TRANSFORMATION OF PROCESSED KAOLIN BY

PLASMA MAGMAVICATION

A Thesis
Presented to
The Academic Faculty

by

Josepha D. Celes

In Partial Fulfillment of the Requirements for the Degree of

Master of Science in Civil and Environmental Engineering

Georgia Institute of Technology

August 1999
TRANSFORMATION OF PROCESSED KAOLIN BY
PLASMA MAGMAVICATION

Approved:

n
Paul W. Mayne, Chairman
 iii

DEDICATION

Chamorro: Para i henerasion antes ki guaho ni muna posipble, yan para i henerasion ni

tatati ki guaho ni muna baii todo. Na tatfe'na i kommunidat, kostumbre, yan kottura siha,

ya in fanacho gi direchon miyo.

(English: To the generations before me who made it possible, and for the generations

after me who make it all worthwhile. Step beyond societal, traditional, and cultural

boundaries and set your own standards.)

 ACKNOWLEDGEMENTS

I would first like to thank my advisor, Dr. Paul W, Mayne, to whom I owe many

sleepless nights and a lot of stress & frustration ©. I will always admire his combination

of intelligence, practical experience, and sharp wit that makes him one of the best

professors I have worked for and learned from. My sincere appreciation is extended to

Dr. Marion Wampler (EAS) and Dr. Joseph Dove (CEE) for their advice and insight on

aspects of my research. My deepest gratitude and friendship goes to Mr. William

Waggener (EAS). He has been an invaluable source of information, guidance, personal

advice, and support (now you can go home on time without the fear of hearing "Bill, I

have a question..."). Appreciation is given to Dr. Lou Circeo, Bob Newsom, and Lamar

Carney for the use of the Plasma Applications Research Facility resources and their

assistance. I would also like to recognize the Defense Special Weapons Agency,

Education and Research Development Agency of Georgia, and the National Science

Foundation for funding this research effort. My gratitude to those who assisted in lab

testing: Alec McGillivray, Tracy Hendren, Gye-Chun Cho, Julio Valdes, Amr El-Hakim,

Gautam Patel, and Lisa Detter-Hoskin. I would also like to thank Dr. KK.

Muraleetharan (University of Oklahoma) who inspired me to pursue geotechnical

engineering.

Finally, my undying love and appreciation to all whom have helped me towards the

light at the end of the tunnel. I might not have all the names down, but that is only
 V

because I have run out of space, not heart: Joshua (hu giiaiya hao\ Chingachcook,

{Catherine, Alec, Merten, Tracy, Julio, Sarah, Josephine, Mischa, Cihan, Jamie, Ryan,

Charles, Mark & Astrid, Chris, Somying, Brindha, Leslie, Amata, Nina & Nino Duncan,

Laura, Jane, Nicole, Rocio, Mich, Rika, Kathy, Meks, Marie, Therese, Manuel, my

family...and my paternal grandmother, Victoria San Nicolas Celes (rest in peace).

 vi

TABLE OF CONTENTS

THESIS APPROVAL PAGE ii

DEDICATION iii

ACKNOWLEDGEMENTS iv

TABLE OF CONTENTS vi

LIST OF TABLES x

LIST OF FIGURES xi

SUMMARY xiii

CHAPTER I. INTRODUCTION 1

1.1 Purpose of Research 3

1.1.1 Remediation of Contaminated Processed Kaolin 4

1.1.2 Geomaterial Characterization 5

1.1.3 Petrography 5

CHAPTER II. PRECEDING RESEARCH ON THERMAL HEATING OF SOILS 12

2.1 In-Situ Thermal Treatment of Soils 12

CHAPTER III. LABORATORY EQUIPMENT 19

3.1 Non-Transferred Arc Plasma Torch Equipment 19

3.1.1 General Components for the Plasma Torch Systems 20

3.1.2 PT50 Non-Transferred Arc Plasma Torch System 20

3.1.3 PT150 Plasma Torch System 22

3.2 Off-Gas Scrubber System 22

 3.2.1 Laboratory Gas Collection System 23

3.3 Chamber Dimensions and Description 25

3.4 Instrumentation 27

3.4.1 Standard K-Type Thermocouples 27

3.4.2 Time Domain Reflectometry 28

3.5 Summary 32

CHAPTER IV. PROPERTIES AND PREPARATION OF GEOMATERIAL 33

4.1 Geology of Source Area 33

4.2 Formation and Structure of Kaolinite 34

4.3 Grain Size Distribution 39

4.3.1 Hydrometer 39

4.3.2 Laser Light-Scattering 40

4.3.3 Scanning Electron Microscopy 41

4.3.4 Discussion 42

4.4 Index Properties 47

4.5 Activity 48

4.6 General Kaolin Preparation 51

4.7 Chamber Deposit Preparation 52

4.8 Synopsis 54

CHAPTER V. SURROGATE MATERIAL PREPARATION AND PLACEMENT 56

5.1 Surrogate Contaminant Materials 56

5.2 Preparation of Surrogate Materials 58

 viii

5.2.1 Nuclear Surrogate Preparation 59

5.2.2 Chemical Surrogate Preparation 59

5.2.3 Biological Surrogate Preparation 60

5.2.4 Mixed Surrogate Preparation 61

5.3 Placement of Contaminants in Kaolin Deposit 62

CHAPTER VI. GENERAL TESTING PROCEDURES 68

6.1 Plasma Torch Initiation and Termination Process 69

6.2 General Torch Operations 70

6.3 Dissection Procedure 71

CHAPTER VII. GEOCHEMICAL ANALYSES OF CONTAMINANT

REMEDIATION 75

7.1 Scanning Electron Microscopy and X-Ray Diffraction 75

7.2 Uncontaminated Processed Kaolin 78

7.3 JDC-1: Uncontaminated Test (Control) 78

7.4 JDC-2: Nuclear Surrogate Contaminant Test 81

7.5 JDC-3: Chemical Surrogate Contaminant Test 84

7.6 JDC-4: Biological Surrogate Contaminant Test 90

7.7 JDC-5: Mixed Waste Surrogate Contaminant Test

Using 100-kW Torch System 92
7.8 JDC-6: Mixed Waste Surrogate Contaminant Test
Using 200-kW Torch System 93

7.9 Discussion 95

CHAPTER VIII. CHARACTERIZATION OF PRE-TEST KAOLIN AND

POST-TEST TRANSFORMED ROCK 97
 ix
8.1 Preparation of Kaolin Specimens for Testing 97

8.2 Compressive Strength Testing 101

8.3 Initial Small-Strain Stiffness 103

8.4 Porosity 107

8.5 Unit Weight 107

8.6 Results of Mass, Power Consumption, and Time Observations 108

CHAPTER IX. PETROGRAPHY OF THE TRANSFORMED ROCK 116

9.1 Preparation of the Rock for Thin Sections 116

9.2 Mineral Determination and the Becke Line Test 118

9.3 Petrographic Results and the Classification of the Rock 120

9.4 Mullite Formation 126

9.5 Discussion on Influencing Post-Test Rock Formation 129

CHAPTER X. CONCLUSIONS 132

CHAPTER XI. RECOMMENDATION FOR FUTURE RESEARCH 135

APPENDIX A (TEST INFORMATION FOR JDC-1 TO JDC-9) 137

APPENDIX B (RESULTS OF SCANNING ELECTRON MICROSCOPY) 173

APPENDIX C (RESULTS OF X-RAY DIFFRACTION) 190

APPENDIX D (RESULTS OF LABORATORY TESTS ON KAOLIN) 211

APPENDIX E (RESULTS OF LABORATORY TESTS ON ROCK) 220

APPENDIX F (PETROGRAPHIC SLIDES) 223

APPENDIX G (TIME DOMAIN REFLECTOMETRY) 226

REFERENCES.... 243
 X

LIST OF TABLES

TABLE PAGE

1.1 List of EPA Regulations 2

1.2 Soil Remediation Techniques 8

2.1 Developments in In-Situ Thermal Heat Treatment of Soils 15

3.1 Equipment Used for Experiments 32

4.1 Breakdown of Oxides in Processed Kaolin 46

4.2 Clay Fraction Determined by Particle Measurement Techniques 46

4.3 Index Properties of Processed Kaolin 49

4.4 Range of Kaolin Characteristics 49

4.5 Parameters of Kaolin Deposits Prepared for Tests JDC-1 through JDC-9 54

5.1 Experiments Performed Using Surrogate Contaminants 58

7.1 Weights and Dimensions of Dissected Rocks 82

8.1 Summary of Experiments 98

8.2 Results of Laboratory Tests on Kaolin and Transformed Rock 99

9.1 Results of Point-Counting on Petrographic Slides 125

9.2 Characteristics of Mullite 128

 Xi

LIST OF FIGURES

FIGURE PAGE

1.1 Illustration of Selected Soil Remediation Techniques 10

1.2 Illustration of Soil Remediation Techniques Using Very High Temperatures 11

3.1 Transferred Arc and Non-Transferred Arc Plasma Torches 21

3.2 (A) Off-Gas Scrubber System (B) Cutaway View of Off-Gas Scrubber Detail 24

3.3 Schematic Drawings of Steel Chambers 26

3.4 (A) "Seebeck Effect" (B) Standard Thermocouple Configuration 31

4.1 Distribution of Kaolin Mines in Georgia 36

4.2 Experimental and Predicted Phase Relations Among K-Feldspar, Muscovite

Pyrophyllite, and Kaolinite 37

4.3 Symbolic Structure of Kaolinite 38

4.4 Grain Size Distribution of Processed Kaolin by the Laser

Light-Scattering Technique 44

4.5 Scanning Electron Microscopy Image of Kaolin Particles 45

4.6 Casagrande Chart Showing Natural and Processed Kaolin Points 50

4.7 Thermocouple Insertion Ports 55

5.1 Sequence of Contaminant Preparation Prior to Placement in Kaolin Deposit 63

5.2 Steel Can for Containment of Surrogate Contaminants 64

5.3 Illustration of General Can Layout 66

5.4 Photographs of Vertical and Horizontal Layout of Cans During Placement 67

6.1 General Dimensions Noted for Post-Test Calculations and Documentation 73

 xii

6.2 Partially-Dissected Kaolin Deposit 74

7.1 Example of SEM Output Graph 79

7.2 Example of XRD Output Graph 80

7.3 SEM Analyses for Tests JDC-1 to JDC-6 and Processed Kaolin 86

7.4 Detected Elements by SEM with Exception of Oxygen 87

7.5 Minor Elements Detected by SEM Analyses 88

7.6 Nuclear and Chemical Surrogate Contaminant Concentrations for Tests 89

7.7 Biological Surrogate Contaminant Concentration 91

8.1 Slabbing Failure in Rock 104

8.2 Change in Nondestructive Elastic Modulus and Destructive Compressive

Strength Between Original Soils and Magmified Rocks 106

8.3 Change in Shear Modulus and Unit Weight Through Plasma Magmavication 109

8.4 Relationship Between Igneous Rock Mass and Energy Consumption Used
During Magmavication 112

8.5 Relationship Between Igneous Rock Volume and Energy Consumption for
Different Soils 113

8.6 Effect of Treatment Time on Igneous Rock Mass Produced 114

8.7 Effect of Average Power Levels on Igneous Rock Mass Produced 115

9.1 General Counting Course on a Petrographic Slide (No Magnification) 123

9.2 Petrograhic Slide at lOx Magnification 124

9.3 Two-Component System Indication the Boundaries Between

Liquid/Mixed/and Solid States at Atmospheric Pressure 131
 X111

SUMMARY

The current remediation technologies approved by the EPA for Superfund site soil

treatment are bioremediation, capping, excavation, immobilization, in-situ vitrification,

incineration, soil washing, and thermal desorption, electrokinetics, and air sparging. Of

these technologies, in-situ vitrification (1SV) and in-situ plasma magmavication are the

only processes that can destroy both inorganic and organic contaminants, regardless of

the concentrations or compositions.

In-situ plasma magmavication (ISPM) is a treatment that uses a non-transferred arc

plasma torch for soil remediation as well as soil strengthening and modification. The

non-transferred arc plasma torch is capable of routinely attaining temperatures from

4000°C to 7000°C, which is above the melting point of all materials known to man.

The effects of ISPM on prepared deposits of uncontaminated and contaminated

processed kaolin were examined in laboratory chamber experiments. Kaolin deposits

were placed and compacted in a uniform manner within steel cylindrical chambers. Nine

laboratory experiments were performed using two sizes of plasma torch systems. The

viability of ISPM for environmental remediation, its effect on the engineering properties,

and identification and classification of the igneous rock produced by the process were

investigated using scanning electron microscopy, x-ray diffraction, ASTM tests, and

petrographic tests.
 1

CHAPTER I

INTRODUCTION

Vitrification is the transformation, by heating, of matter into an amorphous material

(glass). The advent of the non-transferred arc plasma torch, used in this research

program, lends itself to direct insertion in the ground to treat soil by vitrification using

very high temperatures. Temperatures over 4000°C are applied to melt soil that

subsequently cools to form an igneous rock. Since vitrification does not occur with all

soils, the combination of the non-transferred plasma arc torch with in-situ remediation of

soil is a technology more generally termed in-situ plasma magmavication.

st
As the world stands on the threshold of the 2 1 century, mankind has never seen

such immense advances in technology as it has in the past century. Life expectancy has

lengthened, animals have been cloned, computers pontinue to become more efficient, and

artificial intelligence has been developed, to name a few of the accomplishments.

However, with this boon of expanding knowledge comes the misfortune of the

production, management, and disposal of wastes produced by it. The types of wastes are

quite varied and examples include inert organic and inorganic materials, heavy metals,

chemicals, and radioactive wastes.

To address these concerns in the United States, the Environmental Protection

Agency (EPA) was established as an independent federal agency in 1970. Since its
 2

TABLE 1.1: LIST OF EPA REGULATIONS

REGULATION YEAR
IMPLEMENTED
Clean Air Act (CAA) 1970
Federal Insecticide, Fungicide, and Rodenticide Act (FIFRA) 1972
Marine Protection, Research, and Sanctuaries Act (MPRSA) 1972
Safe Drinking Water Act (SDWA) 1974
Resource Conservation and Recovery Act (RCRA) 1976
Toxic Substances Control Act (TSCA) 1976
Clean Water Act (CWA) 1977
Uranium Mill Tailings Radiation Control Act (UMTRCA) 1978
Comprehensive Environmental Response, Compensation, and 1980
Liability Act (CERCLA, or "Superfund")
Hazardous and Solid Waste Amendments (HSWA) 1984
*amendment to RCRA
Superfund Amendments and Reauthorization Act (SARA) 1986
* amendment to CERCLA
Pollution Prevention Act (PPA) 1990

inception, the EPA now oversees ten environmental protection laws, shown in Table 1.1

(EPA/220-B-93-008, 1993).

Of particular interest to this research effort are the CERCLA, RCRA, TSCA, and

related amendments to the legislation. These laws address the generation and disposal of

hazardous wastes from newly-created, closed, and abandoned sites. The current

remediation technologies approved by the EPA for Superfund site soil treatment are

bioremediation, capping, excavation, immobilization, in-situ vitrification, incineration,

soil washing, and thermal desorption (EPA/540-R-94-043, 1994). Electrokinetics and air

sparging (used in conjunction with soil vapor extraction) are also among the more well-

known remediation techniques.

 3

Of these technologies, in-situ vitrification and in-situ plasma magmavication are the

only processes that have the capability to destroy both inorganic and organic

contaminants, regardless of the concentrations or compositions. This significant

advantage over other technologies warrants further investigation into plasma

magmavication of contaminated soils as a thorough solution to waste treatment. Table

1.2 lists the more well-known and commonly used soil remediation techniques. Figure

1.1 shows bioremediation, air sparging, electrokinetics, soil mixing, and excavation.

Figure 1.2 illustrates the high temperature soil remediation techniques of in-situ

vitrification and in-situ plasma magmavication.

1.1 Purpose of Research

The objective of this research program was to conduct laboratory experiments using

in-situ plasma magmavication for soil remediation. Specifically, the tasks included

utilization of non-transferred arc plasma torches to remediate in-place deposits of kaolin

that held contaminants of biological, chemical, and nuclear origins. In addition, the

studies made progress to investigate. (1) the effect of plasma magmavication on the

engineering properties of the project soil, and (2) the classification of the igneous rock

resulting from plasma magmavication through petrographic tests. A total of nine

laboratory experiments were performed on deposits of kaolin prepared in steel chambers.

 4

1.1.1 Remediation of Contaminated Processed Kaolin

Processed kaolin was used for all laboratory experiments in order to allow for a

continuous supply of soil of uniform and constant mineralogy and consistent standards.

Six experiments were done on kaolin deposits that were seeded with surrogate

contaminants prior to magmavication.

Previous experiments performed by Mayer (1996) were the first to establish the

viability of non-transferred plasma arc technology in treating soil seeded with non-toxic

contaminants such as cans, glass, and pieces of concrete, as well as specially-made

briquettes. The briquettes contained 0.92% of RCRA metals and 0.35% radionuclide

surrogates.

In this research effort, focus was placed on treating more hazardous contaminants.

The contaminants used in this research program consisted of biological, chemical, and

nuclear surrogate materials. The surrogate materials were chosen because they reflect the

same range of physical, chemical, and thermodynamic properties as contaminants that

may be found onsite at existing facilities in the U.S. The contaminants were introduced

separately in controlled experiments of compacted kaolin, as well as in combined tests to

determine the effectiveness of the plasma torch in treating mixed wastes.

One significant advantage that the plasma\orch has over all other soil remediation

techniques is its applicability to handle any and all types of wastes in all types of soils.

Past research has proven its effectiveness on incinerator ash (Plumley, DeCesare, and
 5
Hollander, 1992), inert buried contaminants (Mayer, 1996), and asbestos (Circeo and

Newsom, 1996).

1.1.2 Geomaterial Characterization

Various engineering properties of both the pre-test kaolin and the post-test rock

(magmafied kaolin) were examined to determine the changes due to transformation from

soil to rock by plasma magmavication. Laboratory experiments performed on

undisturbed shelby tube specimens were done to determine the changes in compressive

strength (q^), shear modulus ( G x ) elastic modulus (E), porosity (n), unit weight
ma 3 (YT),

and specific gravity (G ) between the processed kaolin and the igneous rock.
s

These results will be compared with those obtained from previous research

performed by Beaver (1995) and Mayer (1996).

1.1.3 Petrography

Petrography is the description and classification of rocks as related to the mineralogy

and texture of intact specimens. Specimens are prepared into thin sections and examined

under a petrographic microscope. A thin section is a slice of rock that has been mounted

on a standard-sized microscope slide and then ground to a thickness of 30 um.

Identification of the minerals present can be made by recognition, comparison with

optical properties and crystal morphology of known minerals, x-ray diffraction, and
 6
differential thermal analysis (Kerr, 1977). For this research effort, x-ray diffraction was

performed to determine the mineralogy of specimens taken from the center of the igneous

rocks produced by magmavication. The x-ray diffraction results are presented in

Appendix C.

Mineral identification was followed by examination of the prepared thin sections.

This entails a process of point counting, which is a manual counting of the constituents

in the rock to determine their relative amounts. The counting was done on a polarizing

microscope in which the mounting plate is controlled by a screw mechanism that allows

movement horizontally and vertically in increments of 0.3 mm. From the eyepiece,

crosshairs determine the counting area. Classification of the rock is finalized when the

identification of mineralogy and constituent amounts are determined. Specific details of

the specimen thin section preparations and the results are located in Chapter IX.

The formation of the rock is essential in determining such properties as hydraulic

conductivity and strength. If plasma magmavication is to be applied for treatment of

hazardous wastes, these properties need to be quantified to determine the leachability and

integrity that can be expected from rocks produced by a soil of given mineralogy.

1.2 Summary

The nine tests performed for this research effort focused on soil remediation,

material properties, and petrography of the rock produced by plasma magmavication.

The applicability of the non-transferred arc plasma torch for in-situ applications is
 7

encouraging because it is neither contaminant-specific nor soil-specific, which are

significant advantages over other technologies.


TABLE 1.2: SOIL REMEDIATION TECHNIQUES
TECHNIQUE MOST EFFECTIVE IN
TREATING:
Bioremediation Petroleum products and
hydrocarbons
Capping Extensive contamination in
which removal poses a threat to (20 yrs); requires periodic
human health and the
environment
Excavation All types of wastes,
particularly hazardous wastes
Immobilization Toxic and hazardous chemicals Soil treatment requires
(Soil Mixing) from soil slurries and waste
sludges
Incineration Organic compounds such as
dioxins and polychlorinated
biphenyls (PCB)
Soil Washing Volatile organic compounds
(VOC) in sands and gravels;
some inorganic compounds
(metals)
Thermal Desorption Organic contaminants like
VOC, PCB, and some
polynuclear aromatic
hydrocarbons (PAH)
s
CONCERNS:
Many conditions (soil pH,
chemical concentrations,
moisture content) must be met
for optimum efficiency of
technique
Relatively short life span
inspection; must be used with
other technologies to prevent
contaminant migration
Requires treatment of soil after
excavation; may require barrier
installation to prevent
migration; soil must be stored
or backfilled
thorough in-situ mixing or ex-
situ processing; sulfate salts
and metallic anions can hamper
solidification
Can not treat inorganic
compounds; not 100%
effective so ash must be
disposed of at a RCRA-
permitted facility
Efficiency ranges between 40%
to 90% depending on
contaminant(s); wash water
requires treatment; very
difficult to treat fine-grained
SOiiS
Can not treat inorganic
contaminants, heavy metals
(except Hg), tars, and heavy
pitches

TABLE 1.2 (CONTINUED)
TECHNIQUE MOST EFFECTIVE IN
TREATING:
Air Sparging VOCs such as benzene, toluene,
ethylbenzene, and xylene
(BTEX) in highly permeable
soils; effectiveness increases
when used with other remedial
methods (soil vapor extraction,
pump-and-treat, etc.)
Electrokinetics Hexavalent chromium-
contaminated unsaturated and
partially-saturated soils
In-Situ Vitrification Radioactive, organic, and
(using embedded inorganic contaminants
graphite electrodes)
In-Situ Plasma Radioactive, organic, and
Magmavication inorganic contaminants in all soil
(using non-transferred types
plasma torch)
*NOTE: This table represents the most commonly used and accepted
it should not be considered exhaustive.
9
CONCERNS:
Can not be used if free
product is present; near
subsurface confined spaces
(basements, sewers, etc);
can not treat confined
aquifers; ineffective in
treating low permeability,
stratified, and/or highly
variable heterogeneous soils
Modification of technology
is necessary to treat other
contaminants, other ions
will compete with
contaminant ions for
removal
High soil moisture increases
power and time for
remediation, low
conductivity must be
improved by addition of
glass frit
High soil moisture increases
power and time for
remediation, technology is
still in development and
requires highly-specialized
equipment
techniques,
 Q
I
Cathode Anode

Pipe-

o
oo oo ff ii
\ \ . J
Microorganisms Contaminated contaminant-free air
soil

A. Boi remediation B. Ari Sparging

Effective in treating
C. Electrokinetics
Effective in
Effective for
treatment of volatile organic treating metallic
petroleum products compounds in species
and hydrocarbons highly-permeable
soil

Treatment by
| f ' Cement ex-situ furnace

Solidified
cement/soil
columns

D. Soil Mxinig
Effective for toxic
E. Excavation
Effective for removal
and hazardous of hazardous wastes
chemicals from for ex-situ treatment
slurries and or landfilling
sludges

FIGURE 1.1: ILLUSTRATION OF SELECTED SOIL

REMEDIATION TECHNIQUES
 11

A. In-Situ Vitrification B
Effective for organic,
inorganic, and
M.agInm
-SaituvciaoitPnlasma
Effective for organic,
radioactive wastes with inorganic, and
consideration to soil radioactive wastes in
conductivity and all soil types
moisture content

FIGURE 1.2: ILLUSTRATION OF SOIL REMEDIATION TECHNIQUES

USING VERY HIGH TEMPERATURES:
(A) IN-SITU VITRIFICATION USING EMBEDDED GRAPHITE ELECTRODES
(B) IN-SITU PLASMA MAGMAVICATION USING NON-TRANSFERRED ARC
PLASMA TORCH
 12

CHAPTER II

PRECEDING RESEARCH ON THERMAL HEATING OF SOILS

This section provides a summary of the developments of in-situ thermal heat

treatment of soils for purposes of ground modification or remediation.

2.1 In-Situ Thermal Treatment of Soils

Thermal heat treatment of soils has been used in the past to increase the strength and

stiffness of clays to fabricate building materials (clay bricks) and storage containers (kiln-

fired pots and jars). Present developments of in-situ thermal treatment techniques have

broadened the applications to include remediation, strengthening of foundation soils, and

the stabilization of soils and rocks. In-situ treatment eliminates the added expenses of

excavation, external processing (either onsite or offsite), and/or storage or disposal of the

soil. Table 2.1 is a chronological summary of the important studies on in-situ thermal

treatment on soils using methods such as heaters, furnaces, microwaves, and burning fuel

in borehole. The table was adapted from Mayer (1996) and includes recent developments

in plasma magmavication.

Since 1992, the Georgia Institute of Technology has been involved in research to

validate the capabilities of in-situ plasma magmavication and the in-place melting of soil
 13

by non-transferred arc plasma torch. The initial experiments performed by Circeo and

Mayne (1993) proved the effectiveness of the technique in decreasing porosity, void

ratio, and water content while increasing the stiffness and strength by melting both clay

and silty sand and eventually forming igneous glassy rock.

Further research by Beaver and Mayne (1995) was performed to broaden the range

of soils to include two types of sands (Tyndall Beach sand and 20/30 blasting sand), silt

(Piedmont soil), and locally-obtained clay (Georgia kaolin). In this instance, variables

such as moisture content, soil type, power level, and energy consumption were examined

to determine their effect on the size and weight of the igneous rock produced. A

significant outcome of this study was the finding that initial soil type and mineralogy

affected the igneous rock produced. In general, sands and soils with high quartz contents

tend to produce a glassy rock (non-crystalline), but other soils can produced a layered

multi-crystalline igneous rock with glass inclusions.

Mayer (1996) expanded the research effort by investigating the applicability of in-

situ plasma magmavication in treating soil obtained from Savannah River Site (a clayey

sand). Specific goals were to determine if fluxing agents were needed to melt the soil, to

simulate melting conditions in the presence of a groundwater table, to melt non-toxic

contaminants, and to coalesce two melts. The research was significant in showing the

viability of in-situ plasma magmavication for remediating contaminated soil.

The first plant-scale test was performed at the K-Reactor seepage basin located at the

Savannah River Site (Blundy et al., 1996). This field experiment was performed to verify

the usefulness and effectiveness of the technology in field conditions. A 1-MW non-
 14

transferred arc plasma torch was used in three tests, all of which were successful in

melting the soil. There are still significant issues (such as remote instrumentation,

modeling, and safety concerns) that need to be resolved for future experiments and

ultimately for the commercial application of in-situ plasma magmavication.

Circeo et al. (1998) further investigated the applicability of in-situ plasma

magmavication on weathered argillaceous sedimentary rocks. The research confirmed

that argillaceous rocks could be melted and altered by the non-transferred arc torch. This

effort by use of plasma technology indicated potential applications in stabilizing rock

slopes and treating expansive rocks (such as shales and mudstones).

2.2 Synopsis

The effectiveness of high temperature heating for ground modification and

remediation has been studied by researchers since the early part of the 20 t h
century and

their findings validate further experimentation in this area. The future importance of

plasma magmavication for remediation seems to be more tangible as social, ethical, and

health concerns pressure engineers and scientists to find solutions to waste storage and

cleanup that are safer, more efficient, and faster than the conventional methods.

TABLE 2.1: DEVELOPMENTS IN IN-SITU THERMAL HEAT
TREATMENT OF SOILS (ADAPTED FROM MAYER, 1996)
Author and Year Title
Irvine (1930) "Road making by heat
treatment of soils"
Hill (1934) "Clay stratum dried out to
prevent landslips"
Beles and Stanculescu "Thermal treatment as a
(1958) means of improving the
stability of earth masses"
Litvinov (1960) "Stabilization of settling and
weak clayey soils by thermal
treatment"
Fujii (1971) "The practical application of
thermal and freezing methods
to soil stabilization"
Jankiewicz (1972) "Fusing soils"
Kukanov(1972) "Construction of a continuous
base of an installation under
construction by thermal
stabilization of soils"
Yurdanov (1978) "Characteristics of deep
roasting of soils and prospects
of its improvement"
Litvinov et al. (1979) "Firing of a loess soil to
25 m depth"
15
Synopsis
Used a mobile wood furnace
over to heat treat soils for road
subgrades
Soil moisture content reduction
by forcing heated air through
tunnels.
Burned fuel in boreholes to
strengthen soils, such as
sensitive clays.
Treated settlement in loess by
burning fuel in a burner at the
top of a sealed borehole.
Investigated the applications of
thermal stabilization and
differentiated between open
and closed systems.
Heat treatment of soils
increased shear strength by
reducing the amount of clay-
sized particles and decreasing
moisture content.
Burned natural gas in adjacent
boreholes to form a continuous
area of thermally stabilized
soil.
Presented an in-situ method
using electric heaters blowing
compressed air.
Modified burner so that
bottom-to-top stabilization
treatment of soils was
achieved.

TABLE 2.1 (CONTINUED)
Author and Year Title
Brouns, Buelt, and Bonner "Patent for in-situ
M
(1983) vitrification (ISV)
de Leeuw(1985) Conference on soil
mechanics and foundation
engineering
Buelt et al. (1987) "In situ vitrification of
transuranic wastes: an
updated systems evaluation
and applications
assessment"
Camacho (1988) "Arc plasma processes: a
maturing technology in
industry"
Buelt and Bonner (1989) "In situ vitrification: test
results for a contaminated
soil melting process"
Munz and Chen (1989) "Vitrification of nuclear
waste in a transferred arc
plasma melter"
Spalding and Jacobs (1989) "Evaluation of an in-situ
vitrification field
demonstration of a
simulated radioactive liquid
waste disposal trench"
Sanderson and Verme "Hanford in situ
(1990) vitrification test produces
record size glass block"
16
Synopsis
In-situ treatment using four
embedded electrodes to
melt soil.
Used a burner to treat
excavated contaminated soil
Describes the in-situ
vitrification process in-
depth and the development
of key components.
Synopsis of plasma
technologies (torches,
furnaces, and reactors).
Includes several case
studies.
Proved through material
balance that soil moisture
was completely removed by
the ISV process.
Simulated nuclear waste
remediation in a plasma
melter.
Performed a field
demonstration on simulated
waste at Oak Ridge to prove
viability of ISV in treating
trenches containing
radioactive wastes.
Used ISV at the US DOE
Hanford site to melt soil
contaminated with
radioactive and hazardous
chemical wastes.

TABLE 2.1 (CONTINUED)
Author and Year Title
Sears et al. (1990) "Plasma centrifugal furnace;
a method for stabilization
and decomposition of toxic
and radioactive wastes"
Byers et al. (1991) "Site remediation by in situ
vitrification"
Dragun(1991) "Geochemistry and soil
chemistry reactions
occurring during in situ
vitrification"
Camacho (1992) "Plasma technology for a
better environment"
Staley (1992) "Site demonstration of the
retech plasma centrifugal
furnace. The use of plasma
to vitrify contaminated soil"
Circeo and Mayne (1993) "In-situ thermal stabilization
of soils using plasma arc
technology"
Beaver and Mayne (1995) "Plasma vitrification of
geomaterials"
17
Synopsis
Used a transferred arc
plasma torch in a furnace to
stabilize soil containing solid
waste materials.
Described the ISV process in
which electricity is used to
melt soil.
Studied the effect of ISV on
soil chemical reactions and
the processes that drive
migration and degradation of
chemicals in the soil.
Reported the industrial uses
of plasma technology.
Showed applicability of
transferred arc plasma
furnace for treating
Superfund sites
contaminated with organic
chemicals and metals.
First experiments to prove
viability of non-transferred
plasma arc torch for
effectively and efficiently
melting soils in-situ
Used non-transferred plasma
arc torch to compare the
influence of different
variables on the weight and
size of vitrified products.
Measured changes in
compressive strength,
stiffness, density, and wave
velocities of pre-test and
post-test materials.

TABLE 2.1 (CONTINUED)
Author and Year Title
Blundy, Zionkowski, "Demonstration of plasma in-
Schumacher, and situ vitrification at the K-
Herman (1996) Reactor seepage basin"
Mayer (1996) "Laboratory chamber
experiments simulating in-
situ plasma vitrification for
geoenvironmental concerns"
Circeo, Mayne, Newsom, "In situ stabilization of
and Hendren (1998) geologic materials by
vitrification using plasma arc
technology"
18
Synopsis
First plant-scale field
experiment using non-
transferred arc plasma torch
(1-MW) at Savannah River
Site. Verified usefulness and
effectiveness of process in
field conditions.
Determined effects of high
saturation, fluxing agents,
and buried contaminants
(inert and specially made
briquettes) on the
effectiveness of the non-
transferred arc plasma torch.
Created overlapping vitrified
areas through treatment of
consecutive boreholes.
Treated weathered
sedimentary rock materials
with non-transferred arc
plasma torch and
demonstrated potential in
stabilizing swelling rock or
rock slopes/slides
 19

CHAPTER IH

LABORATORY EQUIPMENT

An overview of the plasma equipment, off-gas treatment system, the steel chambers in

which the kaolin deposits were made is presented in this section including the

instrumentation used in the test program.

3.1 Non-Transferred Arc Plasma Torch Equipment

Two separate plasma systems were used in this research program: (1) a 100-kW rated

system and (2) a 240-kW rated system. Plasma Energy Corporation (PEC) of Raleigh,

North Carolina manufactured both of the systems. 'The 100-kW system was obtained on

loan from Georgia Power in Atlanta, GA. The 240-kW system was provided through

funding by the Army Corps of Engineers in Urbana, IL. Both systems are currently

located at the Plasma Applications Research Facility (PARF) at the Structures and

Materials Testing Laboratory located on North Avenue in Atlanta. For the experiments

reported herein, all tests were done at a temporary testing facility that was located on

Southland Circle. The building was leased to Georgia Tech for the duration of the
 20

construction of the new laboratory. Figure 3.1 shows schematic drawings for both

transferred arc and non-transferred arc plasma torch systems.

3.1.1 General Components for the Plasma Torch Systems

Each plasma torch system consists of additional components necessary for normal

operation. These are: (1) a power supply, either alternating or direct current; (2) a control

panel to regulate the initiation and support of the plasma arc column; ( 3 ) a starting system

to start the torch; ( 4 ) a gas system to provide the gas required to make the plasma; (5) a

closed-loop water system to provide cooling for the torch and the electrodes; and ( 6 ) a

plasma torch (Circeo and Newsom, 1996).

3.1.2 PT50 Non-Transferred Arc Plasma Torch System

The maximum power capacity that the PEC PT50 system is rated 100 kW. The torch

is 1.83 m long and 6.35 cm in diameter. A cylindrical stainless steel housing encloses the

copper electrodes, inlet lines for air, water and electricity, an outlet line for air, and the

3
vortex generator. Compressed air is supplied to the torch at a flow rate of 0.14 m /min,

3
and the flow rate of the water used to cool the system is 0.11 m /min. The DC power

runs off a 220-volt AC source. This plasma system was utilized in all the experiments

with the exception of one contaminated kaolin deposit that was made in the larger

capacity steel chamber.

 21

Electricity Water In Water In Electricity

Water Water
Output \ ^Output

I Rear Copper Rear Copper

Electrode Electrode

Arc at
T = 12,000°C

Stainless Steel
Water-Cooled
Jacket

VORTEX
VORTEX

Collimator
Front Copper
Electrode

Exterior
Electrode Plasma "Flame"
a t T = 4,000°C

Transferred Arc Torch Nontransferred Arc Torch

FIGURE 3 . 1 : TRANSFERRED ARC AND NON-TRANSFERRED
ARC PLASMA TORCHES
 22

3.1.3 PT150 Plasma Torch System

The maximum capacity of the PEC PT150 system is 240 kW in the transferred arc

mode and 200 kW in the non-transferred arc mode. This torch has the same

configuration as the PEC PT50 torch, with the exception of dimensions. The torch is

1.65 m long and 10.2 cm in diameter. Compressed air is supplied to the torch at a flow

3
rate of 1.42 nrVmin, and the flow rate of the water used to cool the system is 0.19 m /min.

The DC power supply for this system requires a 440-volt AC source. This plasma system

was used during one experiment in which a larger chamber deposit of kaolin was seeded

with a combination of nuclear, chemical, and biological surrogate contaminants.

3.2 Off-Gas Scrubber System

During magmavication, vapors produced from the heating of materials migrate

through the soil pores and can be released to the atmosphere. Since the gaseous by­

products of contaminants can be very hazardous or lethal, extreme care must be taken in

collecting and treating all emissions before release to the environment. One way to

accomplish this is to place a sealed hood over the treated area and divert the gases to an

off-gas scrubber system. Gases travel through the scrubber system and are treated using

various methods or chemicals. Samples can be taken during various stages of treatment

to determine the contaminant levels before release.

 23
Vapor collection is easy to accomplish in the laboratory since the soil deposit is

within a steel chamber, and a hood can be placed and secured on top of the chamber.

However, field conditions pose a more serious problem due to soil heterogeneity, which

can lead to vapor migration both vertically and horizontally. The use of only a sealed

hood as a means of vapor collection would be hard to accomplish due to the unknown

size of the migrating plume of vapors. Therefore, field conditions might require a hood

as well as another method of controlling vapor migration, such as soil vapor extraction

and use of wellpoints or a series of prefabricated drains.

3.2.1 Laboratory Gas Collection System

The off-gas scrubber system is a packed rockbed wet-type unit that has been used by

Georgia Tech and PEC for a number of years. Figure 3.2 is a illustration of the system.

Gases produced by the magmavication process are drawn by vacuum into the water

cooling scrubber. As the gases travel up the scrubber and pass through a 61-cm thick bed

of pebbles, they are cooled by water sprayed through three sets of spray nozzles (Circeo

and Newsom, 1996). The water used in the nozzles is mixed with caustic soda to

neutralize any acidic compounds in the gas. A sludge tank holds the caustic soda solution

and pH levels are checked throughout the test in order to maintain the alkalinity. The

sludge pump recirculates the water into the system.

The gases move to the outlet and prior to release are bubbled through a 3-m gas vent

tank which is seperately attached. Gas samples can be taken for chemical and solids

content analysis from the gas vent tank (Circeo and Newsom, 1996).
 24

(B)

& . — C + —

Scrubber water
Gas outlet to
gas vent tank
^zz^xzzz^ spray system

River pebble
bed inlet/outlet

Gas Inlet (shown rotated 90°)

Recycle water from sludge

tank to sprayers

IN II I I / ' F N NIL J II NY - - - • 1 - -N - N • IJ J—NM-N ,vm

Water supply. Recycle sludge to reactor

FIGURE 3.2: (A) OFF-GAS SCRUBBER SYSTEM

(B) CUTAWAY VIEW OF OFF-GAS SCRUBBER DETAIL
(ADAPTED FROM CIRCEO AND NEWSOM, 1996)
 25

3.3 Chamber Dimensions and Description

Two sizes of steel test chambers were used in the experimental program, as shown in

Figure 3.3. The height of both chambers is 0.9 m. The diameter of the smaller chamber,

which was used for the majority of the tests, was 0.6 m. In general, the 100-kW torch

was used in this chamber. The larger chamber was 0.9 m in diameter, and the 200-kW

torch was used in this chamber. The steel used to form both chambers was about 0.5-cm

in thickness. Both chambers were designed to separate into two halves in the lengthwise

direction. The halves have flanges on both sides that are bolted together prior to the

kaolin deposit preparation. This design also facilitates dissection and removal of the soil

and igneous rock after testing.

Within each chamber, a deposit of prepared soil was placed prior to the

magmavication process. The preparation of the kaolin deposits for the tests will be

discussed in Chapter IV. A thin steel stovepipe inserted into the center of the kaolin

deposits simulated a borehole casing. The stovepipe dimensions are shown in Figure 3.3,

and differed depending on the chamber size used. The stovepipe was placed to a depth of

76 cm from the top of the soil to ensure that soil would not collapse into the borehole and

widen its diameter. A widened diameter would have decreased the torch's efficiency by

allowing heat to escape rapidly.

For the majority of the experiments, the 100-kW torch was placed 15 cm from the

bottom of the borehole (30 cm from the bottom of the chamber). In a selected test, the

200-kW torch was placed 23 cm from the bottom of the borehole (38 cm from the bottom
 0.9 m
FIGURE 3.3: SCHEMATIC DRAWINGS OF STEEL CHAMBERS
(DRAWING NOT TO SCALE)
 27

of the chamber). This was done so that enough soil was below the torch to start a magma

pool and to safeguard against the torch burning through the bottom of the chamber.

3.4 Instrumentation

As the soil melts during the magmavication process, a large cavity forms above the

pool of magma. The size of the cavity and the magma pool are of keen interest in

determining the volume of soil melted (and thus treated) at a given time, as well as

important in the overall safety concerning operations of personnel and equipment.

Therefore, instrumentation is necessary to monitor the progress of the magma and cavity

growth.

At the temperature range of the non-transferred arc plasma torch (4000°C to

7000°C), every material known to man will be destroyed. It is of interest to note that

tungsten (W) has the highest melting point of all elemental metals at 3410°C (Zumdahl,

1989). Measurement devices considered for in-situ instrumentation during testing have

to be sturdy and able to perform sufficiently even when encountering the magma, the

plasma "flame", and/or the superheated gases circulating within the cavity and soil.

3.4.1 Standard K-Type Thermocouples

For the majority of the tests performed at Georgia Tech, thermocouples were used to

observe the temperature changes at fixed heights and depths within the side of soil
 28

deposit. The thermocouple placement will be shown in Chapter V. Thermocouples

operate on the "Seebeck Effect" (Pollock, 1971). This is the phenomenon in which a

circuit formed of two dissimilar metals, which are joined at both ends to form junctions,

will develop a voltage proportional to the difference in the junctions' temperatures.

Normally, the junction located furthest from the heat source is referred to as the

"reference junction." The other is called the "measuring junction." Figure 3.4(A) shows

the "Seebeck Effect", and Figure 3.4(B) is an illustration of a standard thermocouple.

In standard thermocouples, like the type used in this research program, the wires are

only joined at one end to form a point-type sensor. Instrumentation converts the millivolt

G
signal to temperatures in either °F or C.

The thermocouples used in this research effort were K-type standard thermocouples.

The wire material for the positive leg was chromel, a chromium-nickel alloy, and the wire

for the negative leg was alumel, an aluminum-nickel alloy. The K-type thermocouple

operating range is -133°C to 1400°C.

3.4.2 Time Domain Reflectometry

Time domain reflectometry (TDR) was used in one test in order to determine its

applicability in defining the size of the magma cavity during the plasma process. TDR is

a remote-sensing electrical measurement technique that can monitor movement or

deformation through physical changes in the length of cable. TDR has been used in

geotechnical engineering for detecting rock movement and deformation, detecting water
 29

migration through soil, and it is being developed for use in detection of soil movement

(Will, 1996).

The earliest form of TDR comes from radar, in which the pulse is sent through air

rather than through a material medium. A voltage pulse is sent down a coaxial cable and

is reflected back when either a change in the capacitance between the inner and outer

conductors is encountered, or the end of the cable is encountered. The size of the

reflected pulse is proportional to the size of the deformation, and is twice its original

amplitude if the pulse is reflecting off the end of the cable. By knowing the propagation

velocity of the pulse and the time of travel, the distance to the cable distortion, or to the

end of the cable, can be determined (O'Connor and Dowding, 1999).

A TDR system has four standard components. These components and associated

functions are as follows (Nissen and Moldrup, 1995): (1) a pulse generator that produces

a wave pulse; (2) a sampling head(s) which consist of a timing device and a voltmeter to

measure voltage between shield and inner/outer conductors with time in order to detect

the waves; (3) a coaxial cable that connects pulse generator and sampler; and an (4)

oscilloscope which produces a trace showing measurements of travel time and reflected

voltage.

These components can be purchased separately or as an "all-in-one" (inclusive) unit

through vendors such as Tektronix and Hewlett-Packard. After the initial equipment

purchase for a standard TDR setup, coaxial cables are the only continuing expense

throughout the life of the equipment (at approximately $1.05/meter).

 30

The Tektronix 1502C/4 TDR measuring unit, which is an inclusive unit with strip

chart printout capability, was used for this test. A Belden 8237 RG-8 coaxial cable was

chosen for the project from several cables that were tested for durability and

compatibility. The details of the test and the results are located in Appendix G.
 31

* ~ Meatl a
Reference Junction Curent Folw Measunrig Junction
—• Meatl b
(A): T>T
M R

FIGURE 3.4(A): "SEEBECK EFFECT"

FIGURE 3.4(B): STANDARD THERMOCOUPLE CONFG I URATO
IN
 32

3.5 Summary

The laboratory equipment used in the plasma magmavication experiments, excluding

the plasma torch system, were basic components that can be modified or excluded if

necessary. The chambers used during these experiments were constructed to facilitate

easy placement and removal of the soil and other materials. However, different

diameters and shapes (prismatic) can also be constructed, depending on the objective of

the test. Standard K-type thermocouples were used to instrument kaolin deposits in the

chambers, but other types of thermocouples or different types of instrumentation (TDR)

can also be used. This section should be viewed as a guideline for the types of equipment

that can be used for plasma magmavication experiments, not a standard. Table 3.1 shows

the experiments done for this research effort.

TABLE 3 . 1 : E Q U I P M E N T USED F O R E X P E R I M E N T S
T E S T T O R C H S Y S T E M C H A M B E R S I Z E U S E D I N S T R U M E N T A T I O N

JDC-1 100-kW 0.6-m diameter Thermocouples

JDC-2 100-kW 0.6-m diameter Thermocouples
JDC-3 100-kW 0.6-m diameter Thermocouples
JDC-4 100-kW 0.6-m diameter Thermocouples
JDC-5 100-kW 0.6-m diameter Thermocouples
JDC-6 200-kW 0.9-m diameter Thermocouples
JDC-7 100-kW 0.6-m diameter Thermocouples
JDC-8 100-kW 0.6-m diameter TDR
JDC-9 100-kW 0.6-m diameter Thermocouples
 33

CHAPTER IV

PROPERTIES AND PREPARATION OF GEOMATERIAL

Laboratory chamber deposits of kaolinitic clay were used in this research program.

This chapter serves to outline the origin and properties of the kaolin used throughout the

research, and to describe the general procedures used to prepare the kaolin for placement

into the chambers prior to the magmavication process.

4.1 Geology of Source Area

Kaolin is a product of intensely chemically-weathered feldspar and is widely used in

the manufacturing industries of paper, porcelain, paint, and pharmaceutical items (Holtz

and Kovacs, 1981). Kaolin has many industrial uses and these depend on its index

properties, viscosity, color, and other specific characteristics. "Soft" kaolins are used for

magazine coatings and filler for paper, paints, and cosmetics, and in the manufacture of

plastics, rubber, ceramics, and china tableware. "Hard" kaolins are used for firebrick,

cement, and mortar. It can be used to replace bauxite as a raw source for the production

of aluminum.

The soil chosen for the project was processed kaolin that was mined from eastern
 34

central Georgia. This area has the most extensive commercial deposits of kaolin in the

world. High-grade kaolins are usually mined to a depth of about 90 m before becoming

too deep to extract economically (Husted et al., 1978).

The kaolin of eastern central Georgia comes from the Tuscaloosa Formation of the

Upper Cretaceous Epoch (ended 65 million years ago). The thickness of this formation

varies from 46 to 244 m, however, most of the commercially-viable kaolin is found at the

top of the layer (about 60 m below the ground surface). The overlying layers are deposits

from the Eocene Epoch (ended 55 million years ago) and consist of sand, clay, marl, and

limestone deposited from a shallow marine sea (Husted et al., 1978).

The particular batches of kaolin used in these experiments were obtained from the

Thiele Kaolin Company, which has mining operations in Washington County near

Sandersville, Georgia. The shaded region in Figure 4.1 is the major area of mining

activity for kaolin in Georgia, and an indication of the approximate location of Thiele's

mining activity is also shown.

4.2 Formation and Structure of Kaolinite

Due to the nature of the research project, the use of processed kaolin was selected to

ensure a steady supply of uniform soil for the tests. Another advantage was that the use

of processed soil minimized the inclusion of external contaminants in the tests. This

could have affected the post-test analyses. In this section, kaolin will refer to the soil and

kaolinite will refer to the mineralogy of the soil.

 35

The kaolin used for the research melts at approximately 173 5°C (Thiele Material

Safety Data Sheet). The stoichiometry of the chemical metamorphosis (when T < 350°C;

pressure = 1 kbar) from parent rock to kaolin is as follows (Krauskopf and Bird, 1995):

+
3KAlSi O +2H
3 i o KAl (AlSi,O )(OH)
2 ]0 2 + 6Si0 2 + 2K\
K-feldspar muscovite quartz

+ +
2KAI (AlSi 0 )(OH) +2H
2 3 ]() 1 + 3H 0
2 o 3Al Si O (OH)
2 2 s 4 +2K .
muscovite kaolinite

Figure 4.2 is a phase diagram representing the possible processes in which feldspar

may be formed or altered in geologic systems (Krauskopf and Bird, 1995). The figure

shows the predicted phase relationships as a function of temperature and ratio of

concentrations of potassium chloride (KC1) to hydrochloric acid (HC1) in solution.

Kaolinite is formed at temperatures below or equal to 275°C if the percentages of metal

oxides are low or absent, and is independent of HCI concentrations (Krauskopf and Bird,

1995). The breakdown of the oxides in the kaolin used for the project is in Table 4.1.

The kaolinite crystalline structure consists of alternating layers of tetrahedral silica

sheets and octahedral alumina (or gibbsite) sheets. The basic layer unit consists of one of

each sheet, making it a "two-layer" mineral (or "1:1" clay mineral) with H-bonding

between the layer units. Hydrogen bonds are very strong and discourage hydration, thus

greatly reducing swell potential (Holtz and Kovacs, 1981). Figure 4.3 is a symbolic

representation of the mineral structure. Due to the nature of the research conducted in
FIGURE 4.1: DISTRIBUTION OF KAOLIN MINES IN GEORGIA
(SHRUM, 1970)
Temperature 600
°C

FIGURE 4.2: EXPERIMENTAL (SYMBOLS: O ) AND PREDICTED

(CURVES) PHASE RELATIONS AMONG K-FELDSPAR, MUSCOVITE,
PYROPHYLLITE, AND KAOLINITE (KRAUSKOPF AND BIRD, 1995)
Note: WKCI - concentration of potassium chloride
=
WHCI concentration of hydrochloric acid
F I G U R E 4.3: S Y M B O L I C S T R U C T U R E O F K A O L I N I T E
( M I T C H E L L , 1993)
 39

this program, verification of the mineralogy by an x-ray diffraction test was performed to

ensure homogeneity of the soil. Materials with consistent or repeating patterns of crystal

structure diffract x-rays in a singular way. The pattern of diffracted x-rays is indicative

of the structure of the material. The test performed revealed the diffraction pattern

characteristic to kaolinite (Weaver, 1989) and without foreign compounds. The x-ray

diffraction results are in Appendix C.

4.3 Grain Size Distribution

Particle gradation sizes are an important characteristic of soils. It is essential to

determine the grain size distribution (GSD) for classification and behavior purposes. The

GSD is used in conjunction with ASTM-approved classification systems (Unified or

AASHTO) to classify soils. Three methods were used to determine the grain sizes

present in the soil. The amount of particles by weight that are less than 2 ftm, otherwise

known as the clay fraction (CF), were determined by the various methods and are

presented in Table 4.2.

4.3.1 Hydrometer

All of the soil passed through a #200 sieve (opening = 0.075 mm), therefore,

hydrometer tests (ASTM D 422) were performed. This test is the traditional test used to

determine the gradation of the soil with silt and clay size particles.

For the first test, the large amount of particles within the micron range (< 0.001 mm)
 40

resulted in many inaccuracies. This could have been due to disturbance to the

hydrometer setup, particle disturbance due to insertion of the hydrometer for readings, or

Brownian motion. Two additional hydrometer tests were performed on decreased kaolin

concentrations in order to get more reasonable results, but these tests proved

unsuccessful. Therefore, it was concluded that the concentration of the

kaolin/water/dispersant solution would have to be much lower than the ASTM standard

indicates in order for the hydrometer test to be effective on this soil. This invalidates the

ASTM guideline, and so the hydrometer results are not reported. Likewise, the

calculated clay fraction was greater than 100%, and was considered erroneous.

Consequently, two alternate particle-size methods were then used: laser light

scattering (LLS) and scanning electron microscopy (SEM). A dispersant (sodium

hexametaphosphate) was added to a dilute suspension of kaolin in water, which was then

allowed to stand for at least 24 hours. The solution was then mechanically-agitated and

tested.

4.3.2 Laser Light-Scattering

The LLS technique is a technique that can determine particles that are micron-sized

or smaller. A dilute dispersion is forced through a cell made of two small panes of glass

pressed together. As the particles travel through the cell, a laser projects a light beam

through the cell. An optical detector array, located on the other side of the cell, measures

the angle and amount of light scattered by the particles. This information is used to

determine the average sizes of the particles in the stream. The size distribution of the
 41
particles in the suspension stream is plotted as a histogram, and the integration of the

histogram is the grain size distribution. The histogram also indicates the bimodal

distribution typical of clays. The peaks at 0.9 urn and 6 jam indicate individual particle

sizes and aggregated particle sizes, respectively. Kaolinite tends to form layers or

"booklets" of particles, and these booklets in turn act as single particles. The Georgia

Tech Research Institute Materials Analysis Center (GTRI-MAC) performed the test on a

Microtrac XI00 instrument, which can measure sizes from 0.12 to 704 urn

The instrument calculates the mean number diameter, m , the mean particle diameter
n

calculated from the number versus diameter distribution (number frequency distribution).

The light scattering technique determined the kaolin particle sizes to be in a range 48 um

to 0.32 [xm, with m = 0.621 f^m. The grain size distribution is shown in Figure 4.4,
n

4.3.3 Scanning Electron Microscopy

A scanning electron microscope is one in which a beam of focused electrons moves

across an object. The object produces secondary electrons and also scatters electrons

from the beam. These electrons are collected to form a 3-D image of the object on a

cathode-ray tube. The GTRI-MAC performed this test on a Hitachi S4100 high

resolution field emission scanning electron microscope.

The SEM measured the dimensions of a particle between crosshairs that are

manually placed by the machine operator. Figure 4.5 is a SEM photo showing individual

and aggregated kaolin particles. The scale on the photo was used to measure the
 42

diameters of the other particles in the picture (it was assumed that the sample was

representative) to determine the clay fraction. "*X" and "*Y" are the x-coordinates and

M
the y-coordinates, respectively, of the particle between the crosshairs. *D" indicates the

diameter (diagonal) of the particle between the crosshairs.

4.3.4 Discussion

The processed kaolin was considered homogenous in mineralogy and particle size,

but the range of particle sizes determined by the LLS and SEM techniques reflected the

strong attractive Van der Waals forces between individual particles.

When soils contain a significant amount of particles that are micron-sized and

smaller (clays and colloids), electromagnetic forces dominate the behavior and properties

of the soil. One such force, Van der Waals, is an attractive force that causes particles to

move towards one another and flocculate. A distinction must be made between

intermolecular and interparticle Van der Waals forces. Intermolecular Van der Waals

forces are weak bonding forces, while interparticle Van der Waals forces are quite strong.

Flocculation forms larger particles, which if the orientation of the particles is face-to-

face, are called aggregates. Aggregates have a smaller specific surface area than an

individual clay particle because specific surface area is inversely proportional to grain

size. An increase in the ratio of larger particles to smaller particles will alter the overall

behavior (swelling, shrinking, plasticity) of a clay significantly. Flocculation can be

promoted by means such as polymer additions, and altering the liquid suspension

concentration and/or pH.

 43

The clay fraction obtained from the SEM was most compatible with the percentage

reported in the Thiele Material Safety Data Sheet. Therefore, calculations performed

with the clay fraction were done with the value obtained from the SEM image.
 44

FIGURE 4.4: GRAIN SIZE DISTRIBUTION OF PROCESSED KAOLIN BY

THE LASER LIGHT-SCATTERING TECHNIQUE
 A- ^
„,«•*»
- - - -<* "-

1i 5. 0k V

F I G U R E 4.5: S C A N N I N G E L E C T R O N MICROSCOPY
IMAGE OF KAOLIN PARTICLES

* X is t h e d i m e n s i o n i n t h e x - d i r e c t i o n : 1.125 u n i
* Y is t h e d i m e n s i o n i n t h e y - d i r e c t i o n : 1 . 2 8 0 j i m
* D is t h e d i a g o n a l ( d i a m e t e r ) : 1.704 ujn
 46

TABLE 4.1: BREAKDOWN OF OXIDES IN PROCESSED KAOLIN

O X I D E P E R C E N T A G E P R E S E N T I N

K A O L I N

A1 0 2 3
37.4
Si0 2
44.6
P 0 2 5 0.07
K 0 2
0.21
Ti0 2
1.91
Fe 0 2 3
0.98
S0 3
0.03
Na 0 2 0.11

TABLE 4.2: CLAY FRACTION DETERMINED BY

PARTICLE MEASUREMENT TECHNIQUES

P A R T I C L E M E A S U R E M E N T T E C H N I Q U E C L A Y F R A C T I O N , C F

HYDROMETER *See note

LASER LIGHT-SCATTERING 30%

SCANNING ELECTRON MICROSCOPY * 65%

VALUE REPORTED IN THIELE MSDS 85%

*Note: Hydrometer tests resulted in unreasonable values for CF (above 100%)

 47

4.4 I n d e x Properties

The grain size distribution is used together with the Atterberg limits (ASTM D 4318)

to classify soils according to the Unified Soil Classification System (USCS) per ASTM D

2487 and 2488. The Atterberg limits are water contents at critical stages in soil behavior

(Holtz and Kovacs, 1981). They are unique to each soil, although generalized ranges are

reported for overall soil types (clays, silts, sands). For geotechnical engineering

purposes, the liquid limit, plastic limit, and plasticity index are reported. The liquid limit

(LL) is defined as the lowest water content in which a soil will behave fluidly. The

plastic limit (PL) is defined as the lowest water content in which a soil will act as a solid.

The plasticity index (PI) is the difference between the LL and the PL, and denotes the

range of water contents in which a soil behaves as a plastic material. The results of the

Atterberg tests on 3 batches of kaolin are summarized in Table 4.3. For 2 batches, the

conventional Casagrande cup method was used to obtain the liquid limit. A fall cone

device was used for the third batch to determine the liquid limit (BS 1377), the results of

which are also in Table 4.3. For comparison, typical values for kaolin compiled by

Lambe and Whitman (1969) are listed in Table 4.4.

According to the Casagrande classification chart, the soil was classified as MH (high

plasticity clayey silt). Natural kaolin typically falls into the CL or CH range, but the

results determined for this indicate siltier composition. This compares well with the laser

light-scattering results seen in Figure 4.4 (70% silt-sized particles, 30% clay-sized

particles). The processing of natural kaolin removes the sand generally found in the soil,
 48

and thus plasticity is increased for the processed soil. The result is a slightly different

classification of the soil (from low/high plasticity clay to high plasticity silt). However, it

must noted that the classification systems for soil (USCS, AASHTO, etc) are not

faultless. In addition, the Atterberg limit test methods have inherent shortcomings.

Additionally, the nature of kaolin to form into stacked "booklets" of particles serves to

increase the effective particle size and behavior. Kaolin may act more closely to a silt

rather than a clay. The Casagrande classification chart with the processed and natural

kaolin data points plotted is shown on Figure 4.6.

The specific gravity, G , was determined according to ASTM D 854 and found to be
s

G = 2.55.
s Although the calculated value is slightly lower than the range of typical

values, it is very close to the reported value of 2.60 stated in the Thiele Material Safety

Data Sheet.

4.5 A c t i v i t y

Kaolinite is the largest-sized clay mineral in the family of clay minerals

(montmorillonite, illite, halloysite, attapulgite, chlorite, and kaolinite). Therefore, it has

the smallest specific surface and is the least "active" of the clay minerals. Activity can be

interpreted as the tendency of a mineral to gain and lose water (which leads to swelling,

shrinking, settlement, etc). The more active a mineral, the more variable its behavior

may be.
 49

The equation used to determine activity is taken from Skempton (1953):

Plasticity Index (PI)

Clay Fraction (CF)

The average activity of the kaolin was determined to be 0.5. The range of typical values

for activity of kaolin is from 0.3 to 0.5 (Holtz and Kovacs, 1981) which includes the

determined value.

TABLE 4.3: INDEX PROPETIES OF PROCESSED KAOLIN

BATCH TEST LL PL PI CF, Activity, A G s

# DATE %

68 \
Batch 1 3/12/98 (ASTM 39 29 65 0.45 2.55
D4318)
78
Batch 2 3/12/98 39 39 65 0.6 2.55
(BS 1377)
72
Batch 3 6/21/98 (ASTM 38 34 65 0.52 2.55
D4318)

TABLE 4.4: RANGE OF KAOLIN CHARACTERISTICS

(LAMBE AND WHITMAN, 1969)
LIQUID PLASTIC PLASTICITY SPECIFIC
ACTIVITY
LIMIT LIMIT INDEX GRAVITY, G 8

2.61 - 2 . 6 2 ±
3 0 - 110 25-40 25-29 0.3-0.5
0.02
 50

60 -

•
U-Llne'.
50 -
A-Line-.,*'
40 - rH .--'^ Bacth 2
/ OHoC
Plasticity 1Index

: /
.--* X Bacth 3
30 -

: B
Neaautvrearl(19k9a5o)nil Ny X Bacth 1 OHoM rH
20 - •
OL or CL
10 -

[ y' CL
M
- L . OL or M L
0
0 10 M L ,
30 30
(

40 50 60 70 80 90 100

i y< Lqiudi Lm
i * 1

i ti
FIGURE 4 . 6 : CASAGRANDE CHART SHOWING NATURAL
AND PROCESSED KAOLIN POINTS

CL: Low plasticity clay

ML: Low plasticity silt
OL: Low plasticity organic silts or clays
CH: High plasticity clay
MH: High plasticity silt
OH: High plasticity organic silts or clays
 51

4,6 G e n e r a l K a o l i n P r e p a r a t i o n

The dry processed kaolin was purchased from Davens Ceramic Center located in

Atlanta, Georgia in pre-packaged 22.6-kg bags at a price of $9.00/bag. The preparation

and storage of the soil was in non-reactive plastic barrels. A barrel was placed on a scale

and the weight noted. One bag was then emptied into the barrel and the weight recorded.

Proportioned water was then added to reach the target moisture content, and the soil was

mixed for about five minutes. This process was repeated until the barrel was filled. The

final weight was recorded then the barrel was placed on a pallet and covered tightly with

plastic wrap to prevent water loss. Another barrel was placed on the scale and entire

process repeated until the desired weight of mixed soil was attained. The kaolin was then

left to hydrate in the barrels for approximately 36 to 48 hours.

The moisture content (w) is calculated as follows:

W d g h t
, = water
W e i
S soil
h t ( }

For the first control test, the moisture content was 6 2 % . However, it was later decided to

lower the moisture content to between 40% and 50% for the remainder of the tests.
 52

4.7 C h a m b e r Deposit Preparation

The general procedure discussed herein was used for both chamber sizes. The

chamber halves were bolted together and the joints were sealed with silicone-based

sealant. The chamber bottom was then lined with 5-cm thick ceramic insulating material.

A layer of kaolin was first placed in a 23-cm thick layer, and then was compacted to

a 15-cm thickness. Compaction was done by dropping a 5.4-kg weight from a 30-cm

height (relative to the top of the soil layer). This amounted to one "blow", for a total of

3
50 blows per layer. The calculated compactive effort was 8424 N-m/in per layer. The

average dry density achieved was about 70% of the standard maximum dry density

3
(ASTM D 698). The overall value of dry unit weight (yo) was 10 kN/m . The initial void

ratio was 1.49. Table 4.5 is a summary of parameters for each deposit made for the

experiments prior to plasma magmavication.

The stovepipe was then placed in the center of the first layer, and soil placed around

it to the same initial height. The soil was then compacted to the same final height in the

same manner as before. The stovepipe was readjusted (if needed) to maintain its

position. The filling and compaction process was continued until the chamber was filled.

Six compacted kaolin layers were placed for each completed deposit in the steel

chambers.

The set of thermocouples were then inserted into the kaolin deposit through pre­

existing holes located on one side of the steel chamber. The location of the thermocouple

ports are illustrated in Figure 4.7 and were constant for both chamber sizes. After
 53

insertion, the ports were sealed completely with ceramic caulk. The TDR cable

placement, used in test JDC-8, is discussed in Appendix G.

The preparation of kaolin deposits for tests that used surrogate contaminants was

similar to the aforementioned process. The contaminant layout within the deposit will be

discussed in Chapter V.

In order to obtain kaolin samples for the laboratory tests, thin-walled shelby tube

samples (ASTM D 1587) were taken from a smaller deposit prepared in another

container. The kaolin was prepared and allowed to hydrate in the manner described in

section 4.6. It was then placed in a plastic non-reactive barrel with dimensions similar to

the 0.6-m diameter steel chamber. The first layer was placed to a 20-cm thickness and

compacted to a height of 15 cm in the manner described in section 4.7. A second layer

was prepared and compacted as the first. The shelby tubes were cut as approximate 18-

cm sections from a longer tube. For each tube, one end was ground to a cutting edge, and

the other was ground to remove rough edges and metal burrs. A drive hammer was used

to insert the tubes into the deposit. The tubes were dug out of the deposit, mechanically

extruded, and prepared for oedometer, resonant column, and triaxial tests according to the

respective ASTM guidelines. Results for these tests are reported later in Chapter VIII.
 54

4.8 Synopsis

Kaolin is the product of intense chemical weathering, and is primarily mined in

Georgia in an expanse stretching along the fall line. The processed kaolin used for this

research was tested to determine its engineering properties according to ASTM

guidelines and other test methods. The preparation of the soil and its subsequent

placement in the chambers was meant as a guideline and the methodology can be

modified as necessary.

TABLE 4.5: PARAMETERS OF KAOLIN DEPOSITS PREPARED

FOR TESTS JDC-1 THROUGH JDC-9

TEST w, % YT, k N / m 3
Yi>> k N / m 3
Void ratio, e

JDC-1 50 14.3 9.54 1.62

JDC-2 40 14.1 10.1 1.48
JDC-3 40 12.0 8.54 1.93
JDC-4 40 16.1 11.5 1.17
JDC-5 50 14.7 9.80 1.55
JDC-6 50 13.8 9.22 1.71
JDC-7 50 14.2 9.44 1.65
JDC-8 40 13.0 9.25 1.70
JDC-9 40 15.1 10.8 132
9 0 c m

7 6 cm

6 1 c m !

X " 4 $ c m

3d c m

0 . 3 0 m o r 0 . 4 5 m
*Note: Thermocouple
( d e p e n d i n g o n t h e
port diameters are 12 mm
c h a m b e r u s e d )

FIGURE 4 . 7 : THERMOCOUPLE INSERTION PORTS

(DRAWING IS NOT TO SCALE)
 56

CHAPTER V

SURROGATE MATERIAL PREPARATION AND PLACEMENT

Clay deposits were intentionally contaminated with different nuclear, chemical, and

biological materials to investigate the remediation capabilities of non-transferred arc

plasma technology. This section provides an overview of the rationale and purpose of

using surrogate materials, preparation of the materials prior to placement in the kaolin

deposits, and the general layout of the surrogate materials within the prepared kaolin

deposits. A total of six tests on kaolin deposits seeded with surrogate contaminants were

performed. Table 5.1 is a summary of the tests.

5.1 Surrogate Contaminant Materials

A portion of the research was funded by the Defense Special Weapons Agency

(DSWA) in order to determine the effectiveness of magmavication on contaminated soil

and stored hazardous wastes located at military installations. Full disclosure of the exact

contaminants was not feasible for national security reasons; therefore, surrogate

contaminants were used in the research program.

A surrogate contaminant is a material that has a similar range of physical, chemical,

and thermodynamic properties as a contaminant that may be found at a particular site.

According to EPA regulations, the surrogate materials must be chemically similar to the
 57

mixed waste and represent the hazardous constituents in the waste mixture (EPA/NRC

Mixed Waste Testing Guide, 1997). In general, surrogate materials are less hazardous to

handle and allow a measure of protection against accidental exposure. This is not to say

that the substances are completely harmless, but they can be more easily obtained,

handled, mixed, tested, and neutralized in a controlled and properly equipped laboratory

environment.

The research required contamination of the kaolin deposits with nuclear, chemical,

and biological surrogates. Nuclear surrogate contaminants included zirconium oxide

(ZrC>2) and cesium chloride (CsCl). Chemical surrogate contaminants were malathion (an

organophosphorus pesticide) and 2-chloroethyl methyl sulfide. Biological surrogate

contaminants were LE392 E. coli bacteria and YPH80 S. cerevisiae yeast strain.

The research was a joint effort of Georgia Tech Research Institute (GTRI) and Clark

Atlanta University (CAU) made possible through funding from the Defense Special

Weapons Agency. The main role of GTRI was experiment setup, non-chemical material

preparation, physical data and torch data collection and interpretation, and pre-treatment

and post-treatment characterization of the material. CAU was responsible for the

contaminant preparation, the off-gas system sampling and analysis, and the chemical

analyses of the post-test material. Dr. Louis Circeo (GTRI), Dr. Eric Mintz (CAU), and

Mr. Bob Newsom (GTRI) selected the surrogate materials for the research project. Ex-

situ tests using the plasma torch were also performed in a specially designed enclosed

furnace. The results will be discussed in the GTRI-CAU report presented to the Defense

Special Weapons Agency.

 58

TABLE 5.1: EXPERIMENTS PERFORMED USING SURROGATE

CONTAMINANTS
T E S T C O N T A M I N A N T S C H A M B E R U S E D T O R C H

S Y S T E M

JDC-l None (Control) 0.6-m diameter 100-kW

JDC-2 Nuclear surrogates: CsCl and Z r 0 2 0.6-m diameter 100-kW
JDC-3 Chemical surrogates: malathion 0.6-m diameter 100-kW
(CioHigO^PSi) & 2-chloroethyl
methyl sulfide ( C 3 H 7 C I S )

JDC-4 Biological surrogates: LE392 e. coli 0.6-m diameter 100-kW

& YPH80 S.cerevisiae yeast
JDC-5 Mixed: nuclear, chemical and 0.6-m diameter 100-kW
biological surrogates
JDC-6 Mixed: nuclear, chemical and 0.9-m diameter 200-kW
biological surrogates

5.2 Preparation of Surrogate Materials

Clark Atlanta University prepared the surrogate materials for placement in the kaolin

deposit. The contaminants were first mixed and placed in small vials that were in turn

arranged into steel cans. The vials were made of glass and were about 8-cm in length and

2-cm in diameter with a screw-on top. The sequence of the contaminant preparation is

shown in Figure 5.1. The can is about 19-cm long and 8-cm in diameter with a screw-on

cap. A picture of a can is shown in Figure 5.2. The cans were pre-filled with kaolin and

water prior to vial insertion. They were then sealed and transported to Georgia Tech for

placement in the kaolin deposits during their construction prior to the magmavication

process.
 59

Georgia Tech did not assist in the contaminant preparations, however the procedures

for each type of surrogate contaminant will be discussed in the following sections for

general understanding.

5.2.1 Nuclear Surrogate Preparation

The batch of nuclear-surrogate contaminated kaolin was prepared by mixing 300 g of

the dry processed kaolin with 18.0 g each of CsCI and Z r 0 . 2 This mixture was then

equally distributed in fifty-four 50-ml glass vials.

The cans were then filled with 90 g of kaolin and 45 ml of water. This was shaken

vigorously to mix the soil and water. Then 3 or 4 vials were inserted into the can, and

another 50 g of kaolin and 25 ml of water were added. At this time, the can was shaken

gently. More vials were then added and the process repeated until the cans were filled.

A total of twelve cans were made in this manner. The overall concentrations of the

contaminants for the test were: (1) CsCI = 5.08E-03% by weight, ( 2 ) Z r 0 = 5.08E-03%
2

by weight.

5.2.2 Chemical Surrogate Preparation

For chemical-surrogate contaminated batches of kaolin, the malathion and 2-

chloroethyl methyl sulfide were not mixed together prior to placement in the vials. They

were prepared separately and the respective vials were put into the cans.
 60

Sixteen 50-ml vials were each filled with 5.4 g of dry processed kaolin. The 2-

chloroethyl methyl sulfide solution was made by mixing 0.4 ml with 8.0 ml of acetone.

1.0 ml of this solution along with 2.0 ml of water was then added to half of the vials. The

vials were temporarily sealed with parafilm, then cooled and sealed by flame. The

malathion solution was made by adding 1.6 ml of 50% malathion to 16 ml of acetone.

2.0 ml of this solution was then added to each of the remaining vials. The vials were

sealed in the same manner as the previous ones.

Each can was prepared by first adding 50 g of kaolin and 25 ml of water and shaking

vigorously. Then one vial each of the 2-chloroethyl methyl sulfide and malathion

solutions was put into the can. After this, 100 g of kaolin and 50 ml of water were added

and the can was gently shaken. Finally, another 75 g of kaolin and 37 ml of water was

added and the can was sealed. A total of eight cans were prepared in this manner. The

overall concentrations of the contaminants for the test were: (1) malathion (CioHi 0 PS2)
9 6

~ 3.00E-04% by weight, and (2) 2-chloroethyl methyl sulfide ( C 3 H 7 C I S ) = 8.20E-05% by

weight.

5.2.3 Biological Surrogate Preparation

Selected tests were conducted using biological contaminants in kaolin deposits. The

yeast and the bacteria solutions were prepared separately from one another. However,

both were made from organisms grown in saturated media and then resuspended in

culture media. Eight cans were filled with 200 g of dry kaolin. Four of the cans had 100

ml of yeast solution added, and the other four had 100 ml of bacteria solution added. The
 61

cans were sealed and vigorously shaken to mix the contents. The amounts of organisms

per can that were prepared for this test were: (1) LE392 e.coli = 3.00E+11, and (2) S.

cerevisiae strain Y2159 = 8.00E+11.

5.2.4 Mixed Surrogate Preparation

For two of the tests in the program, a combination of all surrogate materials was used

to investigate the effectiveness of plasma magmavication on remediating mixed wastes.

The specific surrogate contaminants used for these two tests were as previously

described.

The nuclear contaminants were made by putting 50 g of dry kaolin, 25 ml of water,

and 2 g each of CsCI and Z r 0 into a can. The chemical contaminants were made in vials
2

as previously stated. Then one vial of each chemical contaminant was added into the can.

Another addition of 175 g of kaolin and 87 ml of water followed this. The cans were

sealed and gently shaken to mix. A total of twelve cans were prepared, four of which

were used in the first mixed waste test, and the others were used in the second mixed

waste test. The biological contaminants were prepared in twelve separate cans as

described in Section 5.2.3. Four were used in the first mixed waste test, and eight were

used in the second mixed waste test. All of the cans were layered within the kaolin

deposit. The concentrations (percent by weight) for JDC-5 were: (1) CsCI = 1.58E-03%,

(2) Z r 0 = 1.58E-03%, (3) C i H i O P S = 1.30E-04%, (4)

2 0 9 6 2 C 3 H 7 C I S = 3.55E-05%. The

biological contaminant amounts per can for JDC-5 were: (1) LE392 e.coli = 3.00E+11,

and (2) S. cerevisiae strain Y2159 = 8.00E+11. For JDC-6, which utilized a larger
 62
chamber and higher capacity plasma torch, the concentrations (percent by weight) were:

(1) CsCl = 1.58E-03%, (2) 2 r 0 2 = 1.58E-03%, (3) CioH 1 9 0 PS2

6 = 1.30E-04%, (4)

C 3 H 7 C I S = 3.55E-05%. The biological contaminant amounts per can for JDC-5 were: (1)

LE392 exoli = 6.00E+11, and (2) S. cerevisiae strain Y2159 = 1.60E+12.

5.3 Placement of Contaminants in Kaolin Deposit

The preparation of the kaolin prior to placement within the chambers was previously

described in Chapter IV. The control tests with kaolin clay contained no cans. Tests that

required the seeding of the kaolin deposit with contaminants were prepared in the fashion

discussed herein. In general, any variation of the can layout was done to accommodate

the amount of cans, and to ensure that the contaminants were at least 4 cm from the

borehole for complete treatment.

For each test involving contaminants, three levels of cans were positioned within the

middle layers of the kaolin deposits. Four cans were placed on top of a compacted layer

of soil. The next layer of kaolin was then placed and compacted over the cans. Four

more cans would be laid out, and the procedure continued until all the cans were inserted

into the kaolin deposit. The rest of the deposit was completed in the normal fashion, and

the chamber instrumented. A layer of silicone-based sealant would be placed on the

chamber rim, and the off-gas hood put in place and bolted down. The joint between the

hood and the chamber would then be resealed for redundancy, A specific layout of the

cans for a representative test is illustrated in Appendix A. Figure 5.3 is an illustration of

 65.

Contaminants are
mixed as prescribed
in Section 5.2 I

Contaminants are
placed in glass vials

Vials are placed in cans that

contain kaolin and water. Cans
are sealed and ready for
placement into chamber deposit.

FIGURE 5.1: SEQUENCE OF CONTAMINANT PREPARATION

PRIOR TO PLACEMENT IN KAOLIN DEPOSIT
F I G U R E 5.2: S T E E L C A N F O R C O N T A I N M E N T OF
SURROGATE CONTAMINANTS
 65

a general layout scheme, and Figure 5.4 shows a general vertical and horizontal

orientation of the cans.

The general procedure for preparation of the contaminants and the placement of the

contaminants within the kaolin deposits has been explained. This section is meant to be a

description and the procedure can be modified to fit the needs of the research. If the

contaminants are to be freely introduced into the soil rather than enclosed within a

container, then these procedures are not recommended as guidelines. At all times, proper

safety equipment such as protective clothing, ventilating masks, or even fume hoods

should be employed if the material safety data sheets (MSDS) on the compounds or

biological agents being used specify these precautions.

F I G U R E 5.3: ILLUSTRATION OF GENERAL CAN LAYOUT
(DRAWING NOT TO SCALE)
 F I G U R E 5.4: P H O T O G R A P H S O F V E R T I C A L A N D
HORIZONTAL LAYOUT OF CANS DURING PLACEMENT
 68

CHAPTER VI

PROCEDURES FOR SOIL MAGMAVICATION

The research into the remediation capabilities of the non-transferred (NT) arc plasma

torch was a joint effort between Georgia Tech Research Institute (GTRI) and Clark

Atlanta University (CAU). Magmavication was accomplished using an NT arc plasma

torch centered in a soil deposit. This chapter describes the common procedures used by

GTRI for torch initialization, operation, and termination, and for dissection of the

remaining kaolin and igneous rock mass from the steel chamber after testing.

The off-gas sampling was performed by CAU during the tests. The specific

procedure is described in the GTRI-CAU report to be presented to the Defense Special

Weapons Agency. The Environmental Protection Agency (EPA) guidelines specifying

equipment, sample collection, and sample testing procedures are EPA SW-846 Method

0010, and EPA SW-846 Method 0030. These documents can be obtained through the

EPA website (http://www.epa.gov).

 69

6.1 Plasma T o r c h System I n i t i a t i o n and T e r m i n a t i o n Process

The procedures for both torch systems are the same, but the 200-kW torch system is

fully-automated, so the steps following torch ignition pertain only to the 100-kW torch

system that was manually-operated. GTRI performed the following steps for torch

operation:

The torch cooling water manifold was opened and the water pump activated.

The water pressure was set at 1930 kPa and water circulated through the steel jacket

to cool the torch and electrodes while in operation.

The air compressor was then started to supply the ionizing gas for plasma creation, (a

minimum air pressure of 55 kPa is needed in order to start a plasma column)

The power supply was turned on.

A trigger was initiated and the torch was ignited.

The power is initially raised to 50% capacity while the air pressure is steadily

increased. The power is raised to 100% capacity once the air pressure exceeds 140

kPa. The air pressure is varied throughout the test between 175 kPa and 380 kPa in

order to rotate the plasma column around the electrodes for more uniform wear of the

electrodes. This helps to extend the life of the electrodes.

After the magmavication process has been completed, the above procedure is

reversed to turn off the torch system (lower air pressure and power, turn off power,

turn off air compressor, turn off water pump).

 70

6.2 Genera] Torch Operations

The torch was normally started at a 15-cm height from the bottom of the borehole

(30-cm height from the bottom of the chamber) for the 100-kW system. The torch was

lifted in increments of 8 cm every 15 minutes for the majority of the tests for an average

overall withdrawal rate of 0.53 cm/min. For the kaolin deposit that was seeded with

mixed wastes, the torch was lifted 8 cm every 20 minutes, corresponding to an average

overall withdrawal rate of 0.40 cm/min. This was done to ensure that the contaminants

were fully incorporated into the magma and treated. The exposure time and torch

withdrawal heights were chosen based on experience from previous plasma research

involving fine-grained soils (clays). The details of the total torch withdrawal and test

times for each test are in Appendix A.

The 200-kW system was started at a 23-cm height (3 8-cm height from bottom of the

chamber). The torch was also lifted in increments of 8 cm, but the time between

increments varied between 20 to 45 minutes. This was done to ensure that all the

contaminants were treated. Specific details of the test are in Appendix A.

Amperage, voltage, and temperature readings were taken every five minutes

throughout the test. Additional readings were taken if anything notable occurred (such as

a thermocouple reaching its maximum temperature and being withdrawn from the

deposit). The off-gas scrubber system was always turned on before the torch was

initialized, but the off-gas sampling generally started after the torch was in operation for

at least 15 minutes. The specific details are in Appendix A.

 71
After the torch was turned off, it was left in the chamber to ensure that gas was not

emitted from the torch access hole to the atmosphere during the cooling period. The

entire setup was left to cool for at least 24 hours. Later, the entire deposit was dissected

to evaluate and sample the igneous rock and residual soil.

6.3 Dissection P r o c e d u r e

The kaolin deposits were allowed to cool a minimum of 24 hours after treatment.

The specific cooling times are discussed in Chapter V I I . The torch and instrumentation

were removed, and the entire chamber was moved outdoors. Figure 6.1 shows the general

dimensions of interest. The following is a brief outline of the dissection process;

The off-gas hood was unbolted and removed.

The remaining stovepipe was removed and discarded. After undergoing moisture

reduction and volume reduction from the magmavication process, some settlement of

the kaolin deposit was seen. This settlement, or subsidence, was measured as the

difference in the height to the top of the chamber from the kaolin deposit before and

after the test.

The chamber halves were then unbolted and separated.

• The kaolin was carefully removed from the exposed side using shovels until the rock

was encountered. A partially-dissected chamber deposit is shown in Figure 6.2.

The exposed cavity dimensions and the distance from the top of the igneous rock to

the top of the kaolin deposit were measured.

The rock was carefully removed from the kaolin, and the dimensions and weight were
 72

noted. All the igneous rocks produced during this research effort appeared to be

symmetrical in shape. An asymmetrical shape might indicate a non-uniform deposit

or misalignment of the plasma torch.

The remainder of the kaolin and the ceramic insulation were removed.

For laboratory testing purposes, the rock was sawed in half with a water-lubricated

saw fitted with a diamond-tipped blade that was located on-site.

Samples for the Toxicity Characteristic Leaching Procedure (TCLP), scanning

electron microscopy (SEM), and the x-ray diffraction (XRD) tests were taken from

the center of the rock and delivered to Clark Atlanta University and the Georgia Tech

Research Institute Material Analysis Center for evaluation.

The torch operation procedures outlined here were standardized for all tests and were

applicable to the specific torch systems used by the Georgia Tech Plasma Applications

Research Facility. The dissection procedures are only specific to this research and should

be modified to suit the research objectives. The contaminants were placed close to the

borehole and thus were assumed to be either incorporated into the magma pool, or

pyrolized by exposure to the extreme temperatures and thus treated. If any concerns

should arise regarding post-test contamination during dissection, precautions should be

taken in accordance with requirements found in the MSDS for the contaminant materials.
 73

F I G U R E 6.1: G E N E R A L D I M E N S I O N S N O T E D F O R P O S T - T E S T
CALCULATIONS AND DOCUMENTATION
FIGURE 6.2: PARTIALLY DISSECTED KAOLIN DEPOSIT
 75

CHAPTER VII

GEOCHEMICAL ANALYSES OF CONTAMINANT REMEDIATION

This chapter discusses the results of the quantitative and qualitative analyses

performed on samples of the igneous rock collected from the in-situ contaminant

remediation experiments JDC-1 to JDC-6.

After each test, the kaolin deposit was allowed to cool and was dissected as detailed

in Chapter VI. The center core rock was removed from the kaolin deposit, measured, and

then weighed. A water-lubricated diamond-tipped saw was then used to cut the rock in

half lengthwise. One half was preserved and the other was manually broken down to

obtain a sample of about 200 g from the center. The details of the sample size will be

described in the following sections.

7.1 Scanning Electron Microscopy and X-Rav Diffraction

Scanning electron microscopy (SEM), previously employed to determine the particle

sizes of the soil in Chapter IV, was also used for quantitative elemental analyses of

samples obtained from the center of the igneous rock produced by plasma

magmavication. Electrons are emitted and accelerated from a cathode at 15 kV. When

the electron beam bombards the surface of the object, electrons and x-rays are
 76

produced that are characteristic of the atoms within the specimen (Goodhew and

Humphreys, 1988). The measurement of the wavelengths and intensities of the x-rays

determines the elements present within the sample. A detector collects the secondary

electrons that produce a SEM image like that shown in Chapter IV (Figure 4.5). An

example of a SEM graph is shown in Figure 7.1

For the SEM tests, the nominal diameters of the specimens were between 0.6 and 1.3

cm. The samples were placed on a mounting plate, which was then placed into the

scanning area. The operator had the capability to scan specific areas on the surface of the

specimen to determine its constituents. This allowed the freedom to examine unique

features of heterogeneous samples. For our purposes, three areas on the sample were

analyzed. The specific elemental content was printed out in two forms. One form was a

graphical representation of intensity (related to concentration) on the y-axis and kilovolts

(specific to wavelength and thus to the individual elements) on the x-axis. The other

output form was a quantitative analysis of the percentage of each constituent relative to

the entire sample.

Qualitative analyses using x-ray diffraction (XRD) was performed to detect

crystallized structures within the samples obtained from the center of the rock. X-rays

from the source (a copper-target tube) bombard the sample. The scattering of the x-rays

by the atoms of a crystal produces an interference effect. The result is a unique

diffraction pattern that gives information on the structure of the crystal from which the

identity of the crystalline substance is determined.

For the XRD tests using a powdered specimen, rock samples were manually crushed
 77

using a mortar and pestle into particles that passed a #400 sieve (38-(im opening). The

crushing of specimens can also be done with a ball mill. The powder was then smeared

onto a small slide. The slide was placed on the mounting plate of the instrument, and

testing was performed. The x-rays start angle (start 28) was 10°, and the ending angle

(stop 20) was 70°. The scan speed was 1° per minute, and the sampling interval was 0.2
The results are output as a graph of the x-ray intensity on the y-axis and detector angle on

the x-axis. Narrow sharp peaks at distinct angles on the graph show the presence of a

crystallized species, while glass (non-crystalline) is shown as a wide crest (bump).

Although glass was present in all the XRD analyses, the discussion will focus on the

detection of crystals. Figure 7.2 is an example of the output XRD graph.

Samples were collected and prepared by the author, and the analyses were performed

at the Georgia Tech Research Institute Materials Analysis Center (GTRI-MAC). Lisa

Detter-Hoskin, a Senior Research Scientist, performed the SEM analyses on a Hitachi

S4100 high resolution field emission scanning electron microscope integrated with a

Noran light element energy dispersive x-ray spectrometer (SEM/EDX). Gautam Patel,

Research Engineer II, performed the XRD analyses on a Rigaku DMAX-B 2kW Unit.

The unit has a computer equipped with IBM software that has a complete library of

organic and inorganic powder diffraction databases (JCPDS database). The JCPDS is the

most comprehensive database of compounds to date. SEM and XRD tests were

performed on samples of the igneous rock from tests JDC-1 to JDC-6, and also from

samples of the powdered processed kaolin. Figure 7.3 shows the major and minor

elements detected and the respective element weight percent for each sample tested.
 78
Figure 7.4 is the same graph as Figure 7.3, with the exception o f oxygen. Figure 7.5

shows the amount of each minor element found in the test samples. The SEM graphs of

the complete data results are to be found in Appendix B. The complete XRD graphs and

results are found in Appendix C.

7.2 Uncontaminated Processed Kaolin

In order to confirm the homogeneity of the processed kaolin used for the

experiments, SEM and XRD analyses were performed on samples of the soil. The SEM

results show the presence of elements typical in kaolin. The major constituents were O,

Al, Si, and the minor constituents were K, Ti, and Fe. The XRD analysis detected

patterns indicative of kaolinite. The results of the SEM and XRD are in Appendix B and

Appendix C, respectively.

The rock resulting from the melted kaolin was expected to contain the same elements

as the kaolin with the exception of ions introduced by the addition of the stovepipe, and

the resulting ionic compounds. Any residue remaining from the inserted contaminants

would show up as different constituents in the SEM and XRD analyses.

7.3 JDC-1: Uncontaminated Test (Control)

The kaolin deposit for experiment JDC-1 was prepared without contaminants. After

75 minutes of treatment with the plasma torch, the process was terminated and the
 79

G e o r g i a T e c h R e s e a r c h I n s t i t u t e D i s p l a y - S p e c t r u n l

VFS: 2400 L i v e t i m e : 90
D e a d t i m e : 34%

Si Y
*

• x
At

ii 1 Fe

T1

•
J 0.000
K
. keV
.
Fe
A

10.220

Cursor: 0 . 0 0 0 keV 0 counts

•
Label: OSWA # 1 0 , Area 3
Element: H 1 P
R
>»
FIGURE 7 . 1 : EXAMPLE OF SEM OUTPUT G R A P H
X-axis is kV (specific to elements)
Y-axis is intensity (related to concentration)
 80

2 0 G U 8 . R A H
ttlV) <CENTER>

4 x
>

v.;
FIGURE 7.2: EXAMPLE O F XRD OUTPUT G R A P H
X-axis is detector angle (in degrees)
Y-axis is x-ray intensity
 81
chamber was allowed to cool for 24 hours. Dissection followed and the resulting weight

and dimensions are shown in Table 7.1.

The results of the SEM analysis on samples taken from the center of the rock show

the presence of O, Si, and Al as the major elements, and Fe, Ti, K and P were found as

minor elements. As was expected, most of the results were the same as for the kaolin soil

sample with the exception of phosphorus. Phosphorus is normally used in detergents and

fertilizers, neither of which was purposely introduced into the soil deposit. Its source is

still unclear.

The XRD analysis detected synthetic mullite as the dominating crystals, along with

some synthetic hercynite (FeAl 04) and synthetic almandine (Fe3Al (Si04)3).
2 2 Synthetic

mullite is one of the two final products of the thermal decomposition of kaolin (Deer,

Howie, and Zussman, 1966), hence its presence is not surprising. The additional iron

ions within the magma came from the stovepipe that was used as a borehole casing. The

formation of hercynite and almandine is normally through metamorphic processes, but

they can be found in basic and ultra-basic igneous rocks. Almandine has been

synthesized from the combination of kaolinite, Fe C>3, S i 0 , and FeCl »4H 0 (Deer,
2 2 2 2

Howie, and Zussman, 1966), which may also explain its presence in the rock.

7.4 JDC-2: Nuclear Surrogate Contaminant Test

The contaminants used in experiment JDC-2 were CsCl and Z r 0 . 2 The kaolin

deposit was prepared as described in Chapters IV and V and Appendix A.

 82

TABLE 7 . 1 : WEIGHTS AND DIMENSIONS OF DISSECTED ROCKS

Test Test YT o f Test Rock Max. Max.
and Objective % Soil, Time, Wt,N Rock Rock lit,
Date kN/m 3
min Piam, cm
cm
JDC-1:
Control 50 14.3 75 236 30.5 30.5
5/6/98
JDC-2: CsCl&
40 14.1 155 529 43.2 40.6
6/4/98 Zr0 2

JDC-3: malathion
7/30/98 &
chloroethyl 40 12.0 140 356 38,1 30.5
methyl
sulfide
JDC-4: LE392 E.
8/6/98 coli
bacteria &
40 16.1 160 360 35.6 35.6
YPH80 S.
cerevisiae
yeast
JDC-5: All
50 14.7 140 285 35.6 38.1
8/26/98 surrogates
JDC-6: All
50 13.8 180 792 47.0 38.1
9/3/98 surrogates
JDC-7:
Control 50 14.2 69 93.4 25.4 22.9
10/16/98
JDC-8:
TDR 40 13.0 45 162 29.2 17.8
11/16/98
JDC-9: Cooling
4/9/99 rate&
40 15.1 41 80.1 25.4 11.4
altered
plasticity
 83
After 155 minutes of treatment with the plasma torch, the torch system was terminated

and the chamber was allowed to cool for 24 hours.

Figure 7.6 shows the amounts of nuclear and chemical surrogate contaminants

placed within the kaolin deposits prior to plasma magmavication. The results of the SEM

analysis on samples taken from the center of the rock show the presence of O, Si, and Al

as the major elements, and minor elements found were Fe, Ti, and K. The XRD results

positively identify synthetic mullite in the rock and show very minor amounts of some

iron-alumina species.

Organic materials pyrolize during magmavication, but most inorganic species do not.

Thus, it was expected that the inorganic contaminant components would remain within

the magma, and during cooling would become a linked species within the glass phase.

This would immobilize the inorganic contaminants until devitrification occurred.

However, in both analyses, neither the contaminant compounds nor their metallic

constituents were detected. The fact that SEM and XRD analysis failed to detect their

presence may be due to the following reasons:

The resolution of the SEM and the XRD instruments may be lower than that needed

to detect the contaminant concentration levels within the rock sample. The XRD is

only capable of determining compounds within a sample as low as 0.5%, with this

being the limiting percentage with a degree of uncertainty. Different analytical

instruments such as ion microprobe or inductively-coupled plasma mass spectrometry

(ICPMS) may rectify this. ICPMS is an instrument capable of detection limits as low

12
as parts per trillion (1 in 10 ) and has multi-element capabilities while the ion
 84

9
microprobe has detection sensitivities down to parts per billion (1 in 10 ). However,

both give elemental analyses and do not tell the compounds present.

. The amounts of contaminants were very small relative to the amounts of other

components in the soil deposit, as shown in Figure 7.6 and discussed in Chapter V.

Consequently, if they had become uniformly dispersed throughout the magma their

concentrations would have been below the detection limit of the instruments. Uneven

distribution throughout the rock, which occurs due to differing specific gravities,

would lower the probability of gathering a sample from an area that contained any

residual pollutants. As a result, the proper sampling size (number of samples) of the

rock becomes a concern.

These concerns do not nullify the findings, but they do bring into question the analysis

methodology and techniques currently employed. A few possibilities of addressing these

issues would be to sample the entire rock, increase the levels of contaminants to insure

that ions of the contaminants could distribute more thoroughly in the rock, or use a more

sensitive analytical technique (ICPMS) to test the rock.

7.5 JDC-3: Chemical S u r r o g a t e C o n t a m i n a n t Test

The contaminants used in test JDC-3 were malathion ( C 1 0 H 1 9 O 6 P S 2 ) and 2-

chloroethyl methyl sulfide ( C 3 H 7 C I S ) . The kaolin deposit was prepared as described in

Chapters IV and V and Appendix A. After 140 minutes of treatment with the plasma

torch, the torch system was terminated and the chamber was allowed to cool for 24 hours.
 85

Dissection of the rock followed and the resulting weight of 356 N and associated

dimensions are shown in Table 7.1.

The SEM results show no traces of any of these contaminant constituents remaining

in the sample obtained from the center of the rock. As shown in Figure 7.6, the

concentrations of the seeded contaminants were low, and thus it may be possible that any

remaining contaminants were not detected due to either the limitations of the instruments

(SEM and XRD), or the lack of adequate sampling. However, the contaminants, being

volatile at temperatures below 300°C, were more likely vaporized, then processed and

treated through the off-gas system. Pyrolysis caused thermal "cracking" (Zumdahl, 1989)

of the bonds between the chemical contaminant components. The resulting free carbon

then formed carbon-based gases that were collected and processed through the off-gas

treatment system.

The XRD results, located in Appendix C, show the presence of synthetic mullite as

the dominating crystal along with some magnesium species as secondary crystals. The

appearance of magnesium within the sample was unexpected since it was neither detected

in the SEM analysis, nor was it introduced into the kaolin deposit intentionally. Its

source can not be traced. Nevertheless, the resulting spinel (MgAbC^) that formed from

it is not a hazardous material and so no additional processing was considered necessary

for remediation.

Previous research performed by Soelberg et al. (1995), Carter and Tsangaris (1995),

Krasnoperov et al. (1995), and Mescavage and Filius (1995) on organic, volatile, and

chemical wastes have shown efficiencies of 99.99% or more using plasma processing.
 86

The low contaminant concentrations used in this research indicate a high processing

efficiency. However, in reality the contaminant concentrations found at treatment sites

may be higher than those tested in this research effort. Nevertheless, these results are

considered significant as a pilot program for future experimentation using higher

concentrations and more toxic chemical wastes.

80 -,

I | Al rjFe

• K HTi

UP

h.
Processed JDC-1 (control) JDC-2 (nuclear) JDC-3 JDC-4 JDC-5 (all) JDC-6 (all
Kaolin (chemical) (biological)

FIGURE 7.3: SEM ANALYSES FOR TESTS JDC-1 TO JDC-6 AND

PROCESSED KAOLIN
O: 65% to 74% Al: 10% to 14% Si: 12% to 17%
Fe: 0.17% to 6% K: 0.06% to 0.18% Ti: 0% to 0.75%
P: 0% to 0.07%
 87

N o t e : O x y g e n i s n o t s h o w n a s It

n
constitutes the largest
p e r c e n t a g e ( > 6 5 % ) in all t e s t s .
• Si DAI

• Fe BK

BTi BP

Processed
Kaolin
JDC-1
(control)
r
• JDC-2
(nuclear)
JDC-3
(chemical)
ii
JDC-4
(biological)
JDC-5 (all) JDC-6 (all)

F I G U R E 7.4: D E T E C T E D E L E M E N T S B Y S E M W I T H
EXCEPTION OF OXYGEN
 88

PK ucCle2-ar) (chJD
roceaosnield JDC1- (contro(nJl)D C3-cia)l (bioJDloCg4-ical)
em JDC5
- (al) JDC6
- (al)
FIGURE 7.5: MINOR ELEMENTS DETECTED BY SEM ANALYSES
 89

6 0E 03 -,

JDC-1 (Control) JD02 (Nuclear) JDC-3 (Chemical) JDC-4 (BidogtcaJ) JDC-5 (All) JDC-6 (All)
Test Number

FIGURE 7.6: NUCLEAR AND CHEMICAL SURROGATE CONTAMINANT

CONCENTRATIONS FOR TESTS
 90

7.6 JDC-4: Biological Surrogate Contaminant Test

The contaminants used test JDC-4 were LE392 E. coli bacteria and YPH80 S.

cerevisiae yeast. The kaolin deposit was prepared as described in Chapters IV and V and

Appendix A. The amounts of the organisms are shown in Figure 7.7. After 160 minutes

of treatment with the plasma torch, the torch system was terminated and the chamber was

allowed to cool for 24 hours. Dissection followed and the resulting weight of 360 N and

the rock dimensions are shown in Table 7.1.

The results of the SEM analysis show the same major and minor elements in the rock

sample as previous tests. This was expected since the contaminating organisms would

not be able to survive in the extreme temperature regimes of the plasma torch and the

magma pool. The XRD results show the presence of synthetic mullite as the dominating

crystal with some minor inclusions of fayalite (Fe Si04) which may have formed due to
2

the iron ions available through the melted stovepipe. Although the organisms were not

detected and are likely destroyed, the detection limitations of the instruments are also a

consideration.

There was the possibility that the organisms may have migrated out from the heated

area into the non-melted soil through water movement or by motility. The insulating

properties of the processed kaolin are very effective in containing the melted soil to

within the immediate treatment zone, and so organisms in areas outside of the melted

region may have survived. To address this issue, polymerase chain reaction (PCR)

analyses were performed and will be reported by Clark Atlanta University in a joint
 91

project with the Georgia Tech Research Institute funded by the Defense Special Weapons

Agency. Additional samples of non-melted soil were gathered in areas from outside of

the rock straight across to the chamber wall, and from splash residue on the plasma torch.

The results of these analyses proved negative in detection of the seeded biological

contaminants and confirmed the destruction of the organisms by plasma magmavication.

1.4E+09 -

JDC-1 (Control) JDC-2 (Nuclear) JDC-3 (Chemical) JDC-4 (Biological) JDC-5 (All) JDC-6 (All)

Test Number
FIGURE 7 . 7 : BIOLOGICAL SURROGATE CONTAMINANT CONCENTRATION
 92

7.7 J D C - 5 : M i x e d W a s t e Surrogate C o n t a m i n a n t Test Using 1 0 0 - k W T o r c h System

The kaolin deposit for experiment JDC-5 was prepared as described in Chapters IV

and V and Appendix A. The surrogate contaminants used in this test were the same as

those used in the JDC-2, JDC-3, and JDC-4 tests. After 140 minutes of treatment with

the plasma torch, the torch system was terminated and the chamber was allowed to cool

for 15 days. After dissection, the resulting weight was found to be 285 N. The rock

dimensions and other parameters are shown in Table 7.1.

The SEM analyses detected the same constituents as in previous tests. However, the

absence of the inorganic contaminants ( Z r 0 and CsCI) once again brings into question
2

the sampling size and area, and the detection limits of the instrument. Despite this, it is

very likely that the inorganic contaminants are within the glass, and so the risk of direct

contamination is essentially eliminated. The SEM results also did not find any of the

chemical contaminants planted in the kaolin deposit, which agreed with the JDC-3 test

results. It is conceivable that the contaminants underwent pyrolysis. As was expected,

the XRD analysis detected synthetic mullite as the major crystal in the rock sample. The

scan also detected a minor presence of synthetic ulvospinel (Fe Ti0 ), but it has no
2 4

unfavorable properties and was not considered a contaminant. Clark Atlanta University

performed a PCR analyses on samples of the rock and the surrounding soil from around

the rock to the chamber wall. The results will be included in a joint GTRI-CAU report.

The PCR analyses confirmed the destruction of the biological contaminants by the

plasma magmavication process. This agreed with the findings of the JDC-4 test results.
 93

7 . 8 JDC-6: Mixed Waste Surrogate Contaminant Test Using 200-kW Torch System

The kaolin deposit for experiment JDC-6 was prepared in the manner described in

Chapters IV, V and Appendix A. The surrogate contaminants used in this test were the

same as those used in the JDC-5 test, and were placed in the 0.9-m diameter steel

chamber. After 180 minutes of treatment with the plasma torch, the torch system was

terminated and the chamber was allowed to cool for 12 days. Dissection followed and

the resulting weight and dimensions are shown in Table 7.1.

The same constituents were detected by SEM analyses as in previous tests, with the

same absence of the inorganic contaminants from the scan. However, the assumption

that the inorganic contaminants are within the glass matrix is still viable. The chemical

contaminants and their components are also missing from the SEM results. This agrees

with the JDC-3 and JDC-5 test results, and the same conclusion can be drawn.

Synthetic mullite was identified by the XRD analysis as the major crystal in the rock.

The PCR analysis performed on rock samples established the destruction of the biological

contaminants by through magmavication. These results are in accord with the findings of

JDC-4 and JDC-5 test results.

Although it seemed that the JDC-6 test was presumably successful in destroying the

organic materials and immobilizing the inorganic materials, there are some concerns that

need to be examined. Upon partial removal of the kaolin from the chamber, it was noted

that the solidified crust of the cavity above the rock contained round openings at regular

intervals around the circumference of the crust. The locations of the holes coincided with
 94

the placement of the topmost layer of cans within the soil prior to plasma magmavication.

It is believed that they are the actual voids left when the cans fell into the magma pool.

This may indicate that the time allotted for the treatment of the larger kaolin deposit was

not enough to completely incorporate the contaminants. An increase in treatment times

needs to be implemented for future experiments, not only for thoroughness, but also to

eliminate the risk to personnel who will unearth and examine the rocks afterwards.

Another concern was the discovery of partially-melted kaolin in pockets located

within the rock after it had been cut in half. This came as a surprise since it had never

been observed before, and may be another indication of inadequate treatment time.

These pockets were generally located about 2.5 to 4 cm from the edge of the rock at

various locations at the top and the bottom regions of the rock. Samples were taken from

these pockets by the author but were never tested due to a lack of funding. It is possible

that the partially melted kaolin came from within the contaminant cans placed on the

topmost layer, which were the last to be incorporated into the magma. The surrounding

metal has a melting point of T < 1500°C (Callister, 1994), and thus melted first and

released the kaolin and contaminants into the magma pool. If the soil was unable to

reach its melting point before the process was stopped and the magma began to cool, then

unmelted kaolin would have been incorporated as isolated pockets of soil within the

magma. This is a cause of great concern because complete treatment was not fully

achieved. The rocks formed during the experiments of this research program all

displayed moderate-to-heavy fracturing that increased the rock permeability. If the

pockets of partially-melted kaolin are located near the fractures, water migration through
 95
the rock will leach out any remaining contaminants within the pocket and carry it to the

surrounding soil, thus causing contamination.

7.9 Discussion

In the field, in-situ contaminants will not always be conveniently enclosed within

containers. More extensive modeling needs to be performed to determine the optimum

time and power ranges needed to process a certain volume of soil. Otherwise, inadequate

treatment may lead to future expenses for additional treatments. The question of how to

determine whether treatment goals have been met is another concern. Perhaps a real-time

technique, such as resistivity or electromagnetic conductivity, could be employed during

and after testing to check the contaminant levels and to determine the size of the rock as

it is being created. Mayne, Burns, and Rix (1997) attempted such an experiment at the

Savannah River Site K-reactor seepage basin. However, they were only able to perform

readings before and after treatment, not during treatment. The presence of a large

electrical transformer and metal safety fence on-site interfered with the instrument

readings. Although the researchers were unable to detect the rocks created in-situ by the

process, the difficulties they encountered can be remedied to make the techniques more

effective.

The details and results of the chemical tests performed by Clark Atlanta University

are in a joint GTRI-CAU report to be delivered to the Defense Special Weapons Agency,

and specific details will not be reported in this thesis. The results of the researchers were
 96

that the chemical and biological contaminants and their by-products were undetected by

the Toxicity Characteristic Leaching Procedure (TCLP), gas chromatograph/mass

spectrometry (GC/MS), and inductively coupled plasma mass spectrometry (ICPMS)

analyses that were performed on the off-gas, off-gas system scrubber water, and the rock

samples obtained after from tests JDC-3 through JDC-6. For JDC-2 and JDC-5, cesium

and zirconium in the off-gas samples were detected at levels equivalent to or below

background levels found in the control test (JDC-1). However, cesium was detected in

the off-gas scrubber water of JDC-6 at 1.5% of the amount prepared of CsCl. The

researchers suggested that the source of the cesium was from particulates traveling

through the off-gas system. TCLP tests performed on rock samples from JDC-6 showed

concentrations of cesium and zirconium above baseline levels.

 97

CHAPTER VIII

CHARACTERIZATION O F PRE-TEST KAOLIN AND POST-TEST

TRANSFORMED R O C K

Various engineering properties of both the pre-test kaolin and the post-test igneous

rock were examined to determine the changes due to transformation of soil to rock by

plasma magmavication. This chapter will compare and discuss the results of laboratory

experiments on compressive strength (q ), shear modulus ( G x ) , elastic modulus (E),

u ma

porosity (n), and unit weight (YT) tests performed on samples of the processed kaolin and

the vesicular mullite glass slag. Table 8.1 is a summary of the tests and their objectives,

and Table 8.2 is a summary of the results from tests done on the kaolin and the rock. The

results of all the laboratory tests performed on the kaolin are in Appendix D, and the

results of the tests performed on the rock are in Appendix E. Other parameters

fundamental to the ongoing plasma research goals are reported in Section 8.6. These

include mass of the rocks produced compared to energy consumption, treatment time, and

power level of the experiments produced. The temperature readings obtained from JDC-

1 through JDC-9 are in Appendix A.

8.1 Preparation of Kaolin Specimens for Testing

In order to reproduce the density and compactive effort of the kaolin deposits in the

steel chamber used for testing, a representative container was prepared and shelby tube
 98

samples were taken. These samples were used to perform one-dimensional

consolidation, resonant column, and CU (consolidated undrained) triaxial tests.

The processed kaolin was prepared at w - 40% in two plastic barrels. A barrel was

placed on a scale and zeroed out. A 222-N bag was emptied into the barrel, and 89 N of

water was then added. The soil was then mixed by hand for approximately 7 to 10

minutes, to minimize pockets of dry soil and allow for a more homogenous mixture. The

process was continued until a total weight of 1557 N of kaolin had been combined with

623 N of water. The barrels were then tightly covered with plastic wrap and the clay was

allowed to hydrate for 48 hours.

TABLE 8 . 1 : SUMMARY O F E X P E R I M E N T S
A v e .
T e s t S l a g
T e s t T o r c h P o w e r
D a t e T e s t O b j e c t i v e T i m e , W e i g h t ,
N u m b e r S y s t e m A t t a i n e d ,
m i n N
k W

J D C - 1 5/6/98 Control Test 100 kW 80 75 236

J D C - 2 6/4/98 Nuclear 100 kW 89 155 529
Contaminants
J D C - 3 7/30/98 Chemical 100 kW 86 140 356
Contaminants
J D C - 4 8/6/98 Biological 100 kW 88 160 360
Contaminants
J D C - 5 8/26/98 All 100 kW 88 140 285
Contaminants
J D C - 6 9/3/98 All 200 kW 200 180 792
Contaminants
J D C - 7 10/16/98 Control Test 100 kW 68 68.8 93.4
J D C - 8 11/16/98 TDR 100 kW 85 45 162
J D C - 9 4/9/99 Cooling 100 kW 65 41 80.1
Rate/Plasticity
 99

TABLE 8.2: RESULTS OF LABORATORY TESTS ON KAOLIN AND

TRANSFORMED ROCK
TRANSFORMED
PARAMETER PROCESSED
KAOLIN
KAOLIN
(IGNEOUS ROCK)
COMPRESSIVE
STRENGTH (q ), MPa
u 0.149 121

AVE. SHEAR WAVE

209 2620
VELOCITY (V ), m/s
s

AVE. SHEAR MODULUS

74 16332
(G), MPa
AVE. YOUNG'S
MODULUS (E), MPa 170 36583
(assume v = 0.12)
TOTAL UNIT WEIGHT
3
14.1 23.3
(Y ), kN/m
T

1.48@40%M.C.
VOID RATIO (e) 0.35
1.66 @ 50% M X .

POROSITY (n) 60% @ 40% M.C.

26%
62%@50%M.C.
 100

After hydration, the kaolin was placed in another plastic barrel of known dimensions

(height and diameter). The soil was placed in a 20-cm layer. A 53-N weight was then

used to compact the soil to a 15-cm lift. Another 20-cm layer was then placed inside and

the compaction process repeated. This layering and compaction procedure replicated the

in-situ chamber preparation for the tests performed during the research program.

Four shelby tubes were prepared by cutting 20-cm lengths from a long steel tube.

This was done using a dry saw with a metal cutting blade, A hand-held grinder and metal

files were then used to sharpen one end to a cutting edge. The other end was filed down

to remove sharp edges and metal burrs.

A shelby tube was placed on the top of the deposit, and a drive hammer was used to

pound the sleeve to the bottom of the barrel. This was repeated for the other three tubes.

Due to the driving action of the hammer, localized densification can occur at the interface

of the tube and soil as well as within some radial area of influence around the tube.

Therefore, each tube was placed about 10 cm from the other to minimize this effect on

the specimens. The tubes were dug out from the deposit, tightly wrapped in plastic wrap,

and placed in plastic bags. The tubes were stored in a refrigerator to maintain the

moisture content.

Each specimen was extruded using a mechanized extruding system. The tube was

placed on the lower platen in the direction of sampling so that the specimen would be

removed in the direction it was placed. The screw mechanism then lifted the lower platen

up towards the top platen. The top platen had a 6.35-cm diameter hole for the sample to

move through. The tube was pushed upwards against the lip of the platen, which held it
 101

in place. The sample was then driven upwards through the tube and out of the platen

hole. The sample was prepared according to the respective ASTM procedures.

8.2 Compressive Strength Testing

Compressive strength tests were performed on a specimen obtained from a shelby

tube. The conventional isotropic consolidated undrained triaxial test (ASTM D 4767)

with pore water pressure measurements was used to determine the compressive strength

of the kaolin prior to magmavication. The triaxial test tries to simulate the stresses that a

soil would experience in the field under given loading conditions. The undrained test

was chosen over the drained test because fine-grained soils, like kaolin, drain much more

slowly under loading conditions than a coarse-grained soil. Thus, a consolidated drained

triaxial test would not simulate realistic conditions for fine-grained soil.

The specimen was extruded and trimmed, and a rubber membrane was placed

around the specimen. The specimen was then placed in the test apparatus and

isotropically consolidated at 120 kPa for about 24 hours. The B-value, which indicates

saturation, was checked and the sample was determined to be below S = 100%, but

highly saturated nonetheless. Testing was then performed and the principal stress

difference (ai - 03), which is the compressive strength, was calculated to be q = 149 kPa.
u

The shear strength of the kaolin is determined by the Equation 8-1, and was calculated to

be T a x = 75
m kPa.
 102

(8-1)

The compressive strength of the vesicular mullite glass slag was determined by a

uniaxial compressive test (ASTMD 2938) using a SATEC Systems, Inc. MTS automated

load frame. The specimens were trimmed into cubes of 3 cm x 3 cm x 3 cm and the

loading faces were ground using a sandpaper wheel to ensure parallel sides. Two cubes

were tested in which one was intact, and the other was fractured. This was done

purposely to determine the strength reduction due to the fractures induced during cooling

in the rock. The compressive strength is calculated by:

a =— (8-2)
A

The compressive strength of the rock was found to be 121000 kPa.

The failure mode observed in the rock was slabbing. Slabbing occurs when major

cracks form parallel to the direction of force application. This results in a series of

columns (Vutukuri, Lama, and Saluja, 1974), similar to those shown in Figure 8.1.
 103

8.3 I n i t i a l S m a l l - S t r a i n Stiffness

The small-strain stiffness of the kaolin was determined through resonant column

tests performed according to ASTM D 4015. The cylindrical specimens were 15-cm in

height and 7-cm in diameter. The soil specimens were subjected to small torsional shear

5 4
strains (y = 10" to 10" ) during which the resonant frequencies were measured. Two

specimens were tested at different confining pressures and the results are shown in Table

8.2. The shear modulus ( G max ) is calculated from the shear wave velocity (V ) and the s

mass density (p - v/g) through the equation:

2
G m M =(?V s (8-3)

The elastic modulus (E) can then be calculated by Equation 8-4. The value of

Poisson's ratio used in the calculations was v = 0.1-2.

E = 2G(l + v) (8-4)

Non-destructive ultrasonics was employed to determine the shear wave velocities

(V ) of the rock. Due to the size, shape, and internal fracturing of the rocks, it was not
s
FIGURE 8.1: SLABBING FAILURE IN ROCK
(VUTUKURI, LAMA, AND SALUJA, 1974)
 105

feasible to obtain cores without damaging or destroying the rock during coring. Thus,

various geometries were cut using an oil-lubricated diamond-tipped automatic saw.

Cubes were most common. However, the nature of the fractures within the rock made it

difficult to cut competent specimens with the minimum length-to-width ratio of 2:1.

Shorter specimens with a 1:1 ratio were used, but the values obtained were higher than

those found for massive intact rocks due to boundary effects. Therefore it was necessary

to test a piece of rock that had been trimmed on parallel sides, but still maintained an

irregular geometry. This specimen yielded results that were more reasonable.

Ultrasonic pulse testing (AST3V1 D 2845) imparts a mechanical wave, via a

transmitter, through the rock specimen that is then received at the other end of the rock

by a receiver. The transmitter is hooked up to a trigger that establishes the initial time of

the wave. When the receiver detects the wave, the timing is stopped and the travel time

is determined. The shear wave velocity is then calculated by dividing the length of the

specimen by the arrival time. The use of shear waves was preferred over compression

waves because the moisture content of a substance does not influence shear waves. This

makes the test more convenient and reliable. The shear modulus and elastic modulus of

the rock are obtained through Equation 8-3 and Equation 8-4. The values are shown in

Table 8.2.

Figure 8.2 is a graph of work done at Georgia Tech that illustrates the dramatic gains

in elastic modulus and compressive strength by magmavication of soils into rocks. The

gain of 2 to 3 orders of magnitude that the geomaterials attain bodes well for future

applications of plasma technology in soil strengthening and stabilization.

 106

TransformedMaterials
X

• Georgia Kaolin

• Transformed Georgia Kaolin

O P i e d m o n t Silty S a n d

• Transformed P i e d m o n t Silty S a n d

2 0 / 3 0 Silica S a n d

Original Soils Transformed 2 0 / 3 0 Silica S a n d

OTyndall Beach Sand

• Transformed Tyndall B e a c h S a n d

X Savannah Clayey Sand

O
1 0 0 4
XTransformed Savannah Clayey Sand

Goose Lake Clay

Transformed G o o s e Lake Clay

^ P l a s t i c Kaolin

^ T r a n s f o r m e d Plastic Kaolin

—
0.01 0.1 100 1000
Compressive Strength]fy u (MPa)

FIGURE 8.2: CHANGE IN NONDESTRUCTIVE ELASTIC MODULUS AND

DESTRUCTIVE COMPRESSIVE STRENGTH BETWEEN ORIGINAL SOILS
AND MAGMIFIED ROCKS
 107

8.4 Porosity

The average porosity of the kaolin deposit was determined from the following

equation:

N
= -7^T
L
(8-5)

The porosity of the rock was determined from the point-counting tests discussed in

Chapter IX. The values shown in Table 8.2 show an expected decrease in porosity

between the soil and the rock. However, the rock porosity was higher than had been

reported from past research. Some of the possible reasons for this singular event are

discussed in Chapter IX.

8.5 U n i t W e i g h t

The total unit weight of the soil was calculated from the total weight of soil placed in

the chamber divided by the volume of the chamber (YJ = W T / V T ) . The unit weight of the

rock was determined from a cube of known volume, which was oven-dried for 2 4 hours.

The cube was weighed and the unit weight determined using the same equation as for the

soil. Porosity and unit weight are related through Equation 8-6.

A 65% increase in unit weights between the soil and the rock was observed, which
 108

follows the trend shown from previous research. Figure 8.3 is a comprehensive graph

illustrating the changes in unit weight and shear modulus for all soils that have been

tested here at Georgia Tech. The shear modulus is seen to increase by two orders of

magnitude through the plasma magmavication process. This further confirms the

strength and stiffness advantages that can be obtained through magmavication.

8.6 Results of M a s s , Power C o n s u m p t i o n , and T i m e Observations

During the plasma magmavication tests, power and time levels were recorded to

continue the effort of data collection for modeling purposes. The results are shown in

graphs showing results of all experiments to date utilizing non-transferred arc plasma

technology performed at Georgia Tech.

Mayer (1996) reported general trends between mass and volume with respect to

power consumption that are shown in Figure 8.4 and Figure 8.5. These relationships

correlate well with the masses and volumes determined from the tests performed on

processed kaolin. In Figure 8.4, it is interesting to note that values obtained from Circeo

et al. (1998), which were from argillaceous sedimentary rocks, showed the highest

masses for a given power consumption. Additionally, when comparing the scatter of
 109

O Georgia kaolin

• T r a n s f o r m e d Georgia kaolin

A Piedmont silty sand

a Transformed Piedmont silty sand

• 20730 silica sand

Tr
j Trans formed 20/30 silica sand Material*
+Tyndall Beach sand

X Transformed Tyndall Beach sand

x Savannah River soil

^Transformed Savannah RivBr soil

Processed K a d i n

«• Transformed processed kaolin

O •

A.

Origin* Soil*

_I I 1_
3
15 Total Unit Weight, Y T (kNVrn )
10 25

20
FIGURE 8 . 3 : CHANGE IN SHEAR MODULUS AND UNIT WEIGHT
THROUGH PLASMA MAGMAVICATION
 110

Figure 8.4 and Figure 8.5, it is seen that the sedimentary rocks, Savannah clayey sand and

Piedmont silty sand are further from the trendline, showing slightly higher gains in rock

mass for given power consumption. This may be an influence of particle size, but more

perhaps more of soil fabric and structure. The cohesion of fine-grained soils allows the

deposit to maintain a more stable soil fabric than coarse-grained soils, which are

cohesionless. As melting occurs, the soil structure of coarse-grained soils collapse and

material is incorporated into the magma pool. The cohesion and interparticle forces of

fine-grained soils help to keep the integrity of the deposit, and so caving does not occur

as readily. For the rocks, the large voids in between the individual rocks allowed magma

to flow through the crevices and incorporate more material, thus increasing the rock

mass.

Figure 8.6 is a graph illustrating treatment times in relation to the mass of igneous

rock produced. Figure 8.7 is a graph of average power relative to the igneous rock mass

produced. Both graphs show significant scatter in the data points. However, the very

general trend of increasing time and power levels yielding increased masses is observed.

In Figure 8.6, the data on processed kaolin show a definite trend with minimal scatter.

This may be because the soil tested was similar in composition and preparation. In

comparison, Mayer (1996) shows a general trend of increased average power level

yielding increased mass, Although Mayer tested one type of natural soil throughout, it is

speculated that the scatter was caused by the heterogeneous nature of the soil used in the

tests. Nonetheless, as a whole, there can be no conclusions drawn on the effects of power

levels and treatment times except that in general, increasing one and/or the other will
 Ill

produce more rock mass.

There are other factors that may affect the rock mass which have gone unchecked.

One such factor is the preparation of the soil and its compaction into the chamber. The

layering and compacting method is not standardized, and so there are variations in the

percent of standard compaction achieved for each soil deposit. It seems likely that a

uniformly-compacted soil will allow more even heating and melting of the soil, which

may affect the amount of rock produced.

The borehole-to-torch diameter ratio can affect energy loss that results in inefficient

melting of soil. For laboratory and field use, it is realistic to modify the torch for direct

insertion into the ground using direct push technology or dynamic driving techniques

(similar to pile driving). The close contact that this would allow may prevent excessive

energy loss and allow for better melting and increased rock mass.

The height of the plasma torch above the magma has an effect on the effectiveness of

the process as well, as was suggested by Mayer (1996). There is an optimum height that

the torch should be placed order to eficiently metl the soil

in while maintaining the torch

integrity and electrode life. If the torch is placed within the soil, there is a chance of

permanent damage to the torch and shortened electrode life. This issue is currently under

investigation.
 112

Energy Consumption, kW-hr

F I G U R E 8.4: RELATIONSHIP BETWEEN IGNEOUS ROCK MASS AND

ENEGRY CONSUMPTION USED DURING MAGMAVICATION
 113

F I G U R E 8.5: RELATIONSHIP BETWEEN IGNEOUS ROCK VOLUME AND

ENERGY CONSUMPTION FOR DIFFERENT SOILS
 114

250 -1

200 A

020/30 Silica Sand

SRS Clayey Sand
• Rome Shale
150
x Plastic Kaolin
• Piedmont Silty Sand
o Georgia Kaolin
A Tyndall Beach Sand
rr 100 A
• Rome Mudstone

50 A

X X
X
X

4 5 6

Treatment Time, hour

10
F I G U R E 8.6: E F F E C T O F T R E A T M E N T T I M E O N
IGNEOUS ROCK MASS PRODUCED
 115

020/30 Silica Sand

A SRS Clayey Sand
• Rome Shale
-(-Plastic Kaolin
• Piedmont Sitty Sand
o Georgia Kaolin
• Tyndall Beach Sand
X Rome Mudstone

-rf
10 60 110 160 210

Average Power, kW

F I G U R E 8.7: E F F E C T O F A V E R A G E P O W E R L E V E L S O N
IGNEOUS ROCK MASS PRODUCED
 116

CHAPTER IX

PETROGRAPHIC STUDIES OF THE TRANSFORMED ROCK

Petrography is the description and systematic classification of rocks using geologic

procedures. The rocks are prepared in thin (30 [im) sections onto microscope slides, and

are observed with a polarizing microscope. These tests mark the initial effort to

determine the proper geologic classification of the rock produced from the processed

kaolin by plasma magmavication. Rock cutting, preparation, and testing were performed

at the School of Earth and Atmospheric Sciences under the guidance and assistance of

William Waggener, Laboratory and Field Coordinator. A summary of the component

percentages relative to all the points counted is given in Table 9.1.

9.1 Preparation of the Rock for Thin Sections

The rock used for the petrographic slide material was from test JDC-1 so that there

were no safety concerns during cutting. The rock was first cut in half using a 61-cm x

0.2-cm diamond-embedded blade on a Highland Park Manufacturing Company "Model

U" oil-lubricated saw. Afterwards, a smaller piece was cut from one of the rock halves

using the same saw. Then a 25-cm diameter diamond-embedded blade on a Star

Diamond Industries, Inc. "Model TS-10C Trim-Slab" oil-lubricated saw was used to cut

the rock into a cubic form with dimensions approximately 6-cm x 3-cm x 3-cm.
 117

The rock was moderately fractured and porous, and it was anticipated to be difficult

to mount the rock section onto a microscope slide and grind it without losing the original

rock structure. Therefore, to maintain the rock integrity, structure, and fracture patterns,

it was necessary to impregnate the rock with a two-part epoxy resin (Epo-tek 301). The

epoxy was mixed in the specified proportions and used to coat one face of the rock.

Much of the epoxy was absorbed into the rock pores, so more was added until the pores

were saturated. Hardening at room temperature normally took 24 hours, so to speed up

the process, the rock was placed epoxy-side up on a hot plate set at 93°C for 1 to 1.5

hours. After this time, the epoxied side had cured enough to be handled. The coating and

heating process was repeated on the other sides until completed.

Another specimen was also prepared from a rock produced by Beaver (1995). This

rock had been made by magmavication of natural unprocessed kaolin and produced a

densely-crystallized rock with blue glass inclusions. X-ray diffraction performed on a

sample indicated alumina-silicates, but did not identify the actual mineral (Beaver, 1995).

The rock was prepared in the same manner for the thin sections, while identification of

the actual mineral was done through the Becke line test. The specifics of the Becke test

will be discussed in Section 9.2.

The samples were initially prepared by the author, but Petrographic International,

located in Saskatchewan, Canada, did the actual mounting and grinding of the rock slide.

The broad explanation of the process will be discussed here for general understanding

and was adapted from Kerr (1977).

After the initial cutting and preparation, a chip is either broken or sliced off the rock
 118

sample and the slide surfaces ground flat. Ideally, this chip should have dimensions of

2.5-cm square with a 0.3-cm thickness. With hard rocks, one side is polished with

successively finer grits (100, FFF, 600 carborundum, 302'/2 emery). For soft rocks the

100 grit should be left out to prevent damage to the rock. The ground surface is then

cleaned and dried. Heated epoxy resin is the adhesive used to bind the rock to the slide.

The resin is placed on the slide, and the rock chip, which is heated to 120°C, is placed on

the slide with care to be sure that it is parallel. After cooling, the rock should be tightly

bonded to the slide. In order to achieve the 30-(j.m thickness for evaluation, the mounted

rock chip is ground down further with successively finer emery grits. To determine when

the desired thickness has been achieved, a microscopic observation is done using the

interference colors of a known mineral within the rock (normally quartz) when covered

with a thin film water. The interference colors of quartz at 30-(j.m will be a light straw

color. Once the correct thickness is obtained, the slide face is washed and dried. Finally,

another layer of epoxy is placed on the top surface and a cover slip placed over it. Once

cured, the slide is ready for use.

9.2 Mineral Determination and the Becke Line Test

There are many ways of identifying the minerals present within a rock. The methods

can range from visual recognition to more complicated methods such as x-ray diffraction.

Differential thermal analysis and infrared study are other commonly used techniques.

For the identification of the minerals within the rocks produced in this research, x-
 119

ray diffraction was employed. All results concluded that the main mineral was synthetic

mullite. The x-ray diffraction results are in Appendix C. However, the rock obtained

from Beaver's (1995) experiments had never been fully identified. Since the end

products of extreme thermal decomposition of kaolin have been proven to be mullite and

cristobalite (Deer, Howie, and Zussman, 1966), it was predicted that mullite would be the

main mineral. To confirm this without resorting to XRD, a Becke line test was done on

minute samples (diameter < 0.5 mm) of the rock.

The refraction indices of a mineral are unique and can be determined by comparison

with oils of known refractive indices. The kit used for this test was a Cargille Set RF 1/2

that had a range from 1.400 to 1.700. Since a certain mineral (mullite) presence was

suspected, the range of the oils used was narrowed to represent the range of indices

known for mullite.

The following procedure was adapted from Kerr (1977). Several small mineral

fragments are placed on a microscope slide without a cover slip. A drop of oil is placed

on top of a mineral fragment and is viewed in polarized light through the microscope.

Light enters from the bottom of the microscope and goes through the oil and mineral. At

the boundary between the oil and mineral, refraction and reflection take place and a part

of the light beam is bent to one side or the other, depending on the relative indices of the

oil and mineral. If the indices are the same, then no refraction takes place. If they are

not, then the light will be deflected towards the medium with the greater. This deflection

causes a blurred white line along the mineral boundary, either right within the oil or

within the mineral, depending on which indices are greater. This line is called the Becke
 120

line (for mineralogist F. Becke). As the mounting plate of the microscope is moved up

(closer) the line will move towards the material with lower index. As the plate is moved

down (away) the line will move towards the mineral of higher index. If the line does not

move at all with either motion of the plate, the indices are the same.

The material from Beaver (1996) was tested with the assistance of William

Waggener, Laboratory and Field Coordinator for the School of Earth and Atmospheric

Sciences. Mullite has a range of refractive indices from 1,642 to 1.654 (Kerr, 1977).

Three oils ranging from 1.640 to 1.656 were chosen to bracket the range found in the

literature. After checking the upper and lower refractive index values, a mineral piece

was prepared with the 1.644 oil. The Becke line was observed, and the plate was moved

up and down. The Becke line did not move but only became out-of-focus. This showed

that the indices were the same, and confirmed the identity of the mineral as mullite.

9.3 Petrogranhic Results and Classification of the Rock

Point-counting was performed to determine the classification of the rock produced in

these experiments after the minerals were identified. Point-counting is the process of

counting constituents within a thin section using a polarizing microscope. A manual

point recorder device tabulates the individual components. The microscope used for this

task, as well as for the Becke line test, was a Carl Zeiss "Standard Universal Pol"

polarizing microscope. The eyepiece of the microscope had crosshairs within the sight

that indicated the exact spot upon which a count was taken. The stage can rotate 360° or
 121

be locked into place to prevent motion. The point counter on the platform has two screw

mechanisms which allow the slide to move in perpendicular axes in 0.3-mm increments.

There are five objective lenses, but for the purposes of the test only a lOx objective was

used.

A counting area of a slide was predetermined by visual inspection before it was

mounted on the plate. Then the area was mapped out by determining the start and stop

points in the horizontal and vertical directions. Once this was done, the point recorder

keys were tagged to identify each key with a particular component. The slide was then

moved along one axis and the components under the cross-hairs (points) were identified

and counted along the lines between the predetermined start and stop points. The points

were registered on the point recorder under the respective key. The slide was then moved

one division in the perpendicular axis, and the counting was performed in the other

direction. Figure 9.1 is an exaggerated illustration of a counting course. Once the point-

counting for a slide was completed, the total for each component and the grand total of

points were recorded. The slide was removed and the process repeated for the other

slides. A picture of a slide at lOx magnification is shown in Figure 9.2 with the

components of the rock marked.

Each slide prepared from the rock contained three major constituents: black glass,

mullite crystals, and pores. The mullite crystals were long, needle-like crystals with a

nearly square cross-section. The lengths of the crystals were about 2 mm to 12 mm, and

the cross-sections ranged from 2 mm to 4 mm. A total of 10 slides were counted. The

results are summarized in Table 9.1. Rock classification was done by first naming the
 122

least recognizable characteristic of the rock and progressing to the most recognizable

characteristic of the rock. As shown in Table 9.1, the pores were lowest in the point-

count, followed by the mullite, and finally the glass. At times it was difficult to

distinguish between the components. When this happened, cross-polarized light was

used to view the slide. The crystals appeared as white or very light gray shapes in

polarized light, while glass and pores remained dark-colored. To differentiate between

the pores and crystals, it was always noted that the crystals had definite geometries while

the pores were round or irregularly shaped. From the results of the point-counting and

mineral identification, it was determined that the rock was a vesicular mullite glass slag.

Slag denotes the fact that the rock was man-made.

The slides made from the rock produced by Beaver ( 1 9 9 6 ) have not been through

point-counting yet. However, it is safe to say that the rock is a more densely-crystallized

mullite rock. Nonetheless, point-counting will be needed in the future to determine the

porosity and the other minor components of the rock.

 123

FIGURE 9 . 1 : GENERAL COUNTING COURSE ON A

PETROGRAPHIC SLIDE (NO MAGNIFICATION)

i
 124

FIGURE 9.2: PETROGRAPHIC SLIDE AT lOx MAGNIFICATION

A: FINE NEEDLE-LIKE MULLITE CRYSTALS

B: IRREGULARLY-SHAPED PORES
C: BLACK GLASS
 125

TABLE 9.1: RESULTS OF POINT-COUNTING ON PETROGRAPHIC SLIDES

S L I D E S U R F A C E P O R E M U L L I T E G L A S S T O T A L

N U M B E R A R E A C O U N T C O U N T C O U N T P O I N T S

2
( m m ) C O U N T E D

E20623F-2 466.1 1529 1643 2291 5463

E20623F-1 364.0 1509 1052 1662 4223

E20623-d-2 276.0 558 983 1653 3194

E20623-e-2 135.0 277 533 772 1582

E20623-e-l 132.0 397 488 674 1559

E20623b-2 180.0 650 646 840 2136

E2623b-1 144.0 413 556 733 1702

E20623c-1 165.0 492 687 758 1937

E20623-d-l 240.0 679 914 1198 2791

r
E2063a-1 336.0 980 1431 1489 3900

T O T A L S 2438.1 7484 8933 12070 28487

% OF EACH
C O M P O N E N T — 26.3 31.3 42.4 100

*Note: All slides were made from the rock produced by JDC-1 test
 126

9.4 Mullite F o r m a t i o n

Mullite (3Al203»2Si0 ) is a rare mineral found mainly on the Isle of Mull off the
2

coast of West Scotland. It is the only stable compound in the AI2O3—Si0 2 system

formed under either atmospheric pressure or pressures just a few hundred atmospheres

above atmospheric pressure. Other alumina-silicates are also formed in the system, such

as sillimanite, andalusite, and kyanite. Sillimanite is formed under high pressures and

high temperatures; andalusite is formed under relatively low pressures and temperatures;

and kyanite is formed under high pressure and low temperatures (Grofcsik, 1961).

Mullite forms under the conditions of high Al03 content, low pressure, and high magma
2

temperatures. These conditions were similar to the laboratory conditions under which the

vesicular mullite glass slag was made. Some properties of mullite are listed in Table 9.2.

Mullite is very similar in its properties to sillimanite and was not recognized as a distinct

mineral until the early part of this century (Kerr, 1977).

In explaining the formation of mullite from the kaolin that was used for this research,

an investigation of the A l 0 3 — S i 0 — H 0 system reveals some interesting points. Roy

2 2 2

and Osborn (1954) examined the system at 700 atm, as a function of temperature. It was

discovered that kaolin becomes unstable at temperatures above 405°C, and that mullite

becomes a stable constituent remaining at temperatures above 575°C. This is the reason

that mullite is commonly found in industrial ceramic products, where most ceramic

materials are fired at temperatures well above 575°C.

Formation of mullite from kaolin has been investigated by many researchers and a
 127

number of different hypotheses have been considered (Grofcsik, 1961). However, the

most coherent explanation came from Brindley and Nakahira (1958, 1959) who made

observations of the heating of kaolin through x-ray methods. Kaolin experiences distinct

changes in enthalpy throughout the heating process, which was determined through

differential thermal analysis. The first reaction is endothermic and occurs between 500°C

and 600°C as hydroxyl ions are destroyed and water is released from the kaolin lattice.

The next reaction happens between 900°C and 1000°C and is exothermic (called the

"first" exothermic effect). The "second" exothermic effect occurs between 1200°C and

1300°C. Sometimes a "third" exothermic reaction occurs at temperatures above 1300°C,

but this is largely dependent on the clay (Grofcsik, 1961). Brindley and Nakahira (1958,

1959) explained the thermal effects and formation of mullite in the following sequence:

. Endothermic dehydroxylation of kaolin: Al Si 05(OH)

2 2 4 -> Al Si207 + 2 H 0
2 2

Kaolinite meta-kaolinite
• First exothermic reaction: 2Al Si20 -> Al SijOi + S i 0
2 7 4 2 2

meta-kaolinite Spinel-phase
Second exothermic reaction: AlSi30i —> 2AI Si 0s + S i 0
4 2 2 2 2

Spinel-phase Mullite-type phase

AlSi0i3 +
M u
phase l2

l
i
t
e -
t
y pe
Stable mullite phase formation: 3 A l S i 0 5 —>
Mulite 6 2 Si0 2
 128

TABLE 9.2: CHARACTERISTICS OF MULLITE

(ADAPTED FROM GROFCSIK, 1961)

Formula 3Al 0 «2Si0

2 3 2

Crystal System Orthorhombic

Specific Gravity (G )s
3.03

Mohs Hardness 7.5

Index of Refraction 1.65

Elastic Modulus (E) 34.4 GPa

The presence of foreign materials in the kaolin can positively influence the formation

of mullite (Visconti and Nicot, 1957), which may explain the unique crystallization found

in the rock produced by Beaver (1995). The natural kaolin contained 8 1 % kaolinite, 13%

quartz, 2-3% diaspore, and 1-2% illite. It is obvious that although the rocks produced by

magmavication of the processed kaolin contained mullite crystals, the size and amounts

of the crystals are not comparable with the rock made with natural kaolin. Finally, the

presence of iron species within the magma allowed for formation of other minerals, in

small quantities, as opposed to mullite. Beaver (1995) used a clay stovepipe to simulate

the borehole casing, and thus did not add any iron ions to the magma during treatment.
 129

9.5 Discussion on I n f l u e n c i n g Post-Test R o c k F o r m a t i o n

The natural process of rock formation is much slower and normally occurs under

much higher pressures and sustained temperatures than normal laboratory conditions.

The conditions that natural rocks experience can not be simulated in the lab without

highly-specialized, costly equipment. Additionally, all soils are formed through chemical

alteration of rocks. These rocks can themselves be formed through sedimentary or

metamorphic processes, which makes the likelihood of duplicating the conditions of rock

and soil formation almost impossible. The prediction of mineral formation may be

possible if the constituents of the soil are known to such as degree that a known

temperature-composition diagram (ternary, quaternary, or higher order) can be used.

This diagram illustrates the boundaries to which liquid, liquid-crystal, and crystal phases

can exist under a given pressure. Figure 9.3 is an example of the Fe2Si04—MgSi04

system under atmospheric pressure. The graph clearly illustrates the boundaries between

conditions under which only liquid, liquid + solid, and only solid phases of the system

depending on the percentages of the two components present in the magma.

If the mineral assemblage resulting from melting of a soil of known components can

be predicted from a temperature-composition graph, then it follows that the minerals can

be engineered by the alteration of the soil components. The intentional alteration of the

soil components could be used to influence the mineral formation in a controlled manner.

This suggests the possibility of tailoring a soil to yield a rock of given mineralogy for a

specific purpose. However, more important issues in influencing mineral formation

 130

would be reduction of porosity and understanding the effect of crystals as stress

concentrations or "reinforcement" within the glass phase.

FIGURE 9.3: TWO-COMPONENT SYSTEM INDICATING THE BOUNDARIES
BETWEEN LIQUID/MIXED/AND SOLID STATES AT ATMOSPHERIC
PRESSURE (WILLIAMS, TURNER, AND GILBERT, 1982)
 132

CHAPTER X

CONCLUSIONS

The use of non-transferred arc plasma technology for in-situ soil remediation shows

some potential for immobilization or destruction of nuclear, chemical, biological, and

mixed wastes buried within a clay deposit. In-situ plasma magmavication was shown to

be effective under laboratory conditions in transforming the clay and contaminants into a

stable igneous rock. At the high operating temperatures of the non-transferred arc plasma

torch, organic materials pyrolize and inorganic materials become incorporated into the

magma. During treatment, the inorganic materials are incorporated into magma that

cools into a stable igneous rock with very low teachability and drastically improved

engineering properties, which should have long-term durability.

Quantitative and qualitative tests were performed on the igneous rock produced by

the process to determine the constituents remaining after plasma magmavication. The

tests were unable to detect any traces of contaminants. Nonetheless, there remain some

serious concerns as to the instrument resolution versus the remaining contaminant

concentrations. Although it is highly likely that the organic contaminants underwent

pyrolysis and the inorganic contaminants remain locked within the glass phase, further

analyses using more suitable detection techniques needs to be employed before sound

conclusions can be drawn regarding the fate of the organic and inorganic materials.
 133

Petrographic tests were used to determine the constituents and geologic classification

of the resulting igneous rock. The dominant mineral was confirmed through x-ray

diffraction to be mullite. Mullite is a rare natural mineral, but is found in abundance in

ceramic products due to its formation at low pressures and high temperature. Once the

mineralogy was confirmed, point-counting was employed to determine the amounts of

each constituent. The main constituents detected through point-counting were voids,

mullite, and black glass. Combining the mineral identification and the percentages of

each constituent led to the classification of the igneous rock as a vesicular mullite glass

slag.

The transformed kaolin had greatly improved engineering properties. These positive

gains in material properties, such as compressive strength, shear and elastic modulus, and

unit weight, were noted in all soil types tested by previous researchers. With more

research and development of in-situ plasma magmavication, these benefits may be

directly utilized in construction as a potential method to fabricate pile foundations and

retaining walls, and for underpinning of foundations and piers.

Now more than ever, attention to environmental and societal concerns is of the

utmost importance for all nations as our sources of clean water, clean air, and land

become exhausted. Soil remediation gives the opportunity of opening up expanses of

land for more productive uses. At this intermediate stage of development, in-situ plasma

magmavication shows potential as a remedy for wastes that resist treatment through

conventional methods. The significant advantages of in-situ plasma magmavication over

other soil remediation methods include: (1) it is not contaminant-specific; ( 2 ) in-situ

 134

plasma magmaviation works in any soil type (sands, silts, clays, weathered rock); and (3)

the rock produced can either be left in place with little or no monitoring, or excavated and

disposed of offsite. The process may require some amount of alteration to address

specific off-gas emission concerns, but research has proven its applicability in all soil

types tested. With further investigation, modeling, and refinement of the process, in-situ

plasma magmavication may prove a thorough means to the challenges of solid waste and

contaminated soil treatment and storage.

 135

CHAPTER XI

RECOMMENDATIONS FOR FUTURE RESEARCH

In-situ plasma magmavication holds potential in the area of soil remediation as an

emerging technique. Proper modeling of the magma and cavity growth is crucial in the

development of equations to determine the amount of power and time it will take for

complete and effective treatment under given soil conditions (grain size distribution,

moisture content, overburden, density, volume). For the most part, thermocouples and

infrared thermometers have been used to monitor temperature changes. New techniques,

such as time domain reflectometry, should be further investigated to gather data on

spatial dimensions. This information, along with the temperature changes, will enable

researchers to more fully develop the modeling that is necessary for field implementation

of in-situ plasma magmavication. The commercial viability of plasma magmavication

can only be realized if the process can be made cost-effective and safe.

If the concentrations are suspected to be extremely low, analyses using scanning

electron microscopy (SEM) and x-ray diffraction (XRD) may not prove reliable with

contaminant levels below 0.5% of the entire sample. For future research, a suggestion

would be to either increase the levels of contaminants so they could be detected by SEM

and XRD; or use other detection methods, such as ion microprobe or inductively-coupled

plasma mass spectrometry for analysis.

 136

Petrographic tests should continue to be performed to amass a database and perhaps

develop temperature-composition diagrams to supplement those found in literature. The

rock characteristics and their equilibrium within the environment may play an important

role in determining its permeability or decomposition. Glass devitrifies in a timeframe

dependent on factors such as environmental equilibrium, and pore fluid inclusions, to

name a few. The life span may be shortened considerably if the glass and its structure

(fractures or porosity) and the entrapped and surrounding fluids provide conditions

favoring accelerated disintegration. Petrography may offer one way of determining not

only the type of rock, but its structure and integrity. These are useful factors to know

when considering in-situ treatment without excavation and landfilling of the rock.

The advantageous gains in strength and stiffness make in-situ plasma magmavication

an attractive technique for soil stabilization and improvement. For both soil

improvement and soil remediation, field testing is strongly recommended as the next step

in developing the plasma magmavication process. Field testing will enable future

researchers to determine the logistics of a mobile plasma torch and off-gas scrubber

system. Nevertheless, effective field testing may not be fully realized until the torch

design is modified for subterranean applications and the concern of heat loss through the

borehole is rectified.
 APPENDIX A

EXPERIMENT DETAILS FOR JDC-1 TO JDC-9

 138

The following is a summary of the data collected during the tests. A general

description of the kaolin deposit for each test is given. The raw data collected from the

torch system gauges and thermocouples placed in the deposits are found on pages 155-

168.

A.l JDC-1: Control Test

Test JDC-1 was conducted to determine whether the torch would melt the processed

kaolin. The uncontaminated soil was prepared at a moisture content of 50% and a total

3
unit weight of 14.3 kN/m . The sample was prepared in a steel chamber of 0.9 m height,

and 0.6 m in diameter. A thin steel stovepipe was used to simulate a borehole casing.

The dimensions were 76 cm height and 10 cm diameter. It was inserted to a depth of 76

cm from the top of the soil. The 100-kW torch was placed 15 cm from the bottom of the

borehole (30 cm from the bottom of the chamber). The test duration was 75 minutes

during which the torch was lifted 8 cm every 15 minutes. The total withdrawal distance

was 30 cm with a withdrawal rate of 0.4 cm/min. Figure A.l is a schematic of the

chamber, and the summary of the test parameters is listed in Table A.l.
 139

A.2 JPC-2: Nuclear Surrogate Contaminated Soil

The nuclear surrogates of CsCl and ZrC>2 were prepared in twelve cans by Clark

Atlanta University in the manner previously stated. The uncontaminated soil was

3
prepared at a moisture content of 40% and a total unit weight of 14.1 kN/m . Four cans

were placed vertically on a 38 cm-thick compacted layer of soil, in a square configuration

about 17 cm from the chamber wall (9 cm from borehole). The next layer of 15 cm was

compacted to 10 cm and the cans were placed in the same manner, but staggered from the

previous layer. The subsequent layer of 38 cm was placed and compacted to 30 cm. The

last cans were placed horizontally on the layer in the same configuration. The top layer

was placed and compacted. The stovepipe dimensions and inserted depth are as

previously described. The 100-kW torch was positioned as previously described. The

test duration was 155 minutes during which the torch was lifted 8 cm every 15 minutes.

The total withdrawal distance was 53 cm for a withdrawal rate of 0.34 cm/min. Figure

A.2 is a schematic of the chamber, and the summary of the test parameters is listed in

Table A.l.

A.3 JDC-3: Chemical Surrogate Contaminated Soil

The chemical surrogates of 2-chloroethyI methyl sulfide (CMS) and malathion were

prepared in eight cans by Clark Atlanta University in the manner previously stated. The
 140

TABLE A.1: SUMMARY OF JDC-1 THROUGH JDC-9 TESTS

Test Test Moisture Total Unit Average Energy Time, min
and Objective Content, % Weight of Consumed* kW-hr
3
Date Soil, kN/m
JDC-1:
Control 50 14.3 100 75
5/6/98
Nuclear
JDC-2: Surrogates
40 14.1 231 155
6/4/98 (CsCl &
Zr0 ) 2

Chemical
Surrogates
JDC-3:
(malathion & 40 12.0 201 140
7/30/98
chloroelhyl
methyl sulfide
Biological
Surrogates
( L E 3 9 2 E.
JDC^:
coli b a c t e r i a 40 16.1 235 160
8/6/98
a n d Y P H 8 0 S.
cerevisiae
yeast
JDC-5:
All surrogates 50 14.7 205 140
8/26/98
JDC-6:
All surrogates 50 13.8 600 180
0/3/98
JDC-7:
Control 50 14.2 77 68.8
10/16/98
JDC-8:
TDR 40 13.0 63 45
11/16/98
Cooling Rate
JDC-9:
& Altered 40 15.1 45 41
4/9/99
Plasticity
 141

Test Withdrawal Withdrawal Rock M a x . Rock Max. Rock

and Test Distance of Rate, Weight, Height, Diameter, cm
Date Objective Torch, cm em/miii N cm
JDC-1: Control 30.5
30 0.40 236 30.5
5/6/98
JDC-2: Nuclear 40.6
6/4/98 Surrogates
53 0.34 529 43.2
(CsCI &
Zr0 ) 2

JDC-3: Chemical 30.5

7/30/98 Surrogates
(malathion
& 46 0.33 356 38.1
chloroethyl
methyl
sulfide
JDC-4: Biological 35.6
8/6/98 Surrogates
( L E 3 9 2 E.
coli
bacteria 53 0.33 360 35.6
and YPH80
S.
cerevisiae
yeast
JDC-5: All 38.1
46 0.33 285 35.6
8/26/98 surrogates
JDC-6: All 38.1
38 0.21 792 47,0
9/3/98 surrogates
JDC-7: Control 22.9
30 0.44 93.4 25.4
10/16/98
JDC-8: TOR 17.8
15 0.34 162 29.2
11/16/98
JDC-9: Cooling 11.4
4/9/99 Rate&
15 0.37 80.1 25.4
Altered
Plasticity
 142

uncontaminated soil was prepared at a moisture content of 40% and a total unit weight of

3
12.0 kN/m .

For JDC-3, only two layers were prepared with the contaminants placed vertically.

Four cans were placed on a 38 cm-thick layer of soil, in the layout previously described,

about 17 cm from the chamber wall (9 cm from borehole). The next layer of 38 cm was

compacted to 30 cm thickness, and the cans placed vertically in a staggered manner. The

top layers were placed and compacted.

The stovepipe dimensions and inserted depth are as previously described. The

100-kW torch was positioned as previously described. The test duration was 140 minutes

during which the torch was lifted 8 cm every 15 minutes. The total withdrawal distance

was 46 cm for a withdrawal rate of 0.33 cm/min. Figure A.3 is a schematic of the

chamber for JDC-3, JDC-4, and JDC-5. The summary of the test parameters is listed in

Table A.l.

A.4 JDC-4: Biological Surrogate Contaminated Soil

The biological surrogates for JDC-4 of LE392 E. coli bacteria and YPH80 S.

cerevisiae yeast strain were prepared in eight cans by Clark Atlanta University in the

manner previously stated. The uncontaminated soil was prepared at a moisture content of

40% and a tota!30-cm thickness, and the cans placed vertically in a staggered manner.

The top layers were placed and compacted.

 100-kW Torch Diameter: 6.35 cm

Plasma Torch

Borehole
Steel stovepipe LengtH : 76 cm

15 cm

10 cm

0.6 m

FIGURE A . l : JDC-1 CONTROL TEST (DRAWING NOT TO SCALE)

 144

The stovepipe dimensions and inserted depth are as previously described. The 100-

kW torch was positioned as previously described. The test duration was 160 minutes

during which the torch was lifted 8 cm every 15 minutes. The total withdrawal distance

was 53 cm for a withdrawal rate of 0.33 cm/min. The summary of the test parameters is

listed in Table A.l.

A.5 JDC-5: Mixed Waste Contaminated Soil With 100-kW Torch System

Experiment JDC-5 was conducted to determine whether plasma magmavication was

viable in remediating processed kaolin seeded with mixed wastes (nuclear, chemical, and

biological). The nuclear, chemical, and biological surrogates were the same as

previously tests. Clark Atlanta University prepared eight cans in the manner previously

stated. The uncontaminated soil was prepared at a moisture content of 50% and a total

3
unit weight of 14.7 kN/m .

Two layers were prepared with the contaminants placed vertically. Four cans were

placed on a 36 cm-thick layer of soil, in the layout previously described, about 17 cm

from the chamber wall (9 cm from borehole). The next layer of 15 cm was compacted to

10-cm thickness, and the cans placed vertically in a staggered manner. The top layers

were placed and compacted.

FIGURE A.2: JDC-2 NUCLEAR SURROGATE CONTAMINANT
TEST (DRAWING NOT TO SCALE)
 146

The stovepipe dimensions and inserted depth are as previously described. The 100-kW

torch was positioned as previously described. The test duration was 140 minutes during

which the torch was lifted 8 cm every 15 minutes. The total withdrawal distance was 46

cm for a withdrawal rate of 0.33 cm/min. The summary of the test parameters is listed in

Table A.l.

A.6 J D C - 6 : M i x e d W a s t e C o n t a m i n a t e d Soil w i t h 2 0 0 - k W T o r c h System

Test JDC-6 was conducted with the same objectives as JDC-5, but with the use of

the 200-kW torch system and a larger chamber deposit. The steel chamber is 0.9 m

height, and 0.9 m in diameter. The uncontaminated soil was prepared at a moisture

3
content of 50% and a total unit weight of 13.8 kN/m . The nuclear, chemical, and

biological surrogates were the same as previously tests. Clark Atlanta University

prepared the sixteen cans in the manner previously stated.

A thin steel stovepipe, used to simulate a borehole casing, with dimensions were 76

cm height and 15 cm diameter was used. It was inserted to a depth of 76 cm from the top

of the soil. The 200-kW torch was placed 23 cm from the bottom of the borehole (38 cm

from the bottom of the chamber).

Three layers were prepared with the contaminants placed horizontally. Four cans

were placed on a 42 cm-thick layer of soil, in a square layout. The next layer of 23 cm

was compacted to 15 cm thickness. Eight cans were placed horizontally in a spoked

manner. The process was then repeated for the final seeded layer. The top layers were
 147

then placed and compacted. Figure A.4 shows the can layouts and the chamber

dimensions.

The test duration was 180 minutes during which the torch was lifted 8 cm every 20

to 30 minutes. The total withdrawal distance was 38 cm for a withdrawal rate of 0.21

cm/min. The summary of the test parameters is listed in Table A. 1.

A.7 JDC-7: Control Test

Test JDC-7 was done to complement the information of the initial control test (JDC-

1). The uncontaminated soil was prepared at a moisture content of 50% and a total unit

weight of 14.2 kN/m . The sample was prepared in a steel chamber of 0.9 m height, and

0.6 m in diameter. A thin steel stovepipe was used to simulate a borehole casing. The

dimensions were 76 cm height and 10 cm diameter. It was inserted to a depth of 76 cm

from the top of the soil.

The 100-kW torch was placed 15 cm from the bottom of the borehole (30 cm from

the bottom of the chamber). This test was terminated prematurely when the front

electrode was blown out of the torch. The test duration was 68.8 minutes during which

the torch was lifted 8 cm every 15 minutes. The total withdrawal distance was 30 cm

with a withdrawal rate of 0.44 cm/min. The chamber setup is the same as in Figure A.l,

and the summary of the test parameters is listed in Table A.l.

FIGURE A.3: JDC-3, JDC-4, AND JDC-5: CHEMICAL, BIOLOGICAL, AND
MIXED WASTES SURROGATE CONTAMINANT TESTS
(DRAWING NOT TO SCALE)
FIGURE A.4: JDC-6 MIXED WASTES SURROGATE CONTAMINANT
TEST USING 200-kW TORCH SYSTEM (DRAWING NOT TO SCALE)
 150

A.8 JDC-8: Time Domain Reilectometrv (TDR) Instrumented Test

Experiment JDC-8 was performed to determine the compatibility of TDR with the

plasma magmavication process. The uncontaminated soil was prepared at a moisture

3
content of 40% and a total unit weight of 13.0 kN/m ' The sample was prepared in a steel

chamber of 0.9 m height, and 0.6 m in diameter. A thin steel stovepipe was used to

simulate a borehole casing. The dimensions were 76 cm height and 10 cm diameter. It

was inserted to a depth of 76 cm from the top of the soil.

The 100-kW torch was placed 15 cm from the bottom of the borehole (30 cm from

the bottom of the chamber). The test duration was 45 minutes during which readings

using an inclusive Tektronix 1502C/4 TDR measuring unit were taken every minute. The

torch was lifted 8 cm every 15 minutes. The total withdrawal distance was 15 cm with a

withdrawal rate of 0.34 cm/min. The chamber setup is shown in Figure A.5, and the

summary of the test parameters is listed in Table A.l. The details of the test are in

Appendix G as a report.

A.9 JDC-9: Rate of Cooling and Change in Plasticity Test

This test was to performed to determine the effect of cooling on the crystallization of the

rock and the change in plasticity in the influenced areas surrounding the rock. The

uncontaminated soil was prepared at a moisture content of 40% and a total unit weight of

3
15.1 kN/m . The sample was prepared in a steel chamber of 0.9 m height, and 0.6 m in
 2-Channel Switch Box

1004cW Torch Diameter: 6.35 cm

Radial
TDR
Cable

0.9 m

46 cm

FIGURE A.S: JDC-8 TDR-INSTRUMENTED TEST

(DRAWING NOT TO SCALE)
 152

diameter. A thin steel stovepipe was used to simulate a borehole casing. The dimensions

were 76 cm height and 10 cm diameter. It was inserted to a depth of 76 cm from the top

Of the soil.

In order to slow down the cooling to some degree, 23-cm thick insulation was

wrapped around the chamber and underneath during the torch operation. Additional

insulation was wrapped over the top after the torch was turned off. Two K-type

thermocouples were inserted at 30-cm (TC 1) and 46-cm (TC 2) heights (measured from

the chamber bottom). TC 1 was inserted 16.5 cm into the deposit (8.9 cm from

borehole), and TC 2 was inserted 17.1 cm into the deposit (8.3 cm from borehole).

The 100-kW torch was placed 15 cm from the bottom of the borehole (30 cm from

the bottom of the chamber). The test duration was 41 minutes during which

thermocouple readings were taken every five minutes. The torch was lifted 8 cm every

15 minutes. The total withdrawal distance was 15 cm with a withdrawal rate of 0.37

cm/min. Thermocouple readings were then taken every five minutes for 80 minutes,

every ten minutes for an hour, and then once a day for six days. After the soil had cooled

to the original temperature, the chamber was unwrapped and dissected. The rock and

surrounding zones were carefully removed and brought to the lab for plasticity testing.

The chamber setup is similar to that shown in Figure A.l. The summary of the test

parameters is listed in Table A. 1

Index tests were performed in the George F. Sowers Soil Laboratory located in the

Mason Civil and Environmental Engineering Building at Georgia Tech. Samples were

taken from two distinct layers of altered soil that adhered to the rock and from the
 153

unaltered kaolin located outside the zone of influence. The Fall Cone test (BS 1377), and

the Plastic Limit test (ASTM D 4318) were performed on the soil samples.

Previous experiments on natural kaolin have shown zones of decreased or eliminated

plasticity surrounding the igneous rock. Each of the altered zones were of limited

thickness (~ 3mm) until the unaltered soil area was reached. Beaver (1996) reported that

four zones were distinguished around the rock: a fused black and gray zone of no

plasticity; followed by a white partially-fused zone of no plasticity; then a pink zone of

reduced plasticity, and finally the unaltered natural kaolin. Tests performed on the pink

and unaltered zones resulted in PI = 6% and PI = 20%, respectively.

Upon dissection of the chamber, it was determined that similar distinct layers

encompassed the rock. The innermost layer was a gray to black region fused to the rock,

followed by a white partially-fused zone, a pink altered zone, and finally the original soil.

The layer thicknesses were very small, which was expected in fine-grained soils due to

their excellent insulating properties. Additionally, due to interparticle forces between

water (or other fluids) and the particles, fluid adsorbs and bonds to the particle surface.

This makes it more difficult to drive off the fluid with a given energy input, and limits the

physical area of influence. The result is thin layers of altered soil surrounding the rock.

As particle size increases layer thickness of an altered zone may be expected to be larger

due to the decreased influence of interparticle forces and perhaps a decreased insulating

effect.

The results of the index tests are shown in Table A.2. It is clear that the plasma

magmavication process was effective in reducing plasticity of the kaolin. However, it

 154

must be noted that since the "zone of influence" is very limited in the kaolin, it is more

suitable to consider only the actual rock volume and mass to determine the physical range

of effective treatment.

TABLE A.2: INDEX PROPETIES OF PROCESSED KAOLIN

(PRETEST AND POST-TEST LAYERS)

%
REDUCTION
D I S T ;V N C E
LAYER IN
FR< 3 M
SOIL THICKNESS LL PL PI PLASTICITY
ROCK
(MM) FROM
(M M)
UNTREATED
SOIL
Processed
Kaolin N/A N/A 79 38 41 N/A
(untreated)
Tan Unaltered
12.31 N/A 74 33 41 0
Kaolin

Pink Altered
4.00 8.31 58 26 32 22
Kaolin
White
Partially-Fused 1.00 3.00 0 0 0 100
Zone
Gray/Black
0 1.00 0 0 0 100
Fused Zone
 155

JDC-1 (control)
Y t , kN/m 3
14.3
w 0.5
G, 2.55
e 0
1.62
M a s s of Rock, N 236.00
Max. Height, c m 30.50
Max. Diameter, c m 30.5

Time, min TC 1, C TC 2, C TC 3, C Volts Amps kW Comments

0 0 0 0 0 0 0
4.5 26.3 20.8 21 400 200 80
15 400 200 80 torch up 7.62 cm
20 52.1 21.1 21.1 400 200 80 off-gas on
25 400 200 80 off-gas off
30 89.3 31.1 22 400 200 80 off-gas on, torch up 7.62 cm
35 1000 43 23 400 200 80 off-gas off
40 59.6 24 400 200 80 off-gas on
42 65 24.5 400 200 80
45 87 25.2 400 200 80 off-gas off, torch up 7.62 cm
50 785 26.2 400 200 80 off-gas on
55 26.2 400 200 80 off-gas off
60 26.2J 400 200 80 pH: 3.0, torch up 7.62 cm
75 26.2 400 200 80 torch off
Average Power Consumed, kW-hr 100
Average Torch Withdrawal Rate, cm/min 0.406
Specific Energy Requirement, kW-hr/N 0.424

1200
 156

JDC-2 (CsCI and Z r 0 ) 2

Tr, kN/m J
14.1
w 0.4
Gs 2 55
e
0
1.48
Mass of Rock, N 52900
Max. Height, cm 40.60
Max. Diameter, cm 43.2

Time, min TC 1, C T C 2, C TC 3,C T C 4, C Volts Amps kW Comments

0 start 6" BOH
15 480 200 96 9" BOH
18 500 200 100 off-gas started
20 99 82 91 440 190 83.6
26 100 95 96 420 185 77.7
28 125 96 97
30 300 97 97
32 600 98 95
33 800 99 99
35 12" BOH, TC 1 out
40 109 99
42 205 99
44 380 99
45 525 99
46 700 99
50 99 TC 2 out
55 15" BOH
57 pH=3.3
75 150 80 18" BOH
77 320
78 700
80 92
91 91 pH=11.2
95 96 21" BOH
100 126 pH=11.4
115 485 24" BOH
131 600
135 27" BOH
155 end of test
Average Power Consumed, kW-hr 230.8
Average Torch Withdrawal Rate, cm/min 0.344
Specific Energy Requirement, kW-hr/N 0.436
 157

T h e r m o c o u p l e R e a d i n g s for JDC-2

900 -i—
 158

J D C - 3 ( M a l a t h i o n a n d C h l o r o e t h y l Methyl Sulfide)
yr, kN/m 3
12
w 0.4
G, 2.55
e 0
1.92
Mass of Rock, N 356.00
Max. Heiqht, cm 30.50
Max. Diameter, cm 38.1

1,
Time, min T C 2, C TC3.C TC 4 , C Volts Amps kW Comments
0 28.3 27.3 28.9 27.8 400 175 70 6" BOH
TC C
5 30.7 27 28.5 27.5 380 200 76
10 99.3 35.7 28.5 27.8 480 200 96
20 99.1 79.7 30.2 34 9' BOH
25 98 97.9 33.1 52.5
30 99 98.2 36.5 79.2
35 99.3 97.9 40.5 91.6
40 99.6 232 96.7 12" BOH, off-gas started
45 335.2 689.3
46
49.4 97.3 400 200 80
TC 2 out, TC 4 w/drawn to
50 535 1317
56.3 75.1 4" and changed

50.8 1230 64.2 74 TC 1 w/drawn to 4" depth

55 70.1 78.1
76.8 82.7 15" BOH

60
65
70
75
85.6
99.7
99.9
85.9
87.2
87
add 1 gal, pH 2.9

80 86.5 18" BOH, pH 11.3

85
90
95
100
100
100.1
100.1
69
95.6
94.3
21" BOH, off-gas stopped,
100 100 94.7 pH 11.4
105 les after this time were
110 und, but digital readers
115 tched accordingly. AJI
120 this time are not reliable. 24" BOH
140 end of test
Average Power Consumed, kW-hr 200.7
Average Torch Withdrawal Rate, cm/min 0.327
Specific Energy Requirement, kW-hr/N 0.564
 159

T h e r m o c o u p l e R e a d i n g s for J D C - 3

Time, min
 160

JDC-4 (LE392 E. coli & Y P H 8 0 S.cerevisiae yeast)

Tr, kN/m 3
16.1
w 0.4
e* 2.55
e< 1.18
Mass of Rock, NI 360.00
Max. Height, cm 35.60
Max. Diameter, cm 35.6

Time, min TC 1, C T C 2, C TC 3, C TC 4, C Volt^ Amps kW Comments

0 29 29 29.2 28.9 48 140 6.72 Torch start at 6" BOH
5 29.8 28.9 29.2 28.9 400 200 80
10 69 29 29.2 28.9 480 200 96
15 92.6 29 29.2 28.9
20 99.7 30.3 29.6 28.9 Torch up 3"
25 750 33 30.6 29
30 36.5 32 2 29 2 TC 1 moved to 4"
35 41 24.2 29.6
40 45.3 36 30 Torch up 3"
45 50.5 38.6 31
50 77 45 31.5
55 99 50 32
60 99.7 68 33 Torch up 3"
65 125 90 35
70 202 96 37
75 423 97 43
pH 2.9, TC 2 moved to 4",
add Igallon to scrubber
80 960 97.1 92 water, torch up 3"
85 97.2 93
90 97.3 96
95 98 96.6
100 98.2 97 Torch up 3"
104 800
105 98.3 TC 3 moved to 4"
110 97.6
115 99
TC 1 and TC 2 moved to
120 112 2", torch up 3"
125 1 1 8 pH 12.4
130 600
135 1100 TC 4 to 4"
140 Torch up 3"
145
150 pH 11.3
160 end of test
Average Power Consumed, kvV-hr 234.7
Average Torch Withdrawal Rate, cm/min 0.333
Specific Energy Requirement, kW-hr/N 0.652
 161

Thermocouple Readings for JDC-4

1200

1000

800 TC @ 30-cm From

Bottom of Chamber
TC @ 46-cm From
600 Bottom of Chamber
TC @ 61-cm From
Bottom of Chamber
400 TC @ 76-cm From
Bottom of Chamber

200

0
0 50 100 200
Time, min 150
 162

YT, k N / m
w
3
JDC-5 All Contaminants w/100-kW Torch)
14.7
0.5
G, 2.55

e
0
1.55
M a s s of R o c k , N 285.00
Max. Height, c m 38.10
Max. Diameter, c m 35.6

Th .e, m i n T C 1, C TC 2, C TC 3, C TC 4, C Volts Amps kW Comments

pH 8.7, start torch 6"
0 42 40.5 38.3 34.8 BOH
5 42.4 40,5 47 34.8 400 200 80
10 45.3 40.4 56.8 34.8 480 200 96
15 52.6 40.5 59.9 35.1 pH8.6
20 67.8 43.2 58.2 35.9 torch up 3"
25 78 56,1 57.8 37.3
30 82.2 80.1 57.6 39.2
35 86.1 89.2 58.8 41.2
off-gas on, torch u p
40 88.5 90.8 60.9 43.9 3"
45 91.2 91.3 63 46.8
50 93 93.6 67 49
55 94.6 99.2 71.7 51.3
60 95.7 248 98 53.1 torch u p 3"
65 95.8 715 98 55.2
70 95.8 717 98.2 57.7
75 96.2 546 111.5 60.7
80 95.1 1050 133 63.5 torch u p 3 "
85 95 1290 409 70.5
90 96.1 571.2 97.1
95 97.2 589 97.2
o f f g a s off, p H 1 1 . 1 ,
100 97.7 609 98.2 torch u p 3"
105 97.7 892 97.1
110 98.4 1125.4 98.8
115 98.6 1346 97
120 98.7 145
125 98.8 206 torch u p 3"
130 98.9 400
135 99 786
140 99.1 1053 e n d of t e s t
Average Power Consumed, kW-hr 205.3
Average Torch Withdrawal Rate, cm/min 0.327
Specific Energy Requirement, kW-hr/N 0.720
 163

T h e r m o c o u p l e Readings for JDC-5

— T C @ 3 0 - c m From
Bottom of C h a m b e r f

-a—TC
Bottom
@ 4of
6 - cCmh aFmr ob m
er / /
- * - T C @ 6 1 - c m From
Bottom of C h a m b e r
— K - T C @ 7 6 - c m From
Bottom of C h a m b e r

^A-^B—a—s—EJ—e—

20 40 6 0
-xxx--x—*r
80 100 120 140 160
Time, min
 164

JDC-6 (All C o n t a m i n a n t s w/200-kW Torch)

YT, kN/m 3
13.8
IV 0.5
G, 2 55
e 0
1.72
Mass o t . lock, N 792.00
Max. Height, cm 38,10
Max. Diameter, cm 47

Time, min TC 1, C T C 2, C TC 3, C T C 4, C Volts Amps kW Comments

pH 10.0, start torch at 9"
0 28.2 28.2 28.2 28.3 BOH
5 28.2 28.2 28.2 28.3 200
10 28.2 28.2 28.2 28.3
15 28.2 28.2 28.2 26.3
20 28.2 28.2 28 2 28 3 torch up 3"
30 28.2 28.2 28.2 28.3
40 28.2 28.2 28.2 28.3 off-gas on, torch up 3"
45 28.2 28.2 28.2 28.3
50 28.2 28.2 28.2 28.3 pH 11.2
55 29.2 28.2 28.2 28.3 TC1 to 7"
60 29.8 28.5 28.2 28.3 torch up 3"
65 30.8 29 28.2 28.3
70 32 30 28.2 28.3
80 35 6 33.2 28.2 28.5 TC2-TC4 to 7"
85 37.8 48.4 29.7 28.7
90 40 42 32.5 29 torch up 3"
100 45.3 61.5 48.5 29.8 offgas off
110 49.8 68.4 65.6 33 •

120 54 76 84.2 43
130 56.1 80.8 88.2 63.3
135 59 88 92.2 76.4 torch up 3"
140 60.7 91.8 95.2 93.5 pH 10.9
145 61.1 91.8 99.1 96.2
150 61.8 91.4 329.8 99.7
155 62.5 91.5 344.7 166.1
160 63.2 92.7 406.8 272.8
170 64.7 95.1 543.7 994.3 TC4 to 3"
180 66.9 95.7 714 415 end of test
Average Power Consumed, kW-hr 600.0
Average Torch Withdrawal Rate, cm/min 0,212
Specific Energy Requirement, kW-hr/N 0.758
 165

T h e r m o c o u p l e R e a d i n g s for J D C - 6

1200

200
Time, min
 166

JDC-7 (Control (Electrode Blew Out))

y , kN/m
T
3
14.2
w 0.5
G s
2.55
e 0
1.64
Mass of Rock, N 93.40
Max. Height, cm 22.90
Max. Diameter, cm 25.4

Time, min TC 1, C TC2.C TC 3.C TC 4 , C Volts Amps kW Comments

0 22.3 22.6 22.3 22.7 start 6" BOH
1 22.5 22.7 22.6 22.8 340 145 49.3
3 226 22.7 22.6 22.6 320 200 64
5 22.6 22.7 22.7 22.8 360 200 72
10 23.3 23.1 22.9 22.8 360 200 72
15 28.8 24.4 24 22.8 300 200 60 9" BOH
20 40.5 26.6 25.7 23 320 200 64
25 53.5 29.2 23.2 340 200 68
30
35
40
68.6
80.4
87.8
f 322
29.2
38.3
34.4
39.8
44.1
23.9
24.9
26.1
320
360
340
200
200
200
64
72
68
12" BOH

45
50
55
91.3
94.7
96.2
65
49
91.4
116.2
7 46.6
49.4
51.6
27.4
29.2
31.5
325
340
340
200
200
200
65
68
68
15" BOH

60 97.4 632.8 55.5 33.6 340 200 I 68 18" BOH

63.5 924 TC 1 w/drawn 2"
65 60.9 36.5 360 200 72 I

front electrode blew out,

68.8 76.5 69.6 41.7 end of test
Average Power Consumed, kW-hr 77.4
Average Torch Withdrawal Rate, cm/min 0.443
Specific Energy Requirement, kW-hr/N 0.829

1000

900

TC @ 30-cm From
800 Bottom of Chamber
TC @ 46-cm From
700 Bottom of Chamber
TC @61-cmFrom
°. 600 Bottom of Chamber

I 500
TC @ 76-cm From
Bottom of Chamber

400

300

:<JU

100

0 H 1 1 1— — r — •• t — r — —,
0 10 20 30
Tm
i e, min
40 50 60 70 80
 167

JDC-8 (TDR)
y , kN/m
T
3
13
w 0.4
G s
2.55
e 0
1.69
Mass of Rock, N 162.00
Max. Height, cm 17 80
Max. Diameter, cm 29.2

Time, min TC 1, C T C 2, C T C 3, C Volts Amps kW Comments

0 20.7 21 20.9 start 6" BOH
5 28.4 21 20.8 420 200 84
10 72.8 21 20.8 440 200 88
15 89.3 36 21.1 445 200 89 9" BOH
20 194 68 25.3 440 200 88
25 1200 94 34.3 440 200 88
30 99 44.7 400 200 80 12" BOH
35 98 54.6 420 200 84
40 99 63.3 380 200 76
46 97 72.1 420 200 84 e n d of test
Average Power Consumed, kW-hr 63.4
Average Torch Withdrawal Rate, cm/min 0.339
Specific Energy Requirement, kW-hr/N 0.391
 168

J DC-9 (C
y , kN/m
T
3
15.12
0.4
G s
2.55
e 0
1.32
Mass of Rock, N 80.06
Max. Height cm 11.40
Max. Diameter, cm 25.4

Time, min TC 1, C T C 2, C Volts Amps kW

0 23 23 0 0 0
23 23 380 200 76
10 23.1 23.1 320 200 64
15 43.8 25.2 320 200 64
20 65.9 34.3 340 200 68
26 87.3 42.5 320 200 64
30 97.6 47.3 300 200 60
35 98.9 54 320 200 64
40.3 107.6 85.2 320 200 64
41 127.9 86.6 320 200 64
Average Power Consumed, kW-hr 44.6
Average Torch Withdrawal Rate, cm/min 0.372
Specific Energy Requirement, kW-hr/N 0.558
140

0 -i 1 1 1 ^ 1 ^—i

0 10 20 30 40 50
Time, min
 169

THIELE KAOLIN COMPANY

P . O . BOX 1 0 5 6 -RIV- •
SANDERSVILLC, G A 31082 1 [11816
T E L (912) 5 5 2 - 3 9 5 1
F A X (912) 5 5 2 - 4 1 3 1

B-80
PRODUCT SPECIFICATION SHEET

G . E . BRIGHTNESS
% MINIMUM 81.0

PARTICLE SIZE

FINER THAN 2 MICRONS, % MINIMUM 85.0

SURFACE AREA
SQUARE METER/GRAM, B . E . T . , TYPICAL 21
OIL ABSORPTION
A S T M 2 8 1 - 3 1 , TYPICAL 44

SCREEN RESIDUE RETAINED

3 2 5 MESH, % MAXIMUM , .03

PH

@ 2 0 % SOLIDS > 3.5 - 5.5

MOISTURE

BULK and BAGS, % MAXIMUM 1.5

B-80 IS A FINE PARTICLE SIZE, PULVERIZED, EAST GEORGIA FILLER CLAY.

SAJCX TRT MADE wist, THE UAD*RTTIADXQF; LH«£ PTTRCNAACN WOL DATERMIAE LB* TURUBUIRY OF PRODUCT* FOR [ B U R P A N I C UUR PTTRPOTE* AND
T Y * ! « V U I C A AO * ^ R R M C Y FOR T PARTICULAR PVTPOAC. N O **J-R*NRR OF MERCKAAUBILTTY. AOR OTHER T V N E T Y , EXPRESS OR A&PFICD, IS
M A D « . SIMILARLY , T » I D E KAOLIN COIVPTOY C A A O O T A U M M T R E Q W I U & U I T ) F O R H I K J OR LIAB'JHIEJ,DIRECT, INDIRECT, OR CCFT*CQ»«TTIAL WFEICH
T

A N Y REXUH FROM OK U O OF 1 M PRODUCT! L S C E W U * , NO LIABILITY N U I U O U L FOR U Y C U I M A D « F N N J E M * O ; O C C U N I A F BY REUOO

OF ANY MCIKOD OF U E OF & C I M O M U .

RSL1001.1QR Revision! 11/01/93

 170

MATERIAL SAFETY DATA SHEET

"?.HE
IL0E. 3K cAx ON LICi 5 S CO M P
A N Y N
D aapete P ofreoParraedp:arer:JanuSam ar
y 2J.2.Smhti
S52a0ndK ersavonililIt. R Soeadoreia 3O t S2 R
Teelev:nisioonneD Naota::. 9M :2-5a5crn2-39253:, *3'
SECT O IN I - HATER A IL D IENTFICATO IN
Trade Name: 5-3G. RC3-2
Chemcial Icentity, Commnc Names: Sydrcvs a/.i^nluai silicate; Kaolir.
CAS Numbe:r 2'32-58-7
S
CE CTO IN II - H A Z A RD O US N
I .
G R
S P T EN T D
S
I/
E N T T I
V NIF
O R M A T
OIN
.itrytsutatlinelessSilitncaan (A ixpl.ha Quartz, CAS *7o3i-66-3) is present at levels ve.r : gra =

A
K CGH I TL VT W
- A - 2 ug w
/ re s cir
a ble d us t
5aohlin\g,/misrelistto
:
soirableasfraanctioO nSH.A Ari Conatmniant with a F£_' of 15 mgn/* total
SE CTO
Note: K IN III - P H Y S
CIA L
C/
H E
aocnilompisosedproodfuce2d9 1-n3a35dwM C
I AL CH A R A C TE RSI
TC
IS
ryateforn,n71and- a6s7Sankaaocliunoouasndsluarry.smA queleouvselu
is
T h e i
n f
o rm a t
i
o n i
n th i
s s
e ct
i
o n is ch ara c te r
is t
i
c o f t
h e dry f
o r
m a
l
.
BaooiolnrgPP
V r e osuinret: m
s ( m H Sgo.):lid Scid SpecificMG en
i
t
lgravityPoiH (nt:20 = 1):
Vaoor Densyti A (R I =1): No Vao(B orutyl AEcvetaapteoraoit=1): n Raet
S
Aoplpuebarainltyce 1anndW Oadteor:r: InO soflu-w
bleheti color, odcr^ess
S ECTO IN
FlaxsthinguP V
I
oiningt (M - F RI E
ehetdodai: UseN AND d)o:t A HA 2
A E0 D
Nopneplica'blFA T
a,lmw * mailbel noLtimtuitrsn: None LEL: N O N
E UEL
E i
s
Spneucsuiaall F h M e
U Firiree F anigdhtinE gxpP ^sroionceduHreas:zards:NoN neone
 171

Thiela Kaolin HSO Sheet

Pace 2

HHIS HAZARD CLASSIFICATION:

1 11
Health: O Flaflir.ability: 0 Reactivity: 0 Personal Protection: E
I
No Acute effects. Prolonged breathing c* excess dust without mask may effect luns
capacity.
I I
Use dust rrask in dustv conditions.

SECTION V - REACTIVITY DATA

Stability: Stable
Incompatibility CHaterials to Avoid): Net Reactive
Hazardous Decomoosition or Byproducts; None
Hazardous Polymerization: Will net occur

SECTION. VI - HEALTH HAZAHp DATA

ROUTES OF ENTRY: Inhalation? Yes Skin? NO Ingestion? No Hazard

HEALTH HAZARDS (ACUTE AND CHRONIC)

Oazcmet (tstrahydro-3.5-dinethyl-2H-i,3,S-thiadiazine-2-thione^ biccide used

in sorct slurry shipments may causa lacriraat.on (temporary tearing of the eyes;.

F i l l e r grace kaolin may contain tract levels of crystalline s i l i c a . IARC has

detarrained that there is United evidence of the carcinogenicity of crystalline
silica to humans. The IARC conclusions have been questioned. Our medical experts
h a v e a d v i s e d us that there 1 s n o credible evidence that ...low levels of crystalline
silica such as found in our product would make i t a carcinogen.
r
Long te m exposure to high levels of kaolin aust cculd cause a reduction *n l^ng
capacity.

Carcinogenicity: NT?? IARC Monographs? OSHA Regula:ed?

Not Listed No. Listed Not Listed

Signs and Syrapta-ns of Exposure: Exposure to slurry clay containing seme biccidss may
cause lacrimation.

Hedical Conditions Generally Aggravated by Exposure: None currently known.

Emergency and First Aid Procedures: Remove to fresh a i r , wash skin with water,
and flush eyes with water.
 172

T r i i e l e K a o l i n M$0 S h e e t

P a g e 3

S E C T I O N V I I - P R E C A U T I O N S F O R S A F c H A N D L I N G A N D U S E

S t e p s t o b e t a k e n i n C a s e M a t e r i a l 1« R e l e a s e d o r S p i l l e d :

O r y m a t e r i a l m a n b e s c s o a e d u o , t h e n v e s n a r e a w i t h w a t e r . S s l e a s e d o r s p i l l e c J

s l u r r y car. c e w a s h e d a w a y w i t h w a t e r .

W a s t e D i s p o s a l M e t h o d :

N o s s e c i a l d i s p o s a l a e t h o d r e o u : r e d .

P r e c a u t i o n s t o b e t a k e n i n H a n d l i n g a n d S t o r i n g :

S o i l l e c m a t e r - ; a i m a y c a u s a s l i p p e r y c o n d i t i o n s w h e n w e t .

O t h e r P r e c a u t i o n s :

S n o u i d b e k e p t frora w a s t e e f f l u e n t t o a v o i d h i g n t u r c i d l t y .

S E C T I O N V T I I - C O N T R O L M E A S U R E S

R e s p i r a t o r y P r o t e c t i o n ( S p e c i f y T y p e ) :

U s e K S H A / N I O S H o r O S H A / N I O S H a p p r o v e d r e s p i r a t o r i f o p e r a t i n g c o n d i t i o n s c a u s e heavy
d u s t i n g .

V e n t i l a t i o n : L o c a l E x h a u s t A s n e e d e d t o c o n t r o l d u s t S p e c i a l N o

M e c h a n i c a l ( G e n e r a l ) .AS n e e d e a t o c o n t r o l d u s t O t h e r N o

P r o t e c t i v e G l o v e s : N o t R e q u i r e d Eye P r o t e c t i o n : S a f e t y g o g g l e s f o r h e a v y d u s t i n g

O t h e r P r o t e c t i v e C l o t h i n g o r E c u l p a e n t : N e t r e s i n r t d

W o r k / H y g i e n i c P r a c t i c e s : x o s o e c i t l p r a c t i c e o t h e r t h a n w a s n w i t h s o a o a n d w a t * r .

S E C T I O N I X - T R A N S P O R T I N F O R M A T I O N

c ? A W a s t e « : N o t R e g u l a t e d

D O T C l a s s i f i c a t i o n : N o t R e g u l a t e d

I N T E R N A T I O N A L

U N I : N o t R e g u l a t e d
 APPENDIX B

SCANNING ELECTRON MICROSCOPY OF JDC-1 TO JDC-6

•

Fe

CI0.000 1
keV 10.220
• Ed •
CLuarbseolr:: Kaoli0n.00E3H
0-•keVIc 0 counts
Element: H 1
K a o l i n

C h i - s q d = 6.38 L i v e t i m e = 9 0 . 0 S e c .
S t a r . d a r d l e s s A n a l y s i s
Element; R e l a t i v e E r r o r N e t . E r r o r
k - r a t i o ( 1 - S i g m a ) C o u n t s ( 1 - S i g m a )
0 - K 0.54599 + / - 0 . 0 0 6 7 1 1 0 5 7 9 + / - 1 3 0
S i - K 0 . 2 0 6 1 3 + / - 0 . 0 0 3 5 4 1 6 3 7 5 */- 2 8 1
A l - K 0 . 2 3 7 3 S + /- 0 . 0 0 3 4 4 1 8 3 0 1 + /- 2 6 5
F e - K 0 . 0 0 8 1 1 + / - 0 . 0 0 2 6 1 2 1 1 + /- 66
K -K 0 . 0 0 2 4 3 + / - 0 . 0 0 1 3 9 1 4 0 8 0

A d j u s t m e n t F a c t o r s K L M
2 - B a l a n c e : 0 . 0 0 0 0 0 . 0 0 0 0 0 . 0 0 0 0
S h e l l : 1 . 0 0 0 0 1 . 0 0 0 0 1 . 0 0 0 0

P R O Z A C o r r e c t i o n A c c . V o l t . = 2 0 k V T a k e - o f f A n g l e = 3 9 . 6 2 d e g T i l t = 30 de
N u m b e r o f I t e r a t i o n s = 8

e m e n t Jc-ratio Z A F A t o m % E l e m e n t W t % E r r . S t o i c h -
( c a l c . ) W t % ( 1 - S i g m a ) i o m e t r y
O - K 0 . 2 9 6 2 8 2 .084 7 3 67 6 1 . 7 4 + / - 0 . 7 6 2 4 . 0 0 0
S i - K 0 . 1 1 1 8 5 :: . 6 2 4 12 35 1 8 . 1 7 +/- 0.31 4 . 0 2 3
A l - K 0 . 1 2 8 8 0 i.505 1 3 71 1 9 . 3 8 • 0.28 4 . 4 5 7
F e - K 0 . 0 0 4 4 0 l .241 0 19 0.55 + / - 0.18 0 . 0 6 1
K - K 0 . 0 0 1 3 2 l .252 0 08 0.16 +/- 0.09 0 . 0 2 6
T o t a l 1 0 0 0 0 1 0 0 . 0 0

S t o i c h i o m e t r y r e s u l t s a r e b a s e d u p o n 24 O x y g e n a t o m s
 A TSI D E A D T I M E : 21%

P-J 0.000
L I
J1 K
T I

mm
KEV
FE

10.220

•
Cursor: 0.000 K E V 0 counts
LABEL: K A O L I N -2^

ELEMENT: H 1
L3HE

Kaolin

C h i - s q d = 5.05 Livetime 90.0 Sec.

Sta.idardless A n a l y s i s
Element Relative Error Net Error
k-rat io (1-sigma) Counts (1-Sigma)
0 -K 0.54128 + / - 0.00699 9836 +/ 127
Si-K 0.20956 • / - 0.00366 15613 +/ 273
Al-K 0.24013 + / - 0.00357 17364 253
Fe-K 0.00729 + / - 0.C0275 179 +/- 67
K -K 0 . 0 0 1 7 4 «•/- 0 . 0 0 1 4 4 94 + /- 78

Adjustment F a c t o r s K L M
Z-3alance: 0.0000 0.0000 0 . 0000
Shell: 1.0000 1.0000 1.0000

PROZA C o r r e c t i o n Acc.Volt 20 kV Take-off Angle=39.62 deg Tilt - 30 deg

Number of I t e r a t i o n s = 8

Element k-ratio ZAF Atom % Element Wt % E r r . S t o i c h -

(calc.) Wt % (1-Sigma) iometry
0 -K 0 .29335 2.093 73 . 3 8 61.41 + / - 0 .79 2 4 . 0 0 0
Si-K 0.11357 1.624 12 . 5 6 18 . 4 5 + / - 0 . 3 2 4 . 107
Al-K 0 . 13014 1.501 13 . 84 19 . 53 + / - 0 . 2 9 4 .526
Fe-K 0 . 00395 1.241 0.17 0 . 49 +/- 0.18 0.055
K -K 0.0C094 1.253 0 .06 0.12 +/- 0.10 0.019
Total 100.00 100.00

Stoichiorr.etry results a r e b a s e d u p o n 24 O x y g e n atoms

G Leicvetrauedm
•eorgViaFS:Tec4h400Research Institute Display - SpD titimlee:: 9170%
01
Al

1!
MgBM" T'i Fe

• 00.00 keV A. 5s 102.20

•Cursor: 00.20 keV 0 counts •
Label: DS
V
A #2^ H»3
Element: H 1 |
*'A * I

CBI-SCC = 7 . 1 5 IVETIME = 9 0 . 0 SEC.

£T&R.DA.RDLESS A N A L Y S I S
E 1 ENVEN T RELATIVE ERROR NET ERROR
>; • R A T I O 1 COUNTS (1-SIGMA)
C -3 273 -/- 35
o -x c
5 0 6 6 3 «•/ 0 .00439 26083 252
FE-1 553 -/- 247
AI - X 0 1 7 6 6 2 ... 0 .00215 31352 387
SI -X : 2 3 0 2 5 »/- J . 00230 41891 -/- 455
TI-X J 01409 */~ 0 .00035 1079 »/- 65
067S7 2747
XE-X
? -K
o
:. . C 0 1 2 6
+ /-
+ /-
0
0
.00331
. 0CC56 187 «/-
134
83
MG-X J.00000 *•/- 0 .00001 0 */- 0
X -X 3 .00328 0 .00C47 386 -/- 55

A C " U S — — - -_ • A C T O R S K
Z - 3 A L I R CE 0.0000 0.0000 0 0000
SHELL: 1.0000 1.0000 1.0000

??.GZA C C I RE C T I O N ACC . V O L T . " 1 5 KV TAKE-OFF ANGLE=2 8 . DEG

S O S E R = : : RERATIONS 7

ELEMER,- !< - R A T I O ZAF ATOM % ELEMENT WT % E R R . S T D ICN-

(CALC.) WT % (1-SIGMA) IC SE T R Y
0 -7. 0 .28569 .079 7 3 . 1 1 59.41 24 .000

*}- 6.57
n •
AL - X .09960 .501 1 0 . 9 1 14 .95 R/- 0 . I S .530
;. 1 2 9 8 4 .507 1 3 . 7 1 19.55 */- 0 . 2 1 4 .502
7:. - •" 3 .00795 L .2 0.5S Z.Zi . . J I
FE- X .03827 I .244 1.68 4.76 0.23 .531
? —X
kff-x
.00071
.00000
. 634
1 .7 37
3 5 o.;0
0 . 0 7
0 . 0 0
0.12
0.00
»/- 0-.CS
+/- o.:o c
R . C24
.00 0
:< 0 .00185 :. . 2 1 8 0 . 23 <-/- 0.02 C .037
TOT.IL 100.00 100 . 00

S T O I C * : : C :SETRY RESU S ARE BASED UPON 24 CXYGEN ATOR.S

Georgia Tech R e s e a r c h I n s t i t u t e D i s p l a y - Spectriml

• VFS: 2 800 LU e t irne: 90

Dea d t ime: 16%

A1
0

ill I
•
LLJl 0.000
K Ti
keV
—
Fe
A
c
Le
10.220

Cursor; 0.000 keV 0 counts

•
L a b e l : DSVA #4^
Element: He 2

D S W A *i

C h i - s q d = 3.63 L i v e t i m e = 9 0 . 0 S e c .
3tar.da_rdl e s s A n a l y s i s

R e l a t i v e E r r o r N e t E r r o r
k - r a t i o (1-• S i g m a ) C o u n t s (1- S i g m a )
C - X —- 102 •/- ' 60
0 - X 0 . 5 2 4 1 8 + / - c 0 0 6 9 1 1 6 6 9 0 «-/- 2 2 0

F e - 1 393 + /- 197

A l - K 0 . 1 7 5 7 0 *./- 0 0 0 2 7 2 1 9 5 9 8 +/- 303

S i - * 3 . 2 3 9 7 1 + /- 0 . 0 0 3 1 3 2 6 9 7 4 + /- 352
T i - S 0 . 0 1 3 4 6 0 0 0 1 8 6 6 3 7 • /- 38
0 . 0 4 3 7 6 0 . 0 0 3 7 6 1 0 9 6 +/-

X -X 3 . 0 0 3 1 9 + /- 0 0 0 1 2 2 2 3 3 *•/- 89

A c j u s ~ e r .t F a c t o r s K L
Z-EaLar. 0 . 0 0 0 0 0 . 0 0 0 0 0.
S h e l l : 1 . 0 0 0 0 1 . 0 0 0 0 1.

? R 0 Z A C o r r e c t i o n A c c . V o l t . = 15 k V T a k e - o f f A n g l e = 2 8 . 4 5 c e g T i l t = 15 d a g
N'umber o f I t e r a t i o n s = 8

< - r a t i o Z A F A t o m % E l e m e n t W t % E r r . S t o i c h -
( c a l c . ) W t % ( 1 - S i g m a ) i o m e t r y
0 . 2 9 4 2 6 2 .072 7 3 . 9 7 6 0 . 9 6 + /- 0.30 2 4 . 0 0 0
0 . 0 9 3 6 3 1 . 4 3 8 1 0 . 5 6 1 4 . 6 8 * ] -0 . 2 3 3 . 4 2 7
3 . 1 3 4 5 7 1 . 4 9 6 1 3 . 9 2 2 0 . 1 4 ./«• 0.26 4.516
3 . 0 0 7 5 6 1 .241 0.38 0 .94 +/- 0.13 0.123
3 . 0 2 4 5 6 1 .249 1.07 3.07 «•/- 0.26 0 . 3 4 5
3 . 3 0 1 7 9 1 . 2 2 2 0.11 0.22 + /- Q . 0 8 0 . 0 3 5
1 0 0 . 0 0 1 0 0 . 0 0

St:ichicir.etry r e s u l t s a r e b a s e d u p o n 2 4 Oxyger. atcrr^s

 178

GEORGIA TECH RESEARCH INSTITUTE DISPLAY - SPECTRUM1

• VFS: 1900 LIVETIME: 90

DEADTIME: 21%
A 1

•
• FP

TI

• 0.000

EE2
KEV 10.220

•
CURSOR: 0.020 KEV 0 counts
LABEL: DSVA # 6 , Area I
ELEMENT: H 1
0 H i

D
W
CShA -i
sq d #=
6, A 4 5
.er4a 1
S
EeltamndenatrdleR sselaA t
i
v e nalysisEroL r
viem
it e = 900. Sec.
Netnst (1Erm
or.
0Fe-LK k - ra ti
o (
1 -
- 04.5223 +0/-0.0632 12031999 163 S gim a)
*•/-
+/ -
• /- Co
u
170
-
Sg
i
A
S iK
-K-l 0 0 1
20...9
112
953
242
01 + +0 0 0../-0
/-/-0 0334146 1168595043 272
+ /-
+ /-
297
47

AK T
FdK
-
ei
K
-
u
jsmt e n0
t0 1 . 1F7 9
a 7
ct
o r
s ++ 0
0
/- 00 .
.0
0 5183S3K 2159475L 109
+ /-
+ /-

S-hBealK
Z al:-nc00e.:0287 +0/-0.00170 0..1
00
000 150 7..0
0
10 000 39010
00 0..0
00
00
0
M

0
P
R
N O Z
um Aber C oforeItcetiorantionsAc= cV . o= 6.tl 15 kV Take-of AngelT =396.2 deg
k(c-raalctio.) ZAF A om
t W%t %Eelmen(1t-SgimWat)% o
imilteE
=rr. 30Stoicdheg-
r
t
y
EelO mentK 00 2..8812828853..889186183 21..24512705..73 7283 24460..2003
A K-
l -000.09.84 1400242..0223 10455..22 1192.6.03 310150118048
+ /-

TS-K
K
-ii 00. .07050315832..41195 0314..28 903.52.2 1202441
0
F eK-K «•/- 05

Total-
K 1000.0 1000.0
Stoichiometry results are based upon 24 Oxyqen aotms
 179

G e o r g i a T e c h R e s e a r c h I n s t i t u t e D i s p l a y - S p e c t r u m !

• VFS: 2 200 L i v e t i m e : 90
Deadtime: 1 ? %

1 t i i i i i i
r i 1

B
A1
(]

Fe

1! 1
L
U I mi Ti

COBi
e

• 0 . 0 0 0 k e V 1 0 . 2 2 0

•
f
C u r s o r : 0 . 0 B 0 k e V 0 c o u n t s

L a b e l : DSVA # 6 , A r e a 2^
E l e m e n t : H 1 H
[H [

CHI-SQD = 4 . 8 5 L I V E T I M E * 9 0 . 0SEC
STAR.DARDLESS A N A L Y S I S
E1EMENT RELATIVE ERROR NET ERROR
K-RATIO (1 -SIGMA) COUNTS ( 1- S I G M A )
O -K 0.44057 + / - 0 .00617 11788 + / - 165
FE- L 488 + / - 169
O

AL-K 0.15623 + / - .00307 14407 +A- 266

SI-K 0.24341 + / - 0 . 00356 21134 */- 309
TI-K 0.01621 + / - 0 .00247 578 */- 88
FE-K 0.13359 + / - 0 .00603 2506 */- 113

ADJUSTMENT FACTORS K L M
Z-BALANCE: 0.0000 0.0000 0 .0000
SHELL: 1.0000 1.0000 1. 0000

PROZA C O R R E C T I O N ACC.VOLT. 15 KV TAKE-OFF ANGLE=39.62 DEG TILT = 3 0 DEG

NUMBER O F I T E R A T I O N S * 6

ELEMENT K-RATIO ZAF ATOM % ELEMENT WT % E R R . S T O I C H -

(CALC.) WT % (1-SIGMA) IOMETRY
0 -K 0.28277 1.825 67.72 51. 61 •/- 0 . 7 2 24.000
AL-K 0.10669 1.396 11.59 14.89 0.27 4 .106
SI-K 0.15623 1 .383 16.15 21.61 0.32 5 .723
TI-K 0.01040 1.219 0.56 1 .27 • /- 0 .19 0.197
FE-K 0.08574 1.239 3 .99 10.62 +/- 0 . 4 8 1.415
TOTAL 100 .00 100.00

STOIEHIOMETRY RESULTS A R E BASED UPON 2 4 OXYGEN ATOMS

G pevieacedtrituim
•eorgVaiFS:T6ec02h0 Research Institute Display - SL
D nlee::916%
m 0
s\
1

D A1
•
1!
1
J 1 Ti re
• 00.00 keV M M
A
102.20
• 0 counts •
Cursor: 00.00 keV
L
Eleam
beel:nt:DSVA1#5, Area 3^ H
E H I
Chi-sqd = 5.89 Livetime = 90.0 Sec.
Standardless Analysis
Element Relative Error Net Error
k-ratio (1 - S i g m a ) Counts (1 - Sigma )
O -K. 0.46S98 + / - 0 .00573 1 5 7 0 2 *••/- 193
Fe-L 613 + /- 190
A1 -• K 0.16077 + / - 0 .00268 17547 */- 293
Si-K 0.24236 0 .00315 26500 >/- 344
o

Ti-K 0.01485 +/- .00205 666 */- 92

Fe-K 0.11603 + / - 0 .00500 2740 + /- 118
Adjustment F a c t o r s K L M
Z-Balance: 0.0000 0 . 0000 0 . 0000
Shell: 1.0000 1 . 0000 1 . 0000
PROZA C o r r e c t i o n Acc.Volt 15 kV Take-off Angle=39.62 deg Tilt = 30 d e g
Number o f I t e r a t i o n s = 6

Element k-ratio ZAF Atom % Element wt % E r r . S t o i c h -

(calc.) Wt % ( 1 - Sigma) i o m e t r y
0 -K 0.29874 1 .800 69 . 3 5 53 . 7 9 + / - 0 . 6 6 24 . 000
Al-K 0.10307 1 .395 10.99 14 . 3 8 + /- 0 . 2 4 3 . 804
Si-K 0-15538 1 .379 15.73 21 . 42 *•} - 0.28 5 .445
Ti-K 0.00952 i .225 0.50 1 .17 + /- 0 . 1 6 0.174
Fe-K 0.07439 1 .243 3 .42 9.25 */ - 0 . 4 0 1 .182
Total 100.00 100.00

Stoichiometry results are based upon 24 Oxygen atoms

GEORGIA TECH RESEARCH I N S T I T U T E D I S P L A Y - SPECTRUMI

• VFS: 1 0 0 0 L I V E T I M E :
DEADTIME:
9 0
1 0 %

— a

• 13

FE

| FE

L
1 J

Jl J L
T I
I F E
.... -
• 0 . 0 0 0

•
K E V

E E
10.220

•
CURSOR: 0 . 0 0 0 K E V 0 COUNTS

LABEL: OSVA #8, AREA ^

ELEMENT: H 1 L -

DSWA # 8 ,Area 1

Chi-sqd = 2 . 3 2 L i v e t i m e = 90.0 Sec.

Standardless Analysis
Element Relative E r r o r Net • Error
k - r a t i o (1-Sigirva) Counts (1-Sigma)
0 -K 0.39973 0.00881 5765 + / - 1 2 7
Fe-L 277 + / - 1 2 2
A l - K 0.15346 + / - 0 .00403 7402 *•/- 1 8 8
Si-K 0.21222 0 .00459 9931 + / - 2 1 5
Ti-K 0.01871 0 . 00344 359 + / - 6 6
Fe-K 0.21087 + / • 0 .00980 2132 • 9 9
C - K 63 + / - 2 0

Adjustment Factors K L K
2-Balance: 0.0000 0.0000 0.0000
Shell: 1.0000 1 .0000 1.0000

PROZA C o r r e c t i o n Acc.Volt. 15 KV T a k e - o f f Angle=39.62 d e g T i l t = 3 0 d e g

Number o f I t e r a t i o n s = 5

Element k - r a t i o ZAF Atom % Element Wt % Err. S t o i c h -

(cal c . ) Wt % (1-Sigma) iomet ry
0 - K 0.26 1 61 1.811 65 .29 47 . 39 + /- 1 . 0 4 2 4 . 0 0 0
A l-K 0.10 3 71 1.431 12 .13 14.84 0.38 4.458
S i-K 0.13 8 90 1.399 15 .25 19 .44 +/- 0.42 5 .608
T i-K 0.01 2 24 1. 196 0 .67 1.46 */- 0 . 2 7 0 . 2 4 8
F e-K 0.13 8 01 ]. 2 2 2 6 .66 16 . 87 +/- 0.78 2.443
T otal 100 .00 1 0 0 .00

Stoichiometry r e s u l t s a r eb a s e d upon 2 4O x y g e n atoms

 182

G e o r g i a Tech R e s e a r c h I n s t i t u t e D i s p l a y - Spectrunl

• VFS: 1900 Liv e t i m e : 90

Dea d t ime: 19%

Si

[) A

• Fe

uJ
1

Fe
Ti
^jIL
• • EBB •
K
I —.
0.000 JLkeV 10.220

Cursor: 0 . 0 2 0 keV 0 counts

L a b e l : DSWA #B, Area 2^
Henent: H 1 g Q f~ , g ^

DSWA # 8 , A r e a 2

Chi-sqd = 3.84 Livetime = 90.0'Sec

Standardless Analysis
Element Relative Error Net Error
k-ratio (1-Sigma) Counts (1-Sigma)
O -K 0.45119 +/- 0.00663 12258 *•/- 130
Fe-L 665 +/- 173
Al-K 0 . 1 5 1 7 6 +/• 0 . 00291 13355 + /- 256
Si-K 0.20927 +/- 0.00333 18450 +/- 294
Ti-K 0.01546 0.00235 559 +/- 85
Fe-K 0 . 1 7 2 3 2 «•/- 0 . 00641 3282 +/- 122
C -K 183 + /- 27
K -K 136 +/- 40

Adjustment F a c t o r s L M
2-Balance: 0.0000 0 .0000 0000
Shell: 1.0000 1.0000 1.0000

PROZA C o r r e c t i o n A c c . V o l t .= 15 kV Take-off Angle=39 62 deg Tilt = 30 d e g

Number o f I t e r a t i o n s = 6

Element k-ratio ZAF Atom % Element Wt % E r r . S t o i c h -

(calc. ) Wt % (1-Sigma) iometry
0 -K 0.29405 1.762 68.74 51.82 + / - 0 . 7 6 24 . 0 0 0
Al-K 0.09890 1.427 11.10 14 . 1 2 + / - 0 . 2 7 3 . 877
Si-K 0.13639 1.393 14.36 19 . 0 0 */- 0.30 5.013
Ti-K 0 .01008 1.208 0 . 54 1.22 <-/- 0 . 1 9 0 .188
Fe-K 0.11231 1.233 5.26 13 . 8 5 + / - 0 . 5 1 1.837
Total 100 . 00 100.00

Stoich . ometry r e s u l t s are b a s e d u p o n 2 4 Oxygen atoms

 183

Georgia Tech Research I n s t i t u t e D i s p l a y - Spectruml

• VFS: 1100 Livetime:

Oeadtime:
90
19%

Al

Fe

•
1!
Fe

Ti

• • 0.000 keV

•HI
1 0 . 2 2 0

•
0 c o u n t s
Cursor: 0.000 keV

Label: DSVA # 8 , Area 3^

Element: H 1 ESQ (

DSWA 1 3 , AREA 3

CHI-SQD = 2 . 5 8 LIVETIME = 9 0 . 0 SEC.

STA.NDARDLESS A N A L Y S I S
ELEMENT RELATIVE ERROR NET ERROR
K-RATIO (1-SIGMA) COUNTS ( 1 - SIGM.
0 -K 0.43413 +/- 0.00871 7 3 2 7 + /- 147
FE-L 4 4 4 + /- 144
AL-K 0.17560 + / - 0.00384 9 5 9 9 */- 210
SI-K 0.19433 0.00415 1 0 6 4 2 + /- 227
TI-K 0.01211 + / - 0.00289 273 + / - 65
FE-K 0.17968 + /- 0.00820 2126 9 7
C -K 1 0 1 + /- 24
K -K 0.00414 + / - 0.00190 1 4 5 + /- 66

ADJUSTMENT FACTORS K L M
Z-BALANCE: 0 .0000 0.0000 0.0000
SHELL: 1.0000 1.0000 1.0000

PROZA C O R R E C T I O N ACC.VOLT = 1 5 KV TAKE-OFF ANGLE=39 62 DEG TILT = 3 0 DEG

NUMBER O F I T E R A T I O N S = 6

ELEMENT K-RATIO ZAF ATOM % ELEMENT WT % E R R . S T O I C H -

(CALC.} WT % (1-SIGMA) IOMETRY
O -K 0.28273 1.776 67 . 31 50.21 +/- 1 . 0 1 24,000
AL-K 0 .11436 1.423 12 . 93 16.27 •/- 0 . 3 6 4.611
SI-K 0 .12656 1.411 13 6 3 17 . 86 +/- 0 . 3 8 4 .862
TI-K 0.00789 1 .205 0 . 43 0.95 •/- 0 . 2 3 0.152
FE-K 0.11702 1.230 5 53 14 , 39 +/- 0 . 6 6 1.971
K -K 0.00270 1.183 0 . :I 8 0.32 +/- 0 . 1 5 0 .062
TOTAL 100 . 00 100.00

STOICHIONETRY RESULTS ARE BASED UPON 2 4 OXYGEN ATOMS

G e o r g i a T e c h R e s e a r c h I n s t i t u t e D i s p l a y - S p e c t r u m i

• V F S : 14 0 0 L i v e t i m e :

D e a d t i m e :
9 0

1 7 %

° -i

A l

H
• []

ii
1 F e

J L J L
K
T i
A ,
0 . 0 0 0 k e V 1 0 . 2 2 0

•
• E E •
C u r s o r : 0 . 0 0 0 k e V 0 c o u n t s

L a b e l : D S V A # 9 , A r e a ^

E W n t : H 1 Q Q , 1 flS

^Jim W J , ni?d X
C h i - s q d = 3 . 3 6 L i v e t i m e = 9 0 . 0 S e c .
S t a n d a r d l e s s A n a l y s i s
Element R e l a t i v e E r r o r N e t E r r o r
k - r a t i o (l - S i g m a ) Counts ( 1-Eigm
0 -K 0 . 3 8 6 5 0 */- 0 . 0 0 7 6 4 6 1 2 1 + /- 121
Fe - L 129 + /- 67
A l - K 0 . 2 1 6 9 8 + /- 0 . 0 0 4 2 3 11129 + /- 217
S i - K 0 . 2 5 6 4 6 + /- 0 . 0 0 4 7 7 13178 + /- 245
T i - K 0 . 0 2 3 4 0 + /- 0 . 0 0 1 9 9 493 + /- 42
Fe-K 0 . 1 1 2 2 8 */- 0 . 0 0 5 1 4 1246 * / - 57
C - K 0 */- 0
K - K 0 . 0 0 4 3 9 */- 0 . 0 0 1 0 4 143 */- 34

A d j u s t m e n t F a c t o r s K L M
Z - B a l a n c e : 0 . 0 0 0 0 0.0000 0 . 0 0 0 0
S h e l l : 1 . 0 0 0 0 1.0000 1 . 0 0 0 0

PROZA C o r r e c t i o n A c c . V o l t = 15 k V T a k e - o f f A n g l e = 3 9 62 d e g T i l t = 30 dt
Number o f I t e r a t i o n s = 6

Element k - r a t i o ZAF Atom % E l e m e n t Wt % E r r . S t o i c h -

( c a l c . } Wt % (1-Sigma) i o m e t r y
0 - K 0 . 2 4 4 2 0 1 . 9 5 7 6 3 . 7 3 47 . 8 0 + / - 0 . 9 5 24 .000
A l - K 0 . 1 3 7 0 9 1 . 3 6 0 1 4 . 7 4 1 8 . 6 4 + / - 0 . 3 6 5 . 5 5 1
S i - K 0 . 1 6 2 0 4 1 . 3 9 7 1 7 . 2 0 2 2 . 6 4 •>-/- 0 . 4 2 6 . 4 7 6
T i - K 0 . 0 1 4 7 8 1 . 2 2 2 0 . 8 0 1.81 + / - 0.15 0 . 3 0 3
Fe-K 0 . 0 7 0 9 4 1 . 2 3 7 3 . 3 5 8.76 + / - 0 . 4 0 1 . 2 6 2
K - K 0 . 0 0 2 7 7 1 . 1 9 7 0 . 1 8 0 . 3 3 + / - 0 . 0 3 0 . 0 6 8
Total 1 0 0 . 0 0 1 0 0 . 0 0

Stoichioir.etry r e s u l t s a r e b a s e d upon 24 Oxygen atoms

G
•eorgai Tech Research Institute Display - SL
peivcetraeudtim
D t
i
m iee:: 9190%
VFS: 1500

Al
•
B

ii

• 00.00
m
•
J L
T i JL
Te

hk eV e 102.20
•
Cursor: 00.00 keV 0 c o un t
s
Label: DSVA #9, Area \
Element: H 1 ^ Qj [
C
uintahnr-istqddairpd,le=ssAre2
S A a9.7na4lysis Lviem it e = 900. Sec.
Eelment R k ealatitiove (1E
-
r -
S g
i rmora) C
*7- N oetnst E
u -
S
(1 g
irm
ora)
0FeK -- L03.8791 +0/-0.0747 6284573 13722 *-./-
*/-

A S-K K
i-il 0002 2..7
06
31 12 7 *+ •/-/000/--0.00000434530920 1115648253433 22276983
+ /-

T K
-
FdeuK -sm 0.
01.1F19
00aX2 7 + /-

•/-000468K 132631L 5208

FT*

AC K-
o

j
Kh-BealK t e nt c t
ors • /- 36

SZ :al-nc00e.:0352 +/-001 00 09..90

000 10
00 20
1 09..0
00
00
M
0 0 10..0
0 00
00
0
P
R
NO umZ Aber C oforIetectiorantionsAc= cV . o6lt.
15 kV TaW ke-otf% AnSgetloE=ic3rh9r6..-2 deg Tilt = 30 deg
Eelmentk(c-aralctio. ) ZAFA om
t % EelW (
1-
S gim a)
mtent% 0039..42o2i54m 0..80e50rty
0AK K-0 2.45.64128631139..5581 6133777341774.79.4 000324...706 6012.327
*/- 1 ..59006
S-K -
l 0
ii 000.121.2704891123..2844 1086365 2144.2.91
+ /-
+ /-

00.55
TF eK
-
K- 00. 69 6 6 1 2
. 3 8 3
+ /-

2 9 8
6.
o.ca
2
TKotalK -00.0223 11.99 1000010510002.0.70
Stoichiometry results are based upon 24 Oxygen aotms
•eorgVaiFS:Tec1h200Research Institute Display - SL
G peivecaetrdutim
D nlee:: 9200%
tim
•trr

Fe

Ti
EH!
• A .

• 00.00 keV 102.•20

Cursor: 00.00 keV
Label: DSVA #9, Area 3 0 counts
Element: H 1 ^ Qj [
CHI-SQD = 3 . 1 1 LIVETIME = 9 0 .0 SEC.
STANDARDLESS A N A L Y S I S
ELEMENT RELATIVE ERROR NET ERROR
K-RACIO -SIGMA) COUNTS ( I -SIGMA
0 -K 0.44911 + / - 0 .00886 6489 +/- 128
FE-L 250 +./•- G2
AL-K 0.19583 + / - J .00438 9164 •/« 205
SI-K 0.25200 + /- 0 .00495 11814 +/- 232
TI-K 0.01784 + / - 0 . 00187 343 +/- 36
FE-K 0 . 0 8 2 7 7 «•/- Q .00790 839 +/- NO
C -K 56 +•/•- 21
K -K 0.00245 + / - 0 . 00101 74 '3 0

ADJ US TMENT F A C T O R S
Z-BALANCE;
SHELL:
0.0000
1.0000
K
i
0.0000
1.0000
M
0000
0000
:
PROZA C O R R E C T I O N ACC. VOLT. 15 KV TAKE-OFF ANGLE=39.62 DEG TILT = 3 0 DEG
NUMBER OF I T E R A T I O N S = 6

ELEMENT K-RATIO ZAF ATOM % ELEMENT WT % E R R . S T O I C H -

(CALC.) WT % (1- SIGMA) IOMETRY
O -K 0.28338 J . 870 67 . 97 52 . 9 9 • /- 1.05 24.000
AL-K 0.12356 1 .366 12 . *3 16.87 + /- 0 , 3 8 4 .532
SI-K 0.15901 1 . 387 16 . 11 22.05 •7 - 0 . 4 3 5 .689
TI-K 0.01126 1 .233 0 . R
.9 1.39 + /- 0 . 1 5 0.210
FE-K 0.05223 .1 .247 2. ?9 6.51 + /- 0.62 0 . 845
K - K 0.00155 1 . 203 0. 10 0.19 «-/ - 0 . 0 3 0 .035
TOTAL 100. 00 100.00

Stoichiometry results a r e b a s e d u p o n 24 Oxygen atoms

• iaFS:lec4n020rcesearcninstitute uisplay - specL
ueorgV truviem
D i ee::920%
aedttiim
m 0
SI M
Al
•
• n

1! 11
•0•0.00J K Ti Fe

Cursor: 00.00 keV

t
e c
keV

Label: DSVA #10, Area £

s0 counts
102.20
•
Element: H 1 ,
DSWA # 1 0 , A r e a 1

Chi-sqd = 4 . 4 6 Livetime = 90.0 Sec.

Star.dardless Analysis
Element Relative Error Net Error
k-ratio (1 -Sigma) Counts (1 - S i g m a )
0 -K 0 . 4 5 5 2 1 * / - 0 .00639 11960 + / - 168
F e - L 244 + / - 90
Al-K 0 . 2 1 1 6 1 + / - 0 .00334 18009 + / - 284
Si-K 0.26308 • / - 0 .00374 22429 • / - 319
Ti-K 0 . 0 1 8 8 8 + / - 0 . 00134 660 + / - 47
Fe-K 0.04861 • / - 0 .00277 896 + / - 51
C -K 101 + / - 2A
K -K 0.00261 + / - 0 .00070 142 • 38

Adjustment F a c t o r s K L
Z-Balance: 0.0000 0.0000 0
Shell: 1.0000 1.0000 1.

PROZA C o r r e c t i o n Acc.Volt.= 15 kV Take-off Angle=39.62 deg Tilt = 30 d e g

Number o f I t e r a t i o n s = 6

Element k-ratio ZAF Atom % Element Wt % E r r . S t o i c h -

(calc.) Wt % (1-Sigma) i o m e t r y
0 -K 0 .28447 1 .897 18 53.96 *./-- 0 . 7 6 2 4 . 0 0 0
Al-K 0.13224 1 .346 33 17.80 */- 0.28 4.694
Si-K 0.16440 1 .385 li 39 22.78 • / - 0.32 5 .771
Ti-K 0.01180 1 .243 0 62 1.47 • 0.10 0.218
Fe-K 0 .03038 1 .253 1 30 3 .80 <•/- 0 . 2 2 0 . 4 8 5
K -K 0.00163 1 .209 0 10 0 .20 + / - 0 .05 0 .036
Total 100 UO 100.00

Stoichiometry results a r e b a s e d u p o n 24 O x y g e n atoms

 1 8 8

G e o r g i a T e c h R e s e a r c h I n s t i t u t e D i s p l a y - S p e c t r u m 1

• V F S : 17 0 0 L i v e t i m e :

D e a d t i m e :
9 0

1 6 %

mmwM

M Si

A l

1 n

18

iL JL K
T i F e
A . ,

• • 0 . 0 0 0
1
k e V

E E
1 0 . 2 2 0

•
C u r s o r : 0 . 0 0 0 k e V 0 c o u n t s

L a b e l : D S V A # 1 0 , A r e a 2^

E l O T e n t : H 1 , ^

DSWA # 1 0 , A r e a 2

Chi-sqd = 2 . 4 1 Livetime =90.0 Sec.

Standardless Analysis
Element Relative Error Net ' Error
k-ratio -Sigma) Counts (1-Sigma)
0 -K 0.43423 +/- 0 00952 7843 +/- 172
Fe-L 96 +/- 75
Al-K 0.19194 + / - 0 00393 11230 • /- 230
Si-K 0.27476 * / - 0 00454 16104 */- 266
Ti-K 0.02725 • 0 00179 655 */- 43
Fe-K 0.06921 +/- 0 00640 876 • /- ei
C -K 650 */- 55
K -K 0.00261 + / - o 00094 97 • is

Adjustment F a c t o r s K L H
2-Balance: 0 .0000 0 .0000 0. 0000
Shell: 1.0000 1.0000 1 . 0000

PROZA C o r r e c t i o n Acc • V o l t = 15 kV Take-off A n g l e = 3 9 62 d e g

Number of I t e r a t i o n s > = 6

Element k-ratio ZAF Atom % Element Wt % E r r . S t o i c h -

(calc.) Wt % (1-Sigma) i o m e t r y
0 -K 0.27116 .936 67 . 39 52.48 + / - 1.15 2 4 . 0 0 0
Al-K
Si-K
Ti-K
Fe-K
0.11986
0.17157
0 .01702
0.04322
1
1 .356
1 .374
1 .236
1 .248
12.37
17.24
0.90
1.96
16.25
23.57
2 .10
5.39
0.33

+ / - 0.14
+/- 0.50
4 .406
+/- 0.39 6 .141

07
0..3077
K -K .204 0.10 + / - 0.07 0.321
Total
0.00163 1 000.20
100.00 1 . 00
0

Stoichiometry results a r e b a s e d u p o n 24 Oxygen atoms

 189
U E U T Y I D IFCFL.II n e b c t i r u i I R I B L I i u m u t a p l a y - o p e c x r u n i

• V F S : 2 4 0 0 L i v e t i m e :

D e a d t i m e :
9 0

3 4 %

S i

A l

ii 1 n

F e

•
J 0 . 0 0 0
L
K
T i
.A

k e V
F e

A .
1 0 . 2 2 0

C u r s o r : 0 . 0 0 0 k e V 0 counts
•
L a b e l : D S V A # 1 0 , A r e a ^

E l e m e n t : H 1 |

DSWA # 1 0 , A r e a 3

Chi-sqd = 3.8 6 Livetime = 90.0 Sec.

Standardless Analysis
Element Relative Error Net Error
k-ratio (1-Sigma) Counts (1 - S i g m a
0 -K 0 . 4 0 4 2 3 + /- 0 . 0 0 6 4 8 9 6 1 1 + /- 154
Fe-L 333 */- 83
Al-K 0 . 1 8 3 0 6 *•/- 0 . 0 0 3 3 8 1 4 0 9 7 + /- 260
Si-K 0 . 2 9 3 3 2 */- 0 . 0 0 4 0 4 2 2 6 2 9 */- 312
Ti-K 0 . 0 2 1 2 4 */- 0 . 0 0 2 9 7 672 + /- 94
Fe-K 0 . 0 9 4 3 5 */- 0 . 0 0 3 9 0 1S73 +/- 65
C -K 34 23
K -K 0 . 0 0 3 8 0 + /- 0 . 0 0 0 8 6 166 + /- 42 */-
Adjustment F a c t o r s K L M
Z-Balance: 0.0000 0.0000 0.0000
Shell: 1.0000 1.0000 1.0000

FROZA C o r r e c t i o n A c c . V o l t = 15 kV Take-off Angle=39 62 d e g Tilt = 30 d e g

Number o f I t e r a t i o n s * 6

Element k-ratio ZAF Atom % Element Wt % E r r . S t o i c h -

(calc.) Wt % (1-Sigma) iometry
0 -K 0.25479 1.952 65.27 49 . 7 4 + / - 0 . 8 0 24 . 0 0 0
Al-K 0.11538 1.357 12 . 1 9 1 5 . 66 + / - 0.29 4.481
Si-K 0.18438 1 .367 18.90 25.28 +/- 0.35 6.948
Ti-K 0 . 01339 1 .230 0.72 1.65 • / - 0.23 0.265
Fe-K 0 , 05947 1 .242 2.78 7.39 • / - 0.31 1.021
K -K 0 .00240 1.202 0.15 0.29 +/- 0.07 0.057
Total 100.00 100.00

Stoichiometry results a r e b a s e d u p o n 24 O x y g e n atoms

 APPENDIX C

X-RAY DIFFRACTION RESULTS OF JDC-1 TO JDC-6

 191

R E A L T I M E D I S P L A Y

F i l e : 2 8 8 1 2 2 . R A H I t e r a t i o n 1 o f 1
S i d e : R I G H T 2 T h » t a / T h # t « : ?e.euu
S a n p l c : K A O L I N ( R E P E A T ) I n t e n s i t y ;

110 C P S

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 192

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D/MAX-B PEAK FINDING PROGRAM VI. 8

DATA F I L E : A:\DATA\Z00121.RAW
C O L L E C T E D ON 2 3 - O C T - 9 8 AT 08:20:18
SAMPLE IDENTIFICATION: KAOLIN
DATE OF PEAK SEARCH: 11-30-98 AT 0 8 : 1 0 : 1 3

START 2THETA: 10.000 STOP 2THETA: 70.000

STEP SIZE: 0.200 SCAN SPEED: 1.000

PEAK FINDING PARAMETERS

THRESHOLD VALUES 5.0, 10.0

RELATIVE CUTOFF INTENSITY 0.0
T Y P I C A L F U L L W I D T H - H A L F MAXIMUM 0.20
M I N I M U M F U L L W I D T H - H A L F MAXIMUM 0.08
PEAK SPAN 15

B A C K G R O U N D - S U B T R A C T E D DATA W I L L BE I N FILE A:\DATA\Z00121.BSD

P E A K S DATA WILL BE I N T H E NEW FILE A:\DATA\Z00121.PKS
T H R E S H O L D DATA WILL BE I N FILE A:\DATA\Z00121.THD

PEAK 2-THETA D-SPACE I(REL) I(CPS) FWHM

1 12. 200 7, 2489 100. 00 3271. 3 0. 649

2 15. 600 5 .6758 1 20 39. 4 2. 1 0 8
3 17. 600 5. 0351 0 58 19. 0 0. 100
4 19. 800 4803 3 90 291 . 0 2 .176
5 20. 400 1 .3499 8 16 267. 0 2, 285
6 21. 200 4 .1875 (-• 85 224 . 1 1 .599
7 22. 400 3 . 9658 3 28 107 . 2 2. 0 0 0
2609 . 7
Dp

24 . 800 ).5872 79. 78 0 .670

9 26 .600 3 . 3484 5. 56 181 . 9 0. 718
10 28. 200 3 .1620 1 52 49 . 8 2. 400
11 32. 400 ?.. 7 6 1 0 .1 4 2 . 46 . 6 4 .400
12 34 . 800 2 . 5759 6 73 220 . 0 1 .600
13 35. 800 2 .5062 S 03 262. 8 1 .531
14 37. 400 2 .4026 7 82 255. 8 0. 745
15 38 . 200 2 .3541 12. 38 405 . 0 1 .9 3 6
L6 39. 000 2 .3076 7 09 231. 9 0 .799
17 41 .000 2 .1996 2 12 69. 4 3 .382
8 45. 400 1 .9961 6 64 217, 3 0 .947
19 46 . 600 1 .9474 2 95 96. 6 2 .000
20 47 .800 1 .9013 3 .63 118 . 8 2 .993
21 49. 200 1 .8504 2 11 68 . 9 2, 199
22 50. 800 1 .7958 4 . 49 146 . 9 0. 731
2 3 55 .000 3 .6682 7 74 253 . 3 1. 355
3 4 56 . 6 0 0 1 .6248 3 .73 122. 2 1 .585
2 5 58 . 000 1 .5889 2 12 69 . 2 2. 600
26 59. 800 1 .5453 2 78 91 0 3 .792
27 62 . 200 1 .4913 6 77 221. 3 0. 712
28 63 . 800 1 .4577 1 .65 54 0 0. 100
29 65 .000 1 -4336 3 .12 69. 4 3 . 392
3 0 66 . 600 1 4030 3 . 50 49 0 0. 100
31 68 . 000 I . 3775 I 47 48 . 0 0. 100
32 69 . 800 i 3463 2 .02 66 2 5. 593
 194

R E A L T I M E D I S P L f t V

7 i l e : 2 3 9 0 9 T \ J W W I t e r a t i o n 1 o f 1
S i J * : R I G H T - T
I n t e n s i t y :
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RX OF T 05SITR7ED LSIES* 33
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294,, 59336 A FLE2Z - TI3FE2X TM I 04/ CLVOSPD EfL,S Y N321873..63 0055.. 1n4'i 10q 2263
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2I20033 /C CRUN D
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D M/ AXB - PEAK FN IDN IG PROGRAM VIS .

D
C A
O TLA L ECT E FD ILEO :NAD \:03A
-
A TU AG 2\00-90e99R.AAT W12:56:51
S
D AAM TEPLEOFD I EN PEA TKF
IC
IAST EOIAN RC :H: D SWA9-#29-98 AT 03:30:28
S
STTAER PTS2IZ THEE
:TA: 100.2.00000 SSC TAONPS 2T
PHED
EETA :: 10
.7050.000
PEAK FN IDN IG PARAMETERS
R E L A TVI E THC REU SHT OOF LFDN I V
TAE L
N USETISY:: 5. 0 .00, 10.0
T
MY
NIIPC
M IUA ML FF U
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PEAK SPAN : 15
BACKGRO PUEANDKSU
-SBTRA D CT
A TAED W DA
LIT
L ABE WL ILINBE T H E INN E
WFILEFILAE D
\: AA TD
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THRESHOLD DATA WL IL BE IN FILE AD \:ATAZ \00099T .KD
PEAK 2T -HETA DS -PACE I(PEL) I(CPS) W FH M
12 2116.0.20000 45.2.4266699 1531.9.285 27509.7 .2 30.9.77092
4 2213.6.40000 43.1.7190896 1 12 4-.6
85 3 6 754.0
.0 0.63060.551
 196

5 2 6 . 0 0 0 3 ., 4 2 4 3 0 0 . 0 0 5 0 5 . 3 0 . 7 1 1

6 2 9 . 8 0 0 2 ., 9 9 5 7 1 4 . 2 3 7 2 . 0 - 5 4 . 8 4 7
7 3 0 . 8 0 0 2 ,, 9 0 0 7 3 9 . 2 0 1 9 3 . 2 0 . 7 0 3
3 3 ] . 0 0 0 2 ., 7 1 2 2 6 1 . 7 7 3 1 2 . 5 0 , 6 6 5
Q
3 5 . 0 0 0 2 ., 5 6 1 6 4 S . 1 8 2 4 3 . 7 0 . 6 9 7
1 0 3 6 . 2 0 0 2 .. 4 7 9 4 3 5 . 7 2 1 3 0 . 7

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1 1 4
1 1 3 6 . 8 0 0 2 .. 4 4 0 4 2 4 . 1 0 1 2 1 . 9 7 5 2
1 2 2 9 . 0 0 0 2 .. 3 0 7 6 1 9 . 4 1 9 3 . I 0 . 9 1 0
1
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3 1 6 4 . 4 0 0 1 ., 4 4 5 5 3 3 . 0 0 1 6 6 . 9 0 . 9 0 6
3 2 6 5 . 4 0 0 1 .. 4 2 5 8 1 1 . 0 7 5 6 . 0 5 3 . 9 4 4

3 3 6 6 . 2 0 0 \ , 4 1 0 5 1 0 . 4 8 5 3 . 0 2 2 . 1 7 8
3 4 6 9 . 6 0 0 1 . 3 4 9 7 1 2 . 2 6 6 2 . 0 5 . 5 2 0

3 5 7 C . 4 0 0 1 ,. 3 3 6 3 1 7 . 2A 8 7 . 2 1 . 3 6 1

2 6 7 3 . 6 0 0 1 . 3 1 6 8 7 . 5 1 3 8 . 0 0 . 1 0 0

3 7 7 4 . 0 0 0 1 . 2 3 0 0 1 9 . 5 6 9 3 . 9 0 „ 9 3 5

3 3 7 4 . 8 0 0 1 . 2 6 8 2 1 2 . 0 9 6 1 . 1 1 1 6 1

3 3 P E A K S W E R E F O U N D A N D W R I T T E N T O T H E P E A K S F I L E

peak F W K H is less than step width

 197

R E A L T I M E D I S P L * V

F i l e : 2 * 9 1 9 2 . P A W I t e r a t i o n i
of 1
! RtGJIT 2 - I J * t 4 / 7 h # u :
I n t e n s i t y ; 86 CFS

1
ii il 11
ii
t a n , . j i , 11 a I* i . - \\\

AT 5« b y

DSWA /4

ERSOE(DEG): 0.300 3 STRONGEST LIKES DATA BASE: 1 KUHEET? OF OBSERVED LINES- 38

11 PHASE(S) HATCHED SREQ= 0 NELEH= 6 0 AL SI X TI fE

SLOW SEARCH O P CT 0F7 IS 320.

DHAX- 8.838 D K 3 - 1.265

MATCHED WITHCCT O T E S S I 7 ! PREFERRED 0RIEHTATI0H

JCPDS / PHASE OP IC/IOB PDP/HATCH SPATTERS

15. 776 AL6 S I 2 012 / MULLITE, SYK 19.31 1.0 46/ 31 83

33, 20 i£ F E 22.75 0.1 5/ 4 10
1,1257 AL FE 24.91 0.1 5/ 5 13
24, 536 FE2-I FE2* TTl-r 0! / O L V O S P i m , SYS 26.89 0.6 12/ 9 23

12, 234 FE2 SI 04 34.51 0.5 8/ 6 15

3 4 , 180 02 TI / RUTILE, SYM 48.74 0.1 8/ 5 13

22,1118 F E 7 S I 010 71.10 0.4 36/ 16 41
29,1361 T I 0 / BGMGQOIITE 89.77 0.4 V 3 7
10, 63 TI2 03 142.06 0.2 14/ 6 15
16, 895 FE2 03 154.63 0.5 13/ 7 IS
9, 309 TI3 05 165.05 L O 22/ 8 21
D / M A X - B
V I . 8

D A T A F I L E : A : \ D A T A \ Z 0 0 1 0 2 . R A W

C O L L E C T E D O N 0 4 - A U G - 9 8 A T 1 2 : 3 8 : 5 8

S A M P L E I D E N T I F I C A T I O N : D S W A # 4

D A T E O F P E A K S E A R C H : 9 - 9 - 9 8 A T 1 0 : 0 1 : 2 6

S T A R T 2 T H E T A : 1 0 . 0 0 0 S T O P 2 T H E T A : 7 5 . 0 0 0

S T E P S I Z E : 0 . 2 0 0 S C A N S P E E D : 1 . 0 0 0

P E A K F I N D I N G P A R A M E T E R S

T H R E S H O L D V A L U E S : 5 . 0 , 1 0 . 0

R E L A T I V E C U T O F F I N T E N S I T Y : 0 . 0

T Y P I C A L F U L L W I D T H - H A L F M A X I M U M : 0 . 2 0

M I N I M U M F U L L W I D T H - H A L F M A X I M U M : 0 . 0 8

P E A K S P A N : 1 5

B A C K G R O U N D - S U B T R A C T E D D A T A W I L L B E I N F I L E A : \ D A T A \ Z 0 0 1 0 2 . B S D

P E A K S D A T A W I L L B E I N T H E N E W F I L E A : \ D A T A \ Z 0 0 1 0 2 . P K S

T H R E S H O L D D A T A W I L L B E I N F I L E A : \ D A T A \ Z 0 0 1 0 2 . T H D

> E A K 2 - T H E T A D ~ S P A C E I ( R E L ) I ( C P S ) P W H M

1 1 6 . 2 0 0 5 . 4 6 6 9 6 4 . 0 9 3 1 3 . 4 0 . 6 7 3

2 2 1 . 8 0 0 4 . 0 7 3 6 1 4 . 1 1 6 9 . 0 3 9 . 8 3 9

2 2 3 . 4 0 0 3 . 7 9 8 6 1 4 . 7 2 7 2 . 0 4 1 . 2 2 2

4 2 6 . 0 0 0 3 . 4 2 4 3 1 0 0 . 0 0 4 8 9 . 0 0 . 8 7 2

5 2 7 . 6 0 0 3 . 2 2 9 3 1 0 . 0 2 4 9 . 0 0 . 1 0 0

6 2 9 . 6 0 0 3 . 0 1 5 5 1 6 . 1 6 7 9 . 0 *******
7 3 0 . 8 0 0 2 . 9 0 0 7 4 4 . 5 6 2 1 7 . 9 0 . 6 8 0

3 3 3 . 0 0 0 2 . 7 1 2 2 5 0 . 0 1 2 4 4 . 6 0 . 4 7 0
9
3 4 . 0 0 0 2 . 6 3 4 7 6 . 3 4 3 1 . 0 0 . 1 0 0 #
1 0 3 5 . 0 0 0 2 . 5 6 1 6 5 8 . 4 4 2 3 5 . 3 0 . 6 7 6

1 1 3 6 . 2 0 0 2 . 4 7 9 4 4 6 . 7 8 2 2 3 . 7 0 . 7 2 5

1 2 3 5 . 8 0 0 2 . 4 4 0 4 2 7 . 7 3 . 1 3 5 . 6 0 . 9 5 4

1 3 3 9 . 2 0 0 2 . 2 9 6 3 25. 3 6 124.0 0 . 1 0 0 if
1 4 4 0 . 8 0 0 2 . 2 0 9 9 7 1 . 1 3 3 4 7 . 3 0 . 6 3 5

1 5 4 2 . 4 0 0 2 . 1 3 0 1 3 6 . 3 1 1 7 7 , 5 0 . 5 1 8

1 6 4 4 . 2 0 0 2 . 0 4 7 4 1 2 . 6 8 6 2 . 0 4 4 . 8 2 1

1 7 4 8 . 0 0 0 1 . 8 9 3 9 1 5 . 7 5 7 7 . 0 - 3 . 6 9 6 #
1 3 4 9 . 2 0 0 1 . 8 5 0 4 1 3 . 2 9 6 5 . 0 4 2 . 9 2 2

1 9 5 0 . 6 0 0 1 . 8 0 2 5 7 . 9 8 3 9 . 0 4 2 . 4 0 5

2 0 5 3 . 4 0 0 1 . 7 1 4 4 1 4 . 7 2 7 2 . 0 3 . 8 9 6

2 I 5 3 . 8 0 0 1 . 7 0 2 6 2 1 . 1 8 1 0 3 . 6 1 . 1 6 4

2 2 5 4 . 8 0 0 1 . 6 7 3 8 1 1 . 2 5 5 5 . 0 5 9 . 0 7 6

2 3 5 6 . 2 0 0 1 . 6 3 5 4 1 1 . 2 5 5 5 . 0 5 6 . 7 6 3

2 4 5 7 . 4 0 0 1 . 6 0 4 0 3 9 . 6 9 1 9 4 . 1 0 . 4 7 4

2 5 5 8 . 4 0 0 1 . 5 7 8 9 2 0 . 6 5 1 0 1 . 0 1 . 3 1 2

25 5 9 . 6 0 0 1 . 5 5 0 0 7 . 5 7 3 7 . 0 0 . 1 0 0 4
2 7 6 0 . 6 0 0 1 . 5 2 6 8 4 9 . 4 2 2 4 1 . 7 0 . 6 4 6

2 3 6 1 . 8 0 0 1 . 5 0 0 0 1 2 . 4 7 6 1 . 0 - 1 9 . 6 7 6

2 9 6 3 . 4 0 0 1 . 4 6 5 9 1 4 . 7 2 7 2 .0 6 . 4 3 1

30 6 4 . 2 0 0 1 . 4 4 9 6 2 7 . 6 0 1 3 4 . 9 0 . 9 2 4

3 1 6 5 . 4 0 0 1 . 4 2 5 8 1 0 . 4 3 5 1 . 0 4 4 . 5 5 6

3 2 6 6 . 2 0 0 1 . 4 1 0 5 9 . 8 2 4 8 .0 6 2 . 6 9 9

3 3 6 9 . 6 0 0 1 . 3 4 9 7 1 1 . 6 6 5 7 . 0 2 . 4 7 9

3 4 7 0 . 4 0 0 1 . 3 3 6 3 1 8 . 5 5 9 0 . 7 0 . 9 4 0

3 5 7 1 . 4 0 0 1 . 3 2 0 0 6 . 9 5 3 4 . 0 0 . 1 0 0

33 7 2 . 4 0 0 1 . 3 0 4 3 6 . 9 5 3 4 . 0 0 . 1 0 0

3 7 7 4 . 0 0 0 1 . 2 8 0 0 2 5 . 8 7 1 2 6 . 5 0 . 5 3 0

3 3 7 4 . 8 0 0 1 . 2 6 8 2 9 . 4 7 4 6 . 3 0 . 9 1 3
 199

F
Si
dl
e
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M
R
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H1
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5
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l DSIPLAV
SaHPel: DSW
t tr «6 f£) Iteration 1 of 1
T)
Intensity : 38 CPS

D
WSA /6
ERR O
3
2 RD (P
EH
C
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3.S(0)0M AT
C3E
HD S
TRO
NG
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MTA1
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1 0N UM BE
R
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FGO B
SE
R
V
A
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DSILM
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K
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AR
C HTI F OEP C UT13.43
OF IS 320.
M D HA AT
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8
. 38
T
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ITAOTIN
C
JP
2 5 D , S417/ FE5PHASE T I 08 / O LV OS
N
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I0/9.BP
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TE
2RN
0
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LCA1PE8.5 P 8.5 CL1 1.5 15277..25 0025.. 4/ 4 1133
1
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22511,,157540M LM G FE( A L FE )
2 / 04
SPNIEL, FE
RRA
IN 19602.,53 0062.. 84// 64 2103
1
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L
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2 1
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211467,,, 524316655 FMM
G- F
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N 323..02 009..° 180// 78 2247 -
4
29765..95 0099.. 1110// 86 2270
5 , 4 5
3126,, 323948 M 1 M G
G2 A 2
FE 2 SPIE20404 / MAGNEO SIFERR
TIE,32D0916..49 0069., 89// 67 2204
 200

11?9/,762791K FE
G F0E22 04 / MAGNE TE I, S YN332024..93 0095.. 9/57 2147
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1229341,,222308020C A (SIM G A L PE )R A DSVG I2T IEO,0D 6T

A L
U MN
A
IN336380..48 0062.. 1204//175 221
/

N M
NAG 2 T 04
I0SI2 06 N IC O I
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9
3254,,652705K4 5 T 1
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31252!,,628547487CCAA3 NCL2(06SI 03 )2D
A OIPDSIE 445560..09 0092.. 6564//2248 18003
226*/891081N AS72.5 FE 7.5 TI 2.P 5YRT 0I2E,S 46639..75 0101.. 1100//67 2204
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3225,438476N FEA
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A R C A INE
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A R C A N Y N 6
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/ V

NA L 3 /
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N
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890.8 02. 30/ 12 41
D/MAX-B PEAK FINDING PROGRAM VI . 8

DATA F I L E : A:\DATA\Z00115.RAW
C O L L E C T E D ON 2 0 - O C T - 9 8 A T 0 9 M l : 07
SAMPLE IDENTIFICATION: DSWA # 6
DATE OF PEAK SEARCH: 1 1 - 3 0 - 9 8 AT 0 7 : 2 1 : 2 3

START 2THETA 1 0 . 0 0 0 STOP 2THETA 70.000

STEP SIZE: 0 . 2 0 0 SCAN SPEED: 1.000

PEAK FINDING PARAMETERS

THRESHOLD VALUES 5.0, 10 . 0

RELATIVE CUTOFF INTENSITY 0 . 0
T Y P I C A L F U L L W I D T H - H A L F MAXIMUM 0 . 20
M I N I M U M F U L L W I D T H - H A L F MAXIMUM 0 . 08
PEAK SPAN 15

B A C K G R O U N D - S U B T R A C T E D DATA W I L L BE I N FILE A:\DATA\Z00115.BSD

P E A K S DATA W I L L BE I N T H E NEW FILE A:\DATA\Z00115.PKS
T H R E S H O L D DATA WILL BE I N FILE A:\DATA\Z00115.THD

PEAK 2-THETA D-SPACE I(REL) I(CPS) FWHM

1 1 6 . 4 0 0 c
:> 4 0 0 7 7 7 8 7 3 6 8 5 0 . 6 3 5
2 1 8 . 2 0 0 4 8 7 0 4 1 3 1 0 6 2 0 8 0 . 7 8 9
3 2 6 . 0 0 0 3 4 2 4 3 8 8 2 3 4 1 7 5 0 . 7 0 2
4 3 0 . 0 0 0 2 9 7 6 2 2 0 9 2 9 9 0 1 . 2 3 1
5 3 0 . 8 0 0 2 9 0 0 7 5 2 . 7 3 2 4 9 5 0 , 6 6 8
6 3 3 . 2 0 0 2 6963 9 3 9 5 4 4 4 6 0 . 6 1 9
7 3 5 . 2 0 0 2 5475 8 8 7 3 4 1 9 3 0 , 6 6 2
8 3 6 . 2 0 0 2 .4794 5 6 4 1 2 6 6 9 0 . 5 4 5
9 3 7 . 0 0 0 2 4276 3 3 4 0 1 5 8 0 0 . 9 2 4
LO 3 9 . 2 0 0 2 2963 3 9 9 4 • 1 8 9 0 0 . 1 0 0
.1 4 0 . 2 2099 100 00 4 7 3 2 0 . 6 2 1
1 2
1 3
1 4
4 2
4 4
4 8
800
. 6 0 0
. 2 0 0
. 0 0 0
2 1206
2 0474
1 8 9 3 9
4 7
1 5
8
2 0
0 2
6 7
2 2 3
7 1
4 1
3
1
0 - 9 4
0 . 6 6 8
1 . 9 8 5
. 2 8 0
1 5 4 9 . 4 0 0 1 8 4 3 4 1 5 9 1 7 5 3 0 . 7 4 9
1 6 5 0 . 8 0 0 7 9 5 8 7 . 8 2 3 7 0 3 3 . 9 5 0
1 7
1 8
1 9
5 3 .
5 4
5 4
4 0 0
. 0 0 0
. 8 0 0
i i
I
I
7 1 4 4
6 9 6 7
6 7 3 8
1 6
3 7
1 3
9 1
. 4 7
7 4
8 0
1 7 7
6 5
0

0
"i
1 . 6 1 2
0 . 6 9 5
1 7 . 1 6 1
2 0 5 6 . 4 0 0 I . 6 3 0 1 1 2 3 2 5 8 3 0 . 7 7 8
2 1 5 7 . 2 0 0 6 0 9 2 1 3 3 0 6 3 0 1 . 5 5 2
2 2
2 3
5 8
6 0
. 4 0 0
. 6 0 0
i
I . 5 7 8 9
5 2 6 8
2 4
5 4
. 7 3
6 4
1 1 7
2 5 8
0
5
0 . 1 0 0
0 . 6 4 4
2 4
2 5
6 2
6 2
. 0 0 0
. 6 0 0
i
I . 4 9 5 6
. 4 8 2 7
1 6
1 3
. 0 7
5 8
7 6
6 4
0
3
2 . 3 8 8
1 . 6 0 0
2 6
2 7
2 8
6 3
6 4
6 5
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. 2 0 0
4 0 0
i
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4 4 9 6
4 2 5 8
1 4
2 9
9 .
. 1 6
5 6
7 2
6 7
1 3 9
4 6
0
9
0
3 . 8 3 9
0 . 9 3 0
4 0 3
5 0 .
3 9 6 6 . 4 0 0 I . 4 0 6 8 9 . 0 9 4 3 0 44 . 7 3 6
 202

R E A L T I M E D I S P L A V

File : 268116.UAH Iteration 1 of 1

Side : RIGHT Z T h e ta/The U : 7 0 . QWA
S a w p l e : DSWA 1t8 ( C E N T E R ) Intensity : 38 CPS
 203

D
E W
SRR AOR D (/E
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OF IS 320. EL EH - 0 A
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C
J3P 3 D, S20/ A L PHAS
E
FE / 1 7 O9 . P
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4 CHPA
4 tT1T0E
2344,, 513860 T FE I 2X-02FE2x T1IX
/
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Y ,NSY N221722..03 007..1 180//79 2148
1152,, 728746 A F EL 26S SII204013 MULL
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T IE,S YN 22976.6.41 0160.. 387//262 1563
22951,,364117TIFE50 TI 08 /
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213181,,,21771606 T AIL20203 4. SI 02 . M HU2O N T0H O X
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N437740..66 0.101. 5159//299 7246
3 , 4
4116,, 869543 A 00 L82 0FE 2 SI
0.2
51473,.22 07. 7395//1353 9400
FE 3 6
221929,,, 763025431 C 2H 2I 0FE 04 . 2FER HR2OS0L 663212..22 006.1, 2635//1235 6365
/
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FEH034 0 H H
/
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N771063.,67 007.1. 4370//1193 5353
31052,,002136C20A L
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N 871872..81 0122.. 1104//56 1131
33771,,449385AL H 2
33TH SI3 A 1 X
. 0 87675..70 0072.. 2140//150 213?
3187,, 558363 C / L
FEI3 005( 0 H ) GOETH06 TE 8
I 1901230..09 100.1. 25/191 2249
20/
9 , 3 0 9 T
324189,,,226179143A LH-3.A
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/ G O ETHT E
I 11116403..25 001.1. 3390//1131 2395
2190,, 4631 T A L I230T 3I B
I B S
TIE 1077600..42 0022.. 1172//65 1163
23961,,19633SIAL 2
LC( 0 H )3 GB IE 22416667..31 006.1. 3162//150 213?
/
7, 324 A IB5T
 204

D / M A X - B P E A K F I N D I N G P R O G R A M V I . 8

D A T A F I L E : A : \ D A T A \ Z 0 0 1 1 6 . R A W

C O L L E C T E D O N 2 0 - O C T - 9 8 A T 0 9 : 5 0 : 0 6

S A M P L E I D E N T I F I C A T I O N : D S W A # 8 ( C E N T E R )

D A T E O F P E A K S E A R C H : 1 2 - 8 - 9 8 A T 1 1 : 3 8 : 5 6

S T A R T 2 T H E T A : 1 0 . 0 0 0 S T O P 2 T H E T A : 7 0 . 0 0 0

S T E P S I Z E : 0 . 2 0 0 S C A N S P E E D : 1 . 0 0 0

P E A K F I N D I N G P A R A M E T E R S

T H R E S H O L D V A L U E S : 5 . 0 , 1 0 . 0

R E L A T I V E C U T O F F I N T E N S I T Y : 0 . 0

T Y P I C A L F U L L W I D T H - H A L F M A X I M U M : 0 . 2 0

M I N I M U M F U L L W I D T H - H A L F M A X I M U M : 0 . 0 8

P E A K S P A N : 1 5

B A C K G R O U N D - S U B T R A C T E D D A T A W I L L B E I N F I L E A : \ D A T A \ Z 0 0 1 1 6 . B S D

P E A K S D A T A W I L L B E I N T H E N E W F I L E A : \ D A T A \ Z 0 0 1 1 6 . P K S

T H R E S H O L D D A T A W I L L B E I N F I L E A : \ D A T A \ Z 0 0 1 1 6 . T H D

P E A K 2 - T H E T A D - S P A C E I ( R E L ) I ( C P S ) F W H M

1 1 6 . 2 0 0 5 . 4 6 6 9 6 8 . 0 1 3 1 7 . 6 0 . 6 4 9

2 1 8 . 0 0 0 4 . 9 2 4 1 1 2 . 2 1 5 7 . 0 0 . 1 0 0

3 1 9 . 2 0 0 4 . 6 1 9 0 1 3 . 2 8 6 2 . 0 4 0 7 . 2 8 3

1 2 0 . 4 0 0 4 . 3 4 9 9 1 8 . 2 1 8 5 . 0 0 . 1 0 0

5 2 1 . 4 0 0 4 . 1 4 8 8 1 1 . 7 8 5 5 . 0 0 . 1 0 0

6 2 3 . 4 0 0 3 . 7 9 8 6 1 3 . 7 1 6 4 . 0 4 . 9 8 6

7 > 2 4 . 8 0 0 3 . 5 8 7 2 1 1 . 7 8 5 5 . 0 0 . 1 0 0 A
CD

2 6 . 0 0 0 3 . 4 2 4 3 1 0 0 . 0 0 4 6 6 . 9 0 . 8 9 7

9 2 7 . 6 0 0 3 . 2 2 9 3 9 . 4 2 4 4 . 0 0 . 1 0 0 *
1 0 2 9 . 8 0 0 2 . 9 9 5 7 1 7 . 7 8 8 3 . 0 1 . 9 4 8

1 1 3 0 . 6 0 0 2 . 9 1 9 2 6 1 . 5 1 ' 2 8 7 . 2 0 . 7 1 4

1 2 3 3 . 0 0 0 2 . 7 1 2 2 7 4 . 6 4 3 4 8 . 5 0 . 4 3 7

1 3 3 5 . 0 0 0 2 . 5 6 1 6 6 8 . 0 2 3 1 7 . 6 0 . 6 8 6

1 4 3 6 . 0 0 0 2 . 4 9 2 7 6 5 . 9 2 3 0 7 . 8 0 . 9 0 0

1 5 3 6 . 8 0 0 2 . 4 4 0 4 2 0 . 3 5 9 5 . 0 2 . 6 9 2

1 6 3 9 . 2 0 0 2 . 2 9 6 3 2 5 . 7 0 1 2 0 . 0 0 . 1 0 0 i
1 7 4 0 . 6 0 0 2 . 2 2 0 3 4 7 . 1 6 . 2 2 0 . 2 0 . 4 7 5

1 8 4 2 . 4 0 0 2 . 1 3 0 1 2 3 . 5 6 1 1 0 . 0 0 . 1 0 0

1 9 4 4 . 0 0 0 2 . 0 5 6 3 1 9 . 7 0 9 2 . 0 0 . 1 0 0 *
2 0 4 7 . 0 0 0 1 . 9 3 1 8 8 . 7 8 4 1 . 0 6 4 6 . 7 6 0

2 1 4 8 . 0 0 0 1 . 8 9 3 9 1 4 . 3 5 6 7 . 0 2 . 5 0 5

2 2 4 9 . 2 0 0 1 . 8 5 0 4 1 3 . 2 8 6 2 . 0 - 1 . 1 8 7

2 3 5 1 . 2 0 0 1 . 7 8 2 7 8 . 3 5 3 9 . 0 0 . 1 0 0 #
2 4 5 3 . 2 0 0 1 . 7 2 0 3 1 7 . 1 3 8 0 . 0 1 . 6 5 0

2 5 5 3 . 8 0 0 1 . 7 0 2 6 2 1 . 2 0 9 9 . 0 1 . 8 7 4

2 6 5 4 . 6 0 0 1 . 6 7 9 5 1 5 . 2 1 7 1 . 0 2 . 1 3 5

2 7 5 6 . 4 0 0 1 . 6 3 0 1 1 3 . 4 9 6 3 . 0 7 . 4 9 7

2 8 5 7 . 4 0 0 1 . 6 0 4 0 1 8 . 6 3 8 7 . 0 1 . 3 5 8

2 9 5 8 . 2 0 0 1 . 5 8 3 9 3 1 . 3 7 1 4 6 . 5 2 . 5 4 9

3 0 6 0 . 4 0 0 1 . 5 3 1 3 4 5 . 1 4 2 1 0 . 8 0 . 4 7 6

31. 6 2 . 0 0 0 1 . 4 9 5 6 1 3 . 2 8 6 2 . 0 3 . 3 2 1

3 2 6 3 . 4 0 0 1 . 4 6 5 9 2 0 . 7 7 9 7 . 0 1 . 4 0 0
 205

3343 6645.2.20000 1
14
.4
.4
29
96
7 3
1 9
1.861
.
5 15845..09 -109.9.73308 #
3365 6667.2.60000 1
1 .
4
3
. 1
8
40
75 9
7.6
.
9 42 4357..00 -4206.333.9017 §
37 69.600 13.497 9.21 4 3.0 0.100 #
 206

R E A L T I M E D I S P L A V

F i l e : 290117.RAM I t e r a t i o n 1 of 1
Side : RIGHT 2-Theta/Thet»: VB.88«
Sartple: DSWA 119 ( F R O M CENTER) Intensity : 5 5 CPS

DSWA f9 (FROM CENTER)

ERROR(DEG): 0.300 3 STRONGEST LINES DATA BASE: 1 NUMBER OF OBSERVED LINES- 29

11 PHASE(S) HATCHED NREQ- 0 NELEH= 7 H 0 AL SI K TI FE

SLOW SEARCH OP CUT OFF IS 320.

DHAX= 8.838 DHIN= 1.343

HATCHED WITHOUT INTENSITY PREFERRED ORIENTATION

JCPDS f PHA.SE O P IC/I0B PDF/HATCH *PATTERN

15, 776 A L 6 S I 2 013 / M U L L I T E , SYN 25.44 1.0 37/ 21 71

29,1361 TI 0 / HOHOQOIITE 28.03 0.3 3/ 3 10

33, 20 A L FE 28.58 0.1 4/ 4 13

25, 417 FE5 TI 08 / DLVOSPINEL, FERRIA 40.75 0.6 9/ 6 20

24, 536 FE2-X FE2* T I M 04 / ULVOSPINEL, SYN 49.82 0.6 10/ 6 ?0

9, 309 TI3 0 5 67.60 1.0 20/ 10 34

10, 225 TI S I 2 75.93 0.4 16/ 8 27

41,1226 AL .39 FE .85 SI .14 TI .80 101.96 0.1 17/ 7 24

11, 894 AL8 FE2 SI 122.97 0.1 79/ 23 76

26, 38 AL3 TI 126.12 0.2 17/ 6 20

10, 63 T I 2 03 142.28 0.2 12/ 5 17

D / M A X - B P E A K F I N D I N G P R O G R A M V I . 8

D A T A F I L E : A : \ D A T A \ Z 0 0 1 1 7 . R A W

C O L L E C T E D O N 2 0 - O C T - 9 8 A T 1 0 : 5 6 : 0 6

S A M P L E I D E N T I F I C A T I O N : D S W A # 9 ( F R O M C E N T E R )

D A T E O F P E A K S E A R C H : 1 2 - 8 - 9 8 A T 1 5 : 5 9 : 3 0

S T A R T 2 T H E T A : 1 0 . 0 0 0 S T O P 2 T H E T A : 7 0 . 0 0 0

S T E P S I Z E : 0 . 2 0 0 S C A N S P E E D : 1 . 0 0 0

P E A K F I N D I N G P A R A M E T E R S

T H R E S H O L D V A L U E S 5 . 0 , 1 0 . 0

R E L A T I V E C U T O F F I N T E N S I T Y 0 . 0

T Y P I C A L F U L L W I D T H - H A L F M A X I M U M 0 . 2 0

M I N I M U M F U L L W I D T H - H A L F M A X I M U M 0 . 0 8

P E A K S P A N 1 5

B A C K G R O U N D - S U B T R A C T E D D A T A W I L L B E I N F I L E A : \ D A T A \ Z 0 0 1 1 7 . B S D

P E A K S D A T A W I L L B E I N T H E N E W F I L E A : \ D A T A \ Z 0 0 1 1 7 . P K S

T H R E S H O L D D A T A W I L L B E I N F I L E A : \ D A T A \ Z 0 0 1 1 7 . T H D

P E A K 2 - T H E T A D - S P A C E I ( R E L ) I ( C P S ) F W H M

1 1 6 . 2 0 0 5 . 4 6 6 9 5 1 1 5 3 2 4 . 6 0 . 6 6 7

2 2 0 . 8 0 0 4 . 2 6 7 1 1 0 5 8 6 7 . 2 3 . 7 7 9

3 2 1 . 8 0 0 4 .0 7 3 6 1 0 4 1 6 6 . O 3 . 7 7 8

2 6 . 0 0 0 3 4 2 4 3 1 0 0 0 0 6 3 4 . 7 0 . 7 0 2

5 2 9 . 8 0 0 2 . 9 9 5 7 1 4 . 8 1 9 4 . 0 1 3 . 9 2 7

6 3 0 . 8 0 0 2 . 9 0 0 7 3 3 . 9 9 2 1 5 . 8 0 . 6 8 8

7 3 3 . 0 0 0 2 - 7 1 2 2 4 1 . 1 0 2 6 0 . 9 0 . 6 6 7
00

3 5 . 0 0 0 2 . 5 6 1 6 5 7 . 2 0 3 6 3 . 1 0 . 6 7 4

9 3 6 . 0 0 0 2 . 4 9 2 7 1 5 . 6 8 ' 9 9 . 5 1 . 2 0 0

10 3 6 . 8 0 0 Z . 4404 2 5 4 6 1 6 1 . 6 1 . 3 0 0

1 1 3 9 . 2 0 0 2 . 2 9 6 3 2 0 9 6 1 3 3 . 0 0 . 1 0 0

1 2 4 0 . 6 0 0 2 . 2 2 0 3 4 5 8 4 2 9 0 . 9 0 . 5 1 5

1 3 4 2 . 4 0 0 2 . 1 3 0 1 3 1 3 5 1 9 9 . 0 0 . 6 8 5

1 4 4 4 . 0 0 0 2 . 0 5 6 3 7 8 8 5 0 . 0 5 8 . 4 4 4

1 5 4 7 . 0 0 0 1 . 9 3 1 8 7 0 9 4 5 . 0 1 6 4 . 9 2 1

1 6 4 8 . 0 0 0 1 . 8 9 3 9 1 1 . 2 4 7 1 . 3 0 . 7 8 5

1 7 4 9 . 2 0 0 1 . 8 5 0 4 1 2 7 6 . 8 1 . 0 5 . 6 8 3

1 8 5 0 . 4 0 0 1 - 8 0 9 2 6 . 7 7 4 3 . 0 0 . 1 0 0

1 9 5 3 . 6 0 0 1 , 7 0 8 4 1 5 2 5 9 6 . 8 1 . 1 4 5

2 0 5 4 . 6 0 0 1 . 6 7 9 5 6 4 6 4 1 . 0 0 . 1 0 0

2 1 5 6 . 4 0 0 I . 6 3 0 1 7 9 1 5 0 . 2 1 . 7 9 1

2 2 5 7 . 2 0 0 1 . 6 0 9 2 1 0 0 5 6 3 . 8 1 . 7 6 9

2 3 5 8 . 2 0 0 1 . 5 8 3 9 1 4 8 1 9 4 . 0 2 . 3 8 7

2 4 6 0 . 6 0 0 1 5 2 6 8 3 4 . 4 2 2 1 8 5 0 . 6 7 7

;>5 6 2 . 0 0 0 1 . 4 9 5 6 9 . 6 1 6 1 . 0 2 . 6 0 0

2 6 6 3 . 2 0 0 1 . 4 7 0 1 7 . 3 2 4 6 5 1 . 0 0 0

2 7 6 4 . 4 0 0 1 4 4 5 5 2 8 . 9 8 1 8 4 . 0 0 . 7 1 3

2 8 6 5 . 4 0 0 1 4 2 5 8 8 . 5 1 5 4 0 *******
2 9 6 6 . 2 0 0 1 4 1 0 5 1 2 . 5 5 7 9 . 7 0 . 7 4 5

1 0 6 9 . 6 0 0 1 3 4 9 7 9 . 4 5 6 0 0 0 . 1 0 0
 208

DSWA 110 (CENTER)

ERROR(DEG): 0.300 3 STRONGEST LINES DATA BASE: 1 NUMBER OP OBSERVED LINES- 34

21 PHASE(S) MATCHED NREQ= 0 NELEH- 7 H 0 AL SI K TI FE

SLOW SEARCH OP CUT OFF IS 320.

DHAX= 8.838 DMIN- 1.343

MATCHED WITHOUT INTENSITY PREFERRED ORIENTATION

J C P D S / PHASE O P IC/IOB PDF/MATCH tPATTERN

34, 529 F E 1 1 . "75 0.2 4/ 4 11

15, 776 AL6 SI2 013 / MULLITE, SYN 21.05 1.0 37/ 25 71

29,1361 TI 0 / HONOQUIITE 30.36 0.4 3/ 3 8

33, 20 AL FE 30.94 0.1 4/ 4 11

18,1170 SI 0 2 / TRIDYMITE-M, SYN 44.49 0.1 59/ 27 76

9, 309 TI3 0 5 52.06 1.0 20/ 11 32

10, 225 TI SI2 52.82 0.6 16/ 9 26

3 4 , 177 FE2 TI 04 / ULVOSPINEL, SYN 52.89 0.5 10/ 6 17

25, 9 8 2 TI HI .924 54.30 0.6 4/ 3 8

24, 5 3 7 F E 2 TI 04 / DLVOSPINEL, SYN 59.29 0.6 10/ 6 17

41,1226 A L .39 F E .85 SI .14 TI .80 61.61 0.1 17/ 9 26

37,1449 AL3 TI 61.88 0.3 10/ 5 14

14, 260 SI 02 / TRIDYHITE-20H, SYN 65.64 0.1 58/ 24 71

17, 536 FE 0 ( 0 H ) / GOETHITE 74.37 0.1 26/ 12 35

26, 38 AL3 TI 79.83 0.3 1'/ ? 23

41, 894 AL8 FE2 SI 80.80 0.1 79/ 28 83

5, 678 AL TI 82.02 0.3 10/ 6 17

29, 713 FE 0 ( 0 H ) / GOETHITE 149.14 0.1 3C/ 10 29

10, 63 TI2 03 174.06 0.2 12/ 5 14

26,1140 FE2 SI2 05 ( 0 H )4 . 2 H2 0 / HISINGERITE 200.10 0.1 23/ 8 23

 209

D / M A X - B PEAK F I N D I N G PROGRAM VI .8

DATA F I L E : A : \ D A T A \ Z 0 0 1 1 8 . R A W
COLLECTED ON 2 0 - O C T - 9 8 A T 1 4 : 1 3 : 5 8
SAMPLE I D E N T I F I C A T I O N : DSWA # 1 0 ( C E N T E R )
DATE OF PEAK SEARCH: 1 2 - 8 - 9 8 A T 1 6 : 1 4 : 0 0

START 2THETA: 1 0 . 0 0 0 STOP 2 T H E T A : 7 0 . 0 0 0

S T E P S I Z E : 0 . 2 0 0 SCAN S P E E D : 1 . 0 0 0

PEAK F I N D I N G PARAMETERS

THRESHOLD VALUES 5.0, 10.0

R E L A T I V E C U T O F F I N T E N S I T Y 0.0
T Y P I C A L F U L L W I D T H - H A L F MAXIMUM : 0 . 2 0
MINIMUM F U L L W I D T H - H A L F MAXIMUM : 0 . 0 8
PEAK SPAN : 1 5

BACKGROUND-SUBTRACTED DATA WILL BE I N F I L E A : \ D A T A \ Z 0 0 1 1 8 . B S D

PEAKS DATA W I L L B E I N THE NEW F I L E A : \ D A T A \ Z 0 0 1 1 8 . P K S
THRESHOLD DATA WILL BE I N F I L E A : \ D A T A \ Z 0 0 1 1 8 . T H D

;AK 2 - T H E T A D - S P A C E I ( R E L ) I ( C P S ) FWHM

I 16.200 5.4669 62.87 357.9 0.662

?. 20.600 4.3081 13 . 59 77.4 0 , 100
3 21.200 4.1875 12.69 72. 2 3 . 997
4 21.800 4 .0736 11.93 67 .9 3.778
5 23.400 3.7986 14.05 80.0 48.291
6 26.000 3 .4243 100.00 569 . 3 0.728
7 29.600 3.0155 10.01 57.0 0.100
8 30.800 2.9007 33.67 191.7 0 . 702
'•:> 33.000 2.7122 74.49 424.1 0 . 646
10 35.000 2.5616 54.99 313.0 0.524
ii 36.000 2.4927 16.75 95.3 1. 200
12 36.800 2.4404 28.59 162.7 1 .319
13 39.200 2.2963 27.40 156 . 0 0.100
1-1 40.600 2.2203 55.49 315.9 0 .514 if
15 42.400 2. 1301 3 6 . 30 206.7 0 . 668
16 44.000 2.0563 9.38 53 . 4 5.000
17 45.800 1.9796 7 .78 44 . 3 3 .000
18 47.000 1.9318 7.71 43 . 9 5.000
19 47.800 1 .9013 7 . 56 43.0 5 .400
20 49.200 1.8504 1 5 . 26 86 . 9 0 .958
21 50.600 1.8025 8.26 47.0 35.860
22 53.000 1.7264 8 .08 46.0 4 .000
23 53.800 1.7026 21.75 123 .8 1 .150
24 54.600 1.6795 7. 55 43 .0 0 . 100
25 57.400 1.6040 38 . 6 5 220 .0 0 . 100
26 58.400 1.5789 11.48 65. 3 1 . 991
27 60,600 1.5268 54 . 2 5 308 . 8 0 .656
28 61.400 1.5088 8.43 48 . 0 58 . 0 6 1
29 62.000 1.4956 7.93 45.1 2 - 200
30 63.400 1.4659 16 . 4 1 93 . 4 1 . 182
31 64.400 1 .4455 31 . 56 179 . 7 0.712
32 65.200 1 .4297 10.69 60 . 8 1 . 189
 210

33 66.200 1.4105 17 *i ,
34 69
"400 1 3531 8*22 ! « ' o 1
' 3 8 / f

46.8 3.400
 APPENDIX D

LABORATORY TEST RESULTS ON PROCESSED KAOLIN

 212

Oedometer Test
Started 10-11-96
Ended 10-15-98
Soil: processed kaolin
Moisture content
Tin, g wet soil, g dry soil, g m.c.
27.9 62.7 52.4 41.9
27.9 63.5 52.8 43.2
233 59.9 50.3 43.6
Average m.c. 42.9

INITIAL •* J *"r NTS void ratio, e Applied stress, tsf

inches mm
2, , soil ht 0.742 18.90 0.872 0.1
_ , cover & stone h
2 0.853 22.25 0.847868356 0.5
z 3
0.834345553 1
2H , specimen ht 1.484 37.80 0.80817035 2
H solid 0.396 in 0.753170889 4
ring diam 2.436 63.25 0.730843127 8
upper si one 0.730843127 2
& cover 0.853 22.25 0.734753639 0.5
ring vA 76.650 grams

Ykadin © 4 0 % 90.000 pcf o ", tsf

p 1.3
V_ring 3.458 in*3 <V , psf 2600
V_ring 0.002 fl 3
A
a ", kPa
p 124.5
vM_soil 0.180 lbs C e
0.1600
H_solid 0.396 m c, 0.0217 (value taken over 0.1 to 1 Isf range)
FINAL MEASUREMENTS
(rrng+soif) 171.2
rterte- g
(ring+soil) <r34fv.
rt 142.5 g
final m.c, % 43.7

Applied Dial Rdg, Corrected Dal Change in Rdg, Applied

Date Load Applied Time, min Change in Rdg 2H, in Void Ht Void ratio, e
stress, tsf in Rdg. in in stress, tsf
10/11/99 0.00 0.00 16.00 0.00 0.000 0.000 1.484 0.691 0.872 0.01
10/11/99 0.50 0.25 17.34 1.34 1.340 0.013 1.471 0.678 0.855 0.50
10/11/99 0.50 1.00 17*5 1.45 0.110 0.001 1.470 0.677 0.854 0.50
10/11/99 0.50 2.25 17.53 1.53 0.075 0.001 1.469 0.676 0.853 0.50
10/11/99 0.50 4 00 17.57 1.57 0 045 0.000 1.468 0.676 0.352 o.SO
10/11/99 0.50 6.25 17.61 1.61 0.035 0.000 1.468 0.675 0.852 0.50
10/11/99 0 50 9.00 17.63 1.63 0.025 0.000 1.468 0.675 0.851 0.50
10/11/99 0.50 12.25 17.65 1.65 0.018 0.000 1.468 0.675 0.851 0.50
10/11/99 0.50 16.00 17.66 1.66 0.012 0.000 1.467 0.675 0.851 0.50
10/11/99 0.50 20.25 17.68 1.6S 0.017 0.000 1.467 0.674 0.851 0.50
10/11/99 0.50 25.00 17.69 1.69 0.015 0.000 1.467 0.674 0.851 0.50
10/11/99 0.60 30.25 17.70 1.70 0.003 0.000 1.467 0.674 0.851 0.50
10/11/99 0.50 36.00 17,70 1.70 0.007 0.000 1.467 0.674 0.851 0.50
10/11/99 0.50 42 25 17.71 1.71 0.008 0.000 1.467 0.674 0.850 0.50
10/11/99 050 56.25 17.72 1.72 0.010 0.000 1.467 0.674 0.850 0.50
10/11/99 0.50 64 00 17.74 1.74 0.015 0.000 1.467 0.674 0.850 0.50
10/11/99 0.50 1440.00 17.91 1.91 0.178 0.002 1.465 0.672 0.848 0.50
10/12/98 1.00 0.25 18.83 2.83 0.917 0.009 1.456 0.663 0.836 1.00
10/12/98 1.00 1 CO 18.95 2.95 0.120 0.001 1.455 0.662 0.835 1.00
10/12/98 1.00 4.00 18.99 2.99 0.035 0.000 1.454 0.661 0.834 1.00
10/12/98 1.00 6.25 18.99 2.99 0.000 0.000 1.454 0.661 0.834 1.00
10/12/98 1.00 9.00 18.99 2.99 0.000 0.000 1.454 0.661 0.834 1.00
10/12/98 1.00 12.25 18 69 | 2.99 0.000 0.000 1.454 0.661 0.834 1.00
10/12/98 1.00 1440.00 18.99 2.99 0.000 0.000 1.454 0.661 0.834 1.00
10/13/98 2.00 1380.00 21.06 5.06 2 075 0.021 1.433 0.641 0.808 2.00
10/14/98 4.00 592000 25.42 9.42 4.360 0.044 1.390 0.597 0.753 4.00
10/18/98 8.00 1335.00 27.19 11.19 1.770 0.018 1.372 0,579 0.731 8.00
10/19/98 2,00 1065.00 27.19 11.19 0.000 0.000 1.372 0.579 0.731 2.00
1021/98 0.50 1800 00 26.88 10.88 -0.310 -0.003 1.375 0/.. ' 0.735 0.50
 213

1 - D C O N S O L I D A T I O N T E S T ( A S T M D 2 4 3 5 )

S o i l : Processed Kaolin (40% moisture content)

T e s t p e r f o r m e d b y : Josepha Celes and Amr El-Hakim
 214

Compacted Kaolin Properties

w = 40 % w = 50%
y , pcf (average)
T 90 90
YT, k N / m 3
14.08 14.14
YD. k N / m 3
10.06 9.42
PT. k g / m 3
1435.76019 1441.09759
p . kg/m
d
3
1025.543 960.731728

2.55 2.55

P w . kg/m 3
1000 1000
e, average 1.48648766 1.6542269
n, average 0.59782628 0.62324246

Specific Gravity of Processed Kaolin

(ASTM D 854)

Date: 4/9/99
Performed By: A. El-Hakim

wt of soil (before oven-drying), 100

wt of soil (after oven-drying), g 99.8

wt of flask (empty), g 145.3
wt of flask + water (Ma), g 412.3
wt of flask + dry soil, g 205.4
Mo, g 60.1
wt of soil+water+flask (Mb), g 448.8
Gs = Mo/(Mo+Ma-Mb) 2.55
Thiele MSDS value 2.6
 215
Liqu3id/11L
/9i8
mit by CTestl
asagrande CupTA
(eSsT
tM
2 4318)Test 3 Test 4
Tin, g 27.01 28.62 27.69 32.87
Tin + wet soil, g 49.74 52.84 51.80 67.85
Tin + dry soil, g 40.72 43.22 41.60 53.18
Mass of water, g 9.02 9.62 10.20 14.67
Mass of soil, g 13.71 14.60 13.91 20.31
w, % 65.79 65.89 73.33 72.23
# of blows 27 47 12 14

w @ 25 blows 68.2
6/21/98
Tin, gTestl 27.81 Test 2
27.87 Test 3
27.53 Test 4
28.11
Tin + wet soil, g 42.04 47.28 50.66 48.54
Tin + dry soil, g 36.42 39.50 41.06 39.78
L .lass of water, g 5.62 7.78 9.60 8.76
Mass of soil, g 8.61 11.63 13.53 11.67
65.27 66.90 70.95 75.06
w, %
# of blows 50 43 25 20

w @ 25 blows 72.3
Plastic Limit A
(STM 4318)
3/11/98
Tin, g Test 1
33.00 Test 2
33.18 Test 3
32.81
Tin + wet soil, g 41.88 56.74 52.81
Tin + dry soil, g 39.43 50.35 46.82
Mass of water, g 2.45 6.39 5.99
Mass of soil, g 6.43 17.17 14.01
38.10 37.22 42.76
w, %
Average w, % 39.36

6/21/98
Tin, g Test 1
27.44 Test 2
27.97
Tin + wet soil, g 43.79 46.98
Tin + dry soil, g 39.25 41.82
Mass of water, g 4.54 5.16
Mass of soil, g 11.81 13.85
w, % 38.44 37.26
Average w, % 37.85
 216

LIQUID LIMIT RESULTS (ASTM D 4318)

Soil: Processed Kaolin
Test performed by: J o s e p h s Celes and Alec McGillivray

80

75 L • Test 1: 3/11/98
%

•
A Test 2: 6/21/98

^ ^ ^ ^

1•
60
1
,

10 ^ 100
Number of Blows, N
 217

Fall Cone T e s t on P r o c e s s e d K a o l i n : 6.26.98

Performed by A. McGillivray
Fall Cone Penetration Readings
Initial Second Penetration Ave.
Tin#
Readinq Readinq (mm) Penetration

6.47 21.24 15.23

1 7.25 21.37 15.88 15.63

7.15 21.37 15.78

8.7 21.19 17.51
2 17.35
7.96 20.77 17.19
7.84 20.04 17.80
3
7.93 19.58 18.35 18.25

7.66 19.06 18.60

7.55 14.58 22.97
4 22.79
7.32 14.72 22.60
Fall C o n e Penetrometer
Mass of Tin Tin + Dry Mass of Mass of Ave
Tin# Tin + Soil (g) w/c (%)
(q) Soil (g) Solids (q) Water (q) Penetration

1 28.14 45.25 38.42 10.28 6.83 66 15.63

2 27.82 46.46 38.84 11.02 7.62 69 17.35
3 28.65 58.75 45.80 17.15 12.95 76 18.25
4 27.44 67.45 49,15 21.71 18.30 84 22.79

25

0 A 1 1 i 1 1 1 1
55 60 65 70 75 80 85 90
w, %
Fall Cone Test (BS 1377): 5/1/99
Performed by J. Celes
Altered (Pink) Kaolin Data Unaltered (Off-white) Kaolin Data
Layer Thickness, mm: 8.31 Layer thickness, mm: n/a
Distance from edge of rock, mm 3 Distance from egde of rock, mm: 854
Penetration
Tin* Ave. Penetration Tin# Penetration (mm) Ave. Penetration
(mm)
13.09 12.73
1 13.15 1 12.73
13.20 12.73
17.53 15.48
2 17.67 2 15.51
17.80 15.54
19.65 16.95
3 19.74 3 16.93
19.83 16.91

Altered Kaolin
Test 1 Test 2 Test 3
Tin, g 27.60 27.59 28.25
Tin + wet soil, g 49.86 51.18 50.54
Tin + dry soil, q 42.42 42.98 42.31
50.20 53.28 58.53
Average penetration, mmw, % 13.15 17.67
Jnaltered Kaolin
19.74

Test 1 Test 2 Test 3

Tin, o 27.46 27.59 32.86
Tin + wet soil, g 47.37 54.68 63.16
Tin + dry soil, q 40.22 44.46 51.01
56.03 60.58 66.94
Average penetration, mmw, % 12.73 15.51 16.93

25.00
• Altered Kaolin

H Unaltered Kaolin
y = 0.7483x-23.561
"- 20.00
a

w @ 20mrn for Altered

c
% 15.00
0L
Kaolin = 58%
w @ 20mm for Unaltered
Kaolin = 74% y = 0.3747x -7.8683

10.00
0.00 10.00 20.00 30.00 40.00 50.00 60.00 70.00 80.00
w, %

Plastic Limit Test (ASTM 4318): 5/1/99

Performed by A. El-Hakim
Soil Altered Kaolin Unaltered Kaolin
Tin, g 10.48 2.36
Tin + wet soil, g 17.87 6.58
Tin + dry soil, g 16.03 5.71
w, % 33.15 25.97
 219

C
Peofrom
rnveednoitnably:TJria.xiaC
leC
elsonansoddilaetdAUB
nH
-dranaikm
eid Test on Procesed Kaonil
(4/29/99)
Calibration factors
Load Factor 0.002633628 Pore Factor 0.256637 isplacerre Factor 0.000766
kN/au Offset 43.129 (kN7m2)/au Offset 34.72 cm/au Offset 288

Ho (cm) 11.14433 718,45 Void Ratio 1.20 % =rfi- (kPa) 149.3

Do (cm) 7.1115 Moisture (%)
F 40 s, = 0J1 (kPa) 74.7
Dry Mass (g)
1.623043 AREA (cm2) 39.72 237.2 kPa
P*y. 0/cm3 1.159317 Volume (cm3) 442.66 237.2 kPa
<w 9/cm3 117.2 kPa
Backpressure

Time Load Displacement Excess Pore Strain o,-a Aa, % °Y P' q e

Q.
3

(kN) (cm) (kN7m2) (%) kPa (kPa) (kPa) (kPa) (kPa) (kPa) (kPa) 1.20
0 -0.11 -0.22 -92.19 -1.98 63.66 -28.53 208.66 300.85 222.92 315.11 -14.27 1.20
7 0.14 0.00 20.67 -0.01 14.38 35.06 272.24 251.57 254.72 234.04 1753 1.20
73401 0.42 0.06 34.27 0.51 7040 104.68 341.86 307.59 28953 255.25 52.34 1.20
133133 0.44 0.11 40.69 1.02 69.95 11064 347.83 307.14 292.51 251.82 55.32 1.20
192446 0.46 0.17 45.05 1.53 70.23 115.28 352.47 307.42 294.83 249.78 57.64 1.20
252803 0.48 0.23 48.39 2.05 71.54 119.93 357.11 308.73 297.15 248.76 59.96 1.20
311511 0.49 0.29 51.21 2.57 73.36 124.57 361.75 310.54 299.47 248.26 62.28 1.20
370536 0.51 0.34 53.26 3.08 75.28 128.54 365.73 312.47 XI .46 248.20 64.27 1.20
429973 0.53 0.40 54.80 3.60 77.72 132.52 369.71 314.91 303.45 248.65 66.26 1.20
488668 0.54 0.46 55.83 4.11 80.67 13650 373.69 317.86 305.44 249.61 68.25 1.20
548090 0.56 0.52 56.34 4.62 84.80 141.14 378.33 321.99 307.76 251.42 70.57 1.20
607527 0.57 0.57 57.11 5.14 87.34 144.46 381.65 32453 309.42 252.30 72.23 1.20
666016 0.59 0.63 57.37 5.65 91.07 143.44 385.62 328.25 311.41 254.04 74.22 1.20
725418 0.61 0.69 57.37 6.16 95.04 152.41 389.60 332.23 313.40 256.02 76.21 1.20
785061 0.62 0.74 57.11 6.68 97,95 155.07 392.25 335.14 314.72 257.61 77.53 1,20
844188 0.63 0.80 56.60 7.19 102,44 159.04 396.23 33963 316.71 260.11 79.52 1.20
904222 0.64 0.86 56.09 7.70 105.61 161.70 398.89 342.80 318.04 261.95 80.85 1.20
963549 066 0.92 55.57 8.22 109.44 165.01 402.20 346.63 319.69 264.12 82.51 1.20
1022155 0.67 0.97 55.06 8.73 112.60 167.66 404.85 349.79 321.02 265.96 83.83 1.20
1081591 0.68 1.03 54.29 9.24 116.03 170.32 407.50 353.21 322.35 268.06 85.16 1.20
1141316 0.68 1.09 53.52 9.76 118.79 172.31 409.49 355.97 323.34 269.82 86.15 1.20
1200540 0.69 1.14 5275 10.27 122.21 174.96 412.15 359.40 324.67 271.92 87.46 1.20
1260464 0.70 1.20 51.21 10.78 125.07 176 28 413.47 362.26 325.33 274.12 88.14 1.20
1319283 0.71 1.26 49.41 11.29 126.20 177.61 414.80 365.38 325.99 276.58 88.81 1.20
1378912 0.71 1.32 47.87 11.81 130.40 178.27 415.46 367.59 326.32 278.45 89.14 1.20
1438657 0.71 1.37 47.10 12.32 131.83 178.94 416.12 369.02 326.66 279.55 89.47 1,20
1497572 0.71 1.43 44.60 12.83 134.80 179.60 416.79 371.99 326.99 282.19 89.80 1.20
1557729 0.72 1.49 43.26 13.35 137.01 180.26 417.45 374.20 327.32 284.06 90.13 1.20
1617365 0.72 1.55 42.74 13.86 13752 180.26 417.45 374.71 327.32 284.58 90.13 1.20
1675758 0.72 1.60 41.97 1437 138.29 180.26 417.45 375.48 327.32 285.35 90.13 1.20
1735201 0.72 1.66 40.16 14.89 140.09 180.26 417.45 377.27 327.32 287.14 90.13 1.20
1794020 0.72 1.72 38.38 15.40 142.55 180,93 418.11 379.73 327.65 289.27 90.46 1.20
1852207 0.72 1.77 37.10 1591 144.49 181.59 418.78 381.68 327.98 290.89 90.79 1.20
1911424 0.72 1.83 35.56 16.43 145.37 180.93 418.11 382.56 327.65 292.09 90.46 1.20
1969501 0.72 1.89 34.53 16.94 146.40 180.93 418.11 383.58 327.65 293.12 90.46 1.20
2028024 0.72 1.95 33.50 17.45 147.42 180.93 418.11 334.61 327.65 294.15 90.46 1.20
2086589 0.72 2.00 32.73 17.97 148.86 181.59 418.78 386.04 327.98 295.25 90.79 1.20
2144790 0.72 2.06 32.99 18.48 149,26 182.25 419.44 386.45 328.31 295.32 91.13 1.20
2203663 0.72 2.12 33.25 18.99 149.01 182.25 419.44 386.19 328.31 295.07 91.13 1.20
2262640 0.73 2.17 34.27 19.51 149.30 18358 420.77 386.49 328.98 294.70 91.79 1.20
2320477 0.73 2.23 35.30 20.02 148.28 183.58 420.77 385.47 328.98 293.68 91.79 1.20
2378403 0.73 2.29 36.58 2053 146.99 183.58 420.77 384.18 328.98 29239 91.79 1.20
2436494 0.73 2.35 37.87 21.05 146.37 184.24 421.43 383.56 329.31 291.44 92.12 1.20
2492010 0.73 2.40 39.15 21.54 145.75 184.90 422.09 382.94 329.64 290.49 92.45 1.20
 220

APPENDIX E

LABORATORY TEST RESULTS ON VESICULAR MULLITE GLASS SLAG

Shear Wave Velocity Tests (ASTM D 2845)
erformed by: G.C. Cho and J. Cele
Description Non-uniform piece
Date 7/23/99 7/23/99 7/23/99 7/23/99
length, m 0.0721 0.0359 0.0359 0.0359
time, u - S 25.5 14.5 13.2 14.6
V , m/s
s 2827 2476 2720 2459
P, kg/m 3
2370 2370 2370 2370
G m a x . GPa 18.9 14.5 17.5 14.3
E m a x » GPa 42.4 32.5 39.3 32.1
Average G m a x , GPa 16.3
 Specific Gravity of Vesicular Mullite Glass Slag
Performed by J . Celes (7/19/99)
Correction
Stem Conversion 0.1 1.03
for Gs
Test 1 Test 2 Test 3
Parti
Weights only, g 14.3 14.5 14.5
Stem Reading, cm 3.1 2.5 2
Total Wt, g 14.61 14.75 14.7
Part 2
Dry Wt of Rock +
3.2 0.5 0.2
weights, g
Stem Reading, cm 4.05 1.90 4.40
Total Wt, g 3.605 0.69 0.64
Part 3
Wet Rock +
7.7 6 6
Weights, g
Stem Reading, cm 2.6 3.6 2.3
Total Wt, g 7.96 6.36 6.23
Calculations
Dry Wt of Rock, g 11.005 14.06 14.06
Wet Wt of Rock, g 6.65 8.39 8.47
Gs 2.60 2.55 2.59
Average Gs 2.58

Compressive Strength
Performed by J . Celes
Description lntact-1 lntact-2
Date 11/13/98 11/13/98
Length, in 1.047 1.055
Width, in 0.91 1.055
Height, in 1.071 1
Load, lbs 12570 19590
o = F/A, psi 13193 17601
a = F/A, kPa 90966 121357
Average 0 , kPa 1061 62
 223

APPENDIX F

PETROGRAPHIC TESTS RESULTS ON VESICULAR MULLITE GLASS SLAG

 224

SLIDE AREA P O R E (P) MULLITE GLASS TOTAL % % %

U
2
(mm ) COUNT (M) (G) PTS. P M G
COUNT COUNT
E2063 336 980 1431 1489 3900 25 37 38
a-1
E2623 144 413 556 733 1702 24 33 43
b-1
E20623 180 650 646 840 891 30 30 40
b-2
E20623 165 492 687 758 1937 25 36 39
c-1
 225

SLIDE AREA PORE (P) MULLITE GLASS TOTAL % % %

# (mm ) 2
COUNT (M) (G) PTS. P M G
COUNT COUNT
E20623 240 679 914 1198 2791 24 33 43
d-1
E20623 276 558 983 1653 3194 17 31 52
d-2
E20623 132 397 488 674 1559 26 31 43
e-1
E20623 135 277 533 772 1582 17 34 49
e-2
E20623 364 1509 1052 1662 4223 36 25 39
f-1
E20623 466.07 1529 1643 2291 5463 28 30 42
f-2
 226

APPENDIX G

TIME DOMAIN REFLECTOMETRY REPORT

 227

ABSTRACT

Time Domain Reflectometry (TDR) is an electronic measuring technique for

detecting changes in length or distance. TDR has been used in geotechnical engineering

as a means of detecting rock movement and deformation, water migration through soil,

and is under development for use in detection of soil movement (Will 1996). TDR

involves an expendable coaxial cable whose deformations can be detected by the

reflection of a pulse sent through the cable. This technology was used in a recent

chamber test conducted at the Georgia Tech Plasma Application Research Facility

(PARF) located in Atlanta, Georgia. The purpose was to determine the viability of TDR

applications to monitor the size of the plasma cavity and magma growth rate with time

during magmavication of soils. TDR proved a worthy and cost-effective measuring tool

that merits further investigation and application in future tests, both in the lab and in the

field.

INTRODUCTION

TDR is a remote-sensing, electrical measurement technique that can monitor

movement or deformation through physical changes in the cable. A voltage pulse is sent

down a coaxial cable and is reflected back when a change in the capacitance between the

inner and outer conductors is encountered. The larger the deformation in the cable, the

larger the reflected pulse will be. By knowing the propagation velocity of the pulse and

the time of travel, the distance to the cable distortion can be determined (Will, 1996).
 228

In-situ plasma magmavication is a destructive technique using a non-transferred arc

plasma torch that reaches temperatures of 4000°C to 7000°C. At these temperatures,

every material known to man will be destroyed. All organics and some inorganics will be

pyrolized and escape as vapor, while any material left will become incorporated into a

molten pool of matter (magma), which then cools into a slag. Measurement devices

considered for in-situ instrumentation during testing have to be expendable, sturdy, and

able to perform sufficiently even when encountering the molten soil, plasma "flame",

and/or the hot gases circulating within the cavity and soil.

The commercial viability of plasma magmavication can only be realized if it can be

made cost-effective and safe. Equipment costs aside, major expenses are power

consumption, off-gas collection and treatment, and the time and labor needed to treat a

given volume of soil. Since the focus of Georgia Tech's experiments is not the off-gas

treatment, it will not be discussed further here.

Proper modeling of the magma and cavity growth is crucial in the development of

equations to determine the amount of power and time it will take for complete and

effective treatment for given soil conditions (grain size distribution, moisture content,

overburden, density, volume). A large cavity forms above the magma during treatment.

This cavity, as well as the magma, poses a threat to equipment and personnel if its

dimensions are not known during melting. Past experiments have used physical probes

operated by personnel strapped into safety harnesses suspended above the borehole, and

measuring devices such as thermocouples and infrared thermometers to observe the

melting phenomena. However, the devices are limited in their temperature ratings and
 229

over time become costly when sacrificed during experiments, and physical probes are a

hazardous measurement method. Additional laboratory experiments using both TDR and

thermocouples will gather information necessary to develop TDR for field and laboratory

use. This will eliminate the need for further thermocouple instrumentation and thus

lower costs. After the initial equipment purchase, coaxial cables are the only continuing

expense throughout the life of the equipment (at approximately $1.05/meter).

TDR E Q U I P M E N T

TDR has four standard components. These components and associated functions are

as follows (Nissen and Moldrup, 1995):

• pulse generator

> produces wave (pulse)

• sampler (sampling heads)

> consists of timing device and voltmeter

> detects waves and measures voltage between shield and inner/outer conductors

with time

• coaxial cable

> connects pulse generator and sampler

• oscilloscope

> produces a trace which shows measurements of travel time and reflected voltage
 230

These components can be purchased separately or as an "all-in-one" (inclusive) unit

through vendors such as Tektronix and Hewlett-Packard. For the initial lab trials, an

inclusive Tektronix 1502C/4 TDR measuring unit was rented from McGrath RenTelco at

a cost of $347/two weeks. The Tektronix unit was capable of measuring only one cable

at a time, therefore a two-channel switch box was purchased to increase the measuring

capabilities. The specifications of the unit are found in the appendix.

Four types of coaxial cable were tested for compatibility with the TDR unit,

resistance to heat, and propagation velocity ( V ) . p Belden was the only cable

manufacturer tested due to supply and time constraints. The results are listed in the table

below. The temperature gradient along the cable was considered an important factor

because of potential heat damage to the TDR unit. Therefore, the cables were melted at

one end with an acetylene torch while a thermometer measured temperature at the other

end. None of the cables experienced any temperature change until the flame was about

11 cm from the thermometer. For standard uses, the operating range of the cables is -

4 0 ° C to 8 0 ° C .

1
Cable Diameter, mm
8237 RG-8 10.3 0.66
8240 RG-58 4.90 0.66
9258 RG-8 6.15 0.82
9913 RG-8 10.3 0.82
*Note: V is the ratio of the speed of an electromagnetic
p wave through a dielectric medium to the
speed of light in a vacuum.
TABLE G . l : RESULTS OF BELDEN COAXIAL CABLE

Belden 8237 RG-8 was determined to be the most compliant and sturdy cable. The

V p of this cable matched that of the connecting cable supplied by Tektronix.

 231

Additionally, its larger diameter decreased the possibility of accidental deformation

during the test (i.e. stepping on the cable or rolling the pallet jack over it).

Since TDR is capable of detecting deformations in the cable, it was thought that

crimping the cable would offer a baseline of known measurement while the test was in

progress. It was intended that readings would be taken at 5-minute intervals, as well as

when significant changes were seen. Crimp lengths between 2 mm and 2 cm were tested

with the cable. In order to find the crimp, the waveform averaging (noise filtration) took

up to 35 seconds to stabilize, which was not within an acceptable time frame. As the

cable melted, the readings shown on the LCD display at that time would not reflect the

signal at that time, but the average of a reading from beforehand. Therefore, it was

decided that an open-ended signal, where the pulse reflects back from the end of the

cable, would be measured for this experiment.

TEST C H A M B E R AND TDR INSTRUMENTATION

An experiment was conducted to evaluate TDR during plasma magmavication of

soils on November 16, 1998 at PART located at Southland Civil Engineering Laboratory.

The soil used in this experiment was processed kaolin prepared at 40% moisture content.

The steel chamber dimensions were 61-cm diameter by 91-cm height. The chamber

3
dimensions yielded a gross volume of 0.27 m and a net volume (taking into account the

3
volume of the stovepipe and insulation) of 0.23 m . The 100-kW torch system was used

and the test duration was 45 minutes.

 232

2-channel Switch

Stovepipe

Axial T D R

Radial T D R — •
2.5 c m

insulation

FIGURE GA: AXIAL & RADIAL TDR AND CHAMBER DIMENSIONS

Thermocouples were placed at 30-cm, 61-cm, and 76-cm heights, and at a depth of

10 cm. The two cables were placed in a radial and axial configuration. The axial TDR

was placed down the length of the borehole in order to monitor the height of the cavity

growth. This was the first time that length-wise expansion was monitored during lab

testing. The TDR cables were placed as shown in Figure G. 1.

Thermocouple readings were taken every five minutes and TDR strip chart printouts

were taken every five minutes. Manual TDR measurements were taken whenever a

change was seen in either of the cables.

 233

RESULTS

The results of the thermocouple measurements were compared to the melting rates

calculated from the TDR measurements. This was done to verify the applicability and

appropriateness of TDR instrumentation for future in-situ magmavication experiments.

Furthermore, if this technology proves viable then it can be applied to field experiments

currently under consideration.

Thermocouple Results

The thermocouples used in the experiment resulted in only the lowest probe (at a

height of 30 cm from bottom of chamber) registering any significant temperature

changes. A graph of the results is shown in Figure G.2. The melting point of the K-type

thermocouple is 2000°C, but in order to preserve it for future use, the probe was

withdrawn at 1200°C. Therefore, in order to extrapolate the time that the soil would have

melted, the endpoints of the plot of TC 1 were extended to intersect at the melting point

of processed kaolin (1735°C). Previous experiments have shown that the temperature

increases at an approximate exponential rate as the magma boundary begins to intercept

the thermocouples. The estimated temperature increase and intersection with the kaolin

melting point is illustrated in Figure G.2. Assuming this relationship, the estimated time

of interception was calculated at 27.1 minutes, and approximate melting rate was 0.38
 234

cm/min. This value was compared to the average melting rate found with both the axial

and radial TDR measurements.

TDR Results

The TDR cables performed well throughout the experiment and after the torch

system was turned off. There was still a large temperature gradient and effective heat

transfer from the convective magma boundary layer into the soil matrix which caused

further cable melting.

The axial cable began registering readings 35 seconds after start of test, while the

radial cable registered readings after about 13 minutes of testing. Axial and radial

readings were taken at about 1-minute intervals, and the melting rates between readings

were calculated. Due to heterogeneous soil density throughout the specimen, an average

of the melting rates was calculated. Using these averaged rates, cavity growth was

determined and plotted. The average axial melting rate was found to be 0.23 c m / m i n .

The average radial melting rate was calculated as 0.15 c m / m i n . Figure G.3 is the graph

of the 15-minute, 30-minute, and final cavity dimensions. It must be emphasized that

these graphs are approximations. It is difficult to verify the cavity or the magma pool

dimensions during testing because of the intense heat and safety concerns surrounding the

magmavication process. Table G.2 shows measurements with time using the TDR and

thermocouple rates. There is good agreement ( 1 % difference) between the dimensions

calculated using TDR and the actual measured dimensions, as opposed to the
 235

thermocouple method which overestimated the cavity size by 15%. This further validates

TDR as an effective measurement tool for magmavication.

Time vs. Thermocouple Temperature

S o i l : Processed Kaolin(40%rroisture content)
D a t e : Noverrber 16, 1998

•TC 1 -TC2 •TC 3 - • - X estimated temperature increase

FIGURE G.2: RESULTS OF THERMOCOUPLE READINGS

 236

DISCUSSION

The experiment was positive in indicating a compatibility of TDR instrumentation

with the plasma magmavication process. The sacrificial probes are inexpensive and the

equipment can operate in the laboratory with minimal influence from surrounding

electromagnetic interference. However, a field test performed at Savannah River Site

(Tarpley, 1996) which was instrumented with TDR showed that the higher power

operations created a great deal of electromagnetic interference which affected the

readings. Additionally, a drastic temperature change (-30 °F) occurring in the morning

hours affected the coaxial cable length and the readings. These are concerns that need to

be investigated further.

CAVITY SHAPE

It had been initially assumed that the cavity grew in a consistent cylindrical manner

throughout the test. Hand graphing of the readings suggested an initial cylindrical

expansion that changed to a paraboloid as the experiment continued. Figure G.4 shows

the excavated cavity and slag in which the rounded shape of the cavity can be clearly

seen. The metamorphosis of cavity shape may be a result of the scouring action of the

gases combined with certain soil properties (such as uniformity, cohesion, etc).

Additionally, the fact that the soil around the stovepipe is not as compacted as the outer

areas may have also contributed to the melting phenomena. If the immediate area around

the stovepipe is less-densely compacted, heat traveling upwards will dry the soil out and
 237

leave behind the soil matrix. Depending on the void ratio within the region, the dried

kaolin may either aggregate (low void ratio) or fall into the growing cavity (high void

ratio).

Cavity D i m e n s i o n s
2-channel TDR Instrumentation (Nov. 16,1998)
1 1 1 1 I R-
10 20 30 40 50 60
Radial Dimension, cm

Final Dimension

-65-

-75-

-85-

-95-

F I G U R E G.3: C A V I T Y D I M E N S I O N S A T S E L E C T E D T E S T T I M E S
 238

H i i S i i i i l mmmm
0.23 0.15 0.38

0 ®0.00m&^&k 0.00 0.00

5 1.15 0.76 1.88
10 2.30 1.52 3.75
15 3.44 2.27 5.63
20 4.59 3.03 7.50
25 5.74 3.79 9.38
30 6.89 4.55 11.25
35 8.03 5.31 13,13
40 9.18 6.06 15,00
45 10.33 6.82 16.88
69 15.82

Estimated Diameter, c m (TDR) 28.9

Actual Diameter, c m 29.2
% Difference 1.1
Estimated Diameter, c m (Thermocouple) 33.8
Actual Diameter, c m 29.2
% Difference 15 6
Estimated Cavity Height, c m (TDR) 15.8
Actual Height, c m 17.8
% Difference 11.0

**Note: The axial TDR cable continued to register readings after torch system was
turned off

TABLE G.l: COMPARISON OF CAVITY DIMENSIONS USING TDR

AND THERMOCOUPLE DATA
 239

The torch withdrawal rate influences slag shape and perhaps cavity shape to an

extent. Longer torch application at a given height results in a more rounded magma pool,

while shorter duration gives a more cone-shaped magma pool. Previous laboratory

experiments have not focused on cavity dimensions, though most have reported a

combined (cavity and soil slag) "teardrop"-shaped entity. If the shape of the soil slag has

been approximated as a right circular cone (Mayer, 1997), then the cavity could be seen

as somewhat cylindrical. The teardrop-shaped cavity and slag has not been duplicated in

the DSWA tests conducted. All successful tests have shown a paraboloid-shaped cavity

above the approximate right circular cone-shaped kaolin slag, typical of Figure G.4. This

seems to indicate that the cavity shape differs between soil types and torch withdrawal

rate. It must be noted that the experiment was the first laboratory experiment to use TDR

instrumentation. Thus, further experiments are needed to investigate and optimize the

use of TDR.

COMPACTION EFFECT

The compaction method used in preparing the chamber can leave large voids throughout

the specimen, but especially around the stovepipe. It was expected that in these pockets,

the TDR melt rate would be quicker than in areas of dense soil. This tendency can be

seen in the readings taken throughout the experiment. Therefore, melting rates were
 240

FIGURE G.4: POST-TEST CAVITY AND SLAG

determined between readings, and then averaged to account for soil irregularity. A better

method of soil placement would be to compact the layers without the stovepipe, then to

use a post digger to bore a hole into the soil. The stovepipe can then be placed into the

hole.
 241

CABLE AND DIELECTRIC MELTING (SHORT-CIRCUITS & ERRONEOUS

READINGS)

The dielectric material between the conductors was expected to melt first. If this

happened, the conductors might touch one another and cause a short. Due to orientation,

the radial TDR cable shorted after about 15 minutes of testing and therefore the melting

rate was calculated up to that time. The axial TDR did not short, but the dielectric did

melt faster and probably dripped down into the magma. Cables are available with Teflon

dielectric, metallic separators between conductors, and optical fiber with a higher melting

point than polyethylene.

Another consideration of melting is that the reflected pulse will determine the point

up to intact dielectric material, thereby giving a shorter reading than the actual remaining

length. These problems can be corrected after testing by measuring the distance from the

end of the cable to the boundary of the remaining dielectric material. If it is assumed that

this difference in length is the same, then a correction can be determined and applied.

Lastly, the cable may continue to melt after torch operation due to the high residual

temperature gradient. This dimension may be significant depending on the rate of

dissipation and needs to be accounted for.

CONCLUSIONS AND RECOMMENDATIONS

Comparisons of the cavity dimensions calculated from the TDR agree reasonably

with the actual cavity measurements. This indicates that TDR instrumentation is
 242

compatible with plasma magmavication and is able to operate sufficiently within the

harsh environment of the treatment zone. Experiments should be performed with larger

chambers, various types of cables, different soils, and longer testing times in order to

improve the measuring technique. A major concern that needs to be addressed is the

interference encountered during field testing at higher power levels. Perhaps increased

distance from the torch system will rectify this, but that remains to be seen.

TDR components have a wide range of prices and options. Rental companies can

provide individual components or inclusive units for rent or purchase. GeoTDR, Inc. will

also build a TDR setup to specification and/or obtain refurbished inclusive units. They

also sell software developed for multi-channel TDR called NUTSA. An adequate TDR

setup can be obtained for between $3,500- $10,000 and will be usable both in the

laboratory and the field. It is suggested that separate components be purchased rather

than inclusive units for more freedom in exchangeability and easier maintenance.

Finally, non-penetrating TDR probes can be developed and may be powerful in

discerning changes in the soil during treatment by the difference in reflected pulses. If

this avenue is explored, not only will the cavity and magma pool be detectable, but

differing layers surrounding the slag can be found. This information can be used to

ascertain the complete area of influence induced by plasma magmavication.

Additionally, this information can be used for determining a more accurate volume of

treated material and the degree of treatment of the affected area surrounding the soil slag.
 243

REFERENCES

Andrews, J.R. (1994). Time Domain Reflectometry. Symposium, Time Domain

Reflectometry in Environmental, Infrastructure, and Mining Applications, Northwestern
University, Evanston, Illinois, http7/iti.acnsMM^^f^^si^i^^t^^

ASTM D 422, (1996). Standard Test Method for Particle-Size Analysis of Soils, ASTM
Section 4, Vol. 4.08 Soil and Rock (I): D 420 - D 4914.

ASTM D 698, (1999). Standard Test Method for Laboratory Compaction Characteristics
3 3
of Soil Using Standard Effort (12,400 ft-lbf/fl (600 kN-m/m )), ASTM Section 4, Vol.
4.08 Soil and Rock (I): D 420 - D 4914.

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