DE-A.

R21-95MC311
88-01
,.

Mixed waste Treatment Using the ChemChar Thermolytic

Detoxification Technique

Final Report
June 20,1995- July 31,1996
By
Daniel J. Kuchynka

Work Pefiorrned Under Contract No.: DE-AR21-95MC3

For
U.S. Department of Energy
Offic~of Fossil EnerW-Federal Energy Technology Center

P.O.Box 880
Morganto~

West Virg@ia 26507-0880

By
Mirage Systems
575 Maude Court
Sunnyvale, California 94086-2803

REXXWEX?
Mllfl081999

CxYn

1188

..

Disclaimer

This report was prepared as an account of work sponsored by an

agency of the United StatesGovernment. Neither the United States
Government nor any agency thereof, nor any of their employees,
makesanywarranty,expressor implied, or assumes any legal liability
or responsibilityfor the accuracy, completeness, or usefulness of any
information, apparatus,product, or process disclosed, or represents
thatitsuse would not infringeprivatelyowed rights. Reference herein
to anyspecificcommercialproduct, process, or service by tradename,
trademadqmanufacturer,or otherwisedoes not necessarily constitute
or impIyits endorsement,recommendation, or favoring by the United
StatesGovernmentor anyagencythereof. The views and opinions of
authors expressed hereindo not necessarilystate or reflect those of
the United StatesGovernment or any agency thereof.

DISCLAIMER

Portions of this document

may be illegible
in electronic image products.
Images are
produced from the best available original
document.

FzkalRepoti

Abstract

The ChemChar Thermolytic Detoxification is to be tested under a Research Opportunity

Announcement contract to determine its efficacy for the treatment of surrogate mixed waste
streams. The waste-to-energy gasification process employs a fixed bed of activated carbon on
which the surrogate mixed waste feed is applied. The carbon/waste mixture is treated in a
vertically positioned cylindrical, continuous feed reactor by initiating a thin, annular, thermal
reaction zone maintainedby the addition of a sub-stoichiometric amount oxygen at the top of the
reactor. In batch processing, this thermal zone, initiated at the bottom of the reactor, advances
toward the oxygen source, while the by-product gaseous effluent travels downward, away from
the advancing thermalzone. This mode of operation is referred to countercurrentgasification. In a
continuous feed process, the sumogate mixed waste feed rate is adjusted such that it closely
matches the upward migration rate of the thermal zone. This counter balancing produces an
apparentstatiomuy thermal zone with effluent solids and gas moving in the same direction. This
mode of operation is referred to as cocurrent gasification and is the principle mode of operation
employed under this test program. Both modes of operation result in highly reductive conditions

within the reactor which promote conversion of organic material to synthesis gas, mainly
hydrogen and carbon monoxide. The oxidative thermal zone is very small in proportion to the
remainder of the reactor (=3%) due to the low flow rate of oxygen employed to sustain the
thermal front. The latter generates the necessary heat to drive endothermic reduction reactions.
The fixed bed of carbon performs numerous key functions in the ChemCharprocess. It is the in
situ fuel source, reactive substrate and principle efhent treatmentmaterialfor retention of heavy
metals and radionuclides, particulate, acid gases andproducts of incomplete gasification.
The sub-pilot ChemChar system constructed under this program has a ceramic reactor core that is
30 tall, a 4 inner diameterwith a 0.25 wall thickness.The core is fitted with 25 thermocouples
for monitoring temperature throughout its entire length. Waste solids are metered via a high
temperaturerotary star valve. The maximum solids treatmentcapacity of the reactor depends on
the carbon/waste mix ratio, but it is approximately 20-30 Kg/hour. Gaseous effluent initially
enters a cyclone separator followed by a heat exchanger for water removal, a carbon filter then
flmlly into a flare for combustion of flammable components. Gas phase effluent sampling occurs
after the heat exchanger and again after the carbon filter. The entire system is PC controlled with
sensor outputs also monitored and recorded by PC.
The onset of the testing phase of this program has just begun and the data will be reported in the
final version of the Final Report.

Final Repori

Preface
This R&D program addresses the treatment of mixed waste employing the ChemChar
l?hermolyticDetoxification process. Surrogate rnked waste streamswill be treated m a four inch

diameter, contkmous feed, adiabatic reactor with the goal of meeting all regulatory treatment
levels for the contaminantsin the surrogateswith the concomitant production of contaminantfree
by-products. Successful completion of this program will show that organic contaminantsm mixed
waste surrogates will be converted to a clean, energy rich synthesis gas capable of being used,
without further processhg, for power or heat generation. The inorganic components in the
surrogates will be found to be adsorbed on a macroporous coal char activated carbon substrate
which is mixed with the waste prior to treatment.These contaminantsinclude radioactive metal
surrogate species, RCRA hazardous metals and any acid gases formed during the treatment
process.

The program has three main tasks that will be performed to meet the above objectives. The first
task is the design and construction of the four inch reactor at Mirage Systems in Sunnyvale, CA.
The second task is production and procurement of the activated carbon char employed in the
ChemChartest runs and identification of two surrogate mixed wastes. The last task is testing and
operation of the reactor on char/surrogate waste nixtures to be performed at the University of
Missouri. The deliverables for the project are a Design Review Report, Operational Test Plan,
Topical Report and Final Report.
This report contains only the results of the design and construction carbon production-surrogate
waste identification tasks. Treatment of the surrogatemixed wastes has just begun and will not be
reported in this version of the Final Report. The latter will be reported in the final version of the
Final Report.

Final Report

Acknowledgments
Mirage Systems would like to thankthe Morgantown Energy Technology Center for the Research
OpportunityAnnouncement award for the development of the ChemChar mixed waste treatment
technology. As a small business, these R&D assistanceprograms are imviluablefor the attainment
of our goal producing a commercially salable technology.
,_

We also offer special thanks to Richard Dennis, METC Program Manager and Thomas Martin,
METC Program Contracting Officer for their patience and diJigence m working with Mirage
Systems on a program that had a short timeline and many geographiczillyseparatedprogram team
members. Their efforts on granting Mirage Systems a the

and finds extension is especially

acknowledged.
As Mirage Systems Program Manager, I would like to thank all the program team members who
are responsible for making the program a success. At Mirage Systems the key team members
were Ken Ford, Rick Underwood, Paula H.iatt,Mel Rosowski and Mark Dil?aola.
Professor Robert Gunn, retired from the Universityof Wyoming, for his outstandingperformance
on the preliminarydesign, heat balance and numerous other engineering calculations that formed
the basis of the final design of the ChemCharreactor.
The University of Missouri team who are performing the treatment portion of the program.
Professors StanleyManahan (Columbia campus) and Professor David Larsen (St. Louis campus),
the patent holders of the ChemChar technology, are aclmowledged for their insight and diligence
in all phases of the program. Special thanks to graduate students Bradley Medcalf and Rebecca
Morlando who are actuallythe ones getting their hands &preparing
surrogate waste feeds and
operating the reactor.

Table of Contents
.

Abstract ...................................................................................................................................... 2
Preface........................................................................................................................................ 3
Acknowledgments ....................................................................................................................... 4
Table of Contents........................................................................................................................ 5
List of Figures............................................................................................................................. 7
List of Tables .............................................................................................................................. 8
Executive Summary...................*..,,...**,,,....................................

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .

Introduction .............................................................................................................................. 11
Purpose..................................................................................................................................... 12.
Background .............................................................................................................................. 12
ChemChar Development History ........................................................................................... 12
CountercurrentGasification Features..................................................................................... 13
Physical Process Model ......................................................................................................... 14
Chemical Process Model ........................................................................................................ 15
The GranularCarbon Bed ...................................................................................................... 17
Fate of Organic Heteroatoms................................................................................................. 18
The Final Solid Product......................................................................................................... 18
Methodology ............................................................................................................................. 19
Results and Discussion .............................................................................................................. 19
Task 2,3 Identification of the SurrogateMixed Waste Formulations ...................

.,

. . . . . . . . . . . . . . .

19

Task 1.1 ChemCharReactor Design ...................................................................................... 20

Overview and Critical Design Issues .................................................................................. 20

Mass HOW

AIK@k

. . . . . . . . . . . . . . . . . . . . . . .. . . . . . . . . . . . . . . .. . . . . . . .. .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .. . . . . . . 22

Heat DistributionAnalysis ................................................................................................. 30

General Reactor Features-Reactor Core and Solids TreatmentTrain.................................. 34
General Reactor Features-Gaseous Effluent TreatmentTrain .............................................48
General Reactor Features-DataAcquisition and Process Control Overview ........................49

General Reactor Features-Extemal Hardware and Reactor Support Structure.................... 51

Task 2.0 Carbon/Char Procurement & SurrogateWaste Identilcation .................................. 51

..u-

Final Repod

Task 3.0 SurrogateWaste Treatment and Reactor Operation...............................0..

O..........***

55

PreliminaryTest Results To Date .......................................................................................... 55

Test Procedures for the Treatment of the SurrogateMked Wastes ........................................ 56
Mixed Waste Surrogate Preparation.................................................................................. 56
SurrogateWaste Processing .............................................................................................. 57
Effluent %npling Protocols .................................................................................................. 58
Sampling and Analysis of SurrogateWaste/Carbon Solids Residue .................................... 58
Sampling andAnalysis of ParticulateSolids ....................................................................... 59
Sampling and Analysis of Aqueous Condensate ................................................................. 59
Sampling and Analysis of Gaseous Effluent........................................................................ 60
Energy and Mass Balance ...................................................................................................... 63
Safety and Health .................................................................................................................. 63

Conclusion..0..?..0.0,..,,,

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ..0..0..

64

References ................................................................................................................................ 65
Appendix A ............................................................................................................................... 67
FiniteElementAnalysis Final Report from MCR Associates ...................................................... 67

Final Report

List of Figures

Figure 1. Thermochemical Reaction Zones in the ChemCharProcess ......................................... 13

Figure 2. Temperatureand Oxygen ConcentrationProfiles for Reverse Combustion in
UndergroundCoal Gasification (takenfrom Ref. 20) ,0.00.,....,......0,,,,..,,,,,000,
,,,

,,

. . . . . . . . . . .

14

{_

Figure 3. TemperatureProfile for Reve~se Combustion in Underground Coal Gasification (as in

Ref. 20) Including an EndothermicTerm in the Cooling Region .................................. 15

Figure 4. Electron micrograph of the TlZ13carbon to be used in the program . ............................ 17

Figure 5. Calculated equilibrium composition of the principle gas phase species as a function of
temperaturefor the high organic sludge mass flow analysis. ........................................ 29
Figure 6. Calculatedequilibrium composition of the principle gas phase species as a function of
temperaturefrom the aqueous waste mass flow analysis. .............................................29
Figure 7. Schematic of the three component reactor core used in the heat distributionfinite
element analysis. ......................................................................................................... 32
Figure 8. Schematic diagram of the continuous feed ChemCharreactor constructed under this
program...................................................................................................................... 35
Figure 9. Schematic of the surrogatewaste feed hopper............................................................. 37
Figure 10. Schematic of the reactor waste feed inlet chute. ....................................................... 38
Figure 11. Schematic of the reactor core aluminafeeder section. ..............................................39

Figure 12. Schematic of the reactor core containmentvessel top...............................................40

Figure 13. Schematic of the reactor core containmentvessel body . ...........................................41
Figure 14. Schematic of the reactor core containmentvessel bottom ......................................... 42
Figure 15. Schematic of the I-SIC 495 main reactor core..........................................................43
Figure 16. Schematic of the aluminaRF startersection. ............................................................44
Figure 17. Tuning and network matching circuit diagram for the RF induction coil heater. ........45
Figure 18. Schematic of the effluent solids exit chute andreceiving hopper lid . .........................46
Figure 19. Schematic of the effluent solids receiving hopper. ....................................................47
Figure 20. Photograph of the fully assembled ChemCharreactor. .............................................. 52
Figure 21. Sample gas chromatograrnof authenticsynthesisgas displaying locations of the
principle gaseous components. .................................................................................. 62

FinaJRepoti

List of Tables
Tablel.

High Organic Sludge SurrogateMixed Waste Formulation ......................................... 21

Table 2. NeutralAqueous SurrogateMixed Waste Formulation................................................ 21

Table 3. Input Data for the High Organic Sludge Mass Flow Analysis. .................................... 23
I

Table 4. OutputData@ 625C (40 L/rnin 02 input) for the High Organic Sludge Mass Flow

(_

Anasysis............................................................................................................................. 26

Table 5. Input Data for the Aqueous Mixed Waste Mass Flow Analysis ..................................... 27

Table 6. OutputData@ 625*C (40 L/rein 02 input) for the Neutral Aqueous Waste Mass Flow
Analysis............................................................................................................................. 28
Table 7. Physical Properties of the I-SIC 495 Ceramic. ............................................................. 30

Table 8. 1/0 Utilization for tie DACS Hardware, ..............................00..

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . ...0.

50

Table 9. Ash Mineral Analysis Data for the Arch-HarmahCoal TRB StartingMaterial..............53
Table 10. Proximate, Ultimate and BTU Data for the Arch-Haunah Coal and TRB Carbon....... 54

Final Report

Executive Summary
This Research Opportunity Announcement program will determine the treatmenteffectiveness of
the ChemChar l%ermolytic Detoxification System on two surrogate mixed waste streams. The
principle objectives of the program are to construct a continuous feed, adiabatictreatmentsystem,
demonstratehigh destruction efficiencies for the organic waste contaminantswhile simultaneously
entrappingthe volatile surrogate radionuclides and hazardous metals in a fixed bed of carbon char
within the reactor core. A secondary objective will be to demonstrate the production of a
contaminantfree, energy rich synthesisgas.
As of this writing, the project has just entered the testing phase and there is no surrogate waste
treatment data from the operation of the system. A twelve foot ChemChar reactor system has
been designed, constructed and is in-place at the University of Missouri, Department of
Chemistry.
The ChemChar system constructed under the program consists of a thermallyinsulated,vertically
arrangedceramic reactor core four inches in diameter and thkty inches tall. It is fitted throughout
its length with 25 thermocouples for temperature profiling during operation. The carbon
char/waste feed solids are contained in a hopper attachedto the top of the reactor core. Metering
of the solids is accomplished via a rotary valve at the bottom of the reactor core. The valve is
operated via PC for precise control of the waste solids feed rate. The effluent treatment train
consists of a cyclone separator, heat exchanger (condenser), sensor and sampling manifold,
volumetric flowmeter, activated carbon char filter ending with a flare.

-..

All waste processing and data acquisition is controlled by personal computer. The key controlling
parameters are the mass flow rate of oxygen and the rotation rate of the star valve. The latter
controls solids flow through the reactor which must match the upward migration rate of the high
temperaturethermalzone such that it is held stationary.The migration rate of the thermalzone is
directly proportional to the oxygen flow rate. Data horn 37 thermocouples, two pressure
transducers, star valve rotation rate and oxygen input flow rate is downloaded to disc every ten
seconds for permanent record during operation of the system. Volumetric flow of the gaseous
effluent is monitored and recorded by the flowmeter itself. Once collected, these data will be used
to determinesolids flow rate and overall heat and mass balance for a given test run.
Two surrogate mixed wastes will be subjected to the ChemCharprocess under this program. One
of the surrogates is a high organic sludge with a relativelyhigh solids and low water content with
the second surrogate essentially an aqueous waste with a low solids content. Each surrogate
contains the heavy metals cadrni~ chromium, nickel, lead and the sumogate radionuclides
cerhnn and cesiurn, all at 0.25 weight percent. Hazardous organic contaminantsfor each surrogate
include naphthalene,1,2 dichlorobenzene and chlorobenzene.
Sampling of the gaseous effluent will occur throughout a test run and the samples will be
subjected to GC and GCMS analysis for organic products of incomplete gasification, syngas
constituents (carbon monoxide, carbon dioxide, hydrogen, methane) and inorganic by-products
(hydrogen cyanide, ammoni~ hydrogen chloride and hydrogen sulfide). Pairs of samples will be
taken simultaneouslybefore and after the activated carbon char filter. All effluent sampling will
occur after the cyclone separator and the heat exchanger. Solids collected by the cyclone will be
weighed and tested for metals content only. Aqueous condensate from the heat exchanger will be

Final Report

analyzed for acid content, non-volatile organics, cyanide, sulfide, ammonia and metals. Effluent
solids will be initiallyextracted with an organicsolvent and analyzed for the hazardous organic
constituents that were present in the untreated feed. This will be followed by acid digestion and
metals analysis.
Combined the analyticiil data from the solid, liquid and gas phase samples will allow for an
accurate mass balance computation for each process run. The accumulatedtemperaturedata from
the input and output of the condenser cooling water, reactor core and outer surface of the reactor
containmentvessel will be employed to determineoverall heat balance of the system.

10

:FinalRepoti

Introduction
The mixed waste treatment problem faced by the Department of Energy requires little m
introduction. It has been addressed in countless publications over the past ten years. Although the
exact estimates of the volume vary, one fact remains: that the current stockpile of mixed waste
streams vary greatly in hazardous and radioactive constituents and the matrix in which they are
contained, The implications of this are clear, that there is no panacea mixed waste technology
capable of treatingall of the currentmixed waste streams.
The current Department of Energy strategy of funding the development of new and innovative
mixed waste treatmenttechnologies to the pilot-scale provides proof-of-concept treatmentdata,
~kmy employing surrogates, for which a decision to pursue pilot-or full-scale development is
made. The ChemChar thermolytic detoxification technology, tided
under the Research
Opportunity Announcement, is a proof-of-concept R&D program scheduled for approximately
one year.
The ChemChartechnology employs an inexpensive, activated carbon which is combined with the
mixed waste stream prior to processing. It is this admixing of carbon with the waste stream that
distinguishesthe ChemChar technology from other reductiveprocesses. The carbdn functions as a
fixed bed support, reactive substrate for promotion of chemical reduction reactions, fiel source,
and in situ air pollution control medium. The carbon bed has been shown to retain acid gases,
volatile heavy metals, volatile organic compounds (VOC s) and particulate. Depending on the
inorganic loading of the waste/carbon feed, the effluent materialis readily retied with waste and
subsequentlytreated.
The ChemChar process converts organic matter in a waste stream to synthesis gas (hydrogen,
carbon monoxide, carbon dioxide and water). This gasification is accomplished by operating the
reactor in the reverse burn mode. This mode of operation (employed in batch treatment) is
characterized by the fact that the thermal front migrates in the opposite direction of the input
oxidant and product gas. In continuous feed operations, the solid carbon/waste feed rate is
adjusted such that it corresponds to the thermal front migration rate resulting in a stationary
thermal zone. This mode of operation is termed cocurrent flow gasification and is the principle
operating mode for the testing of the surrogatewaste streamsin this program.
Compared to other thermal mixed waste treatment technologies, the principle advantage
ChemCharmaintainsis one of reduced off-gas treatment.Plasma arc, vitrification, molten salt and
metal melting technologies require extensive off-gas treatment of their effluent. The moderately
mild conditions of the ChemChar process (only one section of the reactor core is subjected to high
temperatures) also reduces corrosion of key components and significantly extends the life of
overall treatmentsystem. The results generated from this program will quantitateand substantiate
these attributesof the ChemChar mixed waste treatmentsystem.

This R&D program addresses the treatment of mixed waste employing the ChemChar
l%ermolytic Detoxification process. Surrogate tied waste streamswill be treated in a four-inch
diameter, continuous feed, adiabatic reactor with the goal of meeting all regulatory treatment
levels for the contaminantsin the surrogates with the concomitant production of contaminantfree
by-products. Successful completion of this program will show that organic contaminantsin mixed
waste surrogates will be converted to a cle~ energy rich synthesis gas capable of being used,

11

Final Report

without further processing, for power or heat generation. The inorganic components in the
surrogates will be found to be absorbed on a macroporous coal char substrate that was mixed
with the waste prior to treatment.These contaminantsinclude radioactive metal surrogate species,
RCW4 hazardous metals and any acid gases formed duringthe treatmentprocess.
\

The program has three main tasks that will be performed to meet the above objectives. The first
task is the design and construction of the four-inch reactor at Mirage Systems in Sunnyvale,
California. The second task is production and procurement of the carbon char employed in the
ChemChartest runs and identification of two surrogate mixed wastes. The last task is testing and
operation of the reactor on char/surrogate waste mixtures to be performed at the University of
Missouri.
The deliverablesfor the program include a Design Review Report, Test Plan, Topical Report and
Final Report.

Purpose
The purpose of this program is to demonstrate the treatment effectiveness of the ChemChar
mixed waste technology on two surrogate mixed waste streams. The program will determine
destruction efficiency of target organic contaminants, retention of volatile metals and
radionuclides within the carbon/waste substrate, production of a contaminant free gaseous

effluent and leaching characteristics of the solid by-products. The successful outcome of this
program will result in data that will allow for the construction of a full-scale ChemChar system
capable of treatingauthenticmixed waste streamsat a specified DOE location.

Background
ChemChar Development History
In the ChemCharProcess, the proper conditions for gasification are created so that a complex set
of chemical reactions can occur, and these chemical processes result in the establishment of a
unique thermalprotlle in the reactor. The resultis a very efllcient conversion process. The process
is an outgrowth of laboratory studiesl-2thatwere undertakento better understandthe chemistrym
undergroundcoal gasitlcation (UCG)3-5.UCG is one of the many well-known methods that can be
used to convert carbonaceous materialto a combustible gas. Of particularinterest for UCG were
hazardous organics that remain underground after gasiilcation, thus presenting a source of
pollution, and the laboratory studies were undertaken to identify these compounds. As an
outgrowth of these studies, a form of low grade activated carbon was prepared in the laboratoryG
by gasification of coal, using the countercurrent gasification mode, one of the modes used m
UCG. In subsequent studies74using this activated carbon, (or char) the ChemCharprocess was
developed9-12.The process thus has its origins in gasiilcation, which is a well-established
technology13.

The gasification step of the ChemCharprocess can be carried out in a simple reactor, a schematic
illustrationof which is shown m Figure 1. Prior to gasification, the waste is mixed with granular
carbon char, to form the porous bed within the reactor which allows for facile gas flow through
the bed, Oxidant gas (oxygen) is introduced at the top of the reactor and the combustible gas
product (waste derived fuel) emerges from the bottom of the reactor. Partialoxidation of organic
components occurs within the therrnochernica.1gasification zone, which moves through the
12

Final Repoti

column of granularcarbon toward an incoming oxygen gas stream. Conversion of these products
to combustible gas occurs primarily at the lower end of the gasification zone and also in the
reduction zone, which extends well into the bed of reactivated carbon directly below the
gasification zone. The reaction zone movement in the direction opposite to that of the gas flow is
termed countercumentmode. This mode of operation occurs during batch processing.
Dlractlon of Gasffloatlon Zone Movement

ttt

Oxfdant Flow In

Combustion Zone
Waste

Oxidation, Pyrolysis

Losded

Combustion

Stswed Alr
Thermochemical
Gasfffcatfon Zone

Partial Oxidation, Pyrolysis

Primary Reduction
Zone

Gasification, Pyrolysis
I

Secondary Reduction
Zone

I
t
Waste Derived Fuaf

Thermochemical

Reaction Zone

(EnlargedView)

Figure 1. Thermochemical Reaction Zones in the ChemCharProcess

.

The conversion of waste organic compounds is dependent on the presence of a thermal reaction
band consisting of three zones: a very narrow, high temperature(>1200C) oxidative combustion
zone which lies directly above a very narrow high temperate (850 to 1000C) partial oxidative
gasification zone, which in turn lies directly above the much longer, lower temperaturereductive
gasification zones, as shown in Figure 1. A this complex thernxilreaction band travels upward
through the granularbed (typically at speeds of a few cm/rnin, depending on the oxidant flow
rate), organic material contained in the column is converted to gaseous products, and as these
products travel throughthe long reductive zone, they are converted to a combustible gas titure.
Countercurrent Gasification Features

Countercurrentmode gasification has several unique and favorable features for treatinghazardous
wastes. First, the solids directly above the thermochemical gasification zone are close to ambient
temperature.This mhimizm volatilization of contaminantsm the waste prior to the solids mass
enteringthe thermalreaction zones. In addition, any volatilized matterwill be swept into the zone
by the gas flow through the reactor, so that it is impossible for these volatilized species to exit the
reactor without being subjected to the high temperaturereaction zone. Second, the gases exit the
reactor through a region of regenerated carbon, which will tend to contain trace amounts of
unreacted organics or volatilized heavy metals. Third, the high temperature reactions are very
localized. On a macroscopic scale, with respect to the reactor, the zone is confined to a small
portion (typically 10% or less) of the tott-dreactor volume, which minimizes the overall thermal

13

Final Repoti

mass. Premixing the waste with the carbon, which results in adsorption of organic and inorganic
contaminants,provides for efficient thermochemicalconversion of the waste to reduced products
with only minimal consumption of carbon. This is a result of carbon being an excellent reducing
agent (source of electrons) and the anoxic environment of the reactor.

-.

The ChemCharprocess has two important, intrinsicsafety features that allow for rapid shut-down
of the system in case of process upset: First, is the smallthermalmass of the reactor, as described
above, and the fact thatthere is no externalheat source. Second, when oxidant flow is stopped, all
exotherrnicreactions cease, while the highly endothermic reduction reactions continue, consuming
significant quantitiesof heat which provide cooling of the reactor.
Physical Process Model

Countercurrent mode gasification has been studied extensivelyl~lg, and a simple model for the
process has been publishedzo. The model is obtained by applying the heat equation in one
dimension, along the axis of the gasifier. Heat is generated in the reaction zone by exothermic
chemical oxidation reactions. A single set of Arrheniusparameters and reaction enthalpyis used
to model the process chemistry. This is an oversknpliflcation, since the process chemistry is
complexzl (18). The heat is carried by conduction upstream, in a direction opposite to the flow of
incoming oxygen, radiation effects are ignored for simplicity. Because of the heat transfer, the
reaction zone advances toward the oxygen source (upstream). The oxygen is rapidly depleted m
the upper-most portion of the reaction zone, and the hot, gaseous chemical products carry heat
away from the reaction zone (downstream) by convection. A term for heat loss to the
surroundings is also provided in the equation, however, the hot gases undergo endothermic
reactions with the solid carbon surface as they continue downstream, which provides additional
cooling.
[02

100[
W lnpion

Rata.

m SC

f7
[Oxygan COhc.ntmtlon)

$$

~$?
10
o

0,4

Y,

Distance (Ft)

Typical Oxygen Concentration

Temperature
Profiles

and

Figure 2. Temperatureand Oxygen Concentration Profiles for Reverse Combustion

in UndergroundCoal Gasitlcation (takenfrom Ref. 20)

.-

14

. .

Final Repoti

The thermalprofile obtained by numerical solution of the heat equation, is shown in Figure 2. This

result can be compared with the observed laboratory reactor profile as described above. This
simple treatrnent20gives a reasonably good description of the observed steep thermal gradient at
the top portion of the reaction band, which is the oxidative combustion zone. However, this
treatment does not adequately describe the observed behavior immediately below the oxidative
combustion zone, where there is a second steep thermalgradient (of opposite sign). This is caused
by the cooling effect of the endothermic chemical processes in this region, which is a reduction
zone. If the heat equation is modified by inclusion of an endothermic term m the reduction zone,
the modified equation does reproduce the observed steep thermal gradient below the combustion
zone. The result is shown in Figure 3.
One Dlmenslonel Model
I

HdJng

COollng

Endothennlc Chernletry

_l__&++

I
-0.2

0.0

0.2

Underground Coal Gasification

Figure 3. TemperatureProf.i.iefor Reverse Combustion in Underground Coal Gasification
(as in Ref. 20) Including an EndothermicTerm in the Cooling Re~on
An importantaspect of the countercurrentmode of operation is the stabilityof the reaction ftont.
This question has been studied in detail both theoretically and experimentally522.Criteria for
stabilityare given, from which it can be concluded that the ChemCharprocess is stable, primarily
due to the features of the well defined granularcarbon bed. The results from the experiments to
be performed under this program, by virtue of the embedded thermocouples the length of the
reactor core, will quantitativelydeterminereaction front behavior.
Chemical Process ModeI
The complex chemical processes occurring in all the zones of the ChemChar process are
reasonably well understood21. Exotherrnic oxidation reactions serve to initiate the process. For
sirnpl.icity,if the waste organics are represented as CHO and the char surface is represented as C,
the initiationreactions involving carbon are:

15

Final Report

C +02 ---> COZ + Heat

C!-t-1/202 ---> C02 + Heat
CO+ 1/2 02---> C02 + Heat

and there are a number of analogous initiationreactions involving the waste:

2 CHO I- 3/2 Oz --->2 COZ + HzO + Heat

These heat generating processes promote a series of complex thermally-induced (pyrolysis)

reactions, which can be wtitten for simplicity as:

2 CHO + Heat --->2 CO + Hz

and they also promote endothermic reactions iwolving the reductive carbon surface:

C02 + C + Heat --->2 CO

H20+ C + Heat ---> CO + Hz

The reaction zone is rich in nascent hydrogen (the hydrogen atom, represented as (H} ), which is
highly reactive. This is formed by free radicil processes of the type:
R-CH2-CH2-R ---> R-cHZ+ CH2-R
R-CHZ-CHZ* ---> R-CH=CHZ + {H}

Nascent hydrogen leads to efficient dehydrohdogenation of organochlorides (e.g., PCBS), which

may be representedsimply as:
RC1 + {H} ---> R+ HC1
Because of the reductive environment, dehydrochlorination proceeds without the formation of
polychlorinated d.ibenzodioxins (PCDDS) and furans (PCDFS).
PCB --8-> PCDD/J?CDF

16

Final Report

The Granular Carbon Bed

The characteristic of the ChemChar process that enhances its performance and distinguishesit
from other gasification technologies is the granularcarbon bed. The ChemCharprocess employs a
particularly useful form of medium grade, granular (l-5 rnxnparticle size) activated carbon,
prepared by the gasification of coal. An electron rnicrograph of carbon prepared horn
subbituminouscod is shown in Figure 4. Note that the surface of the carbon contains very large
pores (macropores) which give it the ability to sorb large quantities of oils and other organic
media The carbon also has a low apparent density, again due to the extensive presence of
macropores.
The ChemChar technology derives the energy (heat) needed fio treatment solely from the
carbon/waste mixture. The process thus contains a built-in improvement in handling
characteristics for difficult materials such as oily sludges and tars. Sorption on the inert,
chemically-reducing carbon also provides a degree of stabilizationand solidification of the waste.

A. Commercial
GAC (35x)

B. TRB

GAC
C. Commercial

Carbon(35x)

D. TRB

(1,000 x)

Carbon(1,000x)

Figure 4. Electron micrograph of the TRB carbon to be used in the program.

17

Final Report

The gasification is carried out in a reactor of simple design in which the carbon/waste mass forms
the porous bed. Gasification is done in the countercurrentmode, for batch processing, in which
organics are converted to fuel gases. Some of the water present in the waste participates in the
chemical process; the remainder evaporates. A small portion of the carbon (typically 10%) is
consumed in the process. The remainderis the solid residue inside the reactor, which retains the
inorganic components of the waste. The porous packed bed configuration eliminatesparticulate
and the carbon has been shown to adsorb and retain heavy metalslG18-19.The natural alkalinity
(derived from carbonates in the coal startingmaterial) of tie carbon also neutralizes acid gases,
retainingthe salts in the packed bed.
Fate of Organic Heteroatoms
The fate of organic heteroatoms during gasification is determined by the strongly reductive
environmentof the carbon bed. Dehydrochlorinationproduces HCl as expected but of particular
significance is the fact that the carbon bed is sufficientlychemically reducing that when C12gas is
introduced into the gasifier under char bed gasification conditions, it is also converted to HC1.The
heteroatoms, sulfur and nitrogen commonly produce oxides designated SOX and NOX,
respectively, under oxidative waste treatmentconditions. Gasification under ChemChar conditions
for waste containing these atoms, produces reduced products. The sulfur moiety in sulfur
containing chemicals is typically converted to hydrogen sulfide, HzS, which being acidic may be
neutralizedby residual carbon bed alkalinity.If HzS is produced in large quantity, it will require
scrubbing from the effluent in the synthesis gas processing section of the reactor. The nitrogen
atoms of N-containing species (e.g. organic arnines or inorganic nitrates) are converted to a
mixture of two reduced forms, ammonia (NH3) and nitrogen gas (NZ). The ultimate ratio of
NHSNZ will depend on the process chemistry, which is determinedlargely by the composition of
the waste mixture. Species containing the heteroatoms sulfur and nitrogen are present in the
mixed waste surrogates to be treated under this program and ihrther data on the fate of these
elements during ChemCharprocessing will be generated.
The Final Solid Product
Based on bench-scale studies, typically 10% or less of the carbon is consumed during the course
of a gasitlcation, This result provides the possibility of recycling the waste/carbon residue from
the process. A net gain of carbon is also possible if the waste feed has a very high hydrocarbon
and low ash or inorganic content. The extent of reuse of the carbon process residue will be
directly proportional to the inorganic content of the original carbon/waste feed mixture. Within
the reactor the active sites of the carbon are ~ed by the inorganic contaminantsorigirdly present
in the waste or produced (e.g. H2S) during treatment. Once saturated, regeneration (md hence
recycling to the front of the process) will not be possible and disposal of the inorganic-saturated
carbon will be necessary.
Final disposition of the carbon residue will depend on the original waste feed and the appropriate
regulations. In the case of mixed and radioactive waste treatmentthe residue is best controlled by
applying a second gasification in the forward burn mode. In this mode, which is performed on a
batch basis, the reactor bed is heated at the same end as that in which oxygen is injected so that
the reaction zone travels in the same direction as the gas flow. The result is that the carbon (and
all combustible material) in the residue is completely consumed and the residual inorganic
components are converted to an inert slag. This forward bum mode generates significantlymore

18
,_

Final Repoti

heat than the countercument or reverse burn mode and this extra heat is responsible for slagging
the inorganic component of the spent ChemChar process residue. This achieves further volume
reduction and may result in a mixed or radioactive waste iinal form capable of passing the PCT or
other rigorous radioactive waste leach tests. Addition of additivesprior to forward burn operation
is also possible to assist in the formation of a more stable, inert glass. This mode of operation is
not part of this program and will not be performed on any of the process residues unless time and
funds are available.

Methodology
This ROA development program was carried out by following the tasks and subtasksbelow:

l.O

2.0

3.0

Design and Construction of ChemChar Reactor

1.1

Design of Reactor

1.2

Fabricate Reactor

1.3

Shakedown Reactor

1.4

Prepare Data Acquisition and Reactor Control Software/Hardware

Carbon/Char Procurement & SurrogateWaste Identification

2.1

Carbon/Char Procurement and Production

2,2

Carbon/Char Characterization

2.3

Identify SurrogateMixed Waste Formulations

SurrogateWaste Treatment and Reactor Operation

3.1

Upgrade Univ. of Missouri Laborato~/ TransportReactor

3.2

PrepareTest Plan

3.3

Execute Test Plan

3,4

EvaluateTest Results/PrepareFinal Report

As of this writing, all tasks and subtasks are complete except for 3.3 and 3.4. Detailed discussions
of each of the completed tasks are in the Results and Discussion section.

Results and Discussion

Thisdata and information described in this section is formatted by task and subtask m the order it
was executed during the course of the program except for a discussion on the identificationof the
mixed waste surrogateformulations chosen for the progrsrn.Familiaritywith these formulations is
necessary since they are consistentlyreferredto in many of the discussion sections below.
Task 2.3 Identification of the Surrogate Mixed Waste Formulations
Evaluationof the ChemCharprocess for this ROA program will be accomplished by treatmentof
two surrogatemixed waste streams.The targetattributesof the streamsincluded the identilcation
of a mixed waste stream that represented a reasonable amount of currently stockpiled mixed
waste within the DOE, streamsthatcontained a range of contaminants,inorganic and organic that

19

Final Report

would challenge the ChemChar process and two different waste matrices for testing the material
handlingcapabtiitiesof the technology.
The DOE approved surrogate formulations, listed below in Tables 1 and 2, were identified and
meet all the target attributes.The formulations were obtained from the DOE MWIP Report23:

Surrogate Formuhtions for Thermal Treatment of Low-Level Mixed Waste, Part II: Selected
Mixed Waste TreatmentProject Waste Stream.
The selected surrogate wastes mimic a high organic sludge and an aqueous waste. The former
waste will test the ChemChar process for destruction and gasification efficiency due to the high
organic content. The latter stream @ test the absorbing characteristicsof the carbon for fiontend materials handling and feeding as well as the behavior of the ChemChar process during
treatment of high water content wastes. The chlorinated organic Resource Conservation and
Recovery Act (RCRA) contaminantsin these wastes are ideal for the purposes of displaying acid
gas adsorption (in this case HC1) within the reactor. The RCRA metals present in the surrogates
have a range volatility (lead and cadmium high, chromium and nickel, low to moderate) that will
test the in situ adsorption behavior of the waste/carbon packed bed in the reactor. These metals
are also found in many of the currently stockpiled mixed wastes. The radioactive metal
surrogates, ceriurnfor uraniumand plutonium and cesiurnfor radioactive cesium isotopes should
also challenge the process, especially cesiurndue to its extreme volatility.
Detailed procedures for the preparation of these surrogates and the subsequent mixing with the
carbon will be discussed in the Test Plan portion of this section.
Task 1.1 ChemChar Reactor Design
Overview and Critical Design Issues
One of the principle objectives of this program is to construct a continuous feed, adiabatic, frilly
PC controlled ChemChar reactor for the treatment of surrogate mixed waste. Except for this
program, all experimentationemploying the ChemCharprocess has been in a non-adiabatic mode
where no attempthas been made to control heat loss in various parts of cylindricalvycor and steel
laboratory-scale test reactors. As an aid to understanding the basis for the reactor design
described in this report, a discussion of the various temperature zones and past processing
observations employing batch ChemCharreactors follows.
Figure 1 (p. 12) displays the various reaction zones within the ChemChar reactor core. Initiating
the process is accomplished by input of oxidant from the top of the reactor and heating a carbon
or carbon/waste mixture at the bottom. Once the mixture reaches its ignition temperature (300400C) a combustion front or thermochemical reaction zone (TRZ) is formed. Since the amount
of input oxidant (~ically pure oxygen) is much less than stoichiometric with respect to complete
combustion of the organic materialin the reactor, the geometry of the TRZ is that of a thin, radial
disc that migrates toward the source of the oxidant. In this example the gaseous products of this
process flow out the bottom of the reactor. If the TRZ is allowed to reach the source of the
oxidant its migration direction will reverse moving in the same direction as the input oxidant and
product gas flow. This forward combustion mode resultsin near complete oxidation of all organic
material and significantlyhigher operating temperatures. This mode of operation is undesirable
since its gaseous output is principtiy made up of carbon dioxide and water, not synthesisgas, the
principle product of reverse combustion and the desired output of the ChemChar reactor.

20

Final Report

Table 1. High Organic Sludge SurrogateMixed Waste Formulation

&

Comuonent
Name

wt. %

BulkIngredients

Comuonent
Name

Wt %

RC!RA
Orwinics

1
2
3
4

Activatedcarbon
Water
Perlite
FezOs

10

5
6
7
8

CaS04*2H20
&03
EthyIeneG1ycol
MineralOil

10
5
14.5
12

20
10
10

13
14
15

Naphthalene
1,2Diehlorobenzene
Chlorobenzene

3
2
2

Total

91.5

RCRAMetals
9
10
11
12

Radionuclide
Surrogates

PbC12
CdClz02.5Hz0

0.25
0.25
0.25
0.25

Total

1.0

CrClso6H20
NiC1206H20

16
17

CeCls
Cscl

0.25
0.25

Total

0.5

Table 2. NeutralAqueous SurrogateMixed Waste Formulation.

&

Comuonent
Name

wt. %

&

BulkIngredients

2
3
4
5

75

CaClz
NaHCOs
MgS0407H20

3
3
3

6
7

Na2HP04*7H20
my Ash(MTM Chss I?)

2.5

Total

97.5

10

13
14

Naphthalene
1,2Dichlorobenzene

0.4
0.3

15

Chlorobenzene

0.3

Total

1.0

RCRAMetals
9

10
11
12

wt. %

RCRAOrimnics

Activatedcarbon
Water

Comuonent
Name

Radionuclide
Surrogates

Cr(N03)309H20
Ni(N03)zo6H20
Pb(NOJz
Cd(JVOJ2.4H20

0.25
0.25
0.25
0.25

Total

1.0

16
17

21

CeCls
CSCI

0.25
0.25

Total

0.5

Final Report

The TRZ generates all the necessary heat to drive the endothermic reforming reactions in the
reduction zones below this region (Figure 1). MinimMng heat loss in the reduction zones is
critical for the conversion of organic waste materials,at appreciable rates, to synthesisgas (CO,
H2). At the same time, cooling of the reactor walls above the combustion zone must occur to
prevent the rapid migration of the TRZ to the top of the reactor and entering into a forward
combustion mode. Although minimization of heat loss is critical for conversion of organic
pollutants to synthesisgas, removal of heat above the TRZ is also just as critical. The following
calculations give an indication of the component temperatures of a near adiabatic ChemChar
reactor and exempli@ the likelihood of the onset of forward burn operation within the reactor.

Assuming a 1500C TRZ peak temperature and 35% heat loss by radial conduction, the inner
wall of the reactor core in contact with the thermal reaction zone will attain a temperature, at
steady state, approaching to 1300C. Conduction of heat by the reactor walls will increase the
temperature of the carbon/waste mixture above the TRZ. This results in an increased rate of
migration of the TRZ upward toward the top of the reactor and increases the likelihood the
process entering into a forward combustion mode. Therefore, the removal of heat in the upper
third of the ChemChar reactor will be necess~ for the successful operation of the overall
process. The project team believes the design described below and subsequently constructed
addressesthis critical concern.
Several intrinsicreactor properties will offset, to some extent, entrance into forward combustion
mode. The flow of cool (room temperature) carbon/waste feed will absorb heat from the walls in
this portion of the reactor as well as the flow of cool oxidant gas. Based on smaller scale test
results, these cooling mechanisms by themselves, may not filly prevent the onset of forward
combustion and thusexternal cooling of the wall was incorporated into the final design.
Before discussing the design of the ChemChar reactor constructed under this program, a detailed
mass flow and reactor core materials analysis will be described. These results will aid in the
understandingof the final design of the adiabatic ChemCharreactor.
Mass Flow Analysis
The following is a detailed mass flow analysis for the processing of the approved high organic
sludge mixed waste stmrogate (Table 1). The aualysis was performed using HSC Chemistry
modeling software by Outokurnpu Research (Finland). The calculation involves the
thermodynamicminimization of the free energy of a system (i.e. equilibrium) based on the input
concentration of startingmaterials,identificationof potential product species (150 maximum) and
specified temperature.The credibility of the output from these simulationsis increased if as many
potential product species as possible (and their phases: gas, liquid, solid) are defined. Table 3
displays the starting materials and their respective concentrations employed while Table 4
summarizes the predicted products and their concentrationsfrom the simulation. The total number
of species is 150 which is the maximum input allowed by the program. The thermodynamic data
(free energy, AG, enthalpy,AH, entropy, AS, and heat capacity, Cp) employed by the program are
included in a database containing over 7000 compounds. All potential products envisioned to be
formed by a ChemChar run were included in the database along with their respective phases,
numbered 1-4. A wdue of 1 corresponds to the gas phase, 2 the liquid phase, 3 the solid phase and
4 newly formed solid phases.

22

FinalReport

Table 3.

hput Data for the High Organic Sludge Mass Flow Analysis.

mass (g)

moles

Species

198.7

13158

I 103.2

I 1858

1827.4

19938

CZHGOZ(ethyleneglycol)

21.8

1353

CGH421(chlorobenzene)

1.65

185

185

CZOHAZ
(mineraloil)

13.96

I 1119

CloHg(naphthalene)

12.18

CL@@~ (dichlorobenzene)

I 1.26

279

CdC12

I0.102

I 18.7

PbC12

0.084

23.6

crcl~

0.087

13.8

10.098
23.2

0.138

Cscl
CeCl~

23.2

0.94
1

CaO

I5.35

[ 300

Fe203

15.82

1929
I

CaSOA~2Hz0 (gypSUIYl)

A1203
Perlite
Total Solids Input Mass:
(a).

5.40

1930

[ (a)

1465

[ (a)

I930

18,586 (excludes OJ

Dueto thesespeciesinertbehaviortheywerenotincludedin thesimulation

23

:Final Repozt

The modeling software does not simulateprocessing parameters such as solids flow rate and
variable temperature zones, in which there are several in the ChemChar process. This is an
equilibriumcalculation and the output should be evaluated based on this fact and only this fact.
The input concentrations for the stinting materials, namely all the high organic sludge
constituents, carbon and oxygen, are based on the processing of three reactor volumes of this
mixture. The project team believes that equilibriumwill be approached or met at this level of
waste/carbon processing. The total input solids mass for the simulation was 18,534 g
composed of a 1:1 by weight mixture of carbon and high organic sludge. This amount was
derived according to the following processing assumptions:

Thermochemical Reaction Zone Velocity:

Volume of Reactor:
Reactor Length:
Single Reactor Volume Process Run Time:
Volumetric Waste Flow:
Density of SurrogateWaste (calculated):

3.81 crnlmin
6178 cm3
76.2 cm
20 rnin
309 cm3/hlin
1.5 g/cm3

Density of SurrogateWaste/Char Feed (calculated):

1.0g/cm3

Mass of Feed for 3 Reactor Volumes:

18,534 g

Recall, that the feed rate of waste for the continuous feed ChernCharprocess is governed by the
velocity of the thermochemical reaction zone (TRZ). The feed rate is adjusted such that the TRZ
is kept stationary. The value of 3.8 lcrn/min employed for this mass flow analysis is an average
velocity based on,previous experimentalprocess runs.
The last critical input to the simulation is the quantity of oxidant. Based on the high organic
content of this waste/char mixture and the desire to obtain upper limit, high volume flow
engineeringdata, a volumetric flow of 40 L/rein of oxygen was used. This represents 98.7 moles
of 02 (3. 16 Kg) required to process three reactor volumes of char/waste feed. Note that this is
several orders of magnitude less oxygen required for complete combustion of all the carbon and
organic compounds in the feed material.
Two compounds in the high organic sludge formulation were excluded from the simulationbased
on their inert chemical properties. They were perlite, which is a silicaceous diatomaceous earth
filtering aid and alumina.Included in the siinulationwas lime (CaO). This was included based on
the fact that the carbon contains ash and significantalkalinity,estimated at 1 milliequivalent/grarn.
Mineral oil was assumed to have the molecular formula of eicosane (C2@l!42).
The resultsof the simulation at a fixed output temperatureof 625 C are displayed in Table 4. The
predicted products in Table 4 represent a concentration cut-off of 1 millimole. The calculated
gaseous output for a three reactor volume process run is 441.6 moles. Employing the ideal gas
law and a 60 minuterun time, the calculated gas flow rate from the reactor at 625 C is 542 L/rnin
at equilibrium. This represents a 13.5 fold increase based on input gas flow (40L/min). The
calculated mass of output solids is 12.9 Kg resulting in a modest mass reduction of 30%. The
calculated carbon consumption is 7Yo, very close to the experimentallyobserved values of 10%
found k smaller laboratory-scale ChemChar process runs. It should be noted that all Resource
24

. ._,

.. . ..

-Final Repoti

Conservation and Recovery Act (RCRA) regulated organic contaminants(the chlorobenzenes and
naphthalene) are predicted to be completed destroyed. The highly reducing conditions of the
ChemCharprocess was also confirmed by the chemical reduction of sulfur containing compounds
(from gypsum in the high organic sludge surrogate) to hydrogen sulfide. Although the shnulation
predicted most of it being neutralized by the alkalinelime and iron oxide, it is prevalent in the
effluent gas at a level of 630 ppm (mole basis). This compound will be monitored closely in the
actual process runs and may require scrubbing in larger scale reactors if it is found at significant
levels in the effluent on this small scale.
The RCIM metals in the surrogate are predicted to be converted to a mixture of the original
chloride starting material, oxides (by hydrolysis), sulfides and elemental (lead, nickel and

cadmium) species. The radioactive surrogate metal cenum is predicted to be converted to the
sulfide. Cesium remained as the chloride thus retaining its high volatility and will have to be
carefully monitored duringthe experimentalprocess runs.
The output temperature of 625 C was chosen based on experimental measurements of smaller
scale ChemChar process runs. Allowing the modeling software to calculate the adiabatic effluent
temperaturebased on the input and output concentrations of the products in Table 4 results m a
value of 800 C. Allowing for 3-5% heat loss the output temperatureof 625 C used for the mass
flow analysisis reasonable.
Mass flow analysisfor the aqueous mixed waste surrogate was attempted, but required the input
of the metal nitratesalts as separate species. This was required due to the lack of thermodynamic
data on the pure nitrate salts of chromium and nickel. Thus, the chlorides of the metals and
sodium nitratewere employed to mimic these compounds. This analysis also employed a carbon
to waste mix ratio of 1:1 with on input oxygen flow of 40 L/rnin. All other conditions were as
described for the high organic sludge mass analysis. The input species and their associated
concentrations arelisted in Table 5.
The results of the aqueous stream mass flow analysis are summarized in Table 6. All the output
data were taken at a temperatureof 625C. The major difference between the waste streams is the
increased mass reduction for the aqueous stream, predicted to be 6090. Clearly, this is from the
high water content of this waste stream. The water is not simply being vaporized, but is
promoting synthesis gas reactions with the organic compounds and carbon in the reactor
producing significantlymore gas phase products. kdeed, this mass amilysispredicts 36% loss of
carbon at 625C compared to only a 7% loss in the high organic sludge mass analysis.Converting
the product gases to flow results in a 845 L/rein effluent flow rate for processing of this waste. All
the RCW3 organics are predicted to be destroyed by this analysis, including the nitrate species,
with the principal nitrogen containing product being nitrogen gas with a small amount of
ammonia. The RCRA metals in the aqueous surrogate are predicted to be reduced to elemental
species (Pb, Ni, Cd) while chromium is hydrolyzed to the oxide Cr203. Unlike the high organic
sludge waste, there is no significant sulfur containing compounds to allow for formation of the
very stable metal sulfides. The radioactive surrogates were maintainedas the chloride for cesium
and converted to the oxide for cerium. This analysispredicted a finite amount of cesium chloride
in the gaseous effluent. Although expected, due to the high vapor pressure of this chloride, it is
anticipatedthatthe packed bed will prevent its volatilization.

25

~Final Repoti

Table 4,

Output Data @ 625C (40 L/rnin 02 input) for the High Organic Sludge Mass
FlowAnalysis.
Species

moles

mole%

co(g)

H2(g)

71.78
103.99
157.14

16.2
23.5
35.6

H20(g)

95.51

2.2

CoQ(g)

m(g)

2.8

12.32
I

HCl(g)

I 0.59

10.13

H2S(g)

0.28

0.063

moles

mass(g)

539.34

C(diamond)
Pbc12

257.16
2.06X1(Y2
8.6x 104

6470
3090

CaO

2.85

CdC12

Fe203
CaC12

Cscl
Cd
Nl

Pb

cr203
Ca(OH)2
CdO
CaS
Nls
Pbs

NiO
CeS2

CaC03
Fe

0.14
2.32
0.138
8.05X 10-2
9.Wx 10-2
6.41X 102
1
I4.36X102
2.65X 103
8.67x 104

0.74
7.72X103
1.91x 10-2
2.54X 104
I
I 9.40x10-2
4.83
0.99

3.8
0.24
159.8
I

22.4
257.5
23.2
9.05

5.3
13.3
I
I6.6

0.2
0.11

53.4
0.7
4.6
0.02
I
I 19.2
4s3.5
55.3

FeO

6S2

439,7

Fe30A

1.88x 10-2

FeS
FeS2

4.17
1.51x 104

4.4
366.6

A1203

N/A

465

Perlite

N/A

930

Total Solids Output Mass (excludes gases):

26

0.02

12,900

FinalReport

Table 5.

Iiput Data for the Aqueous Mixed Waste Mass Flow Analysis.
Species

mole

mass (g)

o~

98.7

3158

CGH@

0.248

27.9

I 0.19

I 27.9

c6H4cl~

403

7254

C10H8

I 0.290

37.2

NaHC03

I 3.32

I 279

I 0.867

I 151

I 2.514

I 279

I
I
I
I

H20

CaCl~
MgSOd

1.132

136

crcl~

0.058

9.2

Niclz

0.08

NaN03

10.4

[ 0.334

I 28.4
16.6

I 0.07
1

Pb(NOJz

Cscl

0.075

24.8

I 0.138

I 23.2

CeCls

0.094

23.2

827.430

9938

CaO

I 5.350

Total

Solids

(excludes Oz):

Input

Mass I

I
I

I 300
I

1S,566

Figures 5 and 6 display the temperatureversus concentrationplot for the major gaseous products
of the of the mass flow analysis for the high organic and aqueous waste surrogates,respectively.
They predict thatif the reductive zones can be maintainedabove 600C an enriched CO and Hz
synthesisgas can be prepared with a reasonably low moisture content. The steep slopes of the CO
and Hz curves predict thatsmall variations in temperatureproduce significant changes in
production of these two compounds-the preferred gas phase product of the ChemChar process.
Thus, a signiilcant effort in maintainingas high a temperatureas possible in the reductive zones of
the reactor was incorporated into the design.

27

Table 6.

Output Data @ 625C (40 L/miu 02 input) for the NeutralAqueous Waste Mass
Flow Analysis.
Species

moles

co(g)

137.2

I 19.9

CoZ(g)

169.2

H2(g)

234.4

124.6
,
I 34.1

H20(g)

I 121.2

I 17.6

mole 70

125.4
HCl(g)

0.44

0.06

Cscl(g)

7.1X10-5

1X10-5

NI&(g)

13.6x10-3

I5.1X104

1498

15978 -

MgSOA

1.13

136

CaO

0.094

5.3

Cscl

0.14

23.6

Cd

0.069

7.8

Ni

0.08

4.7

Pb

0.075

15.5

CaC12

Cr203

10.029

Ca(OH)2

2.9 X 10-3

0.2

CaC03

6.8

681

K@POA

0.8

139.3

P401O

0.017

4.8

KCl

0.14

10

Ce02

0.094

16.2

NaCl

3.65

213

Total Solids Output Mass: (excludes gases)

I
I

I
I

I
I

N2(g)

I7353

Final Repoti

400
mol

350

250
200
150

100
50
0
o

200

400

800

600

1000

1200

1400 c

,..

Figure
5.

Calculated eqtibrium composition of theprinciple gas phase species as a fimction

of temperam-e for the high organic sludge mass flow analysis.

mol

700
600
500

400
300

200
100

0
0

200

400

800

600

1000

1200

1400

Figure 6.

Calculatedequilibriumcomposition of the principle gas phase species as a function

of temperaturefrom the aqueous waste mass flow analysis.
29

Final Report

Based on these amilyses, the reactor components described below are designed for a system
handling a gaseous flow of 500 L/rnin with an exit temperature of 750 C, The condenser (heat
exchanger) on the system wll be capable of removing the water and cooling the gas effluent to
between 50-80C. The impact of this mass flow analysison the reactor core material is minimal
since the simulation did not take into account different reaction zone temperatures within the
reactor. A separate study was undertaken to quant@ the heat distribution throughout all the
components of the reactor core. The results of this study will be discussed below.
This mass analysisassumed an equilibriumprocess and ignored all kinetic factors and thus all the
data must be interpretedbased on these conditions. Due to the complexity of these feed streams,
all possible interactions and catalytic effects cannot be accounted for. This analysis should be
regarded as an upper limit prediction for gaseous effluent and solids conversion. The actual
experimentalresults are likely to display lower flow rates and different contaminant conversion
efficiencies.
Heat Distribution Analysis
The variable temperaturerequirements of the ChemChar process nearly necessitate the use of a
ceramic reactor core if a reasonable life-cycle time is to be expected. The durability,low thermal
conductivity and corrosion resistanceof ceramics make them the materialof choice for the reactor
core. The drawback to a ceramic reactor for the ChemChar process is the widely variable
I
,_

temperature regimes found throughout the length of the reactor core. These temperature
differentialscan impose a significantstrainon the rigid ceramic.

Physical Properties of the I-SIC 495 Ceramic.

Table 7.

Specific Gravity:

2.82 g/cm3
I

Bilk Density:

175 lbs/fi3
i

12%

Apparent Porosity:
I

4800 psi

Tensile Strength(MOR):
1

12,000 psi

Compressive Strength:
I

gray-black

Color:
I

Maximum Use Temperature:

Coefficient of l%enmd Expansion

I 2800F (1535oc)
I
3.6 X 104F (6.5x104C)
60 BTUin/fi2Jm0F @ 70F

Thermal Conductivity:

20 BTUOin/ft2%r0F
@ 2800F
I

Excellent

Thermal Shock Resistance:

30

.,

,-

.. . ,.,

..

-. .

Final Repoti

A ceramic material that fulfilk most of the requirements for the ChemChar reactor core is a
material known as I-SIC 495 (43.390 Aunina, 56.790 silicon carbide) manufactured by Ipsen
Ceramics (l?ecatonica, IL). This commercially available material has tremendous thermal shock
resistance, excdlent chemical stability toward corrosion and plasticity at high temperature.
Although these properties are encouraging for a reactor material, the I-SIC 495 has a very low
tensile strengthof 4800 psi. Table 7 lists the physicil characteristicsof this material.In an attempt
to fully understand the global heat distribution within the ChemChar reactor system a two
dimensional, axisymmetric finite element analysis of a fully insulated system was undertaken.
MCR Associates of Sunnyvale, CA performed the computer analysis according to our
specifications using ANSYS Revision 5.1 finite element analysis program. The full report,
complete with 45 figures, is contained in Appendix A. Only the key results of the analysiswill be
given here with reference to the appropriatefigures in AWendix A.
The reactor core design thatwas subjected to the simulationincluded the three component system
shown in Figure 7. The upper feed tube and lower startersection are composed of 98% alumina
and the middle section of I-SIC 495. This reactor core is contained within a 24 OD schedule 10
steel (0.25 wall) casing packed with Kaowool Bulk Fiber with a thermal conductivity of 0.3 and
1.9 BTUh/hrft20F at 200 and 2000F, respectively. The outside of the steel casing is insulated
with a 3 thick blanket of the same material.
The parameters employed for the first of three analysesincluded the physical properties of the ISIC 495 as dsplayed in Table 7, the thermalconductivities of the insulation,allowance for sliding
between ceramic components and fixed temperatures of 1500C for the TRZ and 200C m the
upper 8 of the reactor core. Figure 1A displays the areas of fixed temperature for the heat
distributionsimulation.Gaseous flow rates of 50 L/rnin of oxygen were assumed from the top of
the reactor to the TRZ and below this, a flow of 250 L/rein of carbon dioxide. Figure 2A displays
the assumptionsemployed for gas flow and convective heat transferfor the reactor system.
The results of the first analysis (Model 1) indicate adequate materials selection throughout the
reactor system and in fact, indicate that mild steel can be used for the 24 OD outer casing due to
the less than 300C temperaturesattainedat this surface (compare Figure 7A). This will result in a
significant cost savings over the use of stainless steel. The analysis also predicted a significant
tensile stress in the thermochemical reaction zone of 38,000 psi (see Figure 13A). The program
predicted a radialexpansion of 0.024 in this area (origimilwall thicknesswas 0.5, see Figure
14A). Based on the physical properties of the I-SIC 495, this program predicts the materialwill
crack in this region. The source of the 38,000 psi tensile stress is the cooling of the reactor
directly above this zone, which the program held constant at 200C. Although failure was
predicted, this first analysis employed a room temperature therrrd expansion coefficient and
ignored the elastic modulus of the I-SIC 495. The latter defines the plasticity of the ceramic and
its tendency to alleviate stress through radial deformations. Unfortunately, the manufacturerhas
not quantitativelydeterrnked the elastic modulus for I-SIC 495.
A second analysis was undertaken (Model 2) with the following changes: the reactor wall
thiclmess was increased to l, top to bottom (no indented region for wall cooling as m the first
model), temperaturedependent thermalparameters were added for the expansion coefficient and
thermal conductivity and the operating temperature at the TRZ was reduced to 1378C. The
results of this analysis showed no major changes in global temperatures of reactor components,
31

L%-(.:4 Irl

. ... . .. ... ... ..

1.. ,. :,....
. ,;.. ..-. *- %.,..: t.:.+...!
Il.
....*
. . . ?;-.,...
..*

Figure 7.

Schematic of the three component reactor core used in tie heat distributionfinite
element analysis.

32

FinalRepori

but the radial stress on the system in the area of the TRZ was predicted to increase to 83,500 psi.
This increase is directly related to the increased wall thickness of the reactor employed for this
model. The predicted radial expansion is the same as the first model (compare Figures 27A and
28A) which imparts an even greaterstrainon the thickerwall.
Discussions with Ipsen Ceramics regarding the results of these first two amdyses on their I-SIC
495 materialresultedin the their concern that ignoring the temperaturedependent elastic modulus
of the materialwas seriously modifying the outcome of the simulations.Although they have never
measured the elastic modulus of I-SIC 495 as a function of temperature, they have performed
extensive physical thermalstress and shock tests on the material,includingheating the materialto
over 1000C followed by immersion in water, without material failure. Engineers at Ipsen
recommended an approximate elastic modulus value be used iu a simulation in an attempt to
model their empirical resultsregarding the thermalshock snd stresstoughness of I-SIC 495.

The elastic modulus for I-SIC 495 was estimated by taking the weighted average of the elasticity
modulii of pure aluminaand pure silicon carbide from the literature.A graphicalrepresentationof
this fabricated elastic modulus is shown in Figure 39A. Although a good first approximation,
typically, physical properties of ceramics are not additive due to the formation of essentiallynew
material after sinteringtwo separateprecursors.
Nonetheless, a third simulationwas attempted employing the above elastic moduIus, the reactor
geometry was as in Model 1 (0.5 wall thickness, 0.25 cooling section wall thickness), the
temperatureof the TRZ was maintained at 1378C andjust above this area of the reactor core the
temperaturewas held at 200C (see Figure 30A).
The heat distribution prediction from this third model produced results similar to the other
models, with the outer steel jacket reaching a maximum of 300C at the very bottom where it
attaches to the reactor core (Figure 37A). Incorporation of the fabricated elastic modulus in he
simulationresulted in significanttensile stress reduction as compared to the other models. Figure
42A and 43A displays the results. A tensile stress of 15,378 psi was calculated reduced from
83,000 psi in Model 2. 7%is tensile stress is still 10,000 psi above the empirically determined
tensile strengthof I-SIC 495, but the value was calculated on an elastic modulus value that may
have considerable uncertainty.
Based on the positive outcome of tlis last simulation,Ipsen Ceramics was instructed to perform
several thermalstress tests on a tube of the I-SIC 495 material,The first test requested involved
cooling the cylinder to liquid nitrogen temperaturesfollowed by rapid heating. The second test
was to immersehalf the cylinder in an ice bath while heating the other half. Heating m both cases
was performed with an oxygen/propane torch. Both tests were performed by Ipsen and there was
no structuralfailure of the cylinder in either test. Jn the case of the ice bath immersion test the
cylinder was heated until all the water in the bath evaporated. Other tests done by Ipsen during
the development of this material include the heating of a cylinder to white hot (>lOOOC)
followed by immediate immersion in cold water, again resulting in no structural failure. These
tests do not completely representthe conditions within the core of the ChemCharreactor but they
attestto the fracturetoughness of the I-SIC 495 when subjected to extreme thermal stress.
On-going duringthe heat and stress distributionmodeling was the evaluation of other reactor core
materials,principallymetals. Steel alloys have to low a melting point and simply cannot be used.

33

Final Repoti

Non-iron containing alloys that contain nickel are also not viable candidates due to corrosion by
carbon monoxide. The latter generatesgaseous nickel tetracarbonyl,which results m pitting of the
slloy and eventualfailure. Potential alternativesincluded the space industryalloys of titaniumand
niobium. Titanium could not be used due to the potential 1500C operating regime of the
ChemCharreactor. Its maximum operating temperatureis approximately 1300C. Niobium has a
very high maximum operating temperature and is readily available (albeit somewhat expensive)
but suffers from high reactivi~ under both oxidizing and reducing conditions. Except under the
most mild of conditions, niobium must be coated with a protective material. Hydrogen readily
permeates into niobium causing it to swell with concordant loss of strength.Silicide coatings for
prevention of hydrogen permeation are available from niobium suppliers, but this process nealy
doubles the price of the component.
The aluminain I-SIC 495 is susceptible to carbon corrosion under reducing atmospheres through
the formation of voIatile aluminaoxycarbide. This corrosion is readily overcome by inexpensively
coating the materialwith a thin (1 mm) layer of ptie silicon carbide.
Clearly there is no ideal material that can meet all the thermal, chemical and mechanical stress
requirements demanded by the continuous feed ChemChar reactor system. Based on the finite
element analysis,empirical fracture tests conducted by Ipsen and evaluation of metal alloys, it is
was decided that the reactor core be constructed of the Ipsen Ceramic I-SIC 495 material. Its
combination of low cost ($2000 for preparation of mold and core, and $800 per replacement
core) high operating temperature, corrosion resistance and thermal shock resistance make it the
logical choice over other materials. The remainder of this section will describe, in detail, the
overall ChemChar reactor system with a reactor core prepared from I-SIC 495.
General Reactor Features-Reactor Core and Solids Treatment Train
Figure 8 is a schematic representation of the entire ChemChar waste treatment system to be
constructed under this program. The description that follows is a top down discussion of the
modular reactor components.
The surrogate waste feed hopper is prepared from a prefabricated 316 stainlesssteel 60 conical
vessel with prefitted lid. Welded to this is a the flange for attachment of a pneumatic actuated
slide valve, several clamps for securing the lid and a pressure relief rupture disc. The slide valve is
strictly for on/off control of the feed. Its approximatelyfour inch dismeter opening is either fidly
opened or fidly closed when actuated. There is no control of feed rate by this valve. The rate of
flow is governed by a rotary star valve discussed below. A rubber gasket between the hopper and
the lid will ensure an airtightseal. The waste feed will be blanketed with inert gas via purge ports
180 opposed near the top of the hopper. This subsystem is shown schematicallyin Figure 9. A
flange held rupture disc, rated for 5 psi, is also mounted on the hopper. Although somewhat low
pressure, any build-up at all indicates improper operation of the reactor and immediate release of
pressure will prevent damage to the reactor core and seals, which were not constructed for
pressure operation.
Attached to the flsnge on the underside the of slide valve is the inlet chute (Figure 10) composed
of316 stainlesssteel. The larger diameterflange on the inlet chute is the reactor core containment
vessel lid. Figures 11 and 12 are the schematics for the reactor core aluminafeeder section and
the top of the reactor core containmentvessel, respectively. The aluminafeeder top is grooved for

_,

34

Final Report

&
Cooling c
Section

Oxygen Mass
Fiow Meter

Ceramic
Reactor Core

Effluent

Solids
Metering
Valve

r7
I

Figure 8.

XParticulate
Collection

Aqueous
Condensate

/
Differential
Pressure
Sensor

Absolute
Pressure
Sensor

Schematic diagram of the continuous feed ChemChar reactor constructed under

this program

35

~Final Report

inclusion of an O-ring for maintenance of a gas tight seal and allowance for vertical expansion.
This is inserted into the reactor containment vessel top and bolted to the ceramic reactor core
(vk!e inj?a). This arrangementallows for vertical expansion of the reactor core during operation
and cool-down while the O-ring maintainsthe gas-tight seal. The reactor top, composed of carbon
steel, widens to 24 ID with 0.25 wall thickness. The anticipated low temperatures (250C)
reaching the containmentvessel walls allows for the use of simple cmbon steel over stainlesssteel
resultingin a substantialcost savings. Threaded fittings are welded directly on to the neck of the
containment vessel top for oxygen snd steam input to the reactor. The top is flanged onto the
containment vessel body, a carbon steel cylinder shown schematically m Figure 13. The

.. ~ containment vessel body h fitteclwith six thermocouples along one side for measurement of the
outer hull temperature, It was also retrofitted with an access panelfor access to the ceramic
reactor core and other internal hardware. This access ptiel (not shown m Figure 13) is
approximately 16 wide by 20 tall. It is readily visible in the full system photograph in Figure 20.

/.

_
I
L

.-

The containmentvessel bottom (Fi~e 14) consists of 24 ID flanged base narrowing to a 4-6-4
ID exit chute. An internal, cocentric reducer is welded inside the upper portion of the exit chute
which extends down to the 6 region of the assembly to allow ample space for exiting of the
gaseous effluent while maintainingthe smooth flow of solids. The exit chute then narrows to 3
for attachmentto the rotary star valve. Not shown in Figure 14 is a pressure relief tube directly
welded to the expanded section of the exit chute at a 45 angle to the gaseous effluent tube. This
tube is approximately 18 long and flanged on the end for fitting of a 5 psi rated rupture disc. The
end of this tube discharges into a fine-mesh screened collection vessel for containment of
carbon/waste blowout pa-titles in the event of a process upset.
This precision controlled volve (Rotolok Valves) regulates the flow of solids through the reactor
system. The vanes and internal components of the valve are gas-tight and have a maximum
operating temperatureof 750C which should be capable of withstandingthe hot solids and gases
exiting the reactor. The valve is PC controlled by the data acquisition and control system and the
unit will be calibrated for the movement of low density carbon. Ihside the carbon steel
containmentvessel will be insertedtheI-SIC 495 reactor core and alumina startersection (Figures
15 and 16, respectively). The main body of the reactor core is 0.5 thick with a 4 ID with the
wall thicknessreducing to 0.3 at ihe top. This thin walled region will be nitrogen gas cooled via a
coil of 3/8 copper tubing. As diagrsmmed in Figure 15, there are 23 thermocouple wells, 0.25
deep, situated throughout the entire length of the ceramic reactor core for monitoring the
temperatureof the various thermal zones of the reactor.
There are twelve thermocouples (type R) in three rings (separated by one inch) of four around the
diameter of the reactor in the area of the TRZ. The signal horn this array of thermocouples will
serve as the principle locator of the TRZ which will thenbe positioned by adjustingthe solids flow
via the rotary star valve. The remaining thermocouples (type K) will monitor temperature m the
reductive zones and the cooled area in upper portion of the reactor. All readings are continuously
read by the data acquisition and control system and displayed, real time on the graphical user
interface GUI control screen. Temperature readings are downloaded to disk every 10 seconds
during a process run for permanent record.
The flanges on the reactor core are part of the monolith and have a tongue and groove
arrangementfor joining of the aluminatop and starter sections onto the core. These joints have

36
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6.275

1. MATERIAIJ ISIC-495

2.

COATING: ISIC-491
ON INSIDE
SURFACE, .015 THK MIN,
.031 THK MAX.

3.

DIMENSIONSARE AHER COATING.

4,

FILLET RADIUS .05 MAX UNLESS

OTHERWISE NOTED.

THRU AT 6 EQUAL SPACES

ON A 06.20 CENTERLINE,
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2

Final Report

been sealed with high density, low porosity ceramic cement which will ensure leak free operation
at temperature. As stated earlier, the inner wills of the core are coated with a silicon carbide
coating for corrosion prevention.
The startersection is wrapped with a copper indtiction coil for heating of the carbon to start the
TRZ. The power source for the coil is an RFPP, 13.56 MHz, 3 kW radio frequency generator.
This non-invasive method of startingthe ChemCharprocess was tested outside of the reactor on
samples of triple reverse burn carbon and found to be highly effective at heating the material.
Temperature measurements taken during the tests revealed values over 800C, well above
temperatures necessary to ignite the carbon m the presence of oxygen. hstallation of the
induction coil and the matching network (Figure 19, mounted on the underside of the conta.hnent
vessel bottom) on the fully assembled reactor and subsequent testing produced much lower
temperatures.This is a result of the highly ferromagnetic environmentof the reactor as compared

RF. Imut -13.65

Shigle-Tum lndtion
Heating Loop

MHz

c-3 - -loopf

1.3kw

0-1

0-2

100 pf

100 pf

0-4

G15

50 pf

50 pf

0-16

---

&

Figure 17. Tuning and network matching circuit diagramfor the RF induction coil heater.
to non-magnetic environmentemployed in the laboratory for the initialdesign and testing. The retuning of the matching network is performed by adjustmentof three variable capacitors, two on
the matching network circuitry (capacitors C3 and C16) and a third on the power source. If the
system cannot be tuned sufficiently to raise the temperature of the carbon, it is likely increased
capacitance will be necessary in the matching network. This is readily accomplished by adding
additional capacitors to the bank labeled C-4 to C-16 in Figure 17. This bank of 12, 50 pf
capacitors was designed for relatively simple incorporation of additionalcapacitors. Tuning of the
RF heating system within the reactor containmentvessel is currentlybeing performed.
The starter section is bolted directly to the carbon steel containment vessel bottom. A gas tight
seal between these dissimilar materials was achieved by employing a high temperature Kalrez
graphite-aluminumgasket. Stainless steel nuts (but not the bolts) are used to secure the starter
section to the steel containment vessel to reduce interference with the RI? induction heating
system. Excess thread on the bolts, after securing the starter section to the containment bottom,
was removed to reduce interference with the induction heater.
Flanged to the exit side of the rotary star valve is an exit chute (which also serves as the M to the
solids receiving hopper, Figure 18) and a solids receiving hopper (Figure 19). These components

45

,..

,.,,.,,,.,,:,

,.,.,,,..=

..L..,,

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.,.

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1.
1

MATERIAG MILD STEEL QQS-741

CLASS 1 OR AM 1020

TYPE IL GRADE A
0.275
A

2.

WORKMANSHIP PER lNDUiTRY STANDARDS.

1
1

23.50,

24.00
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MATERIAL MILD STEEL QQS-741 TYPE II.

GRADE A CIASS 1 OR AISI 1020

2.

WORKMANSHIP PER INDUSTRY STANDARDS.

3.

ALL BEVEL WELDS TO BE 37.

4.

WELD AT 4 PLACES

5.

23.50,
22.50,

GRIND SURFACE SMOOTH AFTER WELD.

INSTALL PER MANUFACTURERS INSTRUCTION

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FinalReport

are composed of carbon steel. The receiving hopper will have purge valves attached to expel any
flammable gas that may accumulate during a process run. The lid and hopper have a gasket
between them for maintenanceof an a$tight seal.
This concludes the description of the vertically arrangedsoIids treatmenttrain. As of this writing,
all components have performed exactly as designed in cold and hot test runs. The RF heating
system is the exception, but appearsto be only out of tune, which can be readily prepared with the
proper equipment. A detailed description of the gaseous effluent treatmenttrainfollows.

General Reactor Features-Gaseous EffIuent Treatment Train

The effluent gas exits through the neck of the containment vessel bottom into a carbon steel
cyclone separator (see Figure 8). The cyclone was custom built and its removal efficiency tested
using powdered activated carbon. It is flanged into the effluent piping system and can be readily
removed if test runs indicate insignificantamounts of particulate entering the gas phase effluent.
It will not be known until surrogate processing if the effluent flow rate will be sufficient to carry
particulatematter into the system. Particulate in the effluent will have an adverse effect on the
analyticalinstrumentationfor on-line, real time sampling of the effluent as well as the volumetric
flowmeter downstream (vide in.a). Testing of the cyclone was performed on powdered activated
carbon at the manufacturers facility (Mello, the manufacturer of the majority of the reactor
components) and although not quantitative, particulate removal at the expected flows of the
ChemChar system was shown. Particulateremoval efficiencies were not measured.
After the cyclone, the hot effluent (estimated to be 500-700C) enters a tube-in-tube condenser
(JFD Tube and Coil) for removal of water. The inlet and outlet cooling water temperatures are
monitored by thermocouple probes and do~oaded
to the data acquisition and control system
(DACS) for heat balance computations. As shown in Figure 8, condensable liquids are collected in
a 4 L, conicsl stainless steel vessel equipped with a stopcock at the bottom for drainage and
sampling. The condensate will be collected, stored and analyzed for mass balance computations.
The next section describes in detail the test to be performed on the condensate.
The cooled, water-flee effluent enters a manifold equipped with a sampling port, absolute
pressure gauge and a port connected to the high pressure side of a differentialpressure gauge.
The other sensing port for this diffe~ntial pressure gauge is located on a second manifold after
the triple reverse burn carbon filter. The absolute pressure gauge measures the effluent pressure
with respect to atmospheric. The signal is displayed real time on the GUI system control panel
and downloaded to disc at ten second intervals. The sampling port (not shown m Figure 8 for
clarity) is simply a tube with an attachedtwo-way valve. The two-way valve allows for purging of
the tube between collection of samples. All the gas phase samples will be collected in gas-tight
Tedlar bags and analyzed by gas chromatography with thermal conductivity and mass spectral
detection. The quantitativedata from the GC analysescoupled with the volumetric flow data will
allow for mass flow information and ultimatelyamass balance for a process run. Furtherdetails of
these analyses is located in the next section. The effluent then enters a volumetric flow meter
where the instantaneousflow rate and total volume of effluent are displayed on a LCD on the
meter. This unit is stand alone and is not connected to the PC and DACS system. The meter has a
self contained microprocessor and all measurements(total volume) are retained in its non-volatile
memory until the unit is reset. Tlms, during and after a process run, the flow rate and total volume

48

Final Report

measured will have to be manually recorded. The unit has PC control capabilities, but requires
special software and was not pursued.
Final polishing of the effluent will be accomplished by a triple reverse bum carbon filter. The
filter, diagrarnmedin Figure 8, is a 12 diameter x 24 high canister packed with approximately
12 of triple reverse burn carbon. The large diameter was required to keep pressure drops to a
minimumThe polished effluent enters a second manifold wherein absolute pressure, differential
pressure and a sampling valve are positioned. The differentialpressure gauge monitors pressure
drop across the filter. This signal wdl be read directly by the DACS and if excessive will terminate
operation of the entire system. Sampling of the polished effluent will be performed as described
above.
The polished effluent is then flared by an in-house fabricated, enclosed system flare. A flame
arrestor specifically designed for hydrogen and carbon monoxide mixtures is in-line before the
flare for prevention back-up of the flame into the effluentpiping. Exhaust gas horn the flare will is
vented to a fiune hood.
Input gases to the reactor include oxygen and steam. The latter will likely not be required under
this program due to the high water content of the surrogate waste streams, but an input
electronically actuated solenoid wdve was designed in the reactor. Mass flow of steam, if used,
will be performed by flash evaporation of known weights of water vaporized in line via heating
tape. The inputport is located in the upper section of the containmentvessel top (see Figure 12).
Opposite to this is the oxygen inlet port. Gaseous oxygen will be fed into the reactor from a
oxygen cylinders via a pressure regulator through an oxygen mass flow meter with an internal,
electronically actuated solenoid valve for control of the mass flow rate (Omega Inc.). The valve
on the oxygen flow meter is normally closed for immediateshut-down of oxygen flow in case of a
power failure. The oxygen mass flow meter is completely controlled at the GUI of the PC control
system, wherein the fidl range of mass flow rates and emergency shut-down are readily adjusted.
General Reactor Features-Data Acquisition and Process Control Overview
Automation of the ChemChar reactor system is accomplished by a combination of hardware and
software components. The system is capable of measuring temperatures, gas flow rates and
pressures, and controlling solid feed rates, gas flow rates and associated on/off valves. The
hardware consists of an IBM PC compatible computer communicating via parallel port with a
National JnstrurnentsSCM 12 bit data acquisition module and several signal conditioning
modules, along with several R type and K type thermocouples, sensors, and valves. The control
software consists of code developed at Mirage Systems using National InstrumentsLab Windows
CVI virtual instrumentsC code development environment and compiler. The control software,
based on a PID feedback loop, will change test parameters according to a programmed sequence,
monitor system parameters and record data periodically during the test. The automated system
will be capable of unattendedoperation for extended periods of time.
The main hardware elements for data acquisition and control include 36 thermocouples, 2 flow
and 2 pressure sensors, 2 feed valves, and the SCXI chassis and modules. The RF induction
heating system is separate and requires manual operation. The hardware has capacity in excess of
thatimmediately needed to operate the ChemChar system as shown in Table 8. These components
were procured and individual component testing, hardware integration and final testing was
completed successfully. The SCXI chassis and modules are assembled and the A/D, D/A, and
,.
49

Final Report

digital channelswere successfully exercised and tested for functiomility.Thermocouple assemblies

consisting of wires, jackets and connectors were constructed, tested and insttdledon the reactor

core and outer body. The assemblies were tested by connection to the SCXL1100 signal
conditioning modules. The hardware control components, namely the oxygen mass flow valve, the
gaseous effluent pressure transducer, the rotary feed valve and pneumatic slide valve were
interfaced and tested with the appropriate SCXI modules. All the testing was successful and the
system is under complete computer control.
Table 8. I/O Utilization for the 1 &CS Hardware.
~

l===
I M level inputchannels

Isolated output channels

I Misc. TTL level 1/0

Type/Model

Capacity

Used

Scx-lloo

16

12

SCXI-11OO

36

24

SCXI-11OO

12

SCM-1124

12

SCXI-1200

1 16/16

10/0

The control program features an intuitivegraphical user interface (GUI) running on an IBM PC
compatible Pentiumcomputer utilizing the Windows 95 operating system. Test parameters are set
and displayed graphically within the main window of the program and a variety of other
parameters are available for setting and viewing from pop-up windows. Critical information
concerning reactor temperatures,flow rates, and pressures are updated and displayed in real-time
(three second delay between updates).
Upon entering the program the user is presented with the main program window. Until some
action is initiated by the user the program is in a quiescent, safe mode which maintah the
oxygen flow valve in the closed position and ensures the rotary char feed valve is shut off. All
sensor inputs are actively monitored and their values are availableto the user. Data logging is not
activated. Any sensor inputs which are out of range for the quiescent state of the system are
flagged for the user.
Three control buttons are availablefrom the main window. The <Start> button activates the PID
(Proportional-Integral-Derivative) algorithm based on a fixed timing loop and the <Shutdow@
button activates a routine which returns the program to the quiescent mode. The third button,
dlecorb,
activates data logging. The <Start> button is used once system ignition has occurred.
Ignition is a manually initiated event involving the application of heat through an induction coil
applied to the lower region of the reactor. Once ignition occurs, oxygen is supplied to the reactor

,_

and the TRZ migrates up the core to the primary burn region. The <Start> button accomplishes
this by fiist opening the oxygen supply valve to a preset flow rate.As the TRZ migrates the length
of the reactor core, the temperature profile of the core changes and the 23 thermocouples
instrumentedwithin the walls of the core provide the temperatureprofile to the program. When
the TRZ is determinedto be within the desired section of the reactor core the PID control loop is
automaticallyactivated. Control of the rotary char feed valve is based upon maintainingthe TRZ
at the optimal point within the reactor core (upper third). H the PID control loop cannot maintain

50

Final Report

the TRZ withk the appropriateregion by automatic control of the rotary valve, a manualoverride
button is available for control of the rotary valve. In this case, the system operator visually
monitors the temperaturesof the core and carefully adjusts the feed rate to maintaina stationary
TRZ. If manual operation does not stabilize the system operation shutdown can be activated by
selecting the <Shutdo~
button. Selecting the dlecorcb button a second time turns off data
logging.
Data logging allows the user to record to a file the full complement of input and output data at ten
second intervals during the course of a test run. The ASCII format text file includes a header
containing the date, time and setupparametersat the beginning of the run. Temperature, pressure,

and oxygenflow rate are recorded in standard units, but control values are recorded as percent of
Wl scale (e.g. percent fdl scrde rpm of the rotary valve). The user selects the name of the file
before recording. Since the computer controlling the system is a PC (as opposed to UNIX based
system) and not multi-tasking,there is a very short release of process control (approximately one
second) duringthe download of data to disk.

General Reactor Features-External Hardware and Reactor Support Structure

The ChemChar reactor system, as designed, has a height of 105 and is supported by a steel
platform that allows personnel access to the feed hopper, the most elevated system component.
The platform has a built-in crane capable of raising and lowering of the feed hopper and lifting of
the fully assembled core section (over 650 pounds). The outer edge of the platform is equipped
with a chain guard for prevention of personnel falling from the platform. The fully assembled
system is pictured in Figure 20.

Task 2.0 Carbon/Char Procurement & Surrogate Waste Identification

The section on surrogatewaste identitlcation is located at the beginning of Results and Discussion
section and will not be discussed further. This subsection will be devoted preparation and
properties of the triple reverse burn carbon to be employed in the ChemCharprocess runs.
The starting materialfor the triple reverse burn (TRB) carbon for this program was coal from the
Arch-Hannah Basin in Wyoming. Table 9 lists the ash mineral composition and other physical
properties of the Arch-Hannah coal starting material. Table 10 displays the proximate, ultimate
and BTU analyticaldata for the Arch-Hannah coal startingmaterial and the TRB carbon derived
from it. The analyses were pelforrned by Wyoming Analytical Laboratories, Inc. m Lararnie,
Wyoming.
The ash mineral analysis data indicate advantageous levels of calcium and iron. As shown in the
mass flow analysis,these species (as the carbonates or oxides) were excellent sulfi.uscavengers.
Their scavenging abilitywiU be offset slightly by the presence of ash derived sulfur (8.95%), but
significant capacity should be available for the removal of waste derived sulfur species (mainly
hydrogen sulfide). The majority of the sulfurin the effluent will, in fact, likely arise from the ash m
the TRB carbon.
The ash fision temperatures are close to the projected operated range of the thermal reaction
zone. The potential for slagging of the ash in TRB carbon/waste feed is low since the ash is
essentiallydiluted in the carbon. Since very little of the carbon is consumed in the ChemChar

51

FinalRepoti

Figure 20. Fully assembled ChemChar reactor. A. Swing cranemast, winch and hook. B.
Contairunentvessel mid-section. C. Personnel platform. D. Containmentvessel bottom (no
effluenl: take-off pipe). E. Solids collection hopper. F. Condensate collection vessel. G. Cy
separattJr.H. Rotary starvalve (chain guard most visible).

52

Final Repoti

process, agglomeration of ash with subsequent formation of a molten mass (1242C from Table
9), which would obstruct the flow of solids through the core, is unlikely. Besides barium, the
elementalanalysisof the ash shows no RCRA metal contaminantsthat would produce a solids byproduct disposal problem. The land disposal restrictionfor barium as a characteristicwaste is 100
ppm by the toxicity characteristicleaching procedure. In an actual waste treatment situation, this
treatmentlevel would easily be met employing the TRB carbon employed for this study.

Table 9. Ash Mineral Analysis Data for the Arch-HannahCoal TRB StartingMaterial.
Quantity (~)

Element

40.80
20.06

Silicon as SiOz
Altil.lm
= Alz03
Iron as FezOs

8.18

Calcium as CaO

14.36

Magnesium as MgO
Sodium as NazO

4.50
0.35
0.87
0.81
0.05
0.62
0.15
0.30
8.95

Potassium as KzO
Titaniumas TiOz
1
,_

Manganese as MnOZ
Phosphoms = P205
Strontiumas SrO
Barium as BaO
Sulfur as S03

Total: I

100.00

Other Physical Characteristics

Silica Ratio

60.14

Base/Acid Ratio

0.46

Silica/AluminaRatio

2.03

Dolomite Ratio

66.74

Basicity (%)
Acidity (%)

31.42
68.58
2300 (1260C)

T250(F)
Ash Fusion Data
Parameter

Reducing Atmosphere

Oxidizing Atmosphere

InithilDeformation

2121 F(11600C)

2300F(12600C)

Softening

2145 F(11740C)

2330F(1277C)

Hemispherical

2155F(11790C)

2352F(12890C)

Fluid

2267F(12420C)

2402F(13170C)

53

FinalReport

Table 10. Proximate, ultimate and BTU Data for the Arch-Hannah Coal and TRB Carbon.
As Received

Moisture Free

(wt. %)

(wt.%)

coal

Proximate:
Moisture

I.._

N/A

N/A

N/A

N/A

5.64

10.76

N/A

N/A

7.70

41.33

7.77

43.80

8.71

80.79

53.03

81.47

56.20

91.29

100.00

100.00

coal

8.69

0.84

5.15

10.67

37.73

~ 48.43

coal
Carbon

Total \ 100.00

Ultimate:

(wt.%)

Volatile Matter \
Fixed Carbon

m!
Carbon

ml
Carbon

~
~

Ash

~ Moisture& Ash Free

100,00 ~ 100.00

100.00 .

Hydrogen

5.53

0.66

4.99

0.57

5.29

0.64

Carbon

67.36

81.29

73.77

81.98

78.18

91.86

Nitrogen

1.35

1.25

1.47

1.26

1.56

1.41

sulfur

0.50

0.52

0.55

0.52

0.58

0.58

Oxygen

20.11

5.61

13.58

4.91

14.39

5.51

5.15

10.67

5.64

10.76

N/A

N/A

Total ~ 100.00

100.00

\ 100.00

100.00

100.00

100.00

Heating Value ~ 11,471

13,064

13,175

13,313

14,764

Ash

(BNJ/lb)

12,562

Inspection of the proximate data in Table 10, readily displayshow the triple reverse burn process
dries and converts the volatile matter to tied carbon in the coal. The somewhat high volatile
matter content (7.7Yo) of the TRB carbon is attributedto the presence of adsorbed oxygen md.
carbon oxides (C02 and CO) which are evolved when the carbon is heated (925C under inert
atmosphere) for the volatile matter determination.The high level of carbon m the TRB product is
attested by the moisture and ash free value of nearly 92%. This high level is responsible for the
adsorbing capabilities of this low cost materialin the ChemCharprocess.

54

Final Report

The macroscopic, physical characteristicsof the TRB carbon are lited below. All analyseswere
Surface Area
Pore Volume:
Total Pore Aea
Median Pore Diameter (Volume):
Median Pore Diameter (Area):
Average Pore Diameter (4V/A):
Bulk Density:

394 m2/g
0.93 cm3/g
40.8 m2/g
1.69 pm
0.0059 pm
0.091 pm
0.62 g/cm3

Apparent (Skeletal) Density:

Porosity:

58.15%

1.49g/cm3

performed by Micromerkics of Norcross, GA. The surface area of the sample submitted is 393.9
m2/g. The surface area was derived by generating a Langmuir isotherm with nitrogen as the
adsorbate. All other data was generated by mercury porisimetry measurements.The median pore
diameter (volume) value represents the TRB carbon pore diameter at which one half of the total
pore volume (0.93/2) was reached. As a testamentto the macroporosity of this material, 87% of
the total pore volume was reached at a pore diameter of 0.23 pm. Sirnikuly,the median pore
diameter (area) value, represents the TRB carbon pore diameter at one half the total pore area
(40.7/2) measured. The average pore diameter value was calculated employing the total pore
volume and total pore area assuming the pores were non-intersecting, uniform spheres. The
density and bulk porosity are consistent with past samples and the porosity should prevent
excessive pressurebuild-up in both the reactor core and the TlU3 carbon canistereffluent filter.
&of this writing there is approximately 80 pounds of TRB carbon for use m the program. Based
on the bed volumes to be treated in the surrogate waste process runs and the amount necessary
for the carbon f.i.iter,a shortage is not anticipated.

Task 3.0

Surrogate Waste Treatment and Reactor Operation

Preliminary Test Results To Date

As of this writing shipment and set-up of the reactor at the University of Missouri is complete.
Shakedown of the reactor revealed only minor operational problems which have been addressed.
Batch process runs have shown the I-SIC 495 ceramic core performance to be exceptional. There
is a distinct time lag in the temperaturemeasurementsfor all the thermocouples embedded in the
wall of the core. These batch runs have displayed temperatures only as high as 200C. TRZ
migration rates on the order of 2.0 crn/rninhave been measured, indicating a slow heat transfer
rate through the core material. No continuous feed trials have been performed to determine the
actual length of time required for full response of the thermocouples and the temperature of the
TRZ. The heat from the TRZ must travel 0.25 of core material to reach the head of the
thermocouple.
Condensation of water in the lower section of the reactor core and solids exit chute has been
observed in the batch operations. This results in a wet solids effluent which becomes very difficult
to move via the rotary valve. Several potential solutions to this problem are being investigated.
The first is the changing of the rotor in the star valve to a deep vaned rotor. The one shipped with
the valve has vane heights of 3 mm which readily moved dry TlN3 carbon/waste material,but fails
if the materialis wet. The new rotor has vane heights of 3.5 cm. Results of solids movement by

55

FinalRepoti

from this new rotor are currentlybeing generated.Second, the solids exit chute will be thoroughly

insulatedto prevent heat loss. Fhally, the exit chute will be wrapped with heating tape and heated
simultaneouslywith the start-upof the TRZ.
There is no data on the effluent composition for the batch runs performed to date. The gas does
flare nicely, producing a light blue flame. Condensate has been collected, but not analyzed.
Virtually no particles have been observed and the cyclone has been taken off-line for these
shakedown batch runs. The TRB carbon iilter has also been taken off-line. The effluent pressure
during the batch runs has been shown to be essentiallyatmospheric. This is not truly indicative of
how the system may behave since the cyclone and TRB carbon ilher are off-line.
The remainder of this Draft Final Report will describe, in detail the testing procedures for he
continuous feed treatmentof the surrogatemixed waste feeds.

Test Procedures for the Treatment of the Surrogate Mixed Wastes

This subsection will describe the experimentalprocedures employed for achieving the goals snd
objectives of this program as well as surrogate waste preparation, loading and operational
procedures, and the sampling methodologies for the solid, liquid and gaseous effluents horn a
ChemChar, continuous feed process run.
Mixed Waste Surrogate Preparation
The surrogate mixed waste formulations to be treated by the ChemChar process under this
program are listed in Tables 1 and 2. These DOE-COR approved surrogate waste formulations
were taken from the DOE publication Surrogate Formulation for Thermal Treatment of LowLevel Mixed Waste - Part II: Selected Mixed Waste Treatment Project Waste Streams,
Publication No. DOE/MWIl?-16, January, 1994. The waste streams represent a challenge to the
ChemCharprocess in terms of treatmentcapability and are representativeof several high volume
mixed waste streamscurrentlystockpiled within the DOE complex.
The high organic sludge (HOS; Table 1) mixed waste formulation wiU test the gasification
efficiency of the ChemChar process for the conversion of hazardous and non-hazardous and
organic components (oil and ethylene glycol).
The neutral aqueous waste (NAS, Table 2) will subject the ChemChar process to high moisture
content waste processing. Both streamswill test the ChemCharprocesses abilityto retain volatile
heavy metals since each surrogate contains the same concentration of hazardous and surrogate
radioactive species.
Prior to ChemChartreatment,each of the surrogate wastes will be mixed with triple reverse burn
carbon. Based on the physical attributes of each of the mixed waste surrogate streams, it is
anticipated a mix ratio of 1:1 (by weight) will be employed for HOS and 2:1 (carbon-to-waste)
ratio for NAS. These ratios may change pending the outcome of preTFU3carbon mix ratio of NAS is required due to its high water content.

test runs. The higher

A process test run for the treatment of surrogate waste/char feed will involve processing
approximately three reactor volumes of material. This amount of feed is a balance between
availabilityof TRB carbon, production of solid waste kept to reasonable levels and the reactor
reaching steady state operation.

56

:FinalRepoti

One reactor volume, based on the current design, represents 6200 cm3. The calculated density of
the high organic sludge (HOS) surrogate is 1.5 g/cm3and that for the neutral aqueous surrogate

(NAS) k 1.3 g/cm3. Carbon to waste mix ratios are anticipatedto be 1:1 (by weight) for HOS and
2:1 for the NAS. Since the carbon has an effective density of 0.5 g/crn3, the il.milwaste feed
densities and total required amounts for a process run are: HOS, 1.0 g/crn3, 18.5 Kg; NAS: 0.76
g/cm3, 14 Kg.
waste feeds will be prepared in single process run batches. All chemicals will be
ordered from reputable laboratory supply companies (Aldrich, Fisher etc.) and be a minimum of
99% purity. Sample batches will be prepared in 10L polyethylene or polypropylene containers.
Surrogates will be mixed by manualstirringand mechanicalrolling. The preparation of NAS is as
follows. Based on the mnount required as calculated above, in a small, separate container the
activated carbon (1) and organics (14) and (15) will be mixed until adsorbed. In a 10 L poly drum
the required amount of water (2) will be added followed by the addition (one at a time) of items
3-13, and 16-17. Each of these salts will be allowed to dissolve completely (except for
naphthalene,13) before addition of the next compound. The activated carbon mixturewill then be
added and the poly drum rolled for 15 minutes. The weight of the tared drum will then be
recorded. After thorough mixing, a two-fold, by weight, amount of TRB carbon will be added and
Surrogate

the drum rolled again for 30 minutes.The entie mixturewill be placed M the reactor feed hopper
and processed.
A similarprocedure for HOS will be followed in a srndl poly container the activated carbon (1)
snd organics (14) and (15) will be mixed until adsorbed. h a large, 10 L poly drum will be added
all the dry, inorganic compounds 3-6,9-12 and 16-17 and the tared drum rolled for 10 minutes. In
a separate container, organic solid 13 will be dissolved in organic liquids 7-8. This solution, the
activated carbon rnkure and water (2) will be added to the large poly drum followed by rolling
for 30 minutes. The weight of the tared drum will be recorded and an equivalent amount of TlU3
carbon will be added and the drum rolled again for thirty minutes. The entire mixture will be
placed in the reactor feed hopper and processed.
These mixing procedures are essentially as described in the DOE report from which the
formulationswere taken and should result in very homogeneous solid mixtures readily handled by
the treatmentsystem.

Surrogate Waste Processing

The rate of waste feed processing is governed by the migration rate of the thermochemical
reaction zone (TRZ), The rotary valve will regulate solids flow such that the thermochemical
reaction zone is stationaryat a point in the upper third of the reactor. The location of the TRZ is
determined via an array of thermocouples along the length of the ceramic reactor. The signals
horn these thermocouples are analyzed by the Data Acquisition and Control System (DACS)
which then sends a signalto the rotary valve to increase its rotation to lower the TRZ or slow the
rotation causing upward migration.
This continuously-monitored system results in PID control of the location of the TRZ and hence
the solids feed rate. Based on past experimentalobservations of TRZ migration rates, a feed rate
for the ChemChar reactor constructed for this program of 300 g/rnin is expected.

,_

57

Final Repod

Effluent Sampling Protocols

Processing of the surrogate wastes will result in the generation of four effluent streams that will
require sampling and analysis for certain constituents. Heat balance will be performed by
analyzing the temperaturedata from 36 thexrnocouplessituatedthroughoutthe reactor system.
The four effluent streams from the ChemChar process are the surrogate waste/carbon processed

solids, particulate matter removed by the cyclone, aqueous condensate and the synthesis gas,
Figure 8 displays the location of each of the effluents and their point of collection in the system.
The sampling and analyticaltestprotocols for each of the effluents will be discussed below.
Most of the analyses will be performed with instrumentationpurchased under the program, m
place and fully tested at the University of Missouri, Department of Chemistry. The
instrumentation,purchased from Shimadzu Scientific Instruments,Inc., includes its GC-14APSTF
gas chromatographywith both flame ionization (FID) and thermal conductivity detection (TCD).
This unitwill perform the majority of the quantitativeanalysesfor organic and gas phase amdytes.
A ShirnadzuLC-1OA High Performance Liquid Chromatography(HPLC)/Ion Chromatographywith
W-Visible and conductivity detection will be used for analysis of water soluble salts such as
chloride and nitrate.To be used primarilyfor compound identificationpurposes, a Shimadzu QP5000 gas chromatographywith mass spectral detection (GC-MS) was also purchased. Samples
from the gaseous effluent, and organic extractions of the solid residues will be analyzed for
identification of unknown or unexpected species thatarein significant concentration.

Sampling and Analysis of Surrogate Waste/Carbon Solids Residue

The process solids from a ChemCharrun will be collected in the solids effluent bin on the bottom
of the reactor. Sampling of the solids residue will occur aftercompletion of au entireprocess run.
After cooling of the solids, the bin will be removed from the reactor assembly and the residue
manually mixed to assure uniformity. The tared bin will be weighed to obtain the mass of the
process residue prior to sampling. The homogenized process residue will be sampled from three
locations within the collection bin. The three sub-samples will be composite into a single sample
with a total mass of approximately one kilogram. This composite sample will then be split, with
one half analyzed as described below and the other half archived for later analysis,if necessary.
The solids residue will be analyzed to show that the hazardous organic components were
completely destroyed by the gasification process and both the hazardous and radioactive
surrogate metals were retained on the carbon during the treatment process. The latter will be
determined by an acid digestion of the sample followed by atomic absorption spectroscopy for
quantification.
The analysisprocedure for the hazardous organic components (naphthalene,chlorobenzene and
dichlorobezene) in the solid residue is a 12-hour soxhlet extraction of a known quantity of sample
with methylene chloride followed by gas chromatographic (GC) analysis with flame ionization
detection (GC-FID). Identification and quantitation of these species will be performed by
preparation of calibration curves employing authentic samples of each compound at several
concentrations.The calibration curves will be prepared in the concentration range that is expected
to be found for these compounds in the process residue. The latter are expected to be in the range
of the detection limit (0.01 ppm) to an upper concentration of 50 ppm. If samples are found to be

58

FinalReport

outside this concentration range,

Smples

will be diluted with a known volume of solvent and

reinfected.
Inithdly, W analyses will be performed in-house at the University of Missouri. The analytical
equipment purchased under the program will be used for qualitative (GC with mass spectral
detection) and quantitative (GC-FID or GC-TCD) use. Samples collected for fial, optimized,
process runs will be collected and sent to outside laboratories that are EPA-approved (QA-GC
protocols) that employ EPA analyticalmethods. The above soxhlet extraction followed by GCFID amlysis for organics is essentiallyEPA-Method 8120, but will not have the extensive QA-QC
(fortiilcation, blind duplicates, etc.) that is performed by EPA-certified analyticallaboratories. It
must be emphasized that the lack of stringentQA/QC for the in-house analyses does not detract
horn its reliability.All proper controls will be employed in-house (accurate calibration curves,
duplicate analyses, blank runs, etc.) to ensure excellent reliability and reproducibility of the
analyticalresults.
In-house metal analyses on the solid residue will be performed by nitric acid digestion (EPA
Method 3050) followed by atomic absorption spectroscopy (EPA Method 7000). This procedure
represents a total metils analysisof the solid residue, as opposed to the leachable metals present
in the residue. The latter will be analyzed by the EPAs Toxicity Characteristic Leaching
Procedure (TCLP) for find process run samples only.
Calibration curves produced from laboratory prepared samples of known concentration of the
metals in the surrogate waste will be prepared prior to analysis.Atomic absorption values from
the process samples will be compared with the calibrationcurves to obtain metal concentrations m
the solid residue. The TCLP analyses will not be performed on preliminaryprocess runs. These
analyses of the solid residue will result in mass balance information, waste volume and mass
reduction data, organic contaminantconversion efficiencies and metals retentionby the carbon.

Sampling and Analysis of Particulate Solids

The particulate solids, removed by the cyclone, will be weighed and subjected to X-ray
microanalysis.The latter technique probes the surface of solids by bombardment with X-rays and
any metal species present will be identified by a metal specific emission resulting from the
bombardment. This technique is available in-house atthe Universityof Missouri and will allow for
the rapid screening of particulate for the metals originatingfrom the surrogatemixed wastes.
If there is positive identification of any of the RCRA metals (Cd, Ni, Cr, Pb) or the surrogate
radionuclides (Cc, Cs) in the particulate, a sample will be subjected to acid digestion followed by
atomic absorption spectroscopy for quantitation.The procedure for the latter will be exactly as
described for the process residue solids.

Sampling and Analysis of Aqueous Condensate

The particulate-free gaseous effluent enters a tube-in-tube heat exchanger that will remove all
condensable material. This condensate will be sampled via a stopcock on the underside of the
condensate collector as shown in Figure 8.
It is likely that non-miscible organics will co-condense with the water resulting in a two-phase
condensate. The quantity of each of the phases is difficult to predict and will vary depending on

59

Final Repoti

the waste being processed and the operating conditions of the reactor. The analysis scheme
described below assumes the aqueous condensate contains anon-miscible organic phase.
The condensate will be withdrawn from the collector, inspected for multiplephases and weighed.
The pH of the condensate will then be measured with a ctilibratedpH meter. This measurement

for the calculation of total acid content (expectedto arise solely from hydrochloric acid,
HC1).After pH measurement, the condensate will be transferred to a separator funnel and the
organic contents extracted with a known quantity of methylene chloride. This extraction will
remove all non-miscibleorganics, but may not remove water soluble organics such as alcohols.
After extraction, the methylene chloride extract will be subjected to GC-MS analysis directly to
identify major components. Quantification of the compounds in the organic phase will be
attempted only if it is found that there are a reasonablenumber of components (5 or less) present

will allow

in this phase at appreciable concentrations. Thus, if it is found that the organic layer of the

aqueous condensate contains 100 compounds at roughly equal concentrations, qualitative

information only will be reported on as many compounds as possible. Only the total mass of
organics extracted will be reported in this case.
The organic extracted, aqueous condensate will be subjected to several analyticalprocedures. A
sub-sample will be taken and its total organic compound (TOC) value determined. This test will
be performed at an outside laboratory and involves oxidizing all the organic material to carbon

dioxide and measuring the latter. Combined, the results of the soxhlet extraction and the TOC
analysis will give the total organic content in the condensate.
A second sub-sample of the aqueous condensate will be tested for the soluble anionic species

chloride (C~) nitrate (~03]-), monohydrogen sulfide (HS-), tide

(S7 and cyanide (CN-). This

in-house analysis will be performed employing Ion Chromatography (IC) with conductivity
detection. This liquid phase analytical technique employs a b~ered eluent which carries the
sample through an ion-exchange-like column that interacts with the anions causing them to

traverse the column at different rates. A they exit the column at the detector, the charged species
alter the conductivity as compared to the pure eluent and are then quantitatively detected. Prior to
analysis, calibration curves for all the above anions will have been prepared for use in determining
their concentration in the condensate.
Before injection into the IC, the condensate will be treated with sodium hydroxide (NaOH) to
raise the pH to approximately 11. This will ensure that all the species to be measured are in the
anionic form and not their corresponding neutral acids. The results horn the IC technique should

result in the quantitative identification of ill the inorganic, water-soluble species expected to be
observed as by-products of the ChemChar process.
The last analysisto be performed on the aqueous condensate is for soluble metals. This will be

performed by atomic absorption spectroscopy as described for the solid residue. A sub-sample of
the condensate will be analyzed as-is, but after the organic extraction. The combined data from all
these analyses on the condensate wiU result in a fidly characterized aqueous condensate. The data
from these critical analyses will be used in calculating amass balance for a Chemchar process run.

Sampling and Analysis of Gaseous Effluent

As shown in Figure 8, sampling of the gaseous effluent first occurs after the condenser. There are

two sampling ports for the effluent where samples will be talcen manually and placed in gas-tight

60

Final Repoti

Tedlar bags. k of this writing, several tests have been performed at the University of Missouri
showing that leakage from these sampling bags is less than 5% over a period of 24 hours. Since
the contents of the Tedlar bags will be analyzed within hours (vide hzjia) of collection, loss of
sample integritywill not be an issue.
Gas phase samples will be collected at ten-minuteinterwdsbeginning after the start of a process
run. This will result in approximately 12 samples (6 at each port) per process run. Analysis of the
sampleswill commence immediately aftercollection.
Analysis of the effluent samples (the main constituentsbeing hydrogen, carbon monoxide, carbon
dioxide and methane) will be performed by GC with therrmdconductivity detection (TCD). The
gas phase nature of the samples requires mild gas chromatographic operating conditions. At the
time of injection of a sample, the separation column (a packed Carbosphere column, 6 by 1/8,
80-100 mesh) is maintainedat 35C and the temperatureramped up to 135C over the course of
10 minutes. The gradual increase in temperature is required to expedite the elution of carbon
dioxide and water in the sample. As of this writing, optimized GC operating parametershave been
determined on authentic ChemChar (batch processing) gaseous effluent. Figure 21 is a sample

chromatogram which displays all the major species (H2, CO, C02, H20, Cl+&)expected to be
observed in the effluent.Baseline separation is observed for all species allowingfor very accurate
concentration determinations. The first peak, which is for hydrogen, is inverted because of
hydrogenslower thermal conductivitythan that of the helium carrier gas. Although inverted, this
does not effect the quantitation of hydrogen. The next pti of peaks (not baseline separated) are
oxygen and nitrogen, respectively. The latter is expected to be a product in the effluent in the
processing of the neutral aqueous waste surrogate. Oxygen arises from the contamination of air
during the manual fijection process. ~
will not intefiere with nitrogen quantitation since the
nitrogen to oxygenratio of air is constant and can be readily compensated for when analyzingthe
nitrogen peak. Indeed, the chromatogram in Figure 21 shows that nitrogen gas was formed m the
ChemCharrun thatproduced this sample since the NX02 ratio is much greater than four. Methane
and carbon dioxide are next to elute with water the last component. The tailingpeak shape of the
water is typical for this species on this column type. Another potential component in the gaseous
effluent is hydrogen sulfide (H2S). Known samples of this species will be injected to determine its
retentiontime and behavior under these GC conditions.
Quantitation of all the aforementioned gas phase species will be performed by preparing
calibration curves from samples containing known concentrations of compound. Since the GC is
fidly automated and controlled via PC, the data from these curves can be input into the computer

and quantitationof experhnental traces determinednear real-time by the GC controlling software.

The volatile organic contaminants (VOCS) in the effluent, depending on their size and molecular
interaction with the GC column, may or may not elute within the 10 minute run-time of these
analyses. Thus, all samples from effluent sampling port 1 will be subjected to GC-MS analysis
under more rigorous conditions (higher column temperature). Potential VOCS include ethane,
ethylene, acetylene, propane and its olefinic congeners. Oxygenated compounds, such as
aldehydes and ketones may also be observed. The use of GC-MS will allow for ready
identification of the VOCS in the effluent. Once identified, authentic samples of the species m
question will be injected for confirmation and quantitation.

61

Figure 21. Sample gas chromatograrnof authenticsynthesis gas displayinglocations of the

principle gaseous components.
C\EZCH~OM\CHRO~TRB.002,
ChaMel
B
Peak

Name

c1

.
m

---

Mhiit&
62

. .-

FrnalReport

The gas chromatograms from the samples taken from effluent port 1 will be compared with the
chromatograrnsfrom samples from effluent port 2. Organic compounds in the effluent will have
been removed by the TIW filter. Removalefficienq datawill be obtained showingthat the overall
ChemChar system is capable of producing a clean, contaminant tiee synthesis gas effluent ready
for immediateuse as an energy source. Volatile metal contaminantswill be condensedby the heat
exchanger or removed by the cycloneif adsorbed onto particulate and are not expected to be m
the effluent beyondthe heat exchanger and thus will not be analyzed.
All the quantitative data from the four sampling sites (solid residue, particu.lates, aqueous
condensate and gaseous effluent) will be tabulatedfor fi.nslcalculation of the overall mass balance
of a ChemCharprocess run.
All analyticalprocedures will be in-house from samples generated during optimization process
runs. For final process runs, the solids residue will be sent to an EPA-certified laboratory for
TCLP and total constituentanalyses (TCA). The number of final process runswill depend on
budget and timelineconstraints.Two optimized process runs for each surrogate waste streamwill
be targeted.

Energy and Mass Balance

Data to be logged during a process run include temperature at 36 locations, oxygen mass flow,
rate of rotation of rotary valve (converted to feed rate), effluent volumetric flow rate, effluent
pressure and differentialpressure across the TIU3filter.
The effluent volumetric flow rate, combinedwith the quantitative analysesof the effluent, will be
converted to mass flow. Overall energy balance of the system will be calculated based on
temperature differences at three locations within the reactor system. The first location is the
cooled portion of the reactor core. This nitrogen gas cooled section (see Figure 8; cooling coils
not shown) will have separate thermocouples at the inlet and outlet fittings, very close to the coil
wrappings on the ceramic core. The second location is the reactor core wall (23 thermocouples
total from top to bottom) and the 13 thermocouples monitorkg temperature on the carbon steel
shell and at the inlet and outlet water fittings of the condenser. The data collected at these points
should allow for a heat balance calculationwith an estimatedprecision of +/- 10%.
Safety and Health
The testing of the ChemChartreatmentsystem will be performed at the Department of Chemistry
at the University of Missouri-Columbia campus. All procedures for preparation of chemical
mixtures and handlingof chemicals will be in accordance with the UniversitysSaiety and Health
Plan. Good Laboratory Practice (GLP) will be required and performed at all times. Proper
personnel protective equipment will be supplied and worn at all times (lab coats, gloves and
protective eye were).

The ChemChar reactor is sited in the Chemistry bukling in a hydrogenation laboratory. This
laboratory is equippedwith steel-reinforced concrete floors, walls and ceiling. The interior of the
laboratory is equipped three, 1/4 thick steel wall bays, seven feet high, with one open side. The
reactor is located outside the bays while the data acquisition and control system and the operator
are inside one of the bays. The flammable effluent produced during the process will be piped to a
fiune hood and flared inside the hood. The piping is equipped with an end-of-line flame arrestor

63

FinalRepoti

constructed specifically for hydrogen/carbon monoxide mixtures just prior to the flare to prevent
flame migration back into the system.
The use of GLP and the experience of the University of Missouri staff in the operation of
ChemChar reactors and the associated handling of the synthesis gas effluent will ensure safe
operation of theChemChar system.

Conclusion
Treatment data is currentlybeing generated employing the continuous feed ChemChar reactor at
the University of Missouri and will be reportedin detail in Monthly reports snd in the final version
of the Final Report. Several very minor problems were identified during the shakedown of the
newly constructed reactor, but were readily addressed. All systems appear to be operating as
designed and it is anticipatedthatthe program will be complete by July 31,1996.

Questions and commentsregarding the content of this report should be addressed to:
DanielJ. Kuchynka,ProgramManager
Mirage Systems
575 Maude Court
Sunnyvale,CA 94086-2803
Ph: 408-752-1600 ext. 30
e-maik dkuchynk@x.netcom.com

64

Final Report

References
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Contaminated Water and Solid Material By-Products from In Situ Coal Gasification
Implications for Pollution Control Technology, Proc. 6th Underground Coal Gasification
symposium, Conf. No. 800716, Nat. Tech. Info. Serv., Springfield, VA, 1980, V-81 to V90.
2. J. Dishinger, D.Bornhop, C. Orazio, S. Kapil~ S.E. Manahan, R,E. Poulson, and D.C.
Sheesley, Some Unique Approaches to the Chromatographic and Spectrophotometric
Analysis of Underground Coal Gasification By-Product Waters and Their Applications to
Environmental Control, Proc. 8th Underground Coal Gasification Symposium, Sand 822355, SandraR. Hudson, cd., USDOE Sandia Natl. Lab., 1982, pp. 345-354.
3. Fabry, R. Underground Gasification, Ann. Mines Belg. 1987,zI,pp.399-432.

4. Krantz, W.B. and Gunn, R.D., Ed. Underground Coal Gasification: State of the Art~ AIChE
SymposiumSer. 1983, ~, p. 185ff.
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Reverse Combustion, In Proc. of the Tenth Annual UndergroundCoal Gasification Symp.;

Williamsburg,VA, 198%pp 357-366.

6. The Adsorption of Trace Heavy Metals from Solution by Coal and Coal Derived Solid
Phases: R.W. Gale, M.A. Thesis, Universityof Missouri-Columbia,1980.
7.

D.W. Larsen and S.E. Manahan, Process for the Regeneration of Activated Carbon Product
by Reverse Burn Gasification, U.S. Patent No. 5,124,292,June 23,1992.

8. .E. McGowin, L.L. I@mer, S.E. Manahan and D.W. Larsen, ChemCharProcess for Cabon
Reactivation,Chemosphere,1991, Vol. 22,1191-1209.
9. D.W. Larsen and S.E. Manahan, Process for the Treatmentof Hazardous Wastes by Reverse
Bum Gasification, U.S. PatentNo. 4,978,477, Dec. 18,1990.

100 Gasification Techniques in Waste Treatment, C.J. Cady, Ph.D. Thesis, University of
Missouri-Columbi~ 1990.
11. The ChemChar Process for Hazardous Waste Treatment, A.E. McGowin, Ph.D. Thesis,
Universityof Missouri-Columbi~ 1991.
12.

ChemChar Gasification for Waste Treatment, L.L. Kinner, Ph.D. Thesis, University of
Missouri-Columbia, 1992.

13. Parkinson,G.; Fouhy, K. Gasification New Life for an Old Technology; Chem. Eng. 1996,
W(3), pp 37-43.
14. A.E. McGowin, L.L. Kinner, S.E. Manahan and D.W. Larsen, Mechanistic Study of the
ChemChar Process using HexachIorobenzene as Surrogate for Monitoring Reaction
Products, Chemosphere,1992, Vol. 24,1867-1884.

65

RinalRepoti

15. L.L. Khmer, A.E. McGowin, S.E. Manahan and D.W. Larsen, ReverseBurn Gasification
for Treatment of Hazardous Wastex ContaminatedSoil, Mixed Wastes, and Spent Activated
CarbonRegeneration, Environmental Science and Technology, 1993, Vol. 27,482-488.
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the ChernC!harProcess, Journal of Environmental Science and Health, 1993, Vol. A28,
697-727.
17. L.L. Ki.nner,A.E. McGowin, S.E. Manahan and D.W. Larsen, ChemChar Process for
Destruction of Sorbed Hexachlorobenzene with Char Sorbent Regeneration; Toxicological
and Environmental Chemistry, 1993, Vol. 37(1-2), 1-10.

18. A.E. McGowin, W. Brendt,. S.E. Manahan, and D.W. Larsen, Behavior of Mercury m
Hazardous Waste Treatment by Reverse-Burn Gasification,
27(5), 807-815.

Chemosphere, 1993, Vol.

19. A.E. McGowin, C. Cady, S.E. Manahan, and D.W. Larsen, Mixed Waste Treatment by
Reverse-Bum Gasification, Chemosphere,1993, Vol. 27(5), 779-794.
20,

V.J,
Berry and D,R. Parrish, A Theoretical Analysis of Heat Flow in Reverse
Combustion~Pet. Trans. AIM!?,1960, Vol. 219, pp. 124-131.

21.

J.G. Burger and B.C. Sahuquet, Chemical Aspects of In-Situ Combustion-Heat of

Combustion and Kinetics, Sot. Pet. Eng. J., 1972, Vol. 253, pp. 410-422.

22. R.D. Gunn and W.B. Krantz, Reverse Combustion Instabilitiesin Tar Sands and Coal,
Sot. Pet. Eng J., 1980, Vol. 20, pp. 267-277.

,_

23. Bostick, W.D. et al. Surrogate Formulations for Thermal Treatment of Low-Level Mixed
Waste, Part II: Selected Mixed Waste Treatment Project Waste Streams, DOE publication
DOE/MWIP-16, January, 1994, p.18 and 28.

66

Final Re~oti

Appendix A.

Finite E1ement Analysis Final Report from MCR Associates

Finite Element Analysis

of a
Carbon Char
Combustion Reactor

Prepared For
Mirage Systems

by MCR Associates,

918195

Inc.

Introduction
This report presents the results of a finite element analysis of a carbon char
combustion reactor designed by Mirage Systems of Sunnyvale, California. The reactor
consists of ceramic cylinders surrounded by a thick layer of insulation. A steel jacket
surrounds the interior insulation followed by a second layer of exterior insulation. The
combustion process is maintained by a continuous feed of carbon char material

down the center of the ceramic cylinders. It is critical to limit the wall temperature of
the ceramic cylinders so that combustion does not propagate along the inside wall.
Consequently, an area above the combustion chamber is liquid cooled using cooling
tubes. Unfortunately, the steep thermal gradient introduced by the temperature
difference between the cooling and the combustion zone can introduce severe
thermal expansion stresses into the ceramic material. The purpose of the analysis is
to establish the thermal temperature distribution in the reactor and the corresponding
stress produced in the reactor. A total of three conditions are evaluated. Each model
is created using a 2D axisymmetric analysis. Each case will be described later in the
report. All calculations are petformed using the ANSYS@Revision 5.1 finite element
analysis program.

Description of First Model

The main reactor is composed of three vertically connected tubes. The bottom
starter tube is composed of 98%0alumina. The center reactor core tube is composed
of a special ceramic material manufactured by lpsen Ceramics. The material for the
core is called I-SIC 495. The top or feeder tube is composed of 98% alumina. The
basic geometry for each of these tubes is obtained from drawings provided by Mirage
Systems. Surrounding the tubes is an interior insulator called Koawool Bulk Fiber.
The interior insulation is in turn surrounded by 24 inch OD, Schedule 10, steel tubing.
The Schedule 10 steel tubing has a wall thickness of .25 inches. Finally, the steel
tubing is insulated with a 3.00 inch thick cerachem blanket.
Mirage Systems initially specified two interface connections will be designed to
slide in order to help reduce thermal expansion stresses. The first sliding connection
is located at the attachment of the bottom starter alumina cylinder to the .25 inch thick
steel end cap that is welded to the steel tubing. The second sliding connection is
located between the OD of the top feed tube and the ID of the steel casing. The first
model has been designed to accommodate the sliding connections at these points.
The first thermal analysis of the reactor assumes the wall temperature of the
reactor core is set to 1500C. The cooling tube region is fixed at 200C. Figure 1
shows a plot of the first model with the temperature boundary conditions shown. The
pink arrows indicate where constraint equations are defined on the sliding surfaces.
The constraint equations impose a continuous temperature field across the sliding
surfaces. The total of 6,622 2D axisymmetric conduction elements are used in the
analysis. The model also has convective boundary conditions. Figure 2 shows a plot
of the model with the convective boundary conditions shown. The calculation of the

film coefficient in the upper reactor is based upon an oxygen flow rate of 50 liters/rein.
The calculation of the film coefficient in the lower reactor is based upon a carbon
dioxide flow rate of 250 liters/rein. The external film coefficient assumes a natural
convection condition. Appendix A shows the equations used to approximate these film
coefficients. The empirical equations are obtained from the first edition of Basic Heat
Transfer written by Kreith and Black, Copyright 1980. The first analysis also uses
constant material properties for the solution. Table t shows the thermal and
mechanical properties used for the first analysis.
Results - First Model
The results for the first thermal analysis are shown in Figures 1 through 8.

Figure 3 shows the steady state temperatures obtained in the bottom starter alumina
cylinder with a maximum value of 335C. Figure 4 shows the temperature for the top
feed tube is much lower with a maximum value of 148C. Figure 5 shows the
temperature for the center reactor core. The maximum temperature is manually fixed
at 1500C. Figure 6 shows the temperature obtained along the inside wall of the
reactor core starting from the bottom and moving to the top. Figure 7 shows a global
temperature plot and Figure 8 shows a plot of the temperature along the outside
surface of the blanket insulation. To reach steady state temperature of 15000C, the
reactor core absorbs a total of 684.3 watts, The cooling tubes remove a total of 256.1
watts.

To perform the structural analysis, the temperature field of the thermal solution is
read into the structural solution. The reference temperature or stress free temperature
for the thermal expansion solution is set to 25C. The boundary conditions for the
structural solution are shown on Figure 9. The nodes located on the sliding surfaces
are coupled normal to the sliding direction. The coupled node surfaces are identified

by the green arrows on Figure 9. The coupled node boundary condition allows normal
loads to be transferred but still allow sliding to occur.
Figures 10 through 15 summarize the structural response of the reactor for the first

iteration. Figure 10 shows a plot of the principle tensile stress in the bottom starter
alumina tube with a maximum stress of 10,333 psi. The principle tensile stress
provides the best indication for stress conditions because brittle ceramic materials
typically form cracks from tensile loads. Figure 11 shows a plot of the principle tensile
stress in the top feeder tube with a maximum stress of 4,049 psi. Figure 12 shows
the principle tensile stress generated in the center reactor core reaches 38,522 psi.
Figure 13 shows a close-up view of the high stress region of the reactor core. The
large tensile stress is well beyond the material limit of 4,800 psi. Figure 14 shows a
plot of the radial expansion of the center core tube. This plot clearly defines the cause
of the high tensile stress. The material near the hot zone simply expands radially
much further than the surrounding material. This introduces large tensile stress
components on the OD of the tube in the hot zone. Figure 15 shows a plot of the
vertical displacement of the reactor assembly. The abrupt change in displacement
values near the top indicates the sliding model is working properly.

Descriptionof Second Model

The second model of the reactor included several changes to the design. The first
change is the wall thickness of the reactor was increased from .05 inch to 1.00 inch.
Second, the reduced diameter of the cooling region was made the same as the main
body. Third, a sliding surface was also added between the bottom of the reactor core
and the top of the starter alumina tube. Figure 16 shows a plot of the model with the
sliding surfaces defined. The total number of elements for the second model
increased to 8,066. Finally, temperature dependent thermal properties are added to
the analysis. The addition of temperature dependent thermal properties is defined by
creating a table of values. Between any two data points in the table, ANSYS will
linearly interpolate the thermal properties. Table 2 shows the values of the properties
used for the analysis. The boundary condition at the hot zone was also changed to an
operating temperature of 1378C.
Results - Second Model
Figures 17 through 23 show a similar series of temperature plots for the second

model. Figure 17 shows a plot of the temperatures

obtained in the bottom starter

cylinder. Surprisingly, even though the operating wall temperature has been lowered
to 1378C from 1500C, the maximum temperature for the bottom alumina cylinder
has increased by 200C to 355oC over the first analysis. This result is produced
because the larger diameter cylinder provides lower axial thermal resistance.
Figure 18 shows the temperature of the top feed cylinder which is also hotter than
before. Figure 19 shows a plot of the temperature of the reactor core with a maximum
temperature set to 1378C. Figure 20 shows a path plot of the inside reactor core wall
temperature. A global temperature plot is shown on Figure 21. The outside wall
temperature is described by a path plot on Figure 22. The maximum outside wall
temperature is reduce by almost 6C. Finally, Figure 23 shows a plot of the
temperature of the steel tubing surrounding the reactor. To reach steady state the
reactor core absorbs a total of 614.9 watts. The cooling tubes absorb a total of 259.5
watts.
The structural solution is obtained using a reference temperature or stress free
temperature of 25C. Figures 24 through 29 summarize the results for the structural
solution of the second model. Figure 24 shows a plot of the principle tensile stress for

the bottom alumina

cylinder with a maximum

stress of 5,243

psi. Allowing the

interface between the reactor core and the bottom cylinder has reduced the stress by
almost a factor of 2.0. Figure 25 shows a plot of the stresses produced in the top
feeder alumina tube with a maximum stress of 5,536 psi. Figure 26 shows a plot of

the tensile stress in the reactor core. The maximum stress has more than doubled to
83,533 psi from the previous maximum of 38,522 psi. Figure 27 shows a close-up of
the maximum stress in the center reactor tube. Figure 28 shows a plot of the radial
displacement

of the

reactor

tube.

The magnitude of displacement is nearly identical to

the original

condition. Figure 29 shows

displacement for the reactor assembly.

a plot of the vertical component

of

Description of Third Model

For the third model, the geometry of the reactor is changed back to the original
shape. Sliding occurs on the three surfaces as described for condition two. The
thermal properties used for the analysis remain temperature dependent. [n addition, a
temperature dependent modulus is defined for both the alumina and the I-SIC 495
reactor core ceramic, Table 3 identifies the values used for the materials at different
temperatures. ANSYS will linearly interpolate the modulus for temperatures that lie
between the values listed in Table 3. The operating wall temperature remains at
1378C. Figure 30 shows a plot of the model used for the third analysis.
Results - Third Model
The results for the thermal solution are shown in Figures 31 through 38. Figures
31 and 32 shows the temperature distribution in the bottom and top alumina pieces
respectively. Figure 33 shows the temperature profile in the center reactor core with
the maximum wall temperature set to 1378C. Figure 34 shows a plot of the
temperature along the inside wall of the reactor core from the bottom to the top. Figure
35 shows a global temperature distribution plot. Figure 36 shows a plot of the
temperature in the steel jacket. Figure 37 shows the temperature profile along the
outside wall of the insulation with the peak temperature of 52.7C. The power required
to keep the wall at 1378C is 403.6 watts. The total power absorbed by the cooling
tubes is 110.5 watts.

The results of the structural analysis are based upon a reference temperature or
stress free temperature of 25C. Figures 38 and 39 show a plot of the temperature
dependent modulus used for the alumina and I-SIC 495 reactor core ceramic. The
high temperature sensitivity of these materials is clearly evident. Figures 40 through
45 show the results of the structural analysis. Figures 40 and 41 shows the tensile
stress in the alumina bottom and top piece respectively. No significant change in
stress is produced in these materials. Figure 42 shows a plot of the tensile stress
generated in the core ceramic and the maximum tensile stress is reduced to 15,378
psi. Figure 43 shows a close-up view of the high stress region. Figure 44 shows a
plot of the radial displacement of the reactor core. This displacement is simply a
result of the thermal expansion of the material. Finally, Figure 45 shows a plot of the
vertical displacement of the reactor assembly.
Conclusion
The analysis of the reactor has shown that the close proximity of the cooling tubes
to the combustion region introduces a large change radial expansion over a short
distance. Consequently, the thermally generated stress has a high tensile component
directly across from the hot zone. The analysis assumes the wall temperature
remains constant and the location does not move Under start-up conditions, the

reaction zone will move until equilibrium is achieved. The worst stress condition
occurs when the combustion zone moves close to the cooling tubes. A larger
4

separation

between

the cooling tubes and the combustion

zone will help reduce

stress.
Based upon current information, the reactor core will crack during operation. The
crack will begin across from the hot zone and is simply the result of radial expansion.
Please note that this cracking conclusion is based upon a room temperature tensile
stress specification for I-SIC 495 ceramic of 4,800 psi. Based upon conversation with
Mirage Systems, the high temperature characteristics of the core material are
substantially different. To insure proper evaluation of the core material, the high
temperature stress vs. strain relationships are needed. Also, the effective modulus of
the I-SIC 495 ceramic drops rapidly above 1380C. It is possible that operating at a
higher temeprature than 1378 will actually reduce the stress in the ceramic material.

.
Table 1
Material Properties
Material

Temperature

FirstModel
98y0Alumina

I-SIC 495
Fiber Insulation (Kaowool)
Blanket (cerachem)
Steel
~
Second Model
Alumina
1-SIC 495

(psi)

,.

65E6
nla
nla

.
/...~ ..
All

30E6

49E6

1535
25
93
425
649
982
1535
25

Blanket

4!2:
649
982
1535
bird Model

All

I
l-sic 495

Fiber Insulation

Blanket

65E6
65E6
65E6
65E6
65E6
nla
nla
nla
nla
nla
nla
nla
nla
nla
nla
nla

6.5 E-6
6,5 E-6
6.5 E-6
6.5 E-6
6.5 E-6
nla
nla
nla
nla
nla
nla
nla
nla
nla
nla
nla

nla

nla

30E6

11.7E-6

44E6

8:IE:6

40E6
20E6
IOE6
28E6
25E6
18E6
1000

8.IE-6
8.IE-6
8.IE-6
6.5 E-6
6.5 E-6
6.5 E-6
6,5 E-6

nla
nla
nla
nla
nla

Thermal
Conductivity

.. ...
. . .
.22
.14
nla
nla

WlinC
~...,,.
,.
,.
.6477
.2198
.00275
.00275

11.7E-[ -

6.5E-6

oisson:
Ratio

,., ~
.~...;
8.IE-6

65E6

.3
,,
.22
.14
.14
.14
.14
.14
.14
nla
nla
nla
nla
nla
nla

nla
nla
nla
nla
nla
nla

-,,,.,.3 ;
.22
.22
.22
.22
.14
.14
.14
.14

A
nla
nla
nla
nla
nla

982

nla

nla

nla
nla
nla
nla
nla
nla
nla
nla
nla
nla
nla

1538
All

nla

nla

nla

nla

nla

nla

nla

Ilimwi!
Steel

6.5 E-6
nla
nla

,.-.,... , .,,,~.. ;, ,.

.,,:. .,,, ,,: ~,.

.$,, .,,.
~,,
25
815
1371
1649
25
815
1371
1537
25
260
538
816
1093
1535
25
93
425
649
982
1535
25

,},~..,,

,..,.-

25
260
538
816
1093

,,...,,
1. .

49E6 8.IE-6

Fiber Insulation

Steel

TCE
in/inlC

..:.,,..,..
,.*, .,. ,

,.
..;,,,.,
~
...
(unacast)

Youngs
Modulus

30E6

11.7E-6 ~ .3

1.27

:,. ,.,
. . ....
.6477
.220
.165
.117
.0879
.0733
.0733
.00092
.00092
.00256
.00366
.00623
.010
.00092
.00092
.0027
.0055
.0095
.0161
1.27
,..
,) ~...
.6477
.6477
.6477
.6477

.220
.165
.117
.0879
.0733
.0733
.00092
.00092
.00256
.00366
.00623
.010
.00092
.00092
.0027
.0055
.0095
,0161
1.27

Calculate Film Coefficient for Inlet Oxygen

501iters~ .001m3 ~ 3937 in 3 lmin

Flowrate =
min

liter

(.)
k

in3

= 50.85
x 60sec
s

50.85fi
flowrate
s = 4.047~
=
Velocity =
area
s
z(2.00in)2

Calculate Reynolds Munber

VD
ReD =
Y
v = velocity in/s
D = diameter in
in2
v = kinematicviscosity=
s

()

4.047~ (4.00in)

ReD =

m2

2=658

(LaminarFlow)

15.86x10-6 X 39.379
s ()
m
.33

()

NUD = 1.86(IleD Pr)33 ~

EQ516

Kreith&B1ack

ReD = Reynolds Number

Pr = Prantl Number
D = Diameter
L = Length of Tube
NUD = 1086(658x.709).33

.33

[)

d.ooin
4oiIl

NUD = 6.61

hD

NUD = ~

hC = film coefilcient w/in2 C

D = Diameter
K= Gas Thermal Conductivity
(6.61)(.02676 w/mC)x
hc=NuD~=
4.00in

hc = .001123 W/m20C

lm
39.37in

CalculateFilm Coeffkient for Outlet Carbon Dioxide

Flowrate =

2501itersx.001m3~ 39 ~7~ 3X lmin = 254 ~113

min
liter () m
60sec
~
:7! 3

.
flowrate 50.85~s
=
Velocity =
= 20.23~
area
s
n(2.00in)2
Calculate Reynolds Number
VD
kq-j =

Y
v = velocity in /s
D = diameter in
inz
v = kinematicviscosity=
s

ReD=

z =

1739

(LarninarFlow)

m2

30.02x10+ X( 39.37~ )
.33

()

NUD = 1.86(IleD Pr)33 ~

EQ516

ReD = Reynolds Number

Pr = Prantl Number
D = Diameter
L = Length of Tube

()

.33

NUD = 1.86(1739x.668)-33 44~~

NUD = 7.22
hCD
NUD =
K

hc = film coefficient w/in2C

D = Diameter
K= Gas Thermal Conductivity
(7.22)(.043 w/mC)x
hc =NuD~=
4.00in

hc = .00197W/m20C

lm
39.37in

Keith&Black

...

AIwYs

AUG 22

5.1
1995

34

13:33:38

PLOT NO.
ELEMENTS
MAT m
TEMP
CE

Zv

=1

DIST=28 .05
XF
=8.5
YF
=22.25
CENTROID HIDDEN
EDGE

200

/ s00

(2.-

Figure 1
Model 1
Thermal
Boundary Conditions

..,

-.

..

-1-1

~r--Fi-_:H

. ...ti

--

iNsYs5.l

34

SEP
8 1995
14:41:46
PLOT NO.
1
ELEMENTS
MAT m
CONV
Zv

=1

DIST=28 .05
XF
=8.5
YF
=22.25
CENTROID HIDDEN
EDGE

.I

Figure 2
Model 1
Thermal
Convective Boundary Conditions

.-

,,

.-

..

ANSYS 5.1
AUG 30 1995
12:53:25

34

PLOT NO.
1
NODAL SOLUTION
STEP=I
SUB =1
TIME=l
TEMP
TEPC=7.524
SMN =245.011
SMX =335.032
245.011
250.012
255.013
260.015
265.016
270.017
275.018
280.019
285.02
290.022
295.023
m
300.024
305.025
310.026
315.028
320.029
325.03
330.031
335.032

Figure 3
Model 1
Bottom StarterTube
Temperature Distribution

--m

,-,

- ---,

- .*,

1
MN

,
-

,-

,
=
.+.

-I

--

ANSYS 5.1
34
AUG 30 1995
12:54.:03
PLOT NO.
2
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=3 .784
SMN =94.794
SMX =148.723
94.794
97.79
100.786
103.782
106.778
109.774
112.77
115.766
118.762
121.758
124.754
m
127.75
I
I
130.746
133.742
136.739
I ~~ I
139.735
142.731
145.727
148.723

Figure 4
Model 1
Top Feeder Tube
Temperature Distribution

-~w-...

-H-3---(

---H

ANSYS 5.1

34

AUG 30 1995
12:54:27
PLOT NO.
3
NODAL SOLUTION
STEP=l
SUB =1
TIME= 1
TEMP
TEPC=9 .491
SMN =148.37
SMX =1500

Eml

148.37
223.46
298.551
373.642
448.732
523.823
598.913
674.004
749.094
824.185
899.275
974.366
1049
1125
1200
1275
1350
1425
1500

Figure 5
Model 1
Center Core Tube
Temperature Distribution

,._

,._,

!,

ANSYS

1365

Zv
1230

a)

34

1095

=1

DIST=O .75
=0.5
XF
YF
=0.5
ZF
=0.5
CENTROID HIDDEN
EDGE

-P
L
CD

5.1

AUG 30 1995
12:55:48
PLOT NO.
4
POST1
STEP=l
SUB =1
TIME=l
PATH PLOT
NOD1=164
NOD2=228

1500

959.348

-P

c
aJ
(.)

(-)

824.185

689.022

0)
/

553,859

418.696

283.

53A

TMP

148,37

I
3

12

15

DIST

24

18

21

I
27

30

Figure 6
Model 1
CenterCoreTube
Inside Wall Temperature

.-I--------++1

-?--r

-+-

-H

..-

ANSYS 5.1
ZAUG 30 1995
12:56:52

34

PLOT NO.
5
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=88 .523

SMJN=31.594
SMX =1500
31.594
113.172
194.75
276.329
357.907
EEl
439.485
REl
521.063
602.641
684.219
765.797
847.375
Eml
928.953
1o11
I
I
1092
I---7
1174
1255
1337
1418
1500

Figure 7
Model 1
Global
Temperature Distribution
.. -

_..._~~

._

,--

-w+

H-

-y

_.

.. ~....

~!

ANSYS 5.1
34
AUG 30
1995
12:58:09
PLOT NO.
6
POST1
STEP=l
SUB =1
TIME=l
PATH PLOT
NOD1=6826
NOD2=6706

63.01

59.868

Zv
=1
DIST=O .75

56.727

XF =0.5
YF =0.5
ZF =0.5
CENTROID
EDGE

53,58kI

50,444
\

47.302

a)

-0
I-I
v)

44,16

-P
3

/
/

41,019

37,877

34,736
TMP

31,594

I
4,625

9,25

18.5

13,875

27,75

37

23.125

32.375

46.25

41,625

Figure 8

DIST

.-.

. ..

.. .

Model 1
Outside Wall
Temperature Profile
I

=a
m
UI
0)

cm
t-l
t-l

II

m
u-)
o
m
.m .
co . CN
N co CN

II II
1!
m
H
n

El

\LJ
.4

-+

-.. ...

-u

-d

L.A

-1

-1-

-L

ANSYS

5.1

34

AUG 30 1995
12:59:41
PLOT NO.
7
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =.O 02j;fi)
SMN =-3465
SMNB=-6373
SMX =10333
SMXB=13843
-3465
-2699
-1932
-1166
-398.988
Eimill
367.554
1134
1901
2667
3434
4200
Eim
4967
5733
6500
7266
8033
8800
9566
10333

Figure 10
Model 1
Bottom Starter Tube
PrincipalTensile Stress

.!----

-. .+

ANSYS

5.1

34

AUG 30 1995
13:00:27
PLOT NO.
8
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =0 l&)
SMN =-~44.246
SMNB=-1234
SMX =4049
SMXB=5550
-444.246
-194.636
54.974
304.585
554.195
IEEm
803.806
1053
1303
1553
1802
2052
EEzl
2301
1
2551
I
2801
I
-1
3050
3300
3550
3799
4049

Figure 11
Model 1
Top Feeder Tube
Principal Tensile Stress

-+--i-- w

_R

--%-

--+.-

..

..

ANSYS

5.1

34

AUG 30 1995

13:00:51
PLOT NO.
9
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =*() 15;;~)
SMN =-4358
SMNB=-11157
SMX =38522
SMXB=40272
-4358
-1976
406.239
2788
5171
IEml
7553
IEmzl
9935
12317
14700
17082
19464
E3m
21846
I
24228
I
1
26611
IIrl
28993
I
I
31375
33757
36139
38522

Figure 12
Model 1
Center Core Tube
Principal Tensile Stress

...H

.. .

M*

-i-

. . . ..

_.

-.

ANSYS

5.1

34

AUG 30 1995
13:01:28
PLOT NO.
10
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =.() 15+;~)
SMN =-4358
SMNB=-11157
SMX =38522
SMXB=40272
-4358
-1976
406.239
2788
5171
m
7553
Em
9935
12317
14700
17082
19464
21846
24228
26611
28993
31375
33757.
36139
38522

Figure 13
Model 1
Center Core Tube
Principal Tensile Stress

+--

H-

%-c

3---C

1,

ANSYS 5.1
34
AUG 30 1995
13:01:48
PLOT NO.
11
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
Ux
RSYS=O
DMX =0.157796
SEPC=14 .9
SMN =0.001745
SMX =0.023826
0.001745
0.002972
0.004199
0.005425
0.006652
0.007879
0.009105
0.010332
0.011559
0.012785
0.014012
m
0.015239
0.016465
0.017692
0.018919
0.020146
0.021372
0.022599
0.023826

Figure 14
Model 1
CenterCoreTube
Radial Displacement UX

ANSYS

5.1

34

AUG 30 1995
13:02:30
PLOT NO.
12
NODAL SOLUTION
STEP=l
SUB =1
TIME= 1
UY
RSYS=O
DMX =0.167433
SEPC=29 .926
SMX =0.167416
o
0.009301
0.018602
0.027903
0.037204
0.046504
0.055805
0.065106
0.074407
0.083708
0.093009
0.10231
0.111611
0.120912
0.130213
0.139513
0.148814
0.158115
0.167416

I
Figure 15
Model 1
ReactorAssembly
Vertical Displacement UY

,7+- l---1- -..*

-t--

-t----c

..

.-

-.

.-

ANSYS 5.1
34
SEP
8 1995
14:44:31
PLOT NO.
2
ELEMENTS
MAT m
=1
Zv
DIsT=28
.05
XF =8.5
YF =22.25
CENTROID HIDDEN
EDGE

Figure 16
Model 2
Geometry

--H-----H-

-&-.+

4-.

- w:--

:7, ,
,.; , ~,,-:
,,4

--,

I
=+

.,,-

.s

H--:

H:

..

..

.-

ANSYS; 5.1

34

AUG 30 1995
13:09:19
PLOT NO.
1
NODAL SOLUTION
STEP=l
SUB =1
TIME= 1
TEMP
TEPC=4 .728
SMN =310.926
SMX =354.933
310.926
313.37
315.815
318.26
320.705
EiEEl
323.15
325.595
328.039
330.484
332.929
335.374
337.819
340.264
342.708
345.153
347.598
350.043
352.488
354.933

Figure 17
Model 2
Bottom Starter Tube
Temperature Distribution

- ...

H-

H----->

bsYs

5.1

AUG 30
13:10:02

34

1995

PLOT NO.
2
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=2 .131
SMN =143 .84
SMX =172 .643

I 1

143.84
145.44
147.04
148.64
150.24
151.841
153.441
155.041
156.641
158.241
159.842
161.442
163.042
164.642
166.242
167.843
169.443
171.043
172.643

Figure 18
Model 2
Feeder Tube
Temperature Distribution
Top

--?41

w-

.--&+
..1

---

-H

-l--

.
-

,--

ANSYS 5.1
34
2NJG 30 1995
13:10:35
PLOT NO.
3
NODAL SOLUTION
STEP=l
SUB =1
TIME= 1
TEMP
TEPC=5 .955
SMN =172 .07
SMX =1378

EmEl

BmEl
-. ..,.
.. .

Em

Ezl

172.07
239.066
306.062
373.058
440.054
507.051
574.047
641.043
708.039
775.035
842.031
909.027
976.023
1043
1110
1177
1244
1311
1378

Figure 19
Model 2
Center Core Tube
Temperature Distribution

. ,

lx
g
H

!1

1-

m
w
.
m

\l

.4

!-

(J)
H
c1

,.,
T

l\

03

[
u-)

m
b
I)

xl
In
N

L
r-J
cl-

4
r-l

u)

g
0
-i
m

04

-i+---m---l--f

-----

-+1----r-k--r

ANSYS 5.1
34
AUG 30 1995
13:12:55
PLOT NO.
5
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=94 .067
SMN =28.649
SMX =1378

EIEEl

I
I

28.649
103.613
178.577
253.541
328.504
403.468
478.432
553.396
628.36
703.324
778.288
853.252
928.216
1003
1078
1153
1228
1303
1378

Figure 21
Model 2
Global
Temperature Distribution

10
N
i

I
1

I
[
I
,--,

1(f)

I .,

T,

,1.

,T1A

H
c1
In
h

co

+r-i

--+-

...->
----

-+-t-

1
m

-3

--

w.

+--+

AKLSYS 5.1
MJG 30 1995
13:15:45

34

PLOT NO.
7
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=5.179
SMN =143.805
SMX =321.348

m
IEEm

DEl
I

143.805
153.669
163.532
173.396
183.259
193.123
202.986
212.85
222.713
232.577
242.44
252.304
262.167
272.031
281.894
291.758
301.621
311.485
321.348

Figure 23
Model 2
Steel
Temperature Distribution

-A

-.

--

?!NSYS 5.1
34
AUG 30 1995
13:52:20
PLOT NO.
1
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX .() 02%)
SMN =-i966
SMNB=-3398
SI!CK =5243
SMXB=5393

-1966
-1566
-1165
-764.561
-364.068
36.425
436.918
837.411
1238
1638
2039
2439
2840
3240
3641
4041
4442
4842
5243

Figure 24
Model 2
Botlom Starter Tube
PrincipalTensile Stress

ANSYS 5.1
34
AUG 30 1995
13:53:35
PLOT NO.
2
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
(AvG)
S1
DMX =0.156394
=-490.735
Sm
SMNB=-1266
SMX =5536
SMXB=7523

m
m

L.L.-l

I
I

-490.735
-155.924
178.887
513.698
848.509
1183
1518
1853
2188
2523
2857
3192
1
3527
I
3862
~ 4197
4531
4866
5201
5536

Figure 25
Model 2
Top FeederTube
Principal Tensile Stress

H.r-l-r--+-+

.---H-

--+-f-+-+

M->

+-- _-

. .

i-+

ANsYs- 5.1

34

AUG 30 1995
13:54:29
PLOT NO.
3
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
(AVG )
S1
DMX =0.142545
SMN =-7890
SMNB=-19284
SMX =83533
SMXB=85128
-7890
-2811
2268
7347
12426
m
17505
m
22585
27664
32743
37822
42901
47980
53059
58138
63217
68296
73375
78454
83533

Figure 26
Model 2
Center Core

Tube

wincipal Tensile Stress

-d--

--+

I
!41W!YS5.1
34
AUG 30 1995
13:58:40
PLOT NO.
4
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =.() 14;;&
SMN =-7890
SMNB=-19284
SMX =83533
SMXB=85128
-7890
-2811
2268
7347
12426
Fn--l
17505
Imzl
22585
27664
32743
37822
42901
47980
53059
58138
63217
68296
73375
78454
83533

Figure 27
Model 2
Center Core Tube
Principal Tensile Stress

-.

. .

,-----

,- ,-.

ANSYS

5.1

-1

34

AUG 30 1995
14:00:42
PLOT NO.
5
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
Ux
RSYS=(I
DMX =0.142545
SEPC=8.761
SMN =0.002053
SMX =0.024217
0.002053
0.003284
0.004516
0.005747
0.006978
m
0.00821
m
0.009441
0.010672
0.011904
0.013135
0.014366
Ex2
0.015598
0.016829
0.01806
0.019292
0.020523
0.021755
0.022986
0.024217

Figure 28
Model 2
CenterCoreTube
Radial Displacement UX
i

,-
,

,,

,.__.,

,-.

.,

,-. .._

. ...-

+~-+

ANSYS

.,..
..
.,!
.. \

5.1

34

AUG 30 1995
14:01:28
PLOT NO.
6
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
UY
RSYS=O
DMX =0.156394
SEPC=12 .033
SMX =0.156326
o
0.008685
0.01737
0.026054
0.034739
0.043424
0.052109
0.060794
0.069478
0.078163
0.086848
0.095533
0.104218
0.112902
0.121587
0.130272
0.138957
0.147642
0.156326

I
Figure 29
Model 2
ReactorAssembly
Vertical Displacement UY

?UNSYS 5.1

34

SEP
8 1995
15:33:30
PLOT NO.
1
ELEMENTS
MAT m
u
CP
Zv
=1
DIST=28.05
XF
=8.5
YF =22.25
CENTROID HIDDEN
EDGE

IL

Figure30
Model 3
Geometry

--H

.-

--

-H

-..

+-

7---

ANSYS

SEP

-..

5.1

34

5 1995

09:41:36
PLOT NO.
1
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=5 .387
SMN =2/5!3
-- .132
-

SMX =340.765

....-.

----..,

,,
,,

,: . . . . . . . .

,, . . . .

285.132
288.223
291.313
294.404
297.495
300.585
303.676
306.767
309.858
312.948
316.039
319.13
322.22
325.311
328.402
331.492
334.583
337.674
340.765

Figure 31
Model 3
Bottom Starter Tube
Temperature Distribution

---

..

.. .-

-----

2WYS 5.1
34
SEP
5 1995
09:42:04
PLOT NO.
2
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=2.46
=126.829
am
SMX =159.337

m
1
Q

126.829
128.635
130.441
132.247
134.053
135.859
137.665
139.471
141.277
143.083
144.889
146.695
148.501
150.307
152.113
153.919
155.725
157.531
159.337

Figure 32
Model 3
Top Starter Tube
Temperature Distribution

. . .. .

---

msYs

5.1

34

SEP
5 1995
09:42:28
PLOT NO.
3
NODAL SOLUTION
STEP=l
SUB =1
TIME= 1
TEMP
TEPC=6.019
=158.844
=1378
158.844
226.575
294.306
362.037
429.767
497.498
565.229
632.96
700.691
768.422
836.153
903.884
971.615
1039
1107
1175
1243
1310
1378

Figure 33
Model 3
Center Core Tube
Temperature Distribution

14
8
H

id

C-mlnl.ncl
. . . .H
L

,-

%
c1

ccl

In

(-i

J.,

1
l-i

107
H
n

-k--

..+

-.W

-+

~...,

?4-

----M-..+

IN

,1

~4-:
AIWYS- 5.1
SEP
5 1995
09:46:33
PLOT NO.
7
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=94 .612
SMN =28.272
SMX =1378

m
r

1{

28.272
103,257
178,242
253.227
328.211
403.196
478,181
553.166
628.151
703.136
778,121
853.106
928.091
1003
1078
1153
1228
1303
1378

Figure 35
Model 3
Global
Temperature Distribution

-!

,--

--

ANSYS

52.7.4

CL

50.293

Zv
=1
DIST=O.75
XF
=0.5
YF
=0.5
ZF
=0.5
CENTROID
EDGE

47,846-

E
0)

-P

5.1

34

SEP
5 1995
09:47:45
PLOT NO.
8
POST1
STEP=l
SUB =1
TIME=l
PATH PLOT
NOD1=6826
NOD2=6706

45.399-

HIDDEN

42.952T

al

40,506-

u
.+
v)

38. 05T

-i-

0
35,612-

33,165

30,71~

TMP2

28,272
u

4,625

9.25

18,5

13,875

I
23.125

DIST

27.75

I
32,375

37

I
41.625

46,25

Figure 36
Model 3
Outer Wall
Temperature Profile

..

, ---

.-

-.

ANSYS

1
m

5.1

34

SEP
5 1995
09:44:55
PLOT NO.
6
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
TEMP
TEPC=5 .752

SMN =126.8
--=295.142
SMX

m
I

126.8
136.152
145.505
154.857
164.209
173.562
182.914
192.266
201.619
210.971
220.323
229.676
239.028
248.38
257.733
267.085
276.437
285.79
295.142

,Y

Figure 37
Model 3
Steel
Temperature Distribution

---~

--~

Ex

.-.---w.

~.-..

~--
FOR

137iTER17&

_ _

.W.-.

-~

+-

ANSYS 5.1

34

SEP
5 1995
09:59:41
PLOT NO.
5
MATERIALS
Zv
=1
DIST=O .75
XF
=0.5
YF
=0.5
ZF
=0.5
CENTROID HIDDEN
EDGE

480C

4400

4000

360U

3200

280d

2400

2000

1600

1200

I
200

400

800
600

I
1000

1200

I
1400

1600

2000

1800

Figure 38

TEMP

Model 3
Alumina
Modulus vs. Temperature

=Y

In

r-mlnlncl
. .

40006:

o
a
o

i$

(N

o
0
co
o
0
a

o
0

04

o
0
0

0
0
cm
N

0
0
a
o
%
o
0
m

ii

)
)
r

X3
,rl

-..

----

-.

Hu+

ANSYS 5.1
34
SEP
5 1995
09:49:10
PLOT NO.
9
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =,O 02~~~~)
Sm =-2325
SMNB=-4275
SMX =6822
SMXB=7228

EEEl

EKEl
I

I
I

-2325
-1817
-1309
-800.511
-292.369
215.773
723.914
1232
1740
2248
2756
3265
3773
4281
4789
5297
5805
6313
6822

Figure 40
Model 3
Bottom Starter Tube
PrincipalTensile Stress

-4---7--

--+.

.,
-+----

+,

L+

-. ...
H!l

XNSYS 5.1
34
SEP
5 1995
09:49:43
PLOT NO.
10
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =.() 15~;~)
SMN =-396.08
SMNB=-1094
SMX =4460
SMXB=6099
-396.08
-126.316
143.449
413.214
682.978
952.743
1223
1492
1762
2032
2302
2571
I
II
2841
t
1
I
I
3111
IzzI
3381
3650
3920
4190
4460
I

Figure 41
Model 3
Top Starter Tube
Principal Tensile Stress

..

ANSYS

5.1

34

SEP
5 1995
09:50:07
PLOT NO.
11
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =.() 14~~~;)
SMN =-1758
SMNB=-4084
SMX =15378
SMXB=15857
-1758
-805.583
146.364
1098
2050
EEl
3002
ZmEi
3954
4906
5858
6810
7762
EE3
8714
9666
10618
11570
12522
13474
14426
15378

Figure 42
Model 3
Center Core Tube
PrincipalTensile
Stress

_-. -m

-,,

,-

-w

-H

- ~

1---

-!-=

ANSYS

5.1

34

SEP
5 1995
09:50:53
PLOT NO.
12
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
S1
DMX =.() 14;;~)
SMN =-1758
SMNB=-4084
SMX =15378
SMXB=15857
-1758
-805.583
146.364
1098
2050
3002
3954
4906
5858
6810
7762
EEEl 8714
I
9666
I
1
10618
11570
1- 1
12522
13474
14426
15378

Figure 43
Model 3
CenterCoreTube
PrincipalTensile Stress

-- _-&+- +---1

.
H

-H

+:

.+

---+

r-~

+-

ANSYS

5.1

34

SEP
5 1995
09:51:30
PLOT NO.
13
NODAL SOLUTION
STEP=l
SUB =1
TIME=l
Ux
RSYS=()
DMX =0.140841
SEPC=ll .144
WIN =0.001884
SMX =0.021566
0.001884
0.002977
0.004071
0.005164
0.006258
0.007351
0.008445
0.009538
0.010632
0.011725
0.012819
0.013912
0.015006
0.016099
0.017193
0.018286
0.019379
0.020473
0.021566

Figure 44
Model 3
CenterCoreTube
Radial Displacement UX

..

..

>
3
b

II-1