ibs/hr (18% Solids)
(a) Water in Kiln 1300 SCFH
(b) Water from Fuel 3880 SCFH
(c) Water in Scrubber 2_1J1P_SC_F_H_
TOTAL 26490 SCFH
Dry Gas from Scrubber (no leakage) •
Ibs of H2O/lb. of dry gas = 0.71
23,890
FIGURE E-S FLOW SCHEMATIC-KIT RUN NO. 7
-------
57,035 SCFH
JKS
3-7-77
Kepone- 0
Acetic Acid - 0
vo
O
(6700 - 6800) Air
(255 - 260) Fuel
0 Water
rr!
30
03
c
30
m
30
Air (19,300-19,500)
Fuel (530 - 600) SCFJi
Propane
50,000 SCFH
Sat. Temp.
180Deg. F
8
30
03
CD
rn
3)
Fuel Air
43 SCFH 6950 SCFH
Caustic 0 gph
Water 117.9 gph (maximum)
Res. Time 2.23 sec.
Sludge 0.15 GPM
0.54 Ibs/hr Kepone
15.66 Ibs/hr Solids
69.20 Ibs/hr Water (1450 SCFH)
_4J80Jbs/nr Acetic Acid (25 SCFH)
90.00 Ibs/hr (18% Solids)
(a) Water in Kiln 1450 SCFH
(b) Water from Fuel 3440 SCFH
(c) Water in Scrubber 20500_§CJFH_
TOTAL 25390 SCFH
Dry Gas from Scrubber (no leakage):
Ibs Water/I b of Dry Gas = 0.66
24,610 SCFH
FIGURE E-9 FLOW SCHEMATIC - KIT RUN NO. 8
-------
58,540 SCFH
JKS
3-7-77
Kepone- 0
Acetic Acid - 0
(6750 - 6850) Air SCFH
260 SCFH Fuel
0 Water
•n
m
30
co
3D
m
31,190 SCFH
(Maximum)
Air (20,500 - 21,000) SCFH
Fuel (540 - 590) SCF.H
Propane
51,670 SCFH
Sat. Temp.
179Deg. F
30
c
00
CO
m
30
Fuel Air
60 6600-6750
Caustic 0 gph
Water 117.5 gph (maximum)
Res. Time 2.20 sec.
Sludge (0.167 GPM)
0.6 Ibs/hr Kepone
17.4 Ibs/hr Solids
5.1 Ibs/hr Acetic Acid (30 SCFH)
_76.9Jbs/hr Water (1610 SCFH)
100.0 Ibs/hr (18% Solids)
(a) Water in Kiln 1610 SCFH
(b) Water from Fuel 3400 SCFH
(c) Water in Scrubber 20480.SCFM.
TOTAL 25490 SCFH
Dry Gas from Scrubber (no leakage) = 26,180 SCFH
IDS H2)/lb of dry gas = 0.62
FIGURE E-10 FLOW SCHEMATIC - KIT RUN NO. 9
-------
56,370 SCFH
JKS
3-7-77
Kepone
Acetic Acid
N>
(6750-6500) SCFH Air
255 - 257 Fuel
0 Water
3)
CD
c
3>
Z
m
33
(2000 Deg. F)
29,220 SCFH
(Maximum)
Air (19.500-19,700)
Fuel (530-600) SCF
Propane
49,520 SCFH
Sat. Temp.
179 Deg. F
3J
CD
CO
m
3J
Fuel Air
53SCFH 6750SCFH
Caustic 6.5 gph
Water 110 gph
Res. Time 2.26 sec.
Sludge (0.133GPM)
3.33 Ibs/hr Kepone
8.67 Ibs/hr Solids
28.30 Ibs/hr Acetic Acid (180 SCFH)
39-70Jbs/hr Water (830 SCFH)
80.00 Ibs/hr (15% Solids)
(a) Water in Kiln 830 SCFH
(b) Water from Fuel 3430 SCFH
(c) Water in Scrubber ?0300J5CF_H_
TOTAL 24560 SCFH
Dry Gas from Scrubber (no leakage)
ibs H2O/lb of Dry Gas = 0.62
24,960 SCFH
FIGURE E-11 FLOW SCHEMATIC-KIT RUN NO. 10
-------
TABLE E-1
KIT RUN NO. 1
DATE: 1-14-77
Time
Variable
1535
1630
1700
1730
1830
1930
COMMENTS
EUMEJ.ICJNIRATO.B.
Incinerator Tenp. {Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCWH)
Gas Input at Pilot No. 2 (SCMH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
1260
560
8.54
8.54
36.40
456
1260
560
8.54
8.54
35.00
459
1260
560
8.54
8.54
_
—
1260
560
8.54
8.54
—
458
1260
560
8.54
8.54
...
411
1260
560
8.54
8.54
_.
407
Methane
Methane
Methane
3.0
4.5
KILN.
Burner Gas Temp. (Deg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M2)
Sludge feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone, (mg/l)
Ash (kg)
Draft in Kiln (cm W. C. )
1066
538
78.4
10.36
0.378
12.04
138
N/A
N/A
N/A
N/A
1016
532
78.4
9.52
0.410
12.04
138
N/A
N/A
N/A
N/A
—
—
—
_.
_
_.
—
N/A
N/A
N/A
N/A
1024
538
89.6
9.80
0.397
12.04
138
N/A
9
0.1
N/A
1015
543
92.6
11.20
0.397
12.04
138
N/A
9
0.1
N/A
1016
538
92.6
11.20
0.397
12.04
138
N/A
9
0.1
N/A
Methane
Methane
-------
TABLE E-l (continued)
Time
Variable
1535
1630
1700
1730
1830
1930
COMMENTS
SCRUBBER
Brine to Fog Nozzle (I/sec.)
Brine to 2" Nozzle (I/sec.)
Brine to 1" Nozzle (I/sec.)
Brine to Cone (I/sec.)
Brine to Scrubber (I/sec.)
Caustic Tank level (cm)
Brine Tank level (cm)
Quench level (cm)
Caustic Flow (l/min)
Press @ Brine Pump (kN/M2)
Press @ Retention Tank (kN/M2)
Press @ Caustic Pump (kN/M
Scrubber pH
FEED STARTED® 1730
,2,
0.441
3.02
0.945
2.52
1.44
310
255
62.1
62.1
9.2
0.416
3.02
0.945
2.71
1.47
302
0.57
262
62.1
62.1
9.2
0.416
3.09
0.945
2.71
1.47
300
0.38
262
55.2
62.1
9.1
0.441
3.09
0.976
2.71
1.51
297
0.38
255
62.1
62.1
9.1
0.441
3.09
0.976
2.71
1.51
292
0.38
255
62.1
62.1
9.1
0.441
3.09
0.976
2.71
1.51
286
0.47
262
62.1
62.1
9.0
FEED STOPPED® 1930
-------
TABLE E-2
KIT RUN NO. 2
DATE: 1-15-77
VO
Ui
Time
Variable
FUMEXNCJNERATOR
Incinerator Temp. (Deg. C)
Total Air Input (SCMH)
Gas Input Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCMH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
1300
1330
1430
1530
1630
1093
560
8.96
8.96
. 28.00
448
1093
568
8.82
8.82
26.88
446
1093
568
8.82
8.82
26.32
444
1093
568
8.54
8.54
21.56
388
1093
560
8.82
8.82
20.30
381
COMMENTS
Methane
Methane
Methane
4.8
KILN_
Burner Gas Temp. (Deg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner U/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M2)
Sludge feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone, (mg/l)
Ash (kg)
Draft in Kiln (cm W.C)
1056
538
106.4
10.36
0.378
12.18
138
N/A
N/A
N/A
N/A
1051
538
98.0
9.52
0.347
12.04
138
N/A
N/A
N/A
N/A
1036
538
103.6
9.52
0.347
12.04
138
N/A
9
0.1
N/A
944
538
103.6
9.52
0.359
12.04
138
N/A
9
0.1
N/A
1031
538
103.6
9.10
0.359
12.04
138
N/A
9
0.1
N/A
Methane
-------
TABLE E-2 (continued)
Time
Variable 1300 1330 1430 1530 1630 COMMENTS,
SCRUBBER
Brine to Fog Nozzle (I/sec.) 0.44 0.18 000
Brine to 2" Nozzle (I/sec.) 3.09 3.09 3.09 3.09 3.09
Brine to 1" Nozzle (I/sec.) 0.977 0.977 0.977 0.977 0.977
Brine to Cone (I/sec.) 1.26 2.08 2.08 2.08 1.64
Brine to Scrubber (I/sec.) 1.32 1.23 1.32 1.27 1.30
Caustic Tank level (cm) 361 359 356 349 344
Brine Tank level (cm) — — — — —
Quench level (cm) — — — — —
Caustic Flow (l/min.) - 0.189 0.284 0.473 0.378
Press @ Brine Pump (kN/M2) 241 276 276 276 276
Press @> Retention Tank (kN/M2) 69.0 138.0 117.0 82.7 82.7
vo Press @ Caustic Pump (kN/M2) 55.2 55.2 55.2 55.2 55.2
"^ Scrubber pH - - - -
FEED STARTED @ 1430
FEED STOPPED® 1640
-------
TABLE E-3
Time
Variable
KIT RUN NO. 3
DATE: 1-22-77
1505
1535
1605
1635
1735
COMMENTS
Incinerator Temp. (Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCMH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
1093 1093 1093
560 552 552
2.94 2.94 2.94
3.50 3.50 3.50
12.88 11.76 11.48
443 451 451
1093 1093
552 552
2.94 2.94
3.50 3.50
12.88 9.52
452 401
Propane
Propane
Propane
Burner Gas Temp (Deg. C)
Gas Discharge Temp (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M2
Sludge feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone, (mg/l)
Ash (kg)
Draft in Kiln (cm W.C.)
r»4*l
1088 1053 1082 1102 1036
538 538 538 538 532
114.8 95.2 98.0 95.2 89.6
4,90 4.34 4.56 4.68 4.48
0.42 0.39 0.39 0.38 0.42
11.62 11.76 11.90 11.90 11.62
124 124 124 124 124
N/A N/A N/A N/A N/A
N/A N/A N/A 9 N/A
N/A N/A N/A 0.1 N/A
N/A N/A N/A N/A N/A
Propane
-------
TABLE E-3 (continued)
Time
Variable 1501 1535 1605 1635 1735 COMMENTS,
SCRUBBER
Brine to Fog Nozlle (I/sec.) — — —
Brine to 2" Nozzle (I/sec.) 3.09 3.09 3.09 3.09 3.09
Brine to 1" Nozzle (I/sec.) 0.98 0.98 0.98 0.98 0.98
Brine to Cone (I/sec.) 2.58 2.71 2.71 2.71 2.71
Brine to Scrubber (I/sec.) 1.04 0.98 0.98 1.02 1.02
Caustic Tank level (cm) 325 323 323 319 312
Brine Tank level (cm) _-_.___ —
Quench Level (cm) __..__ _.
Caustic Flow (i/m'm.) - 0.378 0 0.567 0.473
Press @ Brine Pump (kN/M2) 275.8 289.6 289.6 289.6 289.6
Press @ Retention Tank (kN/M2) 27.58 27.58 27.58 27.58 27.58
^ Press @ Caustic Pump (kN/M2) 62.06 62.06 0 62.06 62.06
oo Scrubber pH — 9.0 9.0 83 9.0
FEED STARTED @> 1638
FEED STOPPED® 1815
-------
TABLE E-4
Time
Variable
1125
KIT RUN NO. 4
DATE: 1-25-77
1155
1230
1330
1430
COMMENTS
vo
Incinerator Temp. (Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCWH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C.)
Stack Flow Rate (SCWH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
%Oxygen in Stack
1093
546
3.14
3.36
11.2
438
1093
546
3.14
3.36
11.2
447
1093
546
3.14
3.36
10.9
448
1093
546
3.22
3.44
8.4
393
1093
546
3.22
3.50
7.84
414
Propane
Propane
Propane
KiLN_
Burner Gas Temp. (Deg. C)
Gas Discharge Temp (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M )
Sludge feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone, (mg/l)
Ash (kg)
Draft in Kiln (cm W.C.)
1080
538
151.2
6.16
0.504
11.48
137.9
N/A
N/A
N/A
N/A
-0.76
1021
538
109.2
5.04
0.397
12.04
137.9
N/A
N/A
N/A
N/A
-1.02
997
538
112.0
5.04
0.410
11.76
124.1
N/A
N/A
N/A
N/A
-1.27
1011
538
109.2
5.04
0.441
11.54
124.1
N/A
9
10
N/A
-0.76
977
538
106.4
4.90
0.473
11.48
124.1
N/A
9
10
N/A
-0.76
Propane
-------
TABLE E-4 (continued)
Time
Variable
1125
1155
1230
1330
1430
COMMENTS
O
O
SCRUBBER
Brine to Fog Nozzle (I/sec.)
Brine to 2" Nozzle (I/sec.)
Brine to 1" Nozzle (I/sec.)
Brine to Cone (I/sec.)
Brine to Scrubber (I/sec.)
Caustic Tank level (cm)
Brine Tank level (cm)
Quench level (cm)
Caustic Flow (l/min.)
Press @ Brine Pump (kN/M2)
Press @ Retention Tank (kN/M2)
Press @ Caustic Pump (kN/M )
Scrubber pH
FEED STARTED® 1240
3.09
0.977
2.71
0.851
304.8
296.5
13.79
0
3.09
0.977
2.71
0.851
304.8
0
296.5
13.79
0
3.09
0.977
2.71
0.851
304.8
0
296.5
13.79
0
3.09
0.945
2.71
0.851
302.3
0.189
296.5
13.79
55.16
3.09
0.977
2.71
0.851
294.6
0.567
296.5
13.79
55.16
FEED STOPPED® 1430
-------
TABLE E-5
Time
Variable
KIT RUN NO. 5
DATE: 1-26-77
1330
1420
COMMENTS
Incinerator Temp (Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCMH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
1093
582.4
3.14
3.44
9.52
437
1093
560.0
3.16
3.42
9.52
437
Propane
Propane
Propane
4.7
K[LN_
Burner Gas Temp. (Deg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M )
Sludge feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone, (mg/l)
Ash (kg)
Draft in Kiln (cm W.C.)
999
538
109.2
4.98
0.36
12.04
124.1
-1.02
Propane
-------
TABLE E-5 (continued)
Time
Variable 1330 1420 COMMENTS.
SCRUBBER
Brine to Fog Nozzle (I/sec.) — —
Brine to 2" Nozzle (I/sec.) 3.09
Brine to 1" Nozzle (I/sec.) 0.98
Brine to Cone (I/sec.) 2.33
Brine to Scrubber (I/sec.) 0.72 —
Caustic Tank level (cm) 293 —
Brine Tank level (cm) — —
Quench level (cm) — —
Caustic Flow (l/min.) 0 —
Press @ Brine Pump (kN/M2) 296.5
Press @ Retention Tank (kN/M2) 13.79 -
Press @ Caustic Pump (kN/M ) 0 —
Scrubber pH -
FEED STARTED®— RUN ABORTED
FEED STOPPED® —
-------
TABLE E-6
KIT RUN NO. 6
DATE: 2-14-77
o
u>
Time
Variable
FUMfiNCINERATgR
Incinerator Temp. (Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCIVH)
Aux. Gas Input (SCMH)
Inlet Gas Temp (Deg. C.)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCIVH)
Stack Temp. (Deg. C)
%Oxygen in Stack
KM-N_
Burner Gas Temp. (Deg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M )
Sludge feed (I /sec.)
Kepone Solution (l/hr.)
Kepone Solution Conc.(%)
Ash (kg)
Draft in Kiln (cm W.C.)
1215
1245
1315
1415
1515
1093
546.0
2.9
3.2
12.7
442
198.8
—
—
77
6.5
993
491
112.0
6.16
0.37
12.0
138
N/A
N/A
N/A
1093
537.6
3.0
3.2
11.9
—
198.8
_
_
77
7.0
952
482
103.6
5.94
0.37
12.3
138
N/A
N/A
N/A
1093
534.8
2.9
3.1
12.5
—
196.0
—
—
74
5.5
1010
410
201.6
9.66
0.55
12.3
138
0.01
N/A
0
1093
537.6
2.9
3.1
11.6
421
194.9
0.17
0.59
116
*""
939
477
168.0
8.54
0.54
11.5
138
0.01
N/A
0
1093
537.6
2.9
3.1
11.9
448
196.0
—
_.
121
~"
893
516
166.6
8.26
0.57
11.5
138
_
N/A
0
COMMENTS
Propane
Propane
Propane
Propane
Feed Line
plugged total
sludge fed =
0.049 M3
-------
TABLE E-6 (continuedI
Time
Variable 1215 1245 1315 1415 1515 COMMENTS^
SCRUBBER
Brine to Fog Nozzle (I/sec.) — —
Brine to 2" Nozzle (I/sec.) 3.0 3.0 3.0 3.0 3.0
Brine to 1" Nozzle (I/sec.) 0.98 0.98 0.98 0.98 0.98
Brine to Cone (I/sec.) 2.7 2.7 2.7 2.7 2.7
Brine to Scrubber (I/sec.) 1.13 1.13 1.12 1.10 1.10
Caustic Tank level (cm) 324 322 320 316 311
Brine Tank level (cm) _ _ _ _ —
Quench level (cm) _.__._ —
Caustic Flow (l/min.) - 0.38 0.28 0.28 0.38
Press @ Brine Pump (kN/M2) 290 293 293 293 293
Press @ Retention Tank (kN/M ) 82.7 82.7 96.5 96.5 96.5
Press @ Caustic Pump (kN/M2) 62.1 55.2 55.2 55.2 55.2
Scrubber pH 9.3 9.4 9.2 9.3 9.3
FEED STARTED® 1308
FEED STOPPED® 1520
-------
TABLE E-7
Time
Variable
1535
1630
KIT RUN NO. 8
1700
1730
1830
1930
2030
DATE: 2-18-77
2115
COMMENTS
O
Ui
Incinerator Temp. (Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCMH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
KILN
Burner Gas Temp. (Oeg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M )
Sludge Feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone. (%)
Ash (kg)
Draft in Kiln (cm W.C.)
1149
512.4
2.82
3.08
12.0
—
195
0.17
0.84
—
4.4
849
364
169.4
8.40
14.3
124
N/A
N/A
N/A
1149
518.0
2.86
3.05
11.5
363
195
0.17
0.84
132
4.7
821
388
168.0
8.26
14.4
124
0.01
N/A
1.2
1149
518.0
2.86
3.05
11.2
349
195
0.17
0.84
132
5.0
824
371
168.0
8.26
14.3
124
0.01
N/A
1.2
1149
518.0
2.86
3.05
11.2
341
195
0.17
0.84
138
5.0
832
366
168.6
8.54
14.3
124
0.01
N/A
1.2
1149
518.0
2.91
3.08
10.9
329
195
0.17
0.84
135
5.0
829
349
169.4
8.57
14.4
124
0.01
N/A
1.2
1149
518.0
2.91
3.08
11.2
299
195
0.17
0.84
132
5.0
838
310
189.0
9.24
14.3
124
0.01
N/A
1.2
1149
518.0
2.94
3.11
10.9
296
195
0.17
0.84
132
4.7
843
316
187.6
9.32
14.4
124
0.01
N/A
1.2
1149
518.0
2.94
3.19
10.6
308
195
0.17
0.84
132
4.6
837
329
189.0
9.24
14.4
124
0.01
N/A
1.2
Propane
Propane
Propane
Propane
Propane
Propane
-0.5
-0.5
-0.5
-0.5
-0.5
0.8
-0.5
-0.8
-------
TABLE E-7 (continued)
Time
Variable 1535 1630 1700 1730 1830 1930 2030 2115 COMMENTS^
SCRUBBER
Brine to Fog Nozzle (I/sec.) _______ _
Brine to 2" Nozzle (I/sec.) 3.0 3.1 3.1 3.1 3.0 3.1 3.0 3.0
Brine to 1" Nozzle (I/sec.) 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0
Brine to Cone (I/sec.) 1.4 1.4 1.4 1.4 1.4 1.4 1.3 1.3
Brine to Scrubber (I/sec.) 0.85 1.0 1.0 1.0 0.95 1.0 - 1.1
Caustic Tank level (cm) 301 300 296 293 287 286 282 278
Brine Tank level (cm) __.__ — — — —
Quench level (cm) — — — — — — — —
Caustic Flow (l/min.) - 0.66 0.57 0.57 0.57 - 0.57 0.47
Press @ Brine Pump (kN/M2) 303 290 290 290 290 290 303 303
Press @ Retention Tank (kN/M2) 117 117 117 124 90 97 103 82
Press @ Caustic Pump (kN/M2) - 55.2 55.2 55.2 69.0 — 62.1 62.1
Scrubber pH — 9.3 9.3 9.4 9.4 9.3 9.3 9.5
FEED STARTED ©1615
FEED STOPPED® 2115
-------
o
--J
TABLE E-8
Time
Variable
KIT RUN NO. 9
Incinerator Temp. (Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCMH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
KU_N_
Burner Gas Temp (Deg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M2)
Sludge Feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone (%)
Ash (kg)
Draft in Kiln (cm W.C.)
1245
1093
546.0
2.7
3.0
11.2
326
194.6
0.36
0.84
143
5.5
755.6
343.3
187.6
7.3
N/A
N/A
N/A
-0.8
1330
1400
1430
1500
1530
1600
DATE: 2-23-77
1630
1700
COMMENTS
1093
546.0
2.7
3.0
11.2
334
194.6
0.36
0.84
143
5.5
755.6
332.2
187.6
7.1
0.01
N/A
0.6
1093
540.0
2.7
2.9
11.2
321
194.6
0.36
0.84
141
6.0
690.0
282.2
190.4
7.3
0.01
N/A
0.6
1093
540.4
2.7
2.9
11.2
260
194.6
0.36
0.84
141
6.0
687.8
280.0
190.4
7.1
0.01
N/A
0.6
1093
540.4
2.7
2.9
11.2
272
194.6
0.36
0.84
138
6.3
688.9
254.4
191.2
7.3
0.01
N/A
0.6
1093
540.4
2.7
2.9
11.5
262
194.6
0.36
0.84
143
6.3
682.8
243.3
190.4
7.1
0.01
N/A
0.6
1093
546.0
2.7
2.9
11.2
254
194.6
0.36
0.84
138
6.1
678.9
226.7
190.4
7.1
0.01
N/A
0.6
1093
546.0
2.7
2.9
11.2
246
194.6
0.36
0.84
138
5.0
678.3
226.7
190.4
7.1
0.01
N/A
0.6
1093
546.0
2.7
2.9
9.2
246
194.6
0.36
0.84
143
6.8
677.2
190.6
190.4
7.1
0.01
N/A
0.6
Propane
Propane
Propane
Propane
Propane
Propane
-1.0
-0.8
•0.8
-1.3
-0.5
-0.5
-0.5
-0.6
-------
TABLE E-8 (continued)
Time
Variable
1245
1330
1400
1430
1500
1530
1600
1630
1700
COMMENTS
O
00
SCRUBBER
Brine to Fog Nozzle (I/sec.)
Brine to 2" Nozzle (I/sec.)
Brine to 1" Nozzle (I/sec.)
Brine to Cone (I/sec.)
Brine to Scrubber (I/sec.)
Caustic Tank level (cm)
Brine Tank level (cm)
Quench level (cm)
Caustic Flow (l/min.)
Press @ Brine Pump (kN/M2)
Press @ Retention Tank (kN/M )
Press @ Caustic Pump (kN/M )
Scrubber pH
3.09
1.0
1.3
1.6
137.75
3.15
1.0
1.4
1.6
137.75
3.15
1.0
1.4
1.6
137.75
3.15
1.0
1.4
1.6
137.75
3.15
1.0
1.5
1.6
137.75
3.15
1.0
1.5
1.6
137.75
3.15
1.0
1.5
1.6
137.75
3.15
1.0
1.5
1.6
137.75
3.15
1.0
1.5
1.6
137.75
0
310.3
96.5
0
9.5
0
317.2
75.8
0
9.3
0
317.2
69.0
0
9.4
0
317.2
89.6
0
9.3
0
317.2
82.7
0
9.4
0
317.2
75.8
0
9.3
0
317.2
69.0
0
9.3
0
317.2
69.0
0
9.3
0
317.2
69.0
0
9.3
FEED STARTED® 1318
FEED STOPPED® 1718
-------
TABLE E-9
Time
Variable
1415
1445
KIT RUN NO. 10
1515
1545
1615
1645
DATE: 2-24-77
1715
1800
COMMENTS
Incinerator Temp. (Deg. C)
Total Air Input (SCMH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCMH)
Aux. Gas Input ISCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
1037.8
588.0
2.5
3.1
9.5
273.9
187.6
0.14
1.5
137.8
5.5
1037.8
579.6
2.7
2.9
10.9
348.9
187.6
0.14
1.5
137.8
6.5
1037.8
574.0
2.7
2.9
10.6
361.7
187.6
0.14
1.5
137.8
6.5
1037.8
574.0
2.7
2.9
10.3
346.7
184.8
0.14
1.5
135.0
6.8
1037.8
588.0
2.7
2.9
10.3
320.6
187.6
0.14
1.46
135.0
6.7
1037.8
579.6
2.7
3.0
10.3
306.7
189.0
0.14
1.46
140.6
6.2
1037.8
588.0
2.7
3.0
9.5
296.7
187.6
0.14
1.46
146.1
7.7
1037.8
588.0
2.7
3.0
9.5
273.9
187.6
0.14
1.46
137.8
8.0
Propane
Propane
Propane
Propane
Propane
KILN_
Burner Gas Temp. (Deg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCM-0
Compressed Air Press (kN/M )
Sludge feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Cone. (%)
Ash (kg)
Draft in Kiln (cmW.C.)
777.2
354.4
190.4
7.3
0
0
0
N/A
N/A
N/A
758.3
398.9
190.4
7.3
0
0
0
N/A
N/A
N/A
765.0
387.8
189.0
7.1
0
0
0
0.01
N/A
0.6
747.2
348.9
189.0
7.3
0
0
0
0.01
N/A
0.6
713.3
315.6
190.4
7.2
0
0
0
0.01
N/A
0.6
748.9
310.0
190.4
7.2
0
0
0
0.01
N/A
0.6
750.0
298.9
191.8
7.2
0
0
0
0.01
N/A
0.6
757.2
265.6
191.8
7.2
0
0
0
0.01
N/A
0.6
-1.0
-1.0
-0.5
-1.3
-1.3
-0.5
-0.5
-1.0
Propane
-------
TABLE E-9 (continued)
Time
Variable
1415
1445
1515
1545
1615
1645
1715
1800
COMMENTS
SCRUBBER
Brine to Fog Nozzle (I/sec.)
Brine to 2" Nozzle (I/sec.)
Brine to 1" Nozzle (I/sec.)
Brine to Cone (I/sec.)
Brine to Scrubber (I/sec.)
Caustic Tank level (cm)
Brine Tank level (cm)
Quench level (cm)
Caustic Flow (l/min.)
Press @ Brine Pump (kN/M2)
Press @ Retention Tank (kN/M2)
Press @ Caustic Pump (kN/M2)
Scrubber pH
FEED STARTED @ 1450
3.1
1.0
1.4
1.6
350
3.1
1.0
1.4
1.6
350
3.1
1.0
1.6
1.6
350
3.1
1.0
1.6
1.6
350
3.1
1.0
1.6
1.6
350
3.1
1.0
1.5
1.6
350
3.1
1.0
1.5
1.6
350
3.1
1.0
1.5
1.6
350
0
317.2
62.1
0
9.3
0
317.2
62.1
0
9.2
0
317.2
62.1
0
9.4
0
317.2
62.1
0
9.3
0
317.2
69.0
0
9.5
0
317.2
62.1
0
9.4
0
296.5
69.0
0
9.5
0
289.6
62.1
0
9.5
FEED STOPPED® 1820
-------
TABLEE-10 KIT RUN NO. 11 DATE: 2-25-77
Time
Variable 1230 1300 1330 1400 1430 1500 1530 1550
FUME JJNCINE RATOR_
Incinerator Temp. (Deg. C)
Total Air Input (SCWH)
Gas Input @ Pilot No. 1 (SCMH)
Gas Input @ Pilot No. 2 (SCMH)
Aux. Gas Input (SCMH)
Inlet Gas Temp. (Deg. C)
Stack Flow Rate (SCMH)
Air in Stack Burner (SCMH)
Pilot Gas to Stack Burner (SCMH)
Aux. Gas to Stack Burner (SCMH)
Stack Temp. (Deg. C)
% Oxygen in Stack
Ki_LN_
Burner Gas Temp. (Deg. C)
Gas Discharge Temp. (Deg. C)
Air Input to Burner (SCMH)
Gas Input to Burner (SCMH)
Water to Burner (l/min.)
Compressed Air to Burner (SCMH)
Compressed Air Press (kN/M2)
Sludge feed (I/sec.)
Kepone Solution (l/hr.)
Kepone Solution Conc.(%)
Ash (kg) _______
Draft in Kiln (cm W.a) -1.02 -0.25 -0.51 -0.76 -0.76 -0.51 -1.02 -0.25
1093.3
551.6
2.7
2.9
10.9
319.4
189
0.22
1.1
132.2
5.0
765.6
393.3
190.4
7.14
0
0
0
N/A
N/A
N/A
1093.3
551.6
2.7
2.9
11.2
374.4
189
0.22
1.3
135.0
6.0
768.8
454.4
189.0
7.20
0
0
0
N/A
N/A
N/A
1093.3
551.6
2.7
2.9
10.6
403.3
189
0.22
1.3
132.2
6.5
763.3
460.0
189.0
7.14
0
0
0
0.1
N/A
4.16
1093.3
551.6
2.7
2.9
9.9
409.4
189
0.22
1.3
132.2
3.2
761.1
457.2
190.4
7.14
0
0
0
0.1
N/A
4.16
1093.3
546.0
2.7
2.9
9.9
423.3
189
0.22
1.3
132.2
3.0
761.1
479.4
190.4
7.14
0
0
0
0.1
N/A
4.16
1093.3
551.6
2.7
2.9
9.9
430.6
189
0.22
1.3
1375
3.0
761.7
482.2
189.0
7.14
0
0
0
0.1
N/A
4.16
1093.3
551.6
2.7
2.9
9.5
432.8
189
0.22
1.3
137.8
3.1
761.1
482.2
189.0
7.20
0
0
0
0.1
N/A
4.16
1093.3
551.6
2.7
2.9
9.2
438.4
189
0.22
1.3
137.8
3.2
757.2
482.2
189.0
7.20
0
0
0
0.1
N/A
4.16
COMMENTS
Propane
Propane
Propane
Propane
Propane
Propane
Dry Basis
-------
TABLE E-10 (continued)
Time
Variable
SCRLBBER
Brine to Fog Nozzle (I/sec.)
Brine to 2" Nozzle (I/sec.)
Brine to 1" Nozzle (I/sec.)
Brine to Cone (I/sec.)
Brine to Scrubber (I/sec.)
Caustic Tank level (cm)
Brine Tank level (cm)
Quench level (cm)
Caustic Flow (l/min.)
Press @ Brine Pump (kN/M2)
Press @ Retention Tank (kN/M )
Press @ Caustic Pump (kN/M )
Scrubber pH
FEED STARTED® 1328
1230
1300
1330
1400
1430
1500
1530
1550
3.15
1.01
1.51
1.59
350
0
310
69
0
9.2
3.15
1.01
1.51
1.59
350
0
310
69
0
9.2
3.06
0.98
1.39
1.59
350
0
310
69
0
9.2
3.15
1.01
1.51
1.59
348
19.05
310
69
55.2
9.2
3.15
1.01
1.51
1.59
344
19.05
310
96.5
55.2
9.3
3.18
0.99
1.51
1.59
342
19.05
310
96.5
55.2
9.6
3.15
0.99
1.51
1.59
342
0
317
69
0
9.8
3.12
0.99
1.76
1.59
342
0
317
69
0
9.8
COMMENTS
FEED STOPPED® 1600
-------
TABLEE-11
KEPONE INCINERATION TESTS DAT.A SUMMARY
Run
No.
1
2
3
4
5
6
7
8
9
10
11
Date Kepone Incinerator*
Feed Temp.
gm/hr. Oeg.C.
1/14/77
1/15/77
1/22/77
1/25/77
1/26/77
2/14/77
2/1 7/77
2/18/77
2/23/77
2/24/77
2/25/77
0.9
0.9
0.9
90
None
None
410
470
250
270
1510
1260
1093
1093
1093
1093
1093
1149
1149
1093
1038
1093
Kiln*
Inlet
Tenp.
Deg. C
1024
1036
1102
997
999
952
877
849
700
758
763
Kiln*
Outlet
Temp.
Deg. C
538
538
538
538
538
482
427
364
343
399
454
Flow thi
Inciner
SCIV
764.4
775.9
771.1
755.3
773.6
998.2
-
814.0
826.0
873.3
818.2
*At Start of Run
*»At
End of Run
Flow through Flow through Incinerator % Residence Kiln** Kiln** Incinerator** Feed
(X, Time Sec. Inlet Outlet Inlet Temp. Time
Hours
1384.6
1315.2
1307.0
1280.3
1311.2
1722.6
1607.2
1597.0
1639.1
1578.4
Deg. C
438
444
452
448
437
442
427
363
326
349
374
•fe
3.75
4.8
—
-
4.7
5.5
3.7
4.4
5.5
6.5
3.1
2.15
2.38
2.39
2.44
2.39
2.06
-
2.18
2.23
2.20
2.26
Temp.
Deg. C
1016
1031
1036
977
999
893
877
837
677
757
757
Temp.
Deg. C
538
538
532
538
538
516
427
329
191
266
482
Deg
407
381
401
414
437
448
427
308
246
274
434
2.0
2.0
1.67
1.67
2.0
0.33
5.0
4.0
3.5
2.5
-------
60
50
UJ
>
UJ
40
30
I
I
I
2.0gpm
AVERAGE WATER CONSUMPTION
IN QUENCH = 1.87 gpm
I
I
l
4=00
5--00
6=00
TIME
7=00
( O'CLOCK)
8 00
9=00
10=00
FIGURE-E12' QUENCH WATER FOR KIT RUN N0.8
-------
60
cc
X
o
_J
UJ
>
UJ
50
40
1.68 gpm
AVERAGE WATER CONSUMPTION
IN QUENCH = 1.67 gpm
30
_L
-L
1 = 00
2=00 3=00
TIME (O'CLOCK)
4=00
6=00
FIGURE-EI3' QUENCH WATER FOR KIT RUN N0.9
-------
63
58
tn
*:
cc
48
I
o
UJ
>
UJ
38
28
I INCH = 4.4 GALLONS
1.61 gpm
AVERAGE WATER CONSUMPTION
IN QUENCH = 1.82 gpm
2 00
3=00
4= 00
TIME (O'CLOCK)
5 = 00
6--00
FIGURE-E14: QUENCH WATER FOR KIT RUN NO.IO
7--00
-------
7O
60
cr
<
2
I
o
£50
UJ
I
AVERAGE WATER CONSUMPTION
IN QUENCH = l.77gpm
69gpm
1= 4.4 GALLONS
I2--00
1-00
4:00
2:00 3-00
TIME (O'CLOCK)
FIGURE- EI5- QUENCH WATER FOR KIT RUNNO.II
5.00
-------
0.3
5
Q_
00
LlJ
CE
O
UJ
UJ
0.1
AVERAGE FLOW 0.145 GPM
I
I
I
0.5
1.5
2 2.5 3
TIME (MRS)
3.5
4.5
FIGURE-E16= SLUDGE FEED RATE FOR KIT RUN NO. 8
-------
VO
0.3
Ul
cr
o
UJ
ui
O.I
AVERAGE FLOW 0.15 GPM
1
1
1
1
0.5
I
1.5
3.5
4.5
2 2.5 3
TIME (MRS)
FIGURE- EI7-. SLUDGE FEED RATE FOR KIT RUN NO. 9
-------
0.3
LU
cr
Q
LU
LU
LL
AVERAGE FLOW 0.167 GPM
I
I
I
I
I
\
I
I
I
0.5
I
1.5
3.5
2 2.5 3
TIME (HRS)
FIGURE-E18= SLUDGE FEED RATE FOR KIT RUN NO. 10
4.5
-------
0.3
UJ
I-
cr
Q
UJ
UJ
U-
0.1
AVERAGE FLOW 0.133 GPM
J I I I I I I L
0.5 I 1.5 2 2.5 3 3.5 4 4.5
TIME (HRS)
FIGURE- E19: SLUDGE FEED RATE FOR KIT RUN NO. 11
-------
FIGURE F-l
TYPICAL CHROMATOGRAM OF STACK GASES
FILTER EXTRACT (10ml) ON GLASS COLUMN
PACKED WITH 1.5% OV-I7+1.95% QF-I ON
GAS CHROM Q
APPENDIX F. TYPICAL CHROMATOGRAMS
K3
-------
to
OJ
FIGURE F-2
TYPICAL CHROMATOGRAM OF KEPONE ON
GLASS COLUMN PACKED WITH 1.5% OV-I7+
1.95% QF-I ON GAS CHROM Q
-------
FIGURE F-3
TYPICAL CHROMATOGRAM OF HIGH VOLUME
AMBIENT AIR SAMPLER NO I ON COLUMN
1.5% 0V-17+1.95% OF-I ON GAS CHROM Q
-------
ho
Ul
FIGURE F-4
TYPICAL CHROMATOGRAM OF INCINERATION
ASH EXTRACT (2ml of I g ash) ON GLASS
COLUMN 15% OV-I7-M 95%QF-I ON GAS
CHROM Q
-------
FIGURE F-5
TYPICAL CHROMATOGRAM OF SCRUBBER
WATER ON GLASS COLUMN PACKED WITH
1.5% OV-I7-H.950/. QF-I ON GAS CHROM Q
Ox
-------
FIGURE F-6
TYPICAL CHROMATOGRAM OF STACK GASES
FILTER EXTRACT (2 ml JON GLASS COLUMN
PACKED WITH 1-5% OV-|7+I.95% OF-I ON
GAS CHROM Q
-------
00
FIGURE F-7
TYPICAL CHROMATOGRAM OF STACK GAS
IMPRINGER EXTRACT ON GLASS COLUMN
PACKED WITH 1.5% OV-I7+I.95% OF-1 ON
GAS CHROM Q
-------
VO
FIGURE F-8
TYPICAL CHROMATOGRAM OF CYCLONE
CONDENSATE EXTRACT OF STACK GASES
ON COLUMN 1.5% 0V-17+1.95% OF-1 ON
GAS CHROM Q
-------
APPENDIX G. LOG OF EVENTS
A.
Date
11/1/76
11/1 to 12/23/76
12/26 to 12/30/76
1/3 to 1/7/77
1/10 to 1/13/77
1/14/77
1/15/77
1/16 to 1/18/77
1/19/77
1/20-21/77
1/24/77
1/25/77
1/26/77
1/27/77
1/28/77
1/31 to 2/11/77
TIME TABLE OF MAJOR EVENTS
Events
Contract awarded to Surface Division
Fabrication, construction and installation of
major equipment
Outside contractor work
Safety training and start-up checkout for
Air Pollution Control System
Troubleshooting for burner system electrical
wiring
Test Run #1
Test Run #2
Changed over to propane, installed a direct
water line for Kepone project as main header
had frozen and burst and heat traced newly in-
stalled water line
Acetic acid spill in mix room and cleanup
Test Run #3
Trouble with removing Kepone from drum
Test Run #4
Test Run #5 (blank run)
Draining and rinsing of scrubber system
Sludge feed system checkout
Removal of old stack, installation of new stack
and installation of a burner in the new stack,
replacing inner layer of insulation inside the
kiln inlet duct
130
-------
Date Events
2/14/77 Test Run #6 (insulated feed line)
2/15-16/77 Water jacieted feed line installed, and a water
trough installed around the kiln inlet duct to
reduce hot spots
2/17/77 Test Run #7 (kiln rotation stopped after 20
minutes of feeding)
2/18/77 Test Run #8
2/22/77 Broken axle replaced for kiln drive system,
frozen core in sludge and required hard work
to chip it off - it was too late to make a run
2/23/77 Test Run #9
2/24/77 Test Run #10
2/25/77 Test Run #11
2/26 to 3/4/77 Major clean-up of test area
3/7 to 3/11/77 Minor clean-up
3/14-15/77 Final clean-up and tearing down of the walls in
control area
B. SUMMARY DESCRIPTION OF KIT RUNS
Run #1 (1/14/77)
Kepone solution in acetic acid with a concentration of 0.1 mg/1 injected
into duct at a rate of 9 1/hr and vapors incinerated at 1260°C. for a period
of two hours. The kiln outlet temperature was maintained at 538 C for entire
test run.
Calculated residence time in the incinerator was 2.15 seconds at the
maximum flow rate through the incinerator. (Air leakage into the system is
not considered for this calculation in all runs.)
Run #2 (1/15/77)
Kepone solution in acetic acid with a concentration of 0.1 mg/1 injected
into duct at a rate of 9 1/hr. and vapors incinerated at 1093 C Qfor a period
of two hours. The kiln outlet temperature was maintained at 538 C.
Calculated residence time in the incinerator was 2.38 seconds at maximum
flow rate through the incinerator.
131
-------
Run #3 (1/22/77)
Fuel system changed to propane gas because of shortage of natural gas.
A separate, heat traced water system installed as the main water heater had
frozen and burst. Kepone solution (0.1 gm/1) injected into duct at 9 1/hr
and vapors incinerated at 1093 C for 1 hour, 40 minutes.
Calculated residence time was 2.39 seconds at maximum flow rate through
the incinerator. The kiln outlet temperature was in the range of 533 - 538
C.
Run #4 (1/25/77)
Versar personnel had difficulties in removing Kepone from the storage
drums as it had lumped, so the run was made at a lower concentration than
planned. The concentration of the solution was 10 gms/1 and it was injected
into the duct at a rate of 9 1/hr for 1 hour, 40 minutes. The vapors were
incinerated at 1093°C.
Calculated residence time in the incinerator was 2.44 seconds at maximum
flow rate. The kiln outlet temperature was 538°C.
Run #5 (1/26/77)
Detectable levels of Kepone were observed by Versar in stack and scrubber
during run #4. No Kepone solution was injected for run #5, but sampling was
carried out for this blank run to understand the causes of detectable levels
of Kepone during run #4. Scrubber system drained and rinsed with water after
the run as 25 mg/1 of Kepone was detected in scrubber liquid.
Run #6 (2/14/77)
A new alloy stack equipped with a 0.147 J/sec capacity burner was in-
stalled to prevent water condensation in the stack. Toledo sewage sludge was
fed through 1.27-cm line into kiln at a rate of 0.01 liters/feec for about 2 hr.
The feed line into the kiln was plugged after about 1 1/2 hr of feeding.
^o"^
The incinerator was operated at 1093 C , and kiln outlet temperature dropped
from 482 C to 410 C and again came up to 515°C.
' Calculated residence time in the incinerator was 2.06 sec. Hot spots
observed on the duct from burner to kiln inlet.
Run //7 (2/17/77)
An insulated feed line was tried prior to this run and a water jacketed
feed line was installed. A water trough was installed around the duct from
burner to kiln inlet to keep the duct cool. Twenty-five liters of Kepone
solution (117 gm/liter)were added to drum of Toledo sewage sludge. The
Kepone sludge mixture was fed to kiln at a rate of .0078 liters^ec for 20 min
and retort rotation stopped. Feed was stopped and retort drive system
132
-------
repaired. Four bolts and a bolting pad were broken. Bolts were replaced and
the pad rewelded.
Run #8 (2/18/77)
The Kepone sludge mixture prepared for run #7 was used for feed. The
mixture was fed atQan average rate of 0.009 liters/sec for 5 hr. The incin-
erator was at 1149 C and kiln outlet temperature dropped from 388°C to 310°C
and came back up to 329 C. Residence time in the incinerator was calculated
to be 2.18 sec at maximum flow rate.
Run #9 (2/23/77)
The friction drive roller had worn out as the axle was broken and was
replaced. The sludge had a frozen core and had to be broken loose. The
operator used a wrong mark on the measuring stick and transferred only 12
liters of Kepone solution instead of 25 liters into a drum load of sludge.
Kepone sludge mixture was fed to the kiln at a rate of 0.0095 liters/sec
for 4 hr. The incinerator was at 1093°C, and the kiln outlet temperature
dropped from 343 C to 190 C. Kiln inlet gas temperature was lower as the
insulation in the duct from the burner to kiln inlet was blown out and
water trough was cooling the inlet gases considerably. The water jacketed
feed line was cooling the gases at the outlet. The retort was stopping
frequently as oil from the drive chain went into clutch.
Run #10 (2/24/77)
The duct from the burner to kiln inlet was insulated. Burner block
refractory was observed to be molten and obstructing the path of gases from
the burner. Noisy burner during previous run was due to this obstruction.
The clutch was cleaned. Kepone sludge mixture was prepared as in run #9
and was fed into the kiln at a rate of 0.0105 liters/sec for 3.5 hr. The in-
cinerator was operated at 1038°C, and kiln outlet temperature dropped from
399°C to 266°C. Calculated residence time in the incinerator was 2.2 sec.
Run #11 (2/25/77)
Two bolts were replaced for the drive system. Approximately 95 liters
of Kepone sludge mixture were left over in the feed tank from run #10. About
59 liters of Kepone solution in acetic acid (117 gm/literjwere added to the
Kepone-sludge mixture left in the tank. This mixture was fed to the kiln at Q
a rate of 0.0084 liters/sec for 2.5 hr. The incinerator was operated at 1093
C. Water flow to the jacketed feed line was reduced fo get higher temperature
at the outlet from kiln. Kiln outlet temperature increased from 454 C to
482°C during the feed time. Calculated residence time in the incinerator
was 2.26 sec for maximum flow. Two holes of 0.32 cm diameter were drilled,
one at each injection point in the duct, after the feed was stopped and air
was blown into duct to clear it from dust.
133
-------
APPENDIX H. EPA (RTP) CONFIRMATORY ANALYSIS RESULTS AND BLOOD TEST RESULTS
1 UNITED STATES ENVIRONMENTAL PROTECTION AGENCY
J ENVIRONMENTAL MONITORING AND SUPPORT LABORATORY
* RESEARCH TRIANGLE PARK
NORTH CAROLINA 27711
April 5, 1977
Dr. Mohamad N. Khattak
VERSAR, Inc.
6621 Electronic Drive
Springfield, Virginia 22151
Dear Dr. Khattak:
Listed below you will find Versar percent recoveries for the quality
assurance spiked kepone filter samples sent to you by Dr. Moseman. In
all cases, other than the blanks, your reported values are lower than
the spiked kepone concentrations reported by Dr. Moseman.
Filter EPA Versar Versar
Number Spiked Concentration Analysis % Recovery
_ _ ng/f i 1 ter _ ng/filter _
004 2500 2200 88
005 1250 760 61
006 0 None detected
007 500 360 72
008 1250 960 77
009 2500 1880 75
010 500 430 86
Oil 1250 950 76
012 0 None detected
013 1250 1010 81
014 500 420 84
015 2500 2470 99
016 500 410 82
017 2500 2070 83
Average 80%
If you have specific questions concerning sample preparation and
analysis, please contact Dr. Moseman directly.
Sincerely yours,
Thomas A. Hartlage
Chief, Field Studies Section
Environmental Monitoring Branch
(MD-76)
cc: Dr. Moseman (MD-69)
R. Carnes, EPA, Cincinnati
134
-------
0,
JAMES B. KENLEY.M.D. Department of Health
COMMISSIONER Richmond. Va. 23219
SUBJECT: KEPONE INCINERATION TEST
25 March 1977
Dr. Prank Whitmore
Versar, Inc.
6621 Electronic Drive
Springfield, Virginia 22151
Dear Dr. Whitmore:
We have received the analyses of the blood samples collected
before and after the Kepone Incineration Test Program on personnel
who were to work on the test program. This is to advise that all
samples were negative and no Kepone was detected.
I would appreciate it if you would pass this information on to
the appropriate personnel.
Sincerely,
Eric H. Bartsch, P. E., Director
Bureau of Sanitary Engineering
EHB/c
135
-------
TECHNICAL REPORT DATA
(Please read Instructions on the reverse before completing)
. REPORT NO.
EPA-600/2-78-108
3. RECIPIENT'S ACCESSION NO.
A. TITLE AND SUBTITLE
KEPONE INCINERATION TEST PROGRAM
5. REPORT DATE
May 1978 (Issuing Date)
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
Bruce A. Bell
Frank C. Whitmore
8. PERFORMING ORGANIZATION REPORT NO.
9. PERFORMING ORGANIZATION NAME AND ADDRESS
Design Partnership
Richmond, Virginia 23226 and
Versar, Inc.
Springfield, Virginia 22151
10. PROGRAM ELEMENT NO. ]DC618
SOS #4, Task 10
11. CONTRACT/GRANT NO.
R-805112-01-0
12. SPONSORING AGENCY NAME AND ADDRESS
Municipal Environmental Research Laboratory—Cin.,OH
Office of Research and Development
U.S. Environmental Protection Agency
Cincinnati, Ohio 45268
13. TYPE OF REPORT AND PERIOD COVERED
14. SPONSORING AGENCY CODE
EPA/600/14
15. SUPPLEMENTARY NOTES
Richard A. Carnes (Project Officer) 513/684-7871
16. ABSTRACT
The Kepone Incineration Test (KIT) program was undertaken to evaluate incineration
as a method of destroying Kepone and Kepone-containing materials and to determine
the range of operating variables required for complete destruction. The program was
divided into two phases: (a) experiments involving the direct injection of low BTU
solutions of Kepone into the afterburner, and (b) experiments involving the co-
incineration of sewage sludge and various amounts of Kepone injected into a rotary
kiln. Each phase was designed so that succeeding experiments involved longer amounts
of Kepone and/or alterations in afterburner temperature and residence time.
17.
KEY WORDS AND DOCUMENT ANALYSIS
DESCRIPTORS
b.lDENTIFIERS/OPEN ENDED TERMS C. COSATI Field/Group
Research
Temperature
Degradation
Organic Compounds
Retention Time
Excess Air
Incineration
Rotary Kiln
13B
8. DISTRIBUTION STATEMENT
RELEASE TO PUBLIC
19. SECURITY CLASS (ThisReport)'
UNCLASSIFIED
21. NO. OF PAGES
146
20. SECURITY CLASS (Thispage}
UNCLASSIFIED
22. PRICE
EPA Form 2220-1 (9-73)
136
ft U.S. GOVERNMENT PRINTING OFFICE: 1978— 7 5 7 -140 /1333
------- |