TECHNICAL REPORT
STUDY OF THE POTENTIAL FOR RECOVERING UNREACTED LIME
FROM LIMESTONE MODIFIED FLYASH BY AGGLOMERATE
FLOTATION
FINAL REPORT
Contract PH 22-68-18
Division of Process Control Engineering
National Air Pollution Control Administration
Departaent of Health, Education and Welfare
COAL RESEARCH BUREAU
MINERAL INDUSTRIES BUILDING
WEST VIRGINIA UNIVERSITY
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STUDY OF THE POTENTIAL FOR RECOVERING UNREACTED LIME FROM
LIMESTONE MODIFIED FLYASH BY AGGLOMERATE FLOTATION
by
Charles F. Cockrell, Supervising Research Engineer
Richard B. Muter, Research Chemist
Joseph W. Leonard, Director
and
Ronald E. Anderson, Assistant Research Technologist
Coal Research Bureau
School of Mines
West Virginia University
Morgantown, West Virginia
FINAL REPORT
May, 1970
Contract PH 22-68-18
Division of Process Control Engineering
National Air Pollution Control Administration
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TABLE OF CONTENTS
SUMMARY
1. Introduction 1
2. Modified Flyash Samples 4
2.1 Detroit Edison Company, St. Clair, Michigan 4
2.2 Tennessee Valley Authority, Colbert, Alabama 4
2.3 Chevrolet Motor Division Plant, St. Louis, Missouri 6
2.4 Kansas Power and Light Company, Lawrence, Kansas 7
2.5 Union Electric, St. Louis, Missouri 7
3. Flotation Studies 8
3.1 Introduction 8
3.2 Purpose of the Flotation Studies 9
3.3 Flotation Results 9
3.4 Experimental Flotation Separations 9
3.41 Preconditioning 11
3.42 Modifier Addition 11
3.43 Carbonation 11
3.44 Emulsion Composition 12
3.45 Flotation Separation 12
3.46 Recleaning 13
3.5 Factorial Design Flotation Tests 15
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TABLE OF CONTENTS (Cont'd)
4. Supportive Flotation Tests 19
4.1 Zeta Potential Studies 19
4.2 Carbonation Studies 26
4.3 Thermogravimetric Analysis 29
4.4 Microscopic Analysis 32
5. Sulfur Recovery 35
6. Agglomerate Sieving 36
7. Conclusions 37
References 39
Appendix A - Flotation Test Data 40
Appendix B - Zeta Potential Data 94
Appendix C - Carbonation Data 170
Appendix D - TGA Data 181
Appendix E - Agglomerate Sieving Data 240
TABLES
Table
1 Chemical and Physical Properties of Modified Flyash Samples 5
2 Typical Results of Lime Recovery by Agglomerate Flotation 10
3 Comparison of Agglomerate Flotation With and Without
Recycling 14
4 Carbonation Test Data 30
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TABLE OF CONTENTS (Cont'd)
Figure
1 The ECMC Process 2
2 Relationship of Potential to Distance From the
Surface of Shear for a Spherical Colloidal Particle 20
3 The Structure of the Double Layer and Potential Distribution
in the Double Layer in Electrolyte Solutions 21
4 The Zeta Potential and Specific Conductance with Change
in pH of Limestone Modified Flyash PID, the Coal Ash
Constituents of PID and the Lime Constituents of PID in
Liquors Containing the Soluble Constituents of PID 23
5 The Effect of the Zeta Potential and Specific Conductance
of the Constituents of Limestone Modified Flyash Sample
PID at Various Levels of pH after the Addition of 4.0
Pounds Per Ton of Trivalent Iron as Ferric Chloride to
a 16.5 Percent Slurry Concentration 25
6 The Effect of Carbonation on the pH of 33 Percent Slurries
of Dolomite Modified Flyash CI 27
7 The Effect of Carbonation on the pH of 33 Percent Slurries
of Dolomite Modified Flyash CM 28
8 The 2.60 Specific Gravity Separation of Limestone Modified
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SUMMARY
As a result of initial promising data obtained on froth flotation of
200 x 325 mesh fractions of limestone modified flyash, extensive studies
were undertaken to determine the feasibility of recovering the unreacted
lime from limestone modified flyash by flotation separation. Grades of
lime recovered were as high as 80 percent in comparison to the 47.6 percent
grade obtained in the preliminary froth flotation tests on the 200 x 325
mesh fraction of a limestone modified flyash. However, as lime grade increased,
the recovery of lime decreased. This was attributed to the embedding of small
siliceous particles in the lime constituents and the coating of the siliceous
coal ash fraction with soluble lime. Tests have indicated that the lime may
be liberated by attritional scrubbing and that carbonation and the use of
chemical modifiers reduce coating of the siliceous coal ash fractions with
lime. Employment of carbonation for pH and soluble lime control, modifiers
for zeta potential control, agglomerate (emulsion) flotation and recleaning
of the lime concentrates did not improve the yield and grade of lime to permit
recovery of a majority of the lime in a highly concentrated form. It was
indicated that lime grade and yield might be improved through further study;
however, the results obtained and the increased interest in wet collection
of limestone modified flyash do not warrant further work in this area at
this time.
Two other areas of investigation have also shown considerable potential.
These are mineral wool production and sulfur recovery; studies will be con-
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I
Section 1
INTRODUCTION
A significant amount of the sulfur oxides emitted to the atmosphere I
by pollution sources results from coal combustion. (1) The Process Control
Engineering Division (PCED) of the National Air Pollution Control Administration
(NAPCA) has been developing processes for reducing or eliminating this source
of atmospheric pollution. One proposed method that has received considerable
attention involves injection of limestone into the boilers of coal fired power
stations for calcination and subsequent sorption of the gaseous sulfur oxides.
Injection of limestone, however, substantially increases the amount of
flyash generated and modifies the chemical and physical properties of the
flyash. The quantities generated and the fact that the modified flyash cannot
be used in current methods of flyash utilization due to changes in chemical
and physical properties could constitute a liability for the limestone injection
process. As a part of NAPCA's overall program to determine the feasibility of
limestone injection for sulfur oxide control, the Coal Research Bureau was
contracted to determine if the potential liability of increased solid wastes
due to the generation of large quantities of limestone modified flyash could
be converted into an asset to help offset part of the limestone injection
process operating costs.
It was observed during initial contract work (2), that such factors as •
small particle size, sulfur content, solubility and overall chemical properties
of the modified ashes precluded concentration of metals or minerals by such
common mineral dressing techniques as sieving, specific gravity separation,
air classification and magnetic separation. The initial contract work was
concentrated on characterizing the physical and chemical properties of limestone-
dolomite modified flyashes to determine if fractions or products of a salable nature
could be obtained. However, preliminary froth flotation tests on the 200 x
325 mesh fractions of PID dry collected limestone modified flyash showed a
recovery of 94.7 percent of the lime in a concentrate of 47.6 percent lime
grade. These initial promising flotation results prompted an intensive'
flotation study for the recovery of unreacted lime. The other most promising
methods for utilization during the initial studies were the production of
mineral wool and recovery of sulfur gases. These three most promising areas
of utilization could be incorporated into a preliminary conceptual plan for
an Emission Control Minerals Complex (ECMC) Process (Figure 1) aimed at complete
utilization of all fractions of modified flyash. (3)
The ECMC Process would consist of (a) a primary phase of recovery for '
reinjection of unspent lime from modified flyash-water slurries by carbona- -
tion followed by agglomerate flotation and secondary phases of (b) manufacture I
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Figure I
THE EMISSION CONTROL MINERALS COMPLEX (ECMC) PROCESS
COAL
PLUS
LIMESTONE
»
AND/OR
DOLOMITE
INJECTION
t
REMOVAL OF STACK GASES
DURING CARBONATION
CO, INPUT FOR
CARBONATION 8 pH CONTROL
TRANSFER OF MODIFIED FLYASH TO CONDITIONING TANK
ALKALINE EARTH
REINJECTION
TRANSFE R OF CONDITIONED FLYASH SLURRY TO FLOTATION CELL
HtO
HEATED
SULFUR GAS REMOVAL AT
A SPECIFIC TEMPERATURE
RANGE
FLOTATION
CELL
©
DEWATERNG
OF
ALKALNE
EARTH
MATERIALS
TRANSFER
OF
FLOTATION
REJECT
DRIED REJECT TO BE
UTILIZED IN
MINERAL WOOL 8
SULFUR COMPOUND
PRODUCTION
GAS
PROCESSING
FOR
SULFUR PRODUCTS
WASTE GAS MANIFOLD
STAGGERED SERIES OF
REVERBERATORY FURNACES
f?
MOLTEN
MINERAL
WOOL
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rejects and (c) recovery of sulfur values when the rejects are heated. Mineral
wool production and sulfur recovery tests were carried out in conjunction with
solid waste disposal utilization procedures under study by the Coal Research
Bureau for the U. S. Bureau of Mines. (A) Therefore, the work performed under ~" _
this contract was essentially concerned with the primary phase of recovering
the unreacted lime. •
All modified flyash samples were subjected to bench scale agglomerate
(emulsion) flotation tests as well as support tests such as (a) zeta potential
measurements to determine the surface potential of particles of limestone modi- I
fled flyash and the effect of chemical modifiers on the surface potential, (b) *
carbonation to determine the reaction of different limestone modified flyashes
to this method of solubility control during flotation and (c) thermogravimetric
analysis (TGA) to determine the amount of both carbonated particles and agglomer-
ating emulsion associated with the different fractions resulting from flotation
separation.
In addition to the extensive tests in these areas, some preliminary
investigations were also undertaken on evolution of sulfur oxides from
limestone modified flyash at high temperatures under oxidizing conditions as
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Section 2
MODIFIED FLYASH SAMPLES
Modified flyashes used in this study were obtained from the following
sources: (a) Detroit Edison Company, St. Clair, Michigan Power Plant; (b)
Tennessee Valley Authority, Colbert, Alabama Power Plant; (c) Chevrolet Motor
Division Plant, St. Louis Missouri; (d) Union Electric Company, Merrimac
Power Plant, St. Louis, Missouri; and (e) Kansas Power and Light Company,
Lawrence, Kansas Power Plant.
Details concerning the development, collection and characteristics of
the samples supplied by each source follow:
2.1 Detroit Edison Company, St. Clair, Michigan
The work undertaken at the St. Clair, Michigan power station was a joint
effort by Detroit Edison Company and Combustion Engineering, Inc. to field
test the limes tone-dolomite injection—wet collection sulfur oxide removal
system under development by Combustion Engineering, Inc. In these tests only
a small amount of the dust-laden stack gases were diverted to a wet scrubber
so that both wet and dry collected modified flyashes were available. When the
dolomite tests were completed, a high purity limestone was tested. Thus, it
was possible to obtain both wet and dry collected limestone and dolomite modified
flyashes. The chemical and physical properties of the limestone dry-collected
sample utilized In this study are given in Table 1.
In these tests, the coal and stone were pulverized to approximately 95
percent passing 200 mesh. The crushed stone was injected through the top
burner, oriented 30° above the horizontal, of a 325 megawatt Combustion
Engineering twin furnace unit. Limestone was fed into the boiler at a rate
of approximately 10 tons per hour (180 percent of the stoichiometric
requirement).
A combination of electrostatic and mechanical precipitators, rated to
be 99.5 percent efficient, was used to collect the dry sample. The dry
modified flyashes from each type of precipitator were admixed after
collection.
2.2 Tennessee Valley Authority, Colbert. Alabama
These limestone modified flyashes were generated at the TVA Colbert,
Alabama power station in separate periods of operation when different lime-
stones were being tested. The chemical analyses of the limestone modified
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TABLE 1
CHEMICAL AND PHYSICAL PROPERTIES OF MODIFIED FLYASH AND
NORMAL FLYASH USED IN FLOTATION AND RELATED
STUDIES
Source
Identification
Modifying Stone
Mode of Collection
Chemical Composition, %
(Dry Basis)
Si02
A1203
Fe203
Ti02
CaO
MC0
Na20
K20
S03
C
Loss on Ignition
Water Soluble Fraction
Moisture
Physical Properties
Melting Properties, "F
Initial Deformation Temperature
Softening Temperature, Spherical
Softening Temperature, Hemispherical
Fluid Temperature
Median Particle Size, Microns
Detroit
Edison
PID
Limes tone
Dry
TVA
DiD2
Limestone
Dry
TVA
D1D2
Limestone
Dry
Chevrolet,
St. Louis
CM
Dolomite
Dry
Chevrolet,
St. Louis
CI
Dolomite
Dry
Union
Electric
SLD
Dolomite
Wet
30.85
13.70
11.59
0.68
29.79
1.49
1.12
0.71
2.20
1.12
1.03
22.11
0.00
2071
2138
2145
2172
9.30
29.52
13.00
14.85
0.53
22.55
1.56
0.59
1.42
3.73
0.88
2.00
21.58
0.10
1740
2100
2120
2140
3.80
31.68
14.29
15.97
0.56
24.94
1.49
0.77
1.63
1.95
0.91
1.30
9.58
0.20
1730
2120
2130
2140
4.40
35.90
14.40
7.76
0.71
22.97
13.93
0.34
0.72
8.05
3.29
3.79
0.24
1870
2260
2270
2300
4.30
33.10
11.80
7.18
0.65
17.92
11.45
0.46
0.72
6.95
5.64
8.34
0.26
1720
2250
2270
2280
4.20
30.80
14.70
7.03
0.64
19.56
4.77
0.36
1.42
15.38
1.49
6.13
25.50
98.00
1780
2140
2150
2160
5.10
Kansas
Power and Light
KPL
Limestone
Wet
29.80
6.79
9.09
0.42
27.13
0.97
0.23
1.29
20.25
1.55
6.01
16.60
99.00
1710
2150
2160
2170
4.00
1702
2400
2410
2460
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In these tests, the particle size of the injected limestone ranged from
70 percent passing 200 mesh to 95 percent passing 325 mesh. Limestone was
injected into the boiler through all sixteen burners by pre-mixing with the
coal in proportions approximately equal to 67 percent of the stoichiometric
requirement for the 6 percent sulfur content coal being burned. These dry-
collected limestone modified flyashes were obtained from standard mechanical
cyclone dust collectors which had been designed to remove approximately 70
percent of the particulate matter in the stack gases. In dust collectors
of this type, the finer size fractions generally escape to the atmosphere.
Thus, the smallest size fractions of modified flyash were not recovered.
2.3 Chevrolet Motor Division Plant. St. Louis, Missouri
The injection tests undertaken by Chevrolet Motor Division at their St.
Louis assembly plant were performed in a small B & W boiler having a capacity
of two tons of coal per hour. Pre-ground commercially available dolomite
was tested both by intermixing and by injection above the flame envelope.
Physical and chemical characteristics of the resultant modified flyashes
produced by this boiler are shown in Table 1.
The CM modified flyash was produced by pre-mixing the dolomite and coal
while the CI material was produced by injecting the material above the flame
envelope.
In these tests, the dolomite, vended as "dolcito," was injected into the
B & W pulverized coal integral furnace type boiler at a rate of 200 percent
of the stoichiometric amount required. The dolomite had been pulverized by
the supplier to 76 percent passing 230 mesh and 4.4 percent passing 325 mesh.
The coal burned during the tests contained 3 1/2 percent sulfur and was obtained
from the River King No. 2 mine of Peabody Coal Company and the Sparta Mine of
Bell and Zoller Company. The coal was fed into a B & W Type E pulverizer in
a ratio of 60 percent River King to 40 percent Sparta where it was pulverized
to 70 percent passing 200 mesh prior to combustion. The dry modified flyash
was collected in an electrostatic precipitator rated to be approximately 99
percent efficient.
In the initial test, dolomite was admixed with the coal by adding 50
pounds of dolomite every three minutes through the exit port of the weight
feeder. A 45 minute delay occurred between the time dolomite was first
added and a stable reduction of sulfur dioxide occurred. After the stable
reduction occurred, the test was continued for three hours.
In the second test, dolomite was injected from a spider system specifically
designed to permit the dolomite to be uniformly sprayed, via six nozzles, into
the boiler above the flame envelope at an angle of approximately 45 degrees
above the horizontal. This test was also of three hours duration; however,
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2.4 Kansas Power and Light Company, Lawrence, Kansas
The tests undertaken at Lawrence, Kansas, were a joint effort by Kansas ^
Power and Light and Combustion Engineering, Inc. on a full-scale, permanent — .
wet scrubbing installation. The scrubbing system is located on the 125 MW,
No. 4 Unit and had been operating for approximately one day prior to sample I
collection. The system used dry injection-wet collection in which limestone, |
ground to approximately 60 percent passing 200 mesh, was injected at the rate
of 110 percent stoichiometric into the 2100°F ter.iperature zone of the furnace. .
Two separated scrubbing units were incorporated, both of which employed an over- I
bed recycle system whereby water and modified ash from the bottom of the scrubber
were passed to a delay and mixing tank and then recycled by being sprayed
above the marble bed in the scrubber. The system used about 3,000 gallons of
water per minute of which 700 gallons per minute was obtained from blow down
of the cooling tower. The remaining water came from a recycle pond adjacent
to the settling pond. Sulfur dioxide was monitored both before and after the
scrubber. The coal being burned contained 1,960 parts per million (ppm) sulfur
as sulfur dioxide and 760 ppm was sorbed by calcined stone in the dry state.
The remaining 1,200 ppm entered the scrubber and 400 ppm were emitted to the
atmosphere after scrubbing. Samples for flotation purposes were obtained
from the 12 inch I. D. exit pipes leading to the settling pond. The slurry
solids were approximately one percent. Physical and chemical analyses of
this sample are shown in Table 1.
2.5 Union Electric Company, St. Louis, Missouri
Samples of wet collected dolomite modified flyash were also obtained
from the Merrimac Plant of Union Electric at St. Louis, Missouri. As was
the case at Lawrence, Kansas, a dry injection-wet collection technique was
employed. When the samples were taken, one of the two scrubbers was shut
down for modification but the water requirement was not reduced. Dolomite
of approximately 85 percent passing through 200 mesh size was added at the
rate of 60 percent stoichiometric to the 2,000°F temperature zone of the furnace.
Approximately 3,000 gallons per minute of water was used, of which 90 percent
could be recycled from a clarification system. The slurry concentration of
the SLD material, even though it contained twice as much water as normal, was
about two percent. Physical and chemical analyses of this sample are also
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Section 3
FLOTATION STUDIES
3.1 Introduction
Flotation is a mineral dressing technique for separating physically
distinct mineral entities which are generally finer than 28 mesh. Specifically,
the objective of froth flotation is to recover valuable metals or minerals by
the addition of chemical additives (collectors) which will make the desired
mineral system hydrophobic, while permitting the other mineral systems to
remain hydrophilic in a water slurry. Usually other chemical additives
(modifiers) and pH controls are utilized to aid this action by altering
the zeta potential or surface charge (discussed in Section 4) of the systems.
Next, the slurry is mechanically or pneumatically agitated to introduce air in
such a manner as to cause collisions between the rising air bubbles and the
liberated hydrophobic mineral system so that each air bubble levitates one
or more of the hydrophobic particles. Other chemicals (frothers) are
generally required to assist the collectors in producing a froth which is
used to stablize the concentrate so that it may be removed from the surface
of the slurry either by displacement or mechanical action. The unlevitated
minerals in the slurry (tails) can be either discarded or subjected to further
treatment.
Agglomerate flotation differs from froth flotation in that oil-water
or water-oil emulsions incorporating both the collector and frother are used
to concentrate the desired mineral by causing it to agglomerate or clump
together by absorption in the oil media prior to attachment to the rising
air bubble.
Flotation separations are usually carried out in a series of basic steps
(flotation circuit) whose order can be varied depending on the prevailing
circumstances. After the addition of the modifier and collectors, the
slurry is usually agitated for a pre-determined period of time (conditioned)
in order to allow the chemicals to react with the mineral systems prior to
flotation. The slurry is then subjected to the first separation step or
rougher separation which produces a concentrate and a tail. The concentrate
can then be refloated or recleaned (utilizing more chemical additives if
desired) as many tines as necessary to obtain the desired concentration.
Further flotation of the tails or unlevitated mineral systems to obtain any
of the desired mineral missed in prior separations is called scavenging.
The results of flotation separations are usually given in terms of
grade and yield. Yield is a percentage measure of the amount of desired
mineral removed from the feed, eg, reporting in the concentrate. .Grade is
a percentage measure of the purity of the concentrate in terms of the
desired mineral. For example, the 47.6 percent grade and 94.7 percent yield
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-9-
of the lime in the feed material was recovered in a concentrate that was
47.6 percent lime.
3.2 Purpose of the Flotation Studies
The intensive flotation studies were undertaken to (a) determine the |
feasibility of recovering major portions of lime from dry collected lime-
stone modified flyash, (b) determine the feasibility of incorporating the .
rejects obtained from the flotation as a raw material for mineral wool pro- I
duction and sulfur recovery in order to utilize all fractions of modified '
flyash and (c) to expand the technology developed to all types of modified
flyash.
3.3 Flotation Results
The flotation data obtained are given in Appendix A. For convenience,
typical data have been abstracted and presented in Table 2. As shown in
Table 2, concentrates in excess of 80 percent lime were obtained; however,
the grade (54.66) and yield (34.99) of Test 85 are more representative of
grades and recoveries usually obtained.
The first phase of flotation work sought to upgrade lime yield and grade
through a series of empirical tests to identify variables that might affect
yield and recovery. The major findings were that process results could be
improved by (a) employment of agglomerate flotation, rather than conventional
froth flotation to more effectively separate the very fine particles of
modified flyash and (b) carbonation of the modified flyash-water slurries
for the reduction in the amount of soluble lime present in the flotation
water and subsequent pH control of the slurry. Other operational variables
which affected process results were (a) percent solids in the slurry, (b)
flotation machine rotor speed, (c) carbonation time (a measure of the rate
of carbon dioxide injection and the capacity of the flotation slurry to
absorb carbon dioxide), (d) slurry pH after carbonation, (e) type of promoter
(collector), frother and modifier, (f) slurry conditioning time and (g) length
of time of the flotation separation.
The second phase of work represents efforts to further improve lime grades
and yields through adjustment of the factors identified in the first phase.
A series of 16 factorially designed flotation tests were also performed during
the second phase. The tests had the objective of Improving lime grades and
yields through determination of the effect of change of (a) emulsion addition
rate, in pounds per ton, (b) agglomeration (conditioning) time after emulsion
addition, (c) impeller rotor speed during flotation separation and (d) rosin
content of the tall oil used in the agglomerating emulsion.
i
3.4 Experimental Flotation Separations . '
( Experimental flotation separations for modified flyash consisted of •
preconditioning, modifier addition, carbonation, agglomerating emulsion
addition, separation of a lime rich fraction by aeration and levitation and I
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TABLE 2
TYPICAL RESULTS OBTAINED FOR LIME RECOVERY BY AGGLOMERATE FLOTATION OF
LIMESTONE MODIFIED FLYASH
(Abstracted From Appendix A)
% CaO
of Limestone
% Grade
CaO in
Agglomerate Calculated
Ratio
Table
1A
3A
8A
16A
Test
No.
79
85
94
115 CC2
115
Modified
Flyash
22.55
29.79
29.79
29.79
29.79
Flotation
Concentrate*
51.98
54.66
32.25
81.45
39.62
CaCO
Equivalent
93.0
97.9
57.7
145.8
53.0
% CaO
Recovered
18.32
34.99
74.75
4.04
30.08
of
Enrichment
2.31
1.85
1.08
2.73
1.33
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-11-
Flotation separations were performed in a WO1CO Fagergren Mineral Master
flotation machine of 600 gram capacity manufactured by Western Machinery.*
The following observations were made concerning the separations:
3.41 Preconditioning. Modified flyash-water slurries were conditioned
as an initial step by intensively mixing water, modified flyash and a collector I
in the flotation cell to insure complete wetting as well as to assure proper I
collector attachment. From the flotation data obtained, it was indicated
that conditioning time was important and that increased conditioning tine •
was beneficial in improving lime grade. No improvement in yield was |
indicated.
During conditioning, the lime particles were softened by the water and
abraded by collisions. This increased the already high solubility of line
in water and required additional carbon dioxide to control the pH. However,
increased conditioning time was found to liberate relatively pure quantities
of lime by the abrasive action on the softened particle. This was indicated
in Test 115 (Table 2) in which an increase in conditioning time from the
normal 15 minutes to one hour was partially responsible for the increase in
grade from 29.79 percent to 81.45 percent in the second cleaner concentrate
(CC2).
As an alternative to increased conditioning time, tests were undertaken
to determine the feasibility of accelerating particle breakdown by attritional
scrubbing of high solid (80 percent) slurries prior to flotation. Some
particle breakdown was observed microscopically; however, further microscopic
analysis and flotation testing would be required to determine the full effect
of particle breakdown by this method.
3.42 Modifier Addition. The purpose of adding chemical modifiers prior
to the addition of the agglomerating emulsion is to selectively alter the
zeta potential (surface charge) of the lime fraction to permit selective
adsorption of the collector by the lime. A wide variety of di- and
trivalent compounds were tested because the effectiveness of a modifier
generally increases with increased valence and decreased ionic radius due
to increased adsorptive capacity of the smaller ions by the mineral.
Additions to the modified flyash-water flotation slurries of divalent
ferrous ammonium sulfate (FAS), usually at one pound per ton (PPT), were
found to be the most effective modifier. The effects of modifiers on the
surface charge were determined by zeta potential measurements and are discussed
in detail in Section 4.1.
3.43 Carbonation. The purpose of carbonating the modified flyash water
flotation slurries was to decrease the amount of undesirable water soluble
line (solubility 1.31 grams per liter) by formation of essentially insoluble
calcium carbonate (solubility 0.014 grams per liter). In agglomerate
flotation tests at 5.4 percent solids up to 35 percent of the lime I
reported in the water if the slurry was not carbonated. However, carbonation
of flotation slurries of the same solids concentration reduced the amount •
of soluble lime five-fold. - . I
t •
*Trade names are used to facilitate understanding and do not imply |
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Carhonation was also found to be necessary for pH control. Carbonation
was found to effectively lower the slurry pH from 12 to 13.5 to a more accept-
able range for flotation separation of 6.5 to 9. Zeta potential data,
reported In Section A.I, showed that such a pll adjustment was necessary to
achieve a suitable difference in surface charges of various modified flyashes
even with the addition of chemical modifiers. Carbonation was selected in
place of such seemingly appropriate mineral acids as hydrochloric acid
because (a) lowering the pH was not possible with practical quantities of
hydrochloric acid because the formation of highly soluble calcium chloride
(745 grams per liter) would result in a decrease of available lime for
flotation and (b) carbonation precipitates any additional lime that might
be brought into solution by equilibrium dynamics for a period of several
minutes to an hour or more which allows sufficient time for the flotation
separation.
The reactions involved in carbonation of lime are well known and would
proceed as follows:
Ca + H20 Ca(01i)2 . (1)
When carbon dioxide is injected,
Ca(UH)2 + C02 CaC03 + H20 . (2)
Any excess carbon dioxide yields carbonic acid by the equation
C02 + H20 li2C03 . (3)
The formation of extremely soluble calcium bicarbonate by the reaction
CaC03 + C02 + 1120 Ca(HC03)2 (4)
was not found to be a problem.
Chemical analysis of the flotation water never indicated the presence of
excess calcium after carbonation as might be predicted by the above equation.
While no tests were run, the absence of bicarbonates might be attributable
to the presence of unreacted lime in the center of particles coated with
calcium carbonate which came into solution slowly and took up any excess
carbonic acid.
After the initial requirement for carbonation was established with one
limestone modified flyash (PID), a systematic study was undertaken to determine
the mechanisms involved. These studies are reported in detail in Section A.2.
3.44 Emulsion Composition. Initial emulsion composition was 50 per-
cent water, 22.5 percent tall oil collector, 25 percent fuel oil dispering
agent and 2.5 percent sodium akylaryl sulfonate (SAAS) frother and was within
the general range used for flotation of other minerals. (5) Subsequent tests
with tall oils of different rosin acid contents showed that more than 28 per-
cent or less than about 15 percent rosin acid content sharply reduced the
grade of lime that could be recovered. This factor was included in factorial
tests (Table 8A, Appendix A) and it was indicated that tall oil containing
22 1/2 percent rosin acid would be best for the emulsion. Later flotation
tests in which the amount of SAAS was varied from 0.5 to 2.5 percent showed
that about 2.0 percent SAAS resulted in the best emulsion composition for optimum
flotation separation.
3.45 Flotation Separation. Agglomerate (emulsion) flotation separations
were made by inducing air as very small bubbles to the bottom of the flotation
cell to levitate the lime rich fraction to the surface for mechanical removal.
-------
-13-
Staged rougher separations (Test 85, Table 2) showed that the grade decreased
sharply after five minutes.
Agglomerate (emulsion) flotation was used, rather than conventional
froth flotation, to more effectively separate the very fine particles of
modified flyash. After numerous tests in the first stages of flotation
testing, it.was indicated that froth flotation would not be as effective in I
lime recovery from unsized modified flyash as it was with the sized (200 x •
325 mesh) flotation feed. In agglomerate flotation, the conventional organic
flotation reagents for collection and froth generation are mixed with oil, I
generally a low grade fuel oil, and then emulsified with water. When added I
to the modified flyash-water flotation slurries, the ultra fine carbonated
calcium rich particles are preferentially absorbed in the oil rich phase of
the emulsion.
3.46 Recleaning. The initial rougher concentrates (RC) were recleaned by
refloating for improvement of lime grades. The recleaning procedures tested
involved both recleaning without recycling of the unlevitated tail products
and with recycling. The purpose of recleaning without recycling was to obtain
maximum grades and highest possible ratio of enrichment (ratio of percent lime
in fraction to percent lime in the feed) whereas recycling was employed as
a means of improving lime yields.
Data from tests (shown in Table 3) have been abstracted from Appendix
A to show typical (Tests 85 and 11) results obtained with and without
recycling the unlevitated tail products when recleaning the rougher con-
centrates (RC). For Test 85, grade, recovery and enrichment values were
respectively, 47.87 percent, 42.80 percent and 1.61 for 1 RC; 26.44 percent,
16.85 percent and 0.89 for 2 RC and 20.97 percent, 30.05 percent and 0.70 for
3 RC. The first fraction (1-CC^) obtained on recleaning for 1 RC yielded a
product containing 60.29 percent lime but recovery, in terms of total lime,
decreased to 24.62 percent. The ratio of enrichment showed a favorable
increase to 2.02. The second recleaning fraction (1-CC ) was obtained by
raising the flotation machine inpellor speed from 1100 to 1700 rpm and a lime
grade of 44.76 and 10.37 percent lime recovery was obtained. Recleaning 2 RC
and 3 RC showed little improvement in lime grade and might be attributed to
the fact that most of the emulsion had been removed from the cell with 1 RC.
The low lime yields and the fact that most of the emulsion was removed
in the initial stages of the rougher separation led to recycling the unlevitated
tail products from recleaning the rougher concentrates. These cleaner tails
were combined with the rougher tails (RT) for further cleaning. To maintain
sufficient froth throughout the recleaning operation, the emulsion was added
in stages. Generally, one-half the emulsion was added prior to the rougher
separation and the rest at various stages of recleaning.
Test 111 is an example of such a test with both recycling the
unlevitated tails and staged emulsion addition. In Test 111, 10 pounds . ~
per ton (PPT) emulsion was added for the rougher separation, five PPT was
later added for the flotation of the total cleaner tails (Scavenger) and I
five PPT was finally added for recleaning the tails (RT and ST). The" - •
cleaner concentrate (CC2) obtained by cleaning the RC twice was 49.47 percent
-------
TABLE 3
AGGLOMERATE FLOTATION OF LIMESTONE MODIFIED FLYASH PID WITH AND
WITHOUT RECYCLING THE UNLEVITATED TAILS
(Abstracted From Appendix A)
Recleaning Without Recycling
Emulsion
Test Addition
Table No. PPT Fraction
3A 85 140.75 1-RC
1-CCi
1-CC2
2-RC
2-CCi
2-CC2
3-RC
3-CCi
3-CC2
Total RC
Total CC
Grade
CaO
%
47.87
60.29
44.76
26.44
28.50
30.46
20.97
21.02
21.08
30.26
54.66
Yield
Recovered
%
42.08
24.62
10.37
16.85
10.51
7.92
30.05
29.21
28.66
89.71
34.99
Ratio
of
Enrichment
1.61
2.02
1.50
0.89
0.96
1.02
0.70
0.71
1.00
1.02
1.17
Recleaning With Recycling
12A 111 10.00 RC Tails Recycled to Scavenger Float—No Data Obtainable
CC Tails Recycled to Scavenger Float—No Data Obtainable
5.0
5.0
CC
SC
TC
TC
j.
2
(CT1 +
1 (RT +
2
CT2)
ST)
Total CC
49
39
•
*
74
72
Recycled — No
27.39
39
•
01
29
20
Data
15
65
.41
.22
Obtainable
.77
.40
1.
1.
0.
1.
67
33
92
-------
-15-
When the total CC from each test is compared, it is evident that sub-
stantially more of the lime was recovered in Test 111 but the lime grade was
lowered by 15.65 percent with 120 PPT less emulsion. The effect of recycling
is best illustrated when the scavenger concentrate is compared with the second
float fraction of 1 RC of Test 85. The recleaning with recycling resulted in
an SC of 39.72 percent and 20.22 percent recovery as compared to 44.76 percent I
grade and 10.37 percent recovery for 1 RC of Test 85. •
In summary, the recleaning tests showed that recycling the unlevitated I
tail products, with staged emulsion addition, would be more applicable because I
yield could be Increased without greatly reducing grade.
3.5 Factorial Design Flotation Tests
The purpose of the factorial design experiment was to optimize the
factors believed to exert the greatest influence on the lime grade and
yield. These factors were chosen as a result of information obtained from
previous flotation tests. The factors studied were emulsion addition rate
(in pounds of emulsion per ton of ash), conditioning or agglomeration time,
flotation cell impeller speed and tall oil rosin content. The factorial
design, standard operating conditions and results are given in Table 8A,
Appendix A.
Since one of the problems attendant to flotation separations was low
lime recovery, a different method of separation and recleaning was incor-
porated in the standard operating conditions of the factorial design
experiments. In the factorial tests, emphasis was placed on shorter periods
of rougher separation (4 minutes versus 10 or more minutes) followed by
cleaning of the combined unlevitated tail products.
The standard operating conditions, with one exception, were those
conditions found in previous flotation tests and zeta potential determinations
to give the highest grades of lime. Make-up water for cleaning and recleaning
stages, however, was recycled from previous flotation steps, when possible,
to reduce the total water volume to a workable level. The recycling of water
between stages was found to have no noticeable effect on grade and yield.
The levels of the factors were within the range of normal separation
conditions except for the emulsion addition rate which was lowered in an
effort to determine what lime grades and yields could be obtained with more
economical additions of emulsion.
The responses measured were grade and yield. Since either grade or
yield may normally be improved at the expense of the other, the product
of grade times yield was also calculated with the objective of maximizing
this function as a means of obtaining a compromise between the divergent I
correlations that would be expected for grade versus yield. The grades
and yields given in Table 8A, Appendix A, were obtained from weighted averages i
-------
-16-
The factorial experiment indicated that:
1. Rosin content and impeller speed were significant at the 95
percent confidence level for yield.
2. Second, third and fourth order interactions accounted for all
other assignable variance. There was no variance accounted
for in the grade times yield data.
3. Rosin content for the tall oil was the most important variable
accounting for 40 percent of assignable variance for the yield
data. Increases in grade might be achieved through increased
rosin content; however, rosin content should be decreased to improve
lime yield. Staged emulsion additions might partially satisfy these
opposing conditions.
4. Emulsion addition rate should be increased to improve yield
but decreased to improve grade.
The presence of substantial higher order interactions and the low variance
accountability indicated that the data could not be used with good reliability
to predict results of future tests outside the range of the experiment.
Further, the tests indicated that there were probably other significant
factors which were not controlled during the factorial tests.
Tests 108 through 115 were undertaken to test the validity of conclusions
within the area of experimentation and to determine how far the experimental
results might be extended. Tests 108 and 110 were performed at the midpoint
of the factorial design (eg, 80 PPT emulsion addition rate, 7.5 minutes condition-
ing, 1425 RPM and 23 percent rosin) to test the practicability of staged
emulsion additions. In these tests 40 PPT emulsion was added to the rougher
separation and 20 PPT to both the cleaner tail separation and the rougher tail
separation. The grades and yields obtained were 31.39 percent and 76.77
percent respectively for 108 and 28.96 percent and 62.20 respectively for 110.
Test 108 was in good agreement with the predicted values and tended to confirm
the validity of the experimental equations within the range of the experiment.
However, the poor results obtained with 110, which was run to confirm the
data of Test 108, indicated that other factors were affecting the grade and
yield results. A review of the carbonation data revealed that the pH values of
Tests 95 and 110, both of which gave poor yields and grades, rose rapidly
during conditioning and were higher than any other tests during rougher
separation, rougher concentrate cleaning, cleaner tail cleaning and rougher
tail cleaning. The cause of this rapid increase in pH was not determined;
however, it did point out the necessity of closer monitoring of carbon dioxide
input.
Test 109 was based on the steepest ascent calculations from the factorial
design data. Factors under study were set as follows:
80 PPT Emulsion Addition Rate (staged addition)
3.5 Minutes Conditioning Time
/ 1681 RP11 Rotor Speed
-------
-17-
The weighted average for CC2, SC and TC. resulted in 32.25 percent lime grade
and 76.22 percent recovery. Agreement between the experimental values and
steepest ascent calculations was not good. The observation during this test »
that the agglomerate was more voluminous with 15 percent rosin and the obser-
vation during Test 110 that there were very little tails when the rougher
concentrate was recleaned indicated that further gains might be made by lowering .
the emulsion addition rate. Thus, Test 111, shown in Table 3, utilized only I
one-fourth the emulsion of Tests 108 through 110 so that the effect of the *
reduced emulsion could not be masked. Overall lime grade for a weighted
average of CC-, SC and TCj was 39.01 percent with a recovery of 65.40 percent. I
The CC2 fraction was 49.74 percent grade and 29.41 percent recovery. The •
rougher concentrate in Test 111 was very light in color and substantial tails
were washed out during cleaning. There did, however, appear to be excessive
froth so that subsequent tests, numbers 112 through 114, were concerned with
determining a better level of SAAS as well as verifying Test 111 and making
carbon dioxide measurements during carbonation. SAAS was cut from 2.5 to
0.5 percent of the emulsion in Test 112. The froth was insufficient and the
sample was not submitted for chemical analysis. SAAS was increased to 1.5
percent of the emulsion in Test 113 and the carbon dioxide was injected slowly
enough to keep the initial pH dip to a minimum. The conditions for Test 113
that varied from standard conditions were:
20 PPT Emulsion Addition Rate
3.5 Minutes Conditioning Time
1700 RPM Rotor Speed
15 Percent Rosin
1.5 Percent SAAS in Emulsion .
The overall lime grade and yield was 41.61 and 54.95 percent respectively
with the CC2 fraction being 52.24 and 14.77 percent respectively. The froth
still appeared to be deficient.
A flowmeter was obtained and installed for Test 114 and the carbon
dioxide flow measured in order to determine the effect of the rate of
carbon dioxide injection on pll stability. The test conditions were:
20 PPT Emulsion Addition Rate
3.5 Minutes Conditioning Time
1700 RPM Rotor Speed
15 Percent Rosin
2.0 Percent SAAS in the Emulsion
1.0 CFM Carbon Dioxide Injection Rate
The overall lime grade and yield for Test 114 were 39.31 and 58.44 percent
respectively with the CC- fraction containing 49.53 percent lime with a
yield of 19.72 percent or the lime. The pll exhibited the same stability
found in other tests and the froth appeared to be adequate. The data
obtained for both Tests 113 and 114 appeared to confirm the conditions of -*
Test 111 as being advantageous over the previous higher rates of emulsion
addition. I
-------
-18-
3.6 Summary
Values were found for the flotation separation parameters that improved
lime grade and/or yield. Some additional improvement in grade and yield was
made and the amount of emulsion drastically reduced as a result of the factorial
design study. However, acceptably higher grades and yields of lime were not
consistently achieved and it must be concluded that further substantial bench
scale study would have to be undertaken to obtain further improvements in grade
-------
-19-
Section A
SUPPORTIVE FLOTATION STUDY TESTS
I
Zeta potential, carbonation, thermal-gravimetric and microscopic analyses I
tests were undertaken to determine the best approach for upgrading flotation I
lime grades and yields. In addition, it was desired to develop technology
for the expansion of flotation recovery of lime to a variety of modified
flyashes.
4.1 Zeta Potential Studies
Zeta potential (ZP) studies were undertaken as a means of determining
the surface chemical charge of constituents of limestone modified flyash
after preliminary ZP measurements. (6,7) Numerous tests, undertaken in the
initial phase of flotation separations, showed that pH adjustment, through
carbonation of the flotation slurries alone would not be sufficient to alter
the surface charge for separation of relatively pure lime. Specific conductance
(SC) data, obtained in the course of making ZP determinations, was also found
to be a convenient way of determining the amount of water soluble material
remaining in solution during and after carbontion.
The ZP of a material is the charge exhibited by a collodial particle and
its hydration sphere with respect to the bulk of the solution in which the particle
is suspended. This is shown diagramatically in Figures 2 and 3. Figure 2
illustrates the environment encountered by a colloidal particle in suspension
and indicates the region of space that zeta potential covers. The zone OA
represents a solid spherical particle of small size having a definite charge
associated with it, zone AB represents both a layer of solvation molecules
and a layer of anchored ions of opposite charge to that of the particle
and is sometimes called the Stern layer or plane. These ions are anchored by
the attractive forces of oppositely charged particles. Zone BC, the Gouy
layer, represents a diffuse layer of counter ions having the same charge as
the solid particle and are the counter ions of the anchored ions. Zone CL
represents the bulk of the solution in which the particle is suspended. The
distance from 0 to L is essentially infinite with respect to the size of the
particle. If a unit charge were brought from L to C, the potential necessary
would be snail; however, it would increase as the charge was brought fron C
to B due to the influence of the Gouy layer containing counter ions. The
potential at point B is called the zeta potential and is illustrated on the
graph at the bottom of Figure 2. Figure 3 gives a better picture of the
electrical phenomena occurring in the two layers. In this figure, the solid
spherical particle is represented by region A and has a negative charge *
resulting from negative ions at the particle surface called potential deter-
mining ions which may be part of the particle itself. Region B illustrates the I
-------
-20-
Diffused
counter
Bulk liquid
Potential necessary to bring
a unit charge from the bulk of the
solution to the surface of the
solid particle.
Zeta potential
Distance from the solid particle
to any point in the surrounding
medium.
Distonce, r
Figure 2 Relationship of potential to distance from
surface of shear for a spherical colloidal particle.
(Gaudin, A. M., Flotation. 2nd ed..
-------
-21-
o
en
UJ
t-
o
Q.
© ©
© ©
Potential necessary to bring a unit charge from
the bulk of the solution to the surface of the
solid particle
POTENTIAL-DETERMINING ION
HYDRATED COUNTER ION
NEGATIVE COUNTER ION
Zeta Potential
Potential necessary to bring E unit charge from the
bulk of the solution to the Gouy layer
DISTANCE —
Figure 3 Schematic representation of the structure
of the double layer and potential distribution in the
double layer in electrolyte solutions.
(Furenstenau, D. W. (ed.), Froth Flotation.
-------
-22-
and held near the immediate surface of the particle. Also shown are counter
ions (ions of opposite charge to that of the particle) surrounding the particle
a short distance away. In this figure, the ions are considered to be hydrated.
Region C contains both counter ions and counter-counter ions, the latter having
the same charge as the particle. The zeta potential is again defined as the
potential necessary to bring a unit charge from the bulk of the solution to
point B, the Stern layer.
All ZP and SC data obtained for the modified flyashes are given in Appendix
B. Typical ZP and SC curves are shown in Figure A. The ZP and SC for whole
modified flyashes and both their coal ash and lime constituents were determined.
The ZP and SC values for lime constituents of modified flyash are not true
values because pure fractions of the lime constituent could not be obtained.
It was found, however, that fractions high in liwe could be separated by a
combination of magnetic and specific gravity separation and that the ZP of
these non-magnetic, 2.96 specific gravity float fractions was a good measure
of the ZP of the lime constituent. In the case of wet collected modified
flyashes, the parent flyash was not available to determine the ZP of the coal
ash constituent; therefore, the magnetic fraction was used to determine the ZP
of the coal ash constituent and the nonmagnetic fraction was used for the lime
constituent. As a result of the inefficiency of the magnetic and specific gravity
separations, it was necessary to separate large amounts of modified flyash to
obtain small quantities of the lime fraction. The scarcity of samples precluded
separation of sufficient amounts of the lime fraction for all ZP tests. It was
found that the parent modified flyash curve generally represented a resultant curve
of the lime and coal ash constituents and that valid interpretations of the ZP
data could be made without determining a lime constituent curve. For this
reason, only the coal ash and parent modified flyash constituent curves were
made for some tests.
In making ZP determinations, the effect of concentration of soluble
electrolytes was determined for modified flyash PID at the natural pH of
33 percent solid-water slurries. The data obtained showed that the ZP of
the materials present in modified flyash is negative at levels of high dilution
where there are only small amounts of soluble electrolytes present. However,
at the higher solids concentration that would be encountered in a flotation
cell, the solution electrolytes make all constituents positively charged
through surface adsorption of postively charged ions.
As indicated in Figure A, there were only small differences in the
ZP of the coal and lime constituent of modified flyash. This unfavorable
situation existed because of absorption of soluble ions from the slurry on
both the coal ash and lime constituents. Therefore, modifier tests were
undertaken to determine the effect of chemical additions for preferential
absorption on either the lime or coal ash constituents to permit selective
flotation collector absorption in the flotation slurry. Postively charged
modifiers tested were trivalent aluminum as aluminum potassium sulfate,
aluminum sulfate and aluminum chloride; trivalent iron as ferric chloride;
and divalent iron as ferrous ammonium sulfate (FAS). Anionic modifiers tested
were trivalent phosphate as phosphoric acid and divalent sulfide as sodium
-------
-23-
FICUKfi. 4
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE WITH CHANGES IN pH
OF LIMESTONE MODIFIED FLYASH PID (St. Clair, Mich.), THi: COAL
ASH CONSTITUENTS OF PID AND THI- LIME CONSTITUENTS OF PID IN
LIOUORS CONTAINING THE SOLUBLE CONSTITUENTS OF PID
10
2
•»
o 0
1
o
N -in
-20
PID
Coal Ash Constituents
Lime Constituents
-30
14
12
•40
6.0
sc~
7.0
8.0
9.0
pH
10.0
12.0
I
-------
-24-
The modifiers tested were those found to be effective in flotation
separation of other minerals and were generally di- or trivalent compounds
because the effectiveness of a modifier usually increases with increased
valence and decreased ionic radius due to increased adsorptive capacity
of the smaller ions by the mineral. The general method of testing each
modified flyash and the effect of each modifier consisted of making a
concentrated 33 percent modified flyash-water slurry, adding the modifier
as required, removing the solid portion of the slurry by centrifuging and
adding back to the supernatant liquid a small amount of the solid material.
The supernatant liquid containing a snail amount of solid material was then
placed in a special electrophoresis cell and a voltage applied to cause the
particles to move toward an electrode of opposite charge. The speed that
the particles traveled to an electrode was proportional to the magnitude
of the surface charge and the ZP was calculated fron the rate of movement.
Typical data obtained in the modifier study are given in Figure 5.
It was found that FAS was the most effective modifier at the level of
addition of 1.0 PPT to a 16.6 percent slurry of PID modified flyash. A
13 millivolt (mv) displacement between the coal ash constituent and
parent modified flyash was obtained at pH 10. The ZP of the line
constituent could not be determined due to a lack of sanple. However, based
on previous ZP tests in which it was determined that the parent modified flyash
curve was a resultant of the lime and coal ash constituent, it was
indicated that the ZP of the line constituent was approximately 57 mv
resulting in a favorable displacement of 26 mv between the line and parent
modified flyash curves. Agglomerate flotation Test 85 was used to test
these ZP findings. As noted in Section 3, an improvement in lime grade was
achieved.
A preliminary investigation was also made on the ZP of calcium sulfate
in order to determine what alteration of surface chemistry might be necessary
to effectively separate this constituent of limestone modified flyash,
especially from wet collected materials. Initial tests involved ZP measure-
ments on 33 percent slurries of calcium sulfate in distilled water at its
natural pH of 6.3 and after lowering the pll to 6.0 by carbonation. The ZP
values at both levels of pll was found to be -9 mv. In subsequent tests,
the ZP was determined on a slurry of line and flyash which was sulfated in
a stirred reactor with sulfur dioxide to pH 2. The ZP was found to be +14
mv and was attributed to a surface absorption of positive charges during pli
adjustment. Further work with high calciuii sulfate wet collected samples
obtained from Kansas Power and Light and Union Electric showed that modifiers
had much less effect than on the dry collected modified flyash. This would
be due to either cementing of the samples or to changes in the physical
composition of the wet collected flyash as compared to dry collected flyash
caused by increased sulfate content.
The ZP studies were beneficial in revealing the nature of the surface
charges present and the effects of modifiers used for their control. Improve-
ments in grade were obtained when the ZP data was applied in flotation separations;
however, ZP control alone was not found to be sufficient in achieving both high
lime yield and recovery. ZP studies of calcium sulfate and wet collected
modified flyash showed that additional work would be required to determine the
true ZP and what modifiers should be used for ZP control. This may be due to
-------
FIGURE 5
THE EFFECT OF THE 2ETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE
CONSTITUENTS OF LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS
LEVELS OF pH AFTER THE ADDITION OF 4.0 POUNDS PER TON OF
TRIVALENT IRON AS FERRIC CHLORIDE TO A 16.5 PERCENT
SLURRY CONCENTRATION
18
5
M
Parent Modified Fly ash
Lime Constituents
Cool Ash Constituents
-10
-40
7.0
8.0
9.0
10.0
110
12.0
13.0
-------
-26-
calcium sulfate.
4.2 Carbonation Studies
Control of the pH of different 33 percent modified flyash flotation
slurries was investigated as a means to determine the mechanism of carbonation.
Preliminary tests were conducted using a magnetically stirred reactor, a
carbon dioxide injection tube, a pll meter interfaced with a recorder and a
constant supply of carbon dioxide. The apparatus was designed to continuously
monitor and record the change in pll with time. The carbonation step, in which
the pH was made as low as possible, and a decarbonation step, in which the pll
increased after the supply of carbon dioxide was shut off, were recorded. The
results of these tests are shown in Appendix C. The following four observations
were noted:
1. Hydrogen sulfide was given off from D]^ and I^D? lines tone
modified flyash during carbonation. The odor and coloration
of a lead acetate paper was very distinct at pll 9.0 to 9.5
with D,D2 and to a lesser degree at pH 9.2 with D D . These
limestone modified fly ashes were produced by TVA by admixing
the limestone with the coal prior to combustion. This gas
evolution could be an indication that with these modified
flyashes the sulfur dioxide was not fixed as calcium sulfate
but as some less stable compound, possibly sulfides, as a
result of the presence of the coal ash constituents, such as
silica, interacting with the line at the high temperatures
present in the boiler.
2. The limestone modified flyashes can be carbonated to pH 6.5
or less while the pH of the dolomite modified flyashes can
only be lowered to about 7.5 by carbonation.
3. Carbonation of limestone modified flyashes proceeds rapidly
once the soluble lime is converted to calciui.i carbonate.
The dolomite modified flyashes, however, increase in alkalinity
once carbonation has lowered the pll to about nine. This increase
is shown by the single and double hunjis in Figures G and 7.
A. The increase in pll after carbonation is slow and proceeds in
distinct steps. These observations primarily indicate that
modified flyash-water slurries can be carbonated and held at
pll values around seven for a sufficient length of tine to
effect flotation separations.
Later tests using modified flyash D D , CI and CM in both 33 and
16.6 percent slurry concentrations showen that the carbon dioxide absorption
rate was generally proportional to the rate of change in pll.
In these tests, the resultant pll and the carbon dioxide absorption was
plotted against tir.iii. The lower slurry concentration was chosnn in order
to prevent cementitious setting of the modified flyash in the reactor during
carbonation. It was indicated that in the initial stages of the reaction,
-------
14.0
13.0
12.0
11.0
10.0
THE EFFECT OF CARBOHATtON OH THE pH OF 33 FERCENT
SLURRIES OF DOLOMITE MODIFIED FLYASH CI
(St. louU, Ho.)
..._!_.. -
4.0
-------
U^j.I'
n
FIGOBE 7
THE EFFECT OF CA1MRATIOH OH TUB pR OF 33 FCIICENT
sunsies OF DOUMITE MODIFIED FLYASH CM
(St. Lout*. HD.)
-------
-29-
and the pH change is slow. At about pH 12.3 most of the soluble line has been
removed and a sharp decrease in pH and carbon dioxide absorption occurs as the
slurry water is titrated. This was seen when comparing the 16.6 percent and
33.0 percent slurry concentration of dolomite modified flyash CM. The increased
amounts of soluble lime resulting from the higher slurry concentration required -
more time and greater amounts of carbon dioxide for precipitation. After
the soluble lime is precipitated, there is a sharp decrease in both pH and I
carbon dioxide absorption as the solution is titrated. Once the equivalence |
point is passed only small amounts of carbon dioxide are required to complete
the titration and precipitate any additional lime brought into solution by •
equilibrium dynamics. The tests also indicated that initially carbon dioxide I
is converted to carbonic acid prior to precipitation of soluble lime as
evidenced by the initial pH reduction and subsequent rise as lime reacts with
carbonic acid. Material balance calculations based on these carbonation tests are
shown in Table A. These calculations indicate that with the exception of the
33 percent CM slurry none of the samples were completely carbonated. The 33
percent CM test resulted in a high value that could not be explained on the
basis of calcium carbonate formation and may point to the formation of some
magnesium carbonate.
4.3 Thennogravimetric Analysis
Thermogravimetric analysis (TGA) of agglomerate flotation fractions of
limestone modified flyash showed that the lime particles were about 2/3
carbonated during pH adjustment for flotation separation. The TGA data,
shown in Appendix D, also indicated that both the lime particles reporting
in the concentrates and those remaining in the unlevitated tails were
carbonated to this degree. It was also indicated from the TGA studies that
carbonation of the agglomerate flotation slurries served only to control the
pH and was not a factor in determining whether a lime particle floated or
remained in the tail. The study also showed that there was generally unused
emulsion remaining after the agglomerate separation.
The TGA studies were undertaken because during the chemical analysis
it was necessary to remove the emulsion before the samples could be
accurately weighed. The temperatures required for removal of the oily
emulsions approached the calcination temperature of calcium carbonate so
that the entire material had to be calcined in order to perform accurate
chemical analysis. Since both the emulsion and the carbon dioxide were
removed by this drying technique, no statement of the amount of either
constituent in a particular flotation fraction could be obtained. It was
of interest to correlate the degree of carbonation with the recovery of the
calcium fraction from the flotation separation to determine if increased carbon
dioxide content yielded a higher lime concentrate and also to observe the
effect of increased emulsion addition on the amount of the calcium material
floated since preliminary correlations of loss on ignition (LOI) and lime
grade indicated that the best recoveries of lime were on fractions having the ,
higher LOI. (8)
Dried TGA samples were weighed on a Calm Model RG Electrobalance. An I
XY* recorder was calibrated to record both the weight loss as registered by the
-------
TABLE 4
CARBONATION TEST
Sample
PID
CM
CI
CM
Slurry
Concen-
tration
Percent
16.6
16.6
16.6
33.0
Feed
Weight
Cms.
50
50
50
100
Grams CaO
In Feed
14.90
9.59
8.96
19.18
Equivalent
Grams
of
CaC03
26.60
17.12
16.00
32.25
Equivalent
Grams
of
CO,
£.
11.80
7.54
7.04
15.07
Percent
Weight
Gain
2.00
3.00
4.00
17.30
Percent
Carbonated
17.09
39.78
56.81
114.79
i
u>
o
-------
-31-
electrobalance and the temperature increase as measured by a chromel alumel
thermocouple. The fusion furnace used for heating the samples was rated for
a maximum of 1200°C.
Agglomerate flotation test fractions chosen for TGA analysis were from
those flotation tests showing distinct differences, either favorable or unfavor-
able, as compared to average test results. The agglomerate flotation tests •
chosen and the reason for their choice are shown in Table 5. I
TABLE 5 I
AGGLOMERATE FLOTATION TESTS ANALYZED BY TGA
Emulsion
Test Number Addition Rates , PPT Reason For Choosing Test
111 20 Good grades - low emulsion
121 20 Recarbonation to maintain pH
at 7 or below
Extensive recleaning
96 60 Good grade and recovery in
relation to other factorial
tests
95 60 Bad grade and recovery in
relation to other factorial
tests
73 112.6 Good grades - tested by NAPCA
for reactivity
84 112.6 Good grades - high emulsion
82 112.6 Bad grades - fair recovery -
high emulsion
85 140.7 High grades - high emulsion -
extensive recleaning
115 20 81.45 percent lime grade - low
recovery
124 Froth flotation
Several pure calcium compounds and a modified flyash were determined as
-------
-32-
The degree of carbonation for the flotation samples, as measured by both
TGA and LOI methods, shows that the highest flotation grades of lime were
generally obtained on the highest carbonated fractions. (8) However, when
the amount of lime in any fraction is considered as the sole carbon dioxide
absorber during carbonation, it is seen that all particles absorb about the
same amount of carbon dioxide. For example, calculation of the degree of
carbonation for the CC3 and RT of Test 84 shows that both are carbonated to
the same degree or about 29.00 percent. The TGA data on Tests 95 and 196
were of special interest because Test 95 showed rapid increases in pH durinp
separation and resulted in poor grades and recoveries while Test 96 showed
good grades and recoveries with stable pH in relation to the other data obtained
in the factorial tests. Calculation of the percent carbonation for this test
showed that the lime particles of Test 95 were carbonated to a slightly higher
degree than those of Test 96.
Since there appears to be essentially no difference in the degree of
carbonation between fractions within a single test and between tests, it
would appear that carbonation serves only to control pll, through precipitation
of soluble lime, and does not affect grade or recovery.
The TGA tests on the tail fractions also showed that unlevitated emulsion
remained after completion of the flotation separation. This was indicated
by weight loses below 400°C and was especially evident with the higher
emulsion addition rates.
4.4 Microscopic Analysis
As a result of the low yields and recoveries of lime obtained and the
failure of the corollary tests to suitably explain these low values, additional
characterization tests were undertaken. Microscopic examination of fractions
of dry collected limestone modified flyash obtained by centrifugation in
liquids ranging in specific gravity from 1.0 to 2.6 indicated that this
material consisted of four distinct particle types. An example of such a
separation is shown in Figure 8. The lightest fraction consisted of bright,
white, hollow siliceous cenospheres (Type I). The second float fraction
Type II, was black irregular shaped carbonaceous particles having much the
same appearance as coked coal particles. Type III, the first sink fraction,
consisted of irregular, dull white or yellow particles which were very high
in lime. The heaviest fraction, Type IV, was comprised of shiny black
spherical particles which were high in iron.
The Type I siliceous cenospheres were found by chemical analysis to
consist of the coal ash constituents of limestone modified flyash. These
cenospheres were comprised of about 50 percent silica, 25 percent alumina
and only about 5 percent lime whereas the Type III irregular dull white or
yellow particles consisted of about 50 percent lime. Type III particles,
when hand crushed, were of low strength and crumbled into smaller uniform
particles, some of which resembled pure calcium carbonate after calcination
while others were glassy like silica. Both the Type I ami Type IV spherical
particles, when crushed, were found to be hollow. The thinner walled Type I
siliceous particles were a uniform white color. However, the high iron Type
IV particles had thicker walls encircling light colored solid spherical
-------
-33-
Figure 8
THE 2.60 SPECIFIC GRAVITY SEPARATION OF HEAD PID
Type I
Bright Spherical White
Particles (Cenospheres)
Type n
Black Irregular Particles
(Carbonaceous)
Float
2.60 Specific Gravity
Liquid Media
Type IE
Irregular, Dull White
And Yellow Particles
Type EZ
Shiny Black Spherica[
Particles
Ferruginous Shell
Unidentified Opaque Particles
Clear Siliceous Center
Siliceous &
Calcium Oxide
-------
-34-
These tests indicated that dry collected linestone modified flyash con-
sists of three coal ash fractions that are unaffected by the injection of
limestone or dolomite, ie, that are similar to unmodified flyash. The Type
III lime fraction is predominately derived from the limestone or dolomite
but appears to contain some of the smaller siliceous coal ash particles.
The low bond strength between the siliceous and lime materials in the
Type III particles partially accounts for the presence of non-lime material
in the lime concentrates and the recovery of relatively pure fractions of
-------
-35-
Section 5
SULFUR RECOVERY
Interest has been expressed in the possibility of recovering sulfur by
heating the different modified flyashes in an oxidizing atmosphere. Preliminary
sulfur balance tests were conducted on the raw modified flyash samples.
These were done using a modified oxidizing combustion furnace-titration
technique. Modified flyash PID having a sulfur concentration of 1.80 percent
as determined by the Eschka method contained 1.72 percent sulfur by the
combustion method. This represents better than a 95 percent recovery of the
sulfur from the sample. This recovery can then be compared with the sulfur
content contained in a sample of dihydrated calcium sulfate which gave a 91
percent recovery and indicates that the decomposition approaches quantitative
yields. In another test using the tailing product from flotation Test 79 which
contained 62.5 percent of the original modified ash (Dj^), the percent sulfur
was found to be 1.30. Since sulfur values have not been determined on all of
the flotation fractions tested to date, a comparison of this result with the
Eschka method for the tailing fraction of flotation Test 79 cannot be made.
However, based on the data available, it would appear that about half of the
sulfur value occurs in the concentrate and half in the tails. Although these
preliminary figures indicate no substantial upgrading of the sulfur value in
either fraction, it should be pointed out that:
1. The sulfur dioxide present in either fraction can be removed
almost quantitatively by melting modified flyash.
2. The form of the sulfur in the modified ash after flotation has
not yet been determined and the decomposition effect may differ
from one ash to another.
3. In Test 79, D^Do modified ash was used which liberates hydrogen
sulfide during carbonation and the resultant sulfur values in the
flotation fractions may be lower due to sulfide evolution during
carbonation.
Further work will be undertaken on Contract CPA 70-66 to compare the
ability of different modified flyashes to liberate hydrogen sulfide during
carbonation and evolve sulfur dioxide when heated in an oxidizing atmosphere.
I
I
-------
-36-
Section 6
AGGLOMERATE SIEVING
Tests were undertaken to determine the feasibility of lime recovery fron
limestone modified flyash by agglomerating the lime fraction in oil-water
emulsions in the same manner as agglomerate flotation and then sieving out
the unagglomerated coal ash fraction rather than by levitation by air lifting.
The results are given in Appendix E, As indicated by the ratios of enrichment
shown in the data of Appendix E, little progress was made toward lime
concentration. Numerous conditions were tested with little success and it
-------
-37-
Section 7 |
CONCLUSIONS -
The results of extensive bench scale agglomerate flotation studies for
recovery of unreacted lime from dry collected limestone modified flyash indicate
that continued study in this area is not feasible. Acceptably high grades
and yields of lime were not consistently achieved and further substantial
bench scale study would have to be undertaken to obtain the required grades
and yields for lime recovery to be effected commercially.
The data accumulated indicates that lime recovery from limestone modified
flyash may be effected to some degree by pH control and soluble lime precipitation
through carbonation, zeta potential control through modifier addition, employment
of agglomerate flotation and by recleaning the initial (rougher) concentrates.
It was found that relatively pure fractions of lime may be obtained through
extended preconditioning. This softens the lime particles in water and the
abrasion of the softened particles results in particles of relatively pure lime.
Attritional scrubbing tests may be a way of breaking down the lime-siliceous
flyash particles; however, no favorable quantitative data were obtained.
Both the physical and chemical characteristics of the constituents of
limestone modified flyash and the flotation separation were studied as a means
of improving lime grade and yield. It was found that agglomerate flotation
was superior to the previously employed froth flotation because of the fineness
of the modified flyash.
It was also found that carbonation was necessary to control the pH of
the flotation slurry and to reduce the amount of water soluble line.
Carbonation tests showed that, while the carbonation mechanism was different
for limestone and dolomite modified flyash, there was sufficient time after
carbonation to permit a flotation separation before the pH rose to unacceptably
high levels. This pll rise was found to result from solution of lime by
equilibrium dynamics.
Zeta potential studies of the surface chemistry of the constituents of
limestone modified flyash showed that chemical modifiers were necessary,
in addition to pH control, to maintain a favorable displacement between the
coal ash and lime fractions. The most effective modifier was di-valent
ferrous ammonium sulfate (FAS). However, it was indicated that different
modified flyashes might require other modifiers and that zeta potential -•
studies should be undertaken before extensive flotation tests are planned.
Thermogravimetric analysis (TGA) showed that even with the lower I
emulsion addition rates obtained as a result of the factorial design •
tests, there was unused emulsion remaining in the unlevitated tail products.
The TGA tests also showed that carbonation served only to control pll and I
-------
-38-
Microscopic studies indicated that modified flyash was made up of four
distinct fractions. The Type III spheres consisted of agglomerated lime-
flyash particles which would appear to preclude effective separation by flotation
or any other available commercially feasible mineral dressing technique.
Agglomerate sieving was tested and found to be unsatisfactory within
the limits of the tests undertaken.
As a result of this investigation, it is concluded that the primary
phase of the ECMC process, flotation recovery of lime does not warrant
further intensive research. The secondary phase of the ECMC process,
mineral wool production in conjunction with sulfur recovery still appears
-------
-39-
REFERENCES I
1. Robinson, Elmer and Robbins, Robert C., "Gaseous Sulfur Pollutants I
from Urban and Natural Sources," Journal of the Air Pollution Control I
Association, ^0, (4) (April, 1970), 233-235.
2. Cockrell, C. F., Muter, R. B. and Leonard, J. W., "Study of the
Potential for Profitable Utilization of Pulverized Coal Flyash
Modified by the Addition of Limestone-Dolomite Sulfur Dioxide
Removal Additives," Final Report, Contract 86-67-122, National
Air Pollution Control Administration, April, 1969.
3. Cockrell, C. F., Muter, R. B., Leonard, J. W. and Lawrence, W. F.,
"Exploratory Studies on New Product and Process Potential of Power
Plant Wastes Originating from Limestone Based Air Pollution Control
Processes," Preprint 36-C, Symposium on Utilization of Mineral Matter
in Coal, 65th National Meeting, American Institute of Chemical Engineers,
Cleveland, Ohio, May 4-7, 1969.
4. "Production of Mineral Wool from Coal Ash Slag," Final Report, U. S.
Bureau of Mines, Solid Waste Disposal Program, Contract No. SWD-9,
September, 1969.
5. Apian, F. F. and Fuerstenau, D. W., "Principles of Non-Metallic
Mineral Flotation," Froth Flotation, D. W. Fuerstenau (ed.), AIJIE
New York, New York, (1960), 211.
6. Personal Communication, Charles T. Ford, Bituminous Coal Research,
Inc., Monroeville, Pennsylvania, October 7, 1968, and November 15,
1968.
7. Personal Communication, Albert F. Baker, Pittsburgh Coal Research
Center, USBM, October 22, 1968.
8. Personal Communication, Thomas A. Kittleman, DPCE, NAPCA, Cincinnati,
-------
-40-
APPENDIX A
-------
MODIFIED FLYASH FLOTATION DATA FOR ASH
PID
PRUMOTOR FROTHER MODIFIER COND. FLOAT
RATE TIME. TIME. PCT.
LB/HR MIN. MIN. FLOAT
O.OO 6O.O 60.00 21.73
O.OO 12O.O 75.00 42.42
0.63 10.0 3O.OO 26.3O
3.0 30.OO 7.14
0.41 6O.O 6O.OO 43.94
0.22 60.0 6O.OO 55.94
O.22 1S.O 60.00 28.O9
O.02 2O.0120.OO 42.11
0.00 10.0 42.00 55.58
6.0 25.00 94.56
3.O 15.00 SO.80
3.0 7.00 44.14
4.O 8.00 10.63
2.0 7.00 40.36
4.0 8.00 20.16
2.5 8.00 50.78
2.0 5.00 9.69
4.0 8.00 49.35
2.0 8.OO 13.54
4.0 9.00 58.04
2.0 9.00 11.13
MODIFIED FLYASH FLOTATION DATA FOR ASH 2X3PID
TtSI bLUfcWY fro TDK T 1 Me
NU. PCT. fit-* MIN.
1 JJ.J.2 l-JtC.
«; jJ.J.2 1450.
J Jj.Jj IbCC.
4 jj.Jj IbOC.
0 jJ.Jj 1450.
7 JJ.JJ 1450.
d JJ.jJ I4b0.
Si c 1 .7 j IbCC.
*A ic.b; itco.
10 5
RATE
LB/HR
0.83
0.60
0. 18
0. 18
0.48
0.48
0.60
1.20
0.30
0.31
0.30
0. 12
0.21
0.12
0.20
O.14
0.05
0. 12
0.24
0. 18
0.28
TYPE
NONE
NONE
40NASI
40NASI
40NASI
EOTA
EDTA
10NASI
NONE
NONE
0.5 HF
0.5 HF
NONE
0.5HF
NONE
0.5HF
NONE
5DE610
NONE
5TANAC
NONE
RATE
LB/HR
O.OO
O.OO
0.63
0.51
0.41
0.22
O.22
O.02
0.00
O.OO
0.02
0.02
O.OO
O.O2
0.00
O.O2
0.00
0.02
O.OO
O.O2
0.00
LIME CONCENTRATIONS
GRADE GRADE RECOVERY RATIO OF
PCT. PCT. PCT. PCT. ENRICH-
FLOAT TAICS FLOAT TAILS MENT
25.40 34.90 16.44 76.36 0.76
27.83 30.57 35.16 43.16 0.83
27.32 27.98 21.40 44.48 0.81
23.51 29.18 5.00 84.17 0.70
29.33 26.99 38.38 45.54 0.87
24.68 24.75 41.12 32.12 0.73
25.64 31.OO 21.45 64.61 O.76
29.46 28.21 36.95 50.22 0.88
31.06 26.25 51.41 34.63 0.92
26.44 26.82 74.45 4.35 0.79
27.67 29.48 41.86 44.53 0.82
28.64 28.32 37.65 47.64 0.85
28.98 28.25 9.17 75.19 O.86
25.6O 29.10 30.77 51.60 0.76
27.59 29.75 16.56 70.73 0.82
26.60 29.40 40.23 44.55 0.79
26.14 29.72 7.55 79.93 O.78
27.90 29.30 41.00 45.28 0.83
27.11 29.60 10.93 78.O9 O.8I
26.04 23.82 45.01 30.60 0.78
22.86 23.95 7.58 63.38 0.68
NL> <
ie
CAMu.
1C* TIMt »-M VALUES
K MIN. IK 1 . FIN.
;C. 0.0 10.0 10.0
PMUMUTUR FROTHER MODIFIER COND. FLOAT
TYPE RATE TYPE RATE TYPE RATE TIME. TIME. PCT.
Lb/HM LB/HR LB/HR MIN. MIN. FLOAT
LIME CONCENTRATIONS
GRADE GRADE RECOVERY RATIO OF
PCT. PCT. PCT. PCT. ENRICH-
FLOAT TAILS FLOAT TAILS MENT
Ai!5
O.b4
A65
0.5O NONE
0.00
-------
MODIFIED FLYASH FLOTATION DATA FOR ASH
PID
LIME CONCENTRATIONS
ca 1
NL>.
19
-------
MODIFIED FLYASH FLOTATION DATA FOR ASH
PID
'cs r
J4
Jb
J»
Jd
J*
40
4 1
«<
4 J
44
43
4C.
47
46
49
to
= 1
t J
b4
bb
bt
b7
tO
ol
jCOKHT FUTLri
b . 4 I - C .
b.41 -C.
t: . 4 £ - I .
b.91 -C.
t.iiS -C.
0.25 -C.
b.bl -C.
4 .-.S -C .
b.7t -C.
C.91 -C.
0.4i -C.
t .bi -C .
0./7 -C.
b.bo -0.
L. ti -C .
L.Bfc -C.
t . 9t -C .
t .47 -C .
c.47 -C.
0 .4 7 -C .
t .bi - C .
b.,1 -C.
b . 9 1 - C .
t . J C - C .
t . Jb -C .
CAWu.
TIMt Fh VALUES
KIN. 1M. FIN.
0.0 12.0
0.0 IJ.O
0.0 li .9
O.O 1 J. 1
0.0 IJ.O
C.O IJ.O
4.0 1 J.O
4.0 li .e
4.0 13.0
0.0 IJ.I
o.o i j . o
4.0 li .E
iOb.O lc .9
4.0 li .9
4.0 13. C
4.0 1J.C
4.0 IJ.O
1
4.0 1 j .0
4 . O 1 j . 1
4.0 1 J . 1
4.0 l-.i
4.0 1 J.2
4.0 1 J .4
4.0 1 j . t
13.0
13.0
12.9
13.1
IJ.O
13.0
7.0
7.0
7.0
13.1
IJ.O
9.6
C.7
7.0
7.0
7.0
7.0
9.9
9.9
9.9
9.9
9.9
9.9
9.9
PHUMUl
irpfc
5.A825
OLACID
A25
OLACID
OLACID
OLACID
OLACID
OLACIO
OLACIO
A25
A25
OLACID
OLACIO
b.OLAA
5.0LAA
b.OLAA
b.OLAA
A25
b.OLAA
b.OLAA
b.OLAA
b.OLAA
b.OLAA
0.bA2b
run
RATE
LH/Hfl
0.91
1 .64
2.36
1 .49
1.69
1.69
1.57
1.73
1.53
1.82
1.97
1.34
1 .29
0.50
0.50
0.50
O.bO
O.bO
0.50
0.50
0.50
O.bO
O.bO
O.bO
0.50
FROTHER
TYPE RATE
LB/HR
0250
D250
F65
O250
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
F65
Fbb
Ftob
0.05
0.20
1.98
0.20
2.07
2.07
1.92
2.18
1.87
1.54
1.67
1.64
1.58
1.95
1.64
1.83
1.80
1 .65
l.bS
1.65
t .64
1 .82
1 .82
2.05
2.02
MODIFIER COND. FLOAT
TYPE RATE TIME. TIME*
.LB/HR MIN. MIN.
NONE
CAL240
5.FECL
NONE
NONE
NONE
NONE
NONE
NONE
NONE
CAL240
5.EDTA
CAL240
NONE
NONE
NONE
NONE
5.FECL
5.FECL
NONE
NONE
NONE
NONE
NONE
NONE
O.OO
0.38
0.23
0.00
0.00
O.OO
O.OO
O.OO
O.OO
O.OO
3.79
0.91
0.36
O.OO
0.00
O.OO
0.00
0.45
0.45
O.OO
0.00
0.00
O.OO
O.OO
O.OO
2.0
2.0
2.O
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
2.0
4.O
2.0
2.0
2.0
2.0
2.0
2.0
3.00
3.50
2.0O
2.00
2.00
2.00
2. SO
2.OO
2.15
2. SO
3.15
3.75
3.0O
3.15
3.50
3.30
3.50
4.00
3.00
3.OO
PCT.
FLOAT
41.00
38.00
19.80
19.09
27.84
31.96
14.42
8.7O
15.89
20.77
26.67
28.69
24.41
18.45
33.61
41.28
54.05
24.79
30.58
29.75
4.10******
4.00
4.OO
4.00
4.0O
36.36
40.91
17.35
21.21
LIME CONCENTRATIONS
GRADE GRADE RECOVERY RATIO OF
PCT. PCT. PCT. PCT. ENRICH-
FLOAT TAILS FLOAT TAILS MENT
31.90
35.70
24. 6O
32.30
29.60
29.60
33. SO
3O.70
33.50
27 .90
27.10
31.OO
31 .40
28.60
27.10
27.70
28.60
3I.9O
30. 7O
32.30
29.60
28.60
27.50
29.90
33.30
35.00
36.20
32.60
28.60
32.10
29.90
29.60
27.10
29.40
29.20
26.30
29.00
30.30
29. OO
31.60
30. IO
31.20
26. 3O
3O. IO
2S.8O
43.90
45.54
16.35
20.70
27.66
31.75
70.49
.75.34
82.35
72.44
77.76
50.70
16.221O4.14
8.96
17.87
19.45
24.26
29.85
25.73
17.71
3O.57
38.39
51.89
26.55
31.51
32.26
27.90******
26. 10
26. 30
26.70
27.50
34.91
37.76
17.41
23.71
9O.97
94. OS
79.17
61. O6
82.19
88.10
91.68
81.73
74.16
72.65
79.53
83.50
79.90
69.09
65.31
63.40
81. 4O
78.33
1.07
1.20
0.83
i.oa
0.99
0.99
1.12
1.03
1.12
0.94
0.91
1.04
1.05
0.96
0.91
O.93
0.96
1.07
1.03
I.O8
0.99
0.96
0.92
1.00
-------
MODIFIED FLYASH FLOTATION DATA FOR ASH
PID
TEbT
NO. FCT.
CARU.
KJ1CH TIMfc
JSF* MIN.
63
64
b.41
5.41
-C.
-C.
o.o
J.O
rest SLURKY
NC. PCT.
65 b.41
67 40.00
69 33.J3
70 £.76
CAKb.
FGTCR TIMt
PFI» MIN.
-C. 4.0
-C. 0.0
I1CC. 55.0
-C. J.O
PROMOTOR FROTHER MODIFIER CONO. FLOAT
Fh VALUES TYPE HATE TYPE RATE TYPE RATE TIME. TIME. PCT.
IM. FIN. LB/HR LB/HR LB/HR MIN. MIN. FLOAT
5.2 9.2 OLACID 0.50 F65 2.00 NONE 0.00 2.0 S.OO 41.00
S.2 6.5 OLACID 0.50 F65 0.50 NONE 0.00 -0.0 5.00 20.00
MODIFIED FLYASH FLOTATION DATA FOR ASH PID
PROMOTOR FROTHER MODIFIER COND. FLOAT
Ph VALUES TYPE RATE TYPE HATE TYPE HATE TIME. TIME. PCT.
IM. FIN. LB/HR LB/HR LB/HR MIN. MIN. FLOAT
12.2 9.2 OLACID 0.50 F6S 0.50 NONE 0.00 2.0 5.00 23.00
12.0 13.0 EfULSN 66.65 NONE 0.00 NONE 0.00 10.0 15.00 65.25
13.1 6.7 EMULSN 112.60 NONE O.OO 5.FECL 2.0O 20.0 15.0O115.75
13.2 9.0 BCACIO 0.50 F6S 0.50 NONE 0.00 2.O 3.OO 14.95
MODIFIED FLYASH FLOTATION DATA FOR ASH OID3
LIME CONCENTRATIONS
GRADE GRADE RECOVERY RATIO OF
PCT. PCT. PCT. PCT. ENRICH-
FLOAT TAILS FLOAT TAILS MENT
33.30 3O.3O 42.07 48.55 1.03
32.30 30.30 19.91 64.43 1.00
LIME CONCENTRATIONS
GRADE GRADE RECOVERY RATIO OF
PCT. PCT. PCT. PCT. ENRICH-
FLOAT TAILS FLOAT TAILS MENT
29.90 30.TO 20.48 83.2O 0.89
33.07 37.00 64.26 10.53 0.98
35.76 16.3O123.26 O.93 1.06
33.90 34.2O 15.10 86.62 1.O1
CAHB. PRUMOTUR
TEST bLUF.RY FC1L& TIMt Fh VALUES TYPE RATE
N(j. PCT. FFH MIN. IM. FIN. LB/HH
FROTHER
TYPE RATE
LB/HR
LIME CONCENTRATIONS
MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. ENRICH-
LB/HH MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
71
5.96
-C ,
0.0 13.4 7.0 OLACID
0.50
F65
0.50 5.FECL 0.5O 2.0 1.30 4.SO 25.60 22.50 4.62 84.46 1.03
MODIFIED FLYASH FLOTATION DATA FOR ASH OID2
LIME CONCENTRATIONS
CARb. PHOMOTOH FROTHER MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
TEST SLUKRY FljlCH TIME PI- VALUES TYPE RATE TYPE RATE TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. ENRICH-
NC. PCT. FFX MIN. IM. FIN. LB/HR LB/HR LB/HR MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
RC1 7J 3J.J2 11CC. J5.0 li.9 7.0 EMULSN 112.6O NONE 0.00 5.FECL 2.00 2O.O S.OO 17.15 30.22 20.96 22.98 77.Ol 1.34
-0.00 20.0 5.00 9.79 36.62 17.37 17.10 74.76 1.75
RC2 7J 25.2S 11CO. -0.0 IJ.S 7.0
RC3 13 ^7.2C 11CO. -0.0 \i .
CC1 7J c.4i I1CC. -0.0 7.0 7.0
CC2 7J J.14 I1CO. -0.0 7.0 7.0
CC3 7J 2.51 I1CO. -0.0 7.0 7.0
7.0
7.0
7.0
7.0
7.0
-0.00
-0.00
-0.00
-0.00
-0.00
-0.00
-0.00
-0.00
-O.OO
-O.OO
-0.00 20.0 5.00 8.59 31.60 16.03 15.64 84.35 1.82
-0.00 1.0 5.00 24.61 49.09 24.06 39.97 60.OO 1.62
-0.00 l.O 5.00 24.53 56.44 30.19 37.80 62.22 1.54
-------
MODIFIED FLYASH FLOTATION DATA FOR ASH PID
LIME CONCENTRATIONS
C"HL" PHUMUTUW FROTHER MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
TtbT aLLHKY M,lLh IIKL ^h VALLti TYPh RATE TYPE RATE TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. 6NRICH-
M.. MCI. t-l-K MIN. IM. FIN. LB/HH LB/HR L8/HR MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
HC1 7o Jo.jj IICO. t^.U 10.b 6.9 EfULSN 112.60 NONE 0.00 5.FECL 4.00 2.0 15.00 55.87 33.26 27.57 62.38 38.90 1.12
CT1 /u lb.<:7 1110. -0.0 6.9 6.9 -0.00 -0.00 -O.OO -0.0 5.00 48.70 38.51 28.27 56.39 43.60 1.16
7o s.a* lice, -o.o 6.9 e.9
-o.oo
-o.oo
-0.00 -0.0 5.00 44.44 40.43 36.97 46.65 53.34 1.05
j li «.ol lltO. -0.0 6.9 e.9
-0.00
-0.00
-0.00 -0.0 5.00 72.37 41.54 37.54 74.36 25.66 1.O3
CT4 7o J.Jb 11CC. -0.0 6.9 6.9
-0.00
-0.00
-O.OO -0.0 5.0O 20.35 45.89 40.43 22.49 77.52 1.10
Lit 7c C.71 lliC. -0.0 6.9 6.9
-0.00
-0.00
-0.00 -0.0 5.00 19.30 50.53 44.80 21.25 78.78 1.10
MODIFIED FLYASH FLOTATION DATA FOR ASH PID
LIME CONCENTRATIONS
PHUMUTUKi FHGTHER MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
Ccol i.LLt«HY fUlCH T1ML f:l- VALUES TYPE RATE TYPE RATE TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. ENRICH—
Nc. PCI. H-F« V>IN. INI. f-lN. LU/HR LB/HR LB/HR MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
7o J.-.J^ 1ILC. oO.O 12.1 6.7 bCULSN 112.60 NONE 0.00 5.FECL 4.0O 20.0 11.OO 49.50 34.71 23.54 57.68 55.31 1.17
CJ1
t
MODIFIED FLYASH FLOTATION DATA FOR ASH DID2
LIME CONCENTRATIONS
l_Arlt). PKUMOTUR FROTHER MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
Itil bLOhhY H,lLh T1 *L PI- VALUES TYPE RATE TYPE RATE TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. EKRICH-
M.. ^Cl. hH» MIN. |M. FIN. LB/HR LB/HR LB/HR MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
WC1 1i JJ.Jj 11CC. jt.O 1I-.C 7.0 EfrULSN 112.60 NONE O.OO 5.FECL 2.0O 20.0 5.00 10.17 47.70 22.39 21.52 89.19 2.12
HC<; ?•»
ltC. -0.0 li.C 7.0
-0.00
-0.00
-0.00 20.0 5.00 12.16 42.19 19.65 22.91 77.09 1.88
HCJ 7t
11CC. -0.0 12.0 7.0
-O.OO
-O.OO
-0.00 20.0 5.00 8.36 39.55 19.78 16.82 92.25 2.01
Ctl ?•< _).<,! IILC. -0.0 7.. 0 7.0
CC«i 7-<
-------
MODIFIED FLVASH FLOTATION DATA FOR ASH PID
LIME CONCENTRATIONS
CAM-. PkUMJTUH FRG1HER MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
fL^I ^LOt-xl l-LlLi« TII»L l-h VALUES IfPt HATt IYPE RATfc TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. ENRICH-
N<_. l-il. l-ff I»IN,. 1M. Flu. LH/MR LB/MH LB/HH MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
RL I cj <.c.t>7 I1CC. O.O I-.4 1J.4 LUiLbN 112.60 NUNt 0.00 S.FECL 2.0O 30.0 13.OO 58.01 24.99 30.89 48.66 29.IS 0.84
Lll to Ifc.ei 1U.C. -0.0 i;.« IJ.4 -0.00 -O.OO -O.OO 1.0 S.OO 66.80 23.92 27.13 63.94 36.OS 0.96
Lit ru U.lc IllC. -U.U li.4 IJ.4 -O.OO -O.OO -0.00 1.0 5.00 77.27 23.72 24.68 76.62 23.39 0.99
Cl- co 1C.CS I1CC. -U.U 1J.1 13.« -0.00 -0.00 -0.00 1.0 5.00 76.63 23.81 23.45 76.93 23.10 1.00
Cl« tu 1.41 11CL. -L.O 1^.4 1J.4 -O.OO -0.00 -0.00 1.0 5.00 74.83 23.76 23.85 74.67 25.32 1.00
MODIFIED FLYASH FLOTATION DATA FOR ASH D1O2
LIME CONCENTRATIONS
CA^c. PkuMOTUH FHOTHER MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
IL-! :,LLt-hY I-L ILH TIM. It- VALUES I YPL HATE TYPE HATt TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. ENRICH— |
M. ( c. 1 . (-I-* .v|i\. IM. HIN. Lb/HH LB/HR LB/HR MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT js^
c | ;,L.JC IlLi,. »U.U IC.t t.V LI»ULoN 112.00 NUNE O.OO 5.FECL 2.0O 20.0 15.00 92.39 25.29 15.14140.76 5.78 1.52 .
MODIFIED FLYASH FLOTATION DATA FOR ASH PID
LIME CONCENTRATIONS
L"w»- PKUMUFUH FHCThtH MODIFIER CUND. FLOAT GRADE GRADE RECOVERY RATIO OF
?L,I .,l.Cl-HV ^ulc^- I IWL l-t- V«LL,tb TYPt HATE TYPE HATE TYPE RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. EKRICH-
K<-- '-'-1- t'^*' "IN- i^l- I-1N. LH/HH Lb/HR LBXHR MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
ct JJ..IJ IILL. l 19.OO 0.96
MUU1FIEU FLYAbH FLOTATION DATA FOR ASH PID
LIME CONCENTRATIONS
LA.-n. PfcUMOTUK FWUTHLH MODIFIER COND. FLOAT GRADE GRADE RECOVERY RATIO OF
TL^| -jLL-l-t-V l-Lll-H 7 I IK_ ^^ VALOLb TYPL HATt TYPE HATE TYPL RATE TIME. TIME. PCT. PCT. PCT. PCT. PCT. EKRICH-
PM_ . (-11. ^ ^ »• fit-. INI. I-IN. Lti/HH LB/HH LB/HR MIN. MIN. FLOAT FLOAT TAILS FLOAT TAILS MENT
HI tj jJ.J." IICC. 11.0 1..S e.O t*"UL^N 112.60 NUN!: O.OO Ft 0.40 5.0 20.OO 80.92 31.07 17.59 84.39 6.28 I.O4
Lll tj .i.eC'IILC. -^.O Ic.S t.O -O.OO -O.OO -O.OO 1.0 10.OO 90.2O 32.24 20.34 93.60 6.42 1.04
Llc;tJ<>./4ll(C. -O.ulr.S (•.() —O.OO -O.OO -0.00 1 .O 1 O.OO 46.98 32.7O 17.SO 98..16 1.64 1.01
CTJ ej ^....l^ 1110. -<,.;i I..S t .') -0.00 -0.00 -0.00 1.0 10.00 97.44 J3.14 15.63 98.75 1.22 1.O1
-------
TABLE 2A
AGGLOMERATE FLOTATION TEST NO. 84 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 80 ml 10,000 PPM Fe solution added (4.0 PPT) and
mixed for 5 minutes.
2. 400 grams of PID flyash added; slurry (16.5%) condition @ 1100 RPM.
3. Carbonate to pH 7 @ 2400 RPM and then add emulsion at rate of 140.75 Ib/ton.
4. Adjust rotor RPM empirically to just maintain suspension.
5. Collect float until froth breaks - 7 minutes.
6. Reclean concentrate.
Log
Number
FEED
690312
690308
690309
690311
690310
Fraction
RT
RC
CT-L
CC1
CT2
cc2
CT3
cc3
Wt.
Rec.
Cms.
400.00
226.00
297.58
116.15
181.08
69.00
112.08
36.08
76.00
L.O.I.
1.03
15.23
23.14
18.54
26.10
21.52
28.92
22.25
32.08
Ignited
Res idue
Cms.
395.88
191.58
228.72
94.90
133.82
54.15
79.67
28.05
51.62
Percent
CaO
29.79
20.26
35.13
26.82
41.02
32.29
46.96
34.53
51.27
Percent
Floated
47.89
57.18
23.72
33.45
13.53
19.92
7.01
12.90
Percent
CaO Rec.
32.57
67.43
21.35
46.07
14.67
31.39
8.12
22.21
Ratio
of
Enrich-
ment
1.18
1.38
1.58
-------
TAI1LF. 3A
AGGLOMERATE FLOTATION TEST NO. 85 LIMESTONE MOUIFIKI) FLYASII PID
1. 2000 nl H.,0 added to flotation cell, 20 ml 10,000 PPM Fe as ferrous ammonium sulfate (1.0 PPT) added and mixed
for 3 minutes.
2. 400 nrams of Pin flyash added; slurry (16.6%), condition P 1700 RPM for 15 minutes.
3. Carbonate to pH 10.0 Q 2200 RPM and then add emulsion at rate of HO.75 PPT.
4. Adjust rotor speed empirically during float.
5. Collect float in 3-5 mimlte increments.
6. Reclean float products separately.
Number
Feed
690363
A-Hi+C
A
1-CC1+1-CC2
690365
ii
1H690367
D
690367
690 J69
690370
F
L9037]
690372
'
i.'-i. ,/ ,
i:
('.'"in/?.
Fraction
RT
Total RC
1-RC
1-CT
Total CC
l-cci (1700)
2-HC
2-CT
Tot.il CC
2-CC!
2-CC (1700)
2-CT-,
2-CC 2
2-CT3
2-i:c,3
2-CC4
1-RC
1-..:)
i-' '' ;,
!"' '. '
Wt.
Rec.
r,ms.
400.00
19.0
437.9
141.7
36.2
105.5
68.5
37.0
93.3
16.6
76.7
56.0
20.7
15.3
40.7
13.8
26.9
21.4
202.9
5.9
4. n
l'i 3.0
3.;;
L.O.I.
1.03
8.55
19.35
24.81
16.40
27.69
28.95
25.35
18.59
11.53
20.12
21.52
16.35
15.28
23.86
13.70
29.08
14.57
32.79
J5.H8
12. V3
U.76
16. 0/
1 1.10
7 'I
Ifinited
Residue
Cms.
395. 9B
17.38
353.20
106.55
30.26
76.29
48.67
27.62
75.96
14.69
61.27
43.95
17.32
12.96
30.99
11.91
19.0.S
4.70
14. 3K
170.69
5.16
Id.'. 00
1.00
Percent
CaO
29.79
19.69
30.26
47.87
30.76
54.66
60.29
44.76
26.44
20.44
27.I-.9
28.50
26.34
23.80
30.46
26.47
32.96
28.44
34.39
20.97
19.38
21.02
18.4.:
21.11
Percent
Floated
4.68
95.31
28.75
8.16
20.59
13.13
7.45
20.49
3.96
16.53
11.85
4.67
3.49
8.36
5.14
1.21.
3.HK
46.06
14 M I'll
O.'l )
4 1 . / 1
O.l.'l
Percent
CaO Rec.
2.77
89.71
42.80
7.81
34.99
24.62
10.37
16.85
2.51
14.34
10.51
3.82
2.58
7.92
2.64
5.27
1.12
4. IS
30.05
O.K3
2" . 2 I
0.54
2;-.. ill.
O.'i 1
2H.14
Ratio
of
Enrich-
ment
1.02
1.61
2.02
1.50
0.89
0.94
0.96
1.02
1.11
1.15
0.70
0.71
1.00
-------
TABLE 4A
EMULSION FLOTATION TEST NO. 86 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20 ml 10,000 PPM FAS added, stirred for 5 minutes.
2. 400 grams PID added, conditioned at 2400 RPM for 15 minutes, carbonated to pH 10.0
3. 2.0 PPT sodium oleate added, conditioned for two minutes.
4. Floated in 5 minute increments, re-cleaned with additions of sodium oleate and F65 frother.
Log
Number Fraction
Wt.
Rec.
Cms. L.O.I.
Ignited
Residue
Cms.
Percent
CaO
Percent
Floated
Percent
CaO Rec.
Ratio
of
E nrich'
ment
FF.ED
400.0
1.03
395.88
27.79
TEST ABORTED
-------
TABLE 5A
AGGLOMERATE FLOTATION TEST NO. 87 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20 ml of 10,000 PPM Fe solution added (1.0 PPT)
and mixed for 5 min.
2. 400 grams of PID flyash added, slurry (16.5%), condition for 15 min. @ 1700 RPM.
3. Carbonate to pH 10.0 and add emulsion at rate of 140.75 Ib/ton.
4. Adjust rotor RPM empirically to just maintain suspension.
5. Collect float in 3-5 min. increments.
6. Reclean products separately.
Log
Number
690399
______
690400
_
690401
_____
690402
......
690403
______
690404
______
690405
690406
690407
690408
Fraction
FEED
RT
RC-I
CT1-I
CC1-I
CT2-I
CC2-I
CT3-I
CC3-I
CT4-I
CC4-I
CT5-I
CC5-I
CT6-I
CCI
RCII
CT1-II
CC-II
Wt.
Rec.
Gins.
400.0
31.2
272.6
50.3
222.3
28.5
193.8
40.8
153.0
26.0
127.0
14.3
112.7
32.8
79.9
150.4
30.3
120.1
L.O.I.
1.03
12.52
20.53
19.89
20.67
19.09
20.90
19.08
21.39
18.80
21.92
20.05
22.15
21.12
22.57
17.72
15.38
18.30
Ignited
Residue
Cms.
395.88
27.29
216.66
40.30
176.36
23.06
153.30
33.02
120.28
21.11
99.17
11.43
87.74
25.87
61.87
123.76
25.64
98.12
Percent
CaO
29.79
14.79
31.63
28.09
32.44
27.17
33.23
31.24
33.78
30.37
34.51
33.12
34.69
33.52
35.18
23.24
20.56
23.94
Percent
Floated
6.82
54.17
10.08
44.09
5.74
38.33
8.23
30.07
5.28
24.79
2.86
21.94
6.47
15.47
30.94
6.41
24.53
Percent
CaO Rec.
3.39
57.51
9.50
48.01
5.26
42.75
8.66
34.10
5.38
28.72
3.18
25.54
7.28
18.27
24.14
4.42
19.71
Ratio
of
Enrich-
ment
1.06
1.09
1.12
1.13
1.16
1.16
1.18
0.78
-------
- - TABLE 6A
AGGLOMERATE FLOTATION TEST NO. 88 LIMESTONE MODIFIED FLYASH PID
1. 1600 ml H20 added to flotation cell, 24 ml of 10,000 PPM Al solution added (0.6 PPT) and
mixed for 5 min.
2. 800 grams of PID flyash added, slurry (33.0%), condition for 15 min. @ 1700 RPM.
3. Carbonate to pH 8 and add emulsion at rate of 140.75 Ib/ton.
4. Adjust rotor RPM empirically to Just maintain suspension.
5. Collect float in 3-5 min. increments.
6. Reclean as conditions indicate.
Log
Number
690409
______
690410
______
690411
690412
______
690413
690414
___ — _
690415
__
690416
690417
690418
690419
690420
690421
Fraction
FEED
RT
RC-I
CT1-I
CC1-I
CT2-I
rr?_ T
\s\s£. J.
CT3-I
CC3-I
CT4-I
CC-I
RC-I I
CT1-II
CC1-II
CT2-II
CC2-II
CT3-II
CC3-II
CT4-II
CC-II
RC-I I I
CT1-III
com
wt.
Rec.
Gms.
800.0
169.4
320.5
148.4
172.1
71.2
inn Q
jLuw • y
43.8
57.1
19.3
37.8
210.1
80.0
130.1
25.7
104.4
11.9
92.5
23.0
69.5
204.6
85.3
119.3
L.O.I.
1.03
16.88
20.69
23.26
18.47
20.07
1 7 TT
JL f • -JJ
15.94
18.39
17.11
19.06
17.95
21.78
15.60
18.68
14.84
15.04
14.82
14.72
14.83
20.35
19.96
20.62
Ignited
Residue
Gms.
791.76
140.81
254.21
113.88
140.33
56.91
8T _?
*JJ • *4 _.
36.82
46.60
16.00
30.60
172.39
62.58
109.81
20.90
88.91
10.11
78.80
19.61
59.19
162.97
68.27
94.70
Percent
CaO
29.79
25.38
30.07
30.80
29.48
30.76
OR Al
A.O . \j j.
26.65
30.16
28.83
30.85
26.19
31.37
23.23
28.00
22.11
22.79
22.32
22.32
21.92
28.72
28.74
28.70
Percent
Floated
17.60
31.78
14.24
17.54
7.11
in &i
JLV/ • t-J
4.60
5.83
2.00
3.83
21.55
7.82
13.73
2.61
11.11
1.26
2.45
2.45
7.40
20.37
8.53
11.84
Percent
CaO Rec.
15.00
32.08
14.72
17.36
7.35
in m
-L.U * UJL
4.12
5.90
1.94
3.96
18.94
82.4
10.70
2.46
8.25
0.97
7.28
1.84
5. 44
19.64
8.23
11.40
Ratio
of
Enrich-
ment
1.01
0.99
Oaf.
• ./D
1.01
1.04
0.88
0.78
0.74
0.74
0.74
0.96
-------
TABLE 7A
EMULSION FLOTATION TEST NO. 89 LIMESTONE MODIFIED FLYASH PID
Log
Number Fraction
FEED
Wt.
Rec.
Cms.
400.0
L.O.I.
1.03
Ignited
Residue
Cms.
395.88
Percent
CaO
29.70
Percent
Floated
Percent
CaO Rec.
Ratio
of
Enrich-
ment
ro
-------
-53-
TABLE 8A
FLOTATION STANDARD CONDITIONS AND VARIABLE FACTORS INCORPORATED
IN TESTS 90 THROUGH 107 WHICH ARE ENCOMPASSED BY THE FACTORIAL
DESIGN EXPERIMENT TO IMPROVE FLOTATION SEPARATION OF LIME
FROM LIMESTONE MODIFIED FLYASH
Standard Conditions
Flyash - Dry-collected limestone modified flyash, Detroit Edison Co.,
St. Clair, Michigan
Pulp Density - 16.67 percent slurry
Mixing - Mix flyash and water for 15 minutes at 1700 RPM rotor speed
before modifier addition
Modifier - 1.0 pound per ton (PPT) ferrous ammonium sulfate
Carbonation - Carbonate immediately upon completion of mixing at 2400 RPM
rotor speed.
pH - Carbonate to pH 10, add emulsion and lower pH to 7 through further
carbonation
Emulsion - 50 percent water, 25 percent #2 fuel oil, 22 1/2 percent tall oil,
2 1/2 percent sodium alkylarylsulfonate
Rougher Separation - four minutes
Cleaner Separations - two minutes
Recleaning - Reclean tail at 1700 RPM except TC, which is recleaned at
1150 RPM
Make Up Water - Use recycle water when possible
Factors
Low Level High Level
Emulsion addition rate in PPT = A 60 100
Conditioning time in minutes after addition of
emulsion - B 5 10
Rotor speed of impeller during separations in
RPM - C 1150 1700
-------
-54-
TABLE 8A (Continued)
FACTORIAL DESIGN RESPONSE DATA AND FACTOR LEVELS
iL ±1
A 60 100
B 5 10
C 1150 1700
D 18 28
I
Flotation
Test No.
98
102
107
99
96
95
103
104
106
93
105
101
100
92
97
94
A
-1
-1
-1
-1
-1
-1
-1
-1
1
1
1
1
1
1
1
1
B
-1
-1
-1
-1
1
1
1
1
-1
-1
-1
-1
1
1
1
1
C
-1
-1
1
1
-1
-1
1
1
-1
-1
1
1
-1
-1
1
1
D
-1
1
-1
1
-1
1
-1
1
-1
1
-1
1
-1
1
-1
1
Grade
30.30
33.31
34.50
31.63
33.13
28.60
30.46
33.61
31.97
32.19
29.43
30.10
29.72
35.40
28.78
32.25
Yield
85.13
69.50
69.40
78.06
86.09
50.06
81.68
72.25
76.76
67.69
85.07
85.03
83.77
56.93
90.10
74.76
Grade x Yield
x 10~2
0.2565
0.2315
0.2394
0.2469
0.2852
0.1432
0.2315
0.2428
0.2454
0.2179
0.2504
0.2559
0.2490
0.2015
0.2593
-------
-55-
TABLE 8A (Continued)
DIAGRAM OF FLOTATION SCHEME OF THE
FACTORIAL DESIGN TESTS 90 THROUGH 107
Mix 16.67% pulp with !
modifier, carbonate and
add emulsion
Rougher Separation
Rougher Concentrate, (RC)
1
1st RC Cleaning
1st Cleaner Tails,
1st Cleaner Concentrate,
(ccp
2nd RC Cleaning
2nd Cleaner Tails, (CTj
2nd Cleaner Concentrate
(cc2)
r
Recleaning of Cleaner —I
•P-4 1 „ I
Tails
Rougher Tails, (RT)
1st RT Cleaning
n
w
1st RT Tail, (TTj)
1st RT Concentrate
(TC,)
2nd RT Cleaning
Cleaner Tail Concentrate,
i .(SCI —
Cleaner Tails, (ST)
2nd RT Concentrate,
(TC2)
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 90 LIMESTONE MODIFIED FLYASH PID
Levels A 60 PPT
B 5 Min.
C 1150 RPM
D 18 Percent
Log
Number Fraction
FEED
Wt.
Rec.
Cms.
400.0
L.O.I.
1.03
Ignited
Res idue
Cms.
395.88
Percent
CaO
29.79
Percent
Floated
Percent
CaO Rec.
Ratio
of
Enrich-
ment
in
PRELIMINARY FACTORIAL TEST
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 91 LIMESTONE MODIFIED FLYASH PID
Levels A 100 PPT
B 10 Min.
C 1700 RPM
D 28 Percent
Lop,
Number Fraction
FEED
Wt.
Rec.
Gr.is .
400.0
L.O.I.
1.03
Ignited
lies i due
Cms .
395.88
Percent
CaO
29.79
Percent
Floated
Percent
CaO Rec.
Ratio
of
Enrich-
ment
I
«J1
•vl
PRELIMINARY FACTORIAL TEST
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 92 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690435
690436
690437
690438
690439
A 100 PI
B 10 Mir
C 1150 I
D 28 Pel
Fraction
cc
2
SC
RT & ST
TTj
TCj
TT2
TC2
/T* r op
L»l>2 " ^**-*
& TC0
»T
i.
1PM
rcent
Wt.
Rec.
Gins.
400.0
63.8
120.8
242.7
151.9
90.8
31.6
59.2
2 A T Q
L.O.I.
1.03
22.55
20.70
15.83
13.83
19.16
14.60
21.59
91 /• 1
£J..'4A
Ignited
Residue
Cms.
395.88
49.41
95.79
204.30
130.89
73.41
26.99
46.42
mAI
• OX
Percent
CaO
29.79
39.64
34.26
23.59
20.65
28.85
21.31
33.25
i1; /. n
JJ .tU
Percent
Floated
12.35
23.94
51.07
32.72
18.35
6.47
11.60
/. 7 on
** / • yu
Percent
CaO Rec.
16.43
27.58
40.45
22.68
17.77
4.82
12.95
jo . y j
Ratio
of
Enrich-
ment
1.33
1.15
0.79
0.69
0.97
0.72
1.12
11 Q
. iy
I
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 93 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690440
690441
690442
690444
690443
A 100 PPT
B 5 Min.
C 1150 RPM
D 28 Percent
Wt.
Rec.
Fraction Gins.
400.0
CC2 94.9
SC 121.3
RT & ST 238.8
T1! 108.5
TCx 130.3
TT2 33.1
TC2 97.2
& TC-,
L.O.I.
1.03
21.08
19.29
16.93
14.52
18.93
15.75
20.01
70 Ofi
i, \i . \j\j
Ignited
Residue
Cms.
395.88
74.90
97.90
198.39
92.75
105.64
27.89
77.75
7^0 ss
£. _/ w • J J
Percent
CaO
29.79
36.19
30.76
26.86
24.28
29.13
26.30
30.15
T9 1 Q
J^ • iy
Percent
Floated
18.72
24.47
49.59
23.18
26.41
6.97
19.43
A9 (.1
OZ . O J
Percent
CaO Rec.
22.74
25.27
44.72
18.89
25.82
06.15
19.67
A 7 f,Q
D / . vy
Ratio
of
Enrich-
ment
1.21
1.03
0.90
0.82
0.98
0.88
1.01
Inft
• Uo
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 94 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690445
690446
690447
690449
690448
A 100 PPT
B 10 Min.
C 1700 RPM
D 28 Percent
wt.
Rec.
Fraction Cms.
400.0
CC2 114.8
SC 123.3
RT & ST 222.0
TT 79.2
TC1 142.8
TT2 43.1
TC2 99.7
CC, (, SC 337.8
L.O.I.
1.03
22.09
18.69
15.97
19.55
13.91
15.76
13.22
18.23
Ignited
Residue
Cms.
395.88
89.44
100.26
186.55
63.72
122.83
36.31
86.52
276.72
Percent
CaO
27.79
42.26
31.94
24.25
27.39
22.63
23.50
22.27
32.25
Percent
Floated
22.36
25.06
46.63
15.93
30.70
9.07
21.63
69.05
Percent
CaO Rec.
31.71
26.87
37.79
14.64
23.33
7.16
16.16
74.75
Ratio
of
Enrich'
ment
1.42
1.07
0.87
0.92
0.76
0.79
0.75
1.08
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 95 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690452
690453
690454
690456
690455
A 60 PPT
B 10 Min.
C 1150 RPM
D 28 Percent
Wt.
Rec.
Fraction Cms.
400.0
CC2 55.2
SC 109.0
RT & ST 305.7
T^ 150.8
K^ 154.9
TT2 68.0
TCo 86.9
*.
ar C f- 7 r: -i i
j n G *>*., Z, _/ J. » X
fv TC2
L.O.I.
1.03
14.23
19.86
18.83
20.72
16.98
19.54
14.96
1 (\ Q '\
j-i> • .' j
Ignited
Residue
Cms.
395.88
47.36
87.35
248.16
119.55
128.61
54.71
73.90
?OK fi
t-\ 'O • \'
Percent
CaO
29.79
22.75
34.43
30.39
32.38
28.54
32.72
25.46
?P, 60
£.O» kl V '
Percent
Floated
11.83
21.83
62.04
29.88
32.15
13.67
18.47
r>? IS
_/ <- • J. -'
Percent
CaO Rec.
9.04
25.23
63.29
32.48
30.81
15.02
15.78
^ ft HA
3\' • UO
Ratio
of
Enrich-
ment
0.76
1.16
1.02
1.09
0.96
1.10
0.85
0 06
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 96 LIMESTONE MODIFIED FLYASH PIU
FACTORIAL DESIGN EXPERIMENT
Levels
Lop,
Number
FEED
690457
690458
690459
690461
690460
A 60 PPT
B 10 Min.
C 1150 RPM
D 18 Percent
wt.
Rec.
Fraction Cms.
400.0
CC 103.3
2
SC 188.1
RT f, ST 1 60 2
TT, 49.1
rr 1111
TT2 13.0
TC2 98.1
CC-, f, SC 389.5
f, TC2
L.O.I.
1.03
24.79
20.00
1 3 74
8.31
1 A 1 A
10.19
16.93
20.50
Ignited
Residue
Cms.
395.88
77.69
150.48
138 19
45.02
QT 17
11.68
81.49
309.66
Percent
CaO
29.79
42.26
34.04
10 iq
14.09
nAA
14.09
22.75
33.13
Percent
Floated
19.42
37.62
34 54
11.25
2.92
20.37
77.41
Percent
CaO Rec.
27.55
42.98
5.32
If. QT
1.38
15.55
86.09
Ratio
of
Enrich-
ment
1.42
1.14
0 64
0.47
O T\
0.47
0.76
1.11
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 97 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels A 100 I
B 10 Mj
C 1700
D 18 P(
LOR
Number Fraction
FEED
690462 CC
2
690463 SC
690464 TT1
TC]L
690466 TT2
690465 TC.,
^.
>PT
Ln..
RPM
jrcent
wt.
Rec.
Cms.
400.0
207.1
197.8
1.5
55.0
1.0
53.2
Ar,« 1
L.O.I.
1.03
19.31
18.23
1 6 64
9.42
16.84
13.70
16.93
IK ^7
Ignited
Residue
Cms.
395.88
167.11
161.74
4710
1.36
45.74
1.55
44.19
T7T HA
Percent
CaO
29.79
29.32
28.75
76 64
22.18
26.77
24.06
26.87
9R 7R
Percent
Floated
41.77
40.43
U77
0.34
11.43
0.38
11.04
QT ?fi
Percent
CaO Rec.
41.11
39.02
in si
J.U. J J
0.25
10.27
0.31
9.96
on i n
Ratio
of
Enrich-
ment
Q
0.98 V
0.97
OOQ
0.74
0.90
0.81
0.90
n QA
& TC
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 98 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690467
690468
690469
690471
690470
A 60 PPT
B 5 Min.
C 1150 RPM
D 18 Percent
Wt.
Rec.
Fraction Gms.
400.0
CC2 126.3
SC - 187.3
RT & ST 145.1
T1l 33.2
TC-L 111.9
TT 15.3
TC2 96.6
rr ~ n QP A 1 n 9
2 H JLU * Z
& TC
L.O.I.
1.03
17.99
18.30
16.95
16.36
17.12
16.79
17.16
1 7 Q4
J. / . y H
Ignited
Residue
Gms.
395.88
103.58
153.02
120.52
27.77
92.75
12.73
80.02
Percent
CaO
29.79
30.45
30.72
28.23
27.83
28.26
26.73
28.62
Tn 1 1
JU. J. J
Percent
Floated
25.89
38.25
30.13
6.94
23.18
3.18
20.00
HA it;
O'*. .0
Percent
CaO Rec.
6.46
39.45
28.56
6.48
22.07
2.85
19.22
OC 1 ">
O_>. I J
Ratio
of
Enrich-
ment
1.02
1.03
0.95
0.93
0.95
0.90
0.96
1m
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 99 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Lop,
Number
FEED
690472
690473
690474
690476
690475
A 60 PPT
K 5 Min.
C 1700 R
D 28 Per
Fraction
cc2
SC
RT & ST
TT
TC1
TT2
TC0
pp~ r cp
v.iv_«2 ** *>*-'
(, TC2
PM
cent
wt.
Rec.
Cms.
400.0
126.4
137.8
192.8
71.5
121.3
23.3
98.0
-If,? 9
J\J /- . t-
L.O.I.
1.03
20.59
19.05
14.89
13.46
15.73
13.71
16.20
1 R ft?
-LO • U£
Ignited
Residue
Cms.
395.88
100.37
111.55
164.11
61.88
102.23
20.11
82.12
9QA DA
£. "H . u1*
Percent
CaO
29.79
34.70
33.07
23.31
20.70
24.89
70.65
25.94
•ji f, -i
J L . O j
Percent
Floated
25.09
27.88
41.02
15.47
25.55
5.02
20.53
Percent
CaO Rec.
29.22
30.95
32.11
10.74
21.36
3.48
17.87
Ratio
of
Enrich'
ment
1.16
1.11
0.78
0.69
0.84
0.69
0.87
i PIA
JL . I'D
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 100 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels A 100 PPT
B 10 Min.
C 1150 RPM
D 18 Percent
LOB
Number
FEED
690477
690478
690479
690481
690480
______
Fraction
cc2
SC
RT & ST
TT
TCX
TT
2
TC2
CC? & SC
Wt.
Rec.
Cms.
400.0
97.8
176.1
194.9
40.3
154.6
13.4
141.2
415.1
L.O.I.
1.03
20.07
18.85
19.04
20.57
18.64
17.43
18.75
19.13
Ignited
Residue
Cms .
395.88
78.17
142.91
152.80
32.01
125.79
11.06
114.73
335.81
Percent
CaO
29.79
34.57
29.80
25.79
24.81
26.05
23.06
26.34
29.72
Percent
Floated
19.54
35.72
39.45
8.00
31.44
2.76
28.68
83.95
Percent
CaO Rec.
22.67
35.73
34.16
6.66
27.50
2.14
26.34
83.77
Ratio
of
Enrich-
ment
1.16
1.00
0.87
0.83
0.87
0.77
0.88
1.00
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 101 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Lop
Number
FEED
6904892
690483
690484
690486
690485
A 100 PPT
B 5 Min.
C 1700 RPM
D 28 Percent
Wt.
Rec.
Fraction Cms.
400.0
CC2 143.0
SC 136.6
RT & ST 195.1
TT 9Q Q
11-1 £-j+j
IC1 165.2
TT2 21.0
TC2 144.2
cr f. ^f A "7° P.
VAy O Of t»Vy '»*-,' »O
& TC0
L.O.I.
1.03
20.60
20.83
19.18
15.36
19.87
4.87
20.30
70 SR
*- •J . j o
Ignited
Residue
Cms.
395.88
113.54
108.15
157.69
25.30
132.39
17.46
114.93
Percent
CaO
29.79
32.38
31.80
25.12
22.92
25.54
20.92
26.25
Percent
Floated
28.38
27.03
39.42
6.32
33.09
4.36
28.73
84 1 S
o*+ . j. j
Percent
CaO Rec.
32.38
31.80
33.24
4.86
28.38
3.06
25.31
Ratio
of
Enrich-
ment
1.09
1.07
0.84
0.77
0.86
0.70
0.88
1 01
J. • \J -L
•vj
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 102 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
6790487
690488
690489
690491
690490
A 60 PPT
B 5 Min.
C 1150 RPM
D 28 Percent
wt.
Rec.
Fraction Cms.
400.0
CC2 112.7
SC 128.7
RT & ST 223.1
TTj, 87.4
TCX 135.7
TT 64.2
TC2 71.5
CC9 & SC 313.0
L.O.I.
1.03
23.93
19.38
16.05
16.16
15.97
14.28
17.48
20.59
Ignited
Residue
Cms.
395.88
85.81
103.76
187.31
73.28
114.03
55.03
59.00
248.57
Percent
CaO
29.79
39.86
31.33
22.30
19.46
24.13
20.74
27.30
33.31
Percent
Floated
21.45
25.94
46.82
18.32
28.50
13.75
14.75
62.14
Percent
CaO Rec.
28.70
27.28
35.06
11.96
23.59
9.57
13.57
69.50
Ratio
of
E nrich-
ment
,
O^
1.34 °°
1.05
0.75
0.65
0.81
0.70
0.92
1.11
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 103 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690492
690493
690494
690496
690495
^•••lu,.
A 60 PPT
B 10 Min.
C 1700 RPM
D 18 Percent
Wt.
Rec.
Fraction Cms.
400.0
CC2 129.1
SC 128.6
RT & ST IQft fi
TT 39.4
T^ 159.2
TT2 24.3
TC2 134.9
CC0 & SC 392.6
L.O.I.
1.03
22.49
18.56
14 70
13.88
14.90
14.35
14.99
18.63
Ignited
Residue
Cms.
395.88
100.07
104.73
169 42
33.93
135.49
20.81
114.68
319.46
Percent
CaO
29.79
37.80
31.24
n96
18.55
22.82
19.86
23.36
30.46
Percent
Floated
25.01
26.18
42 36
8.48
33.87
5.20
28.67
79.87
Percent
CaO Rec.
31.74
27.45
5.28
25.95
3.46
22.48
81.68
Ratio
of
E nrich'
ment
1.27
1.05
0 73
0.62
0.77
0.67
0.78
1.02
vO
I
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 104 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690497
690498
690499
690501
690500
__ __—
A 60 PPT
B 10 Min.
C 1700 RPM
D 18 Percent
wt.
Rec.
Fraction Cms.
400.0
CC2 115.6
SC 100.3
RT & ST 238.8
TTj 103.8
TCX 135.0
TT 26.1
TC 108.9
2
CC0 & SC 324.8
L.O.I.
1.03
23.87
20.90
15.02
12.11
17.26
12.22
18.46
21.14
Ignited
Residue
Cms.
395.88
88.01
79.34
202.94
91.23
111.71
22.91
88.80
256.15
Percent
CaO
29.79
40.25
33.51
22.67
19.71
25.10
17.28
27.12
33.61
Percent
F loated
22.00
19.83
50.73
22.80
27.92
5.72
22.20
64.03
Percent
CaO Rec.
29.72
22.31
38.62
15.09
23.53
3.32
20.21
72.25
Ratio
of
Enrich-
ment
i
1.35 f
1.12
0.76
0.66
0.84
0.58
0.91
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 105 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
NumViPi*
11 UillU C JL
FEED
690502
690503
-Mf^^ ,-!-••_•
690504
^ — — ,»^^
690506
690505
A 100 PPT
B 5 Min.
C 1700 RPM
D 18 Percent
Wt.
Rec.
Fraction Cms.
400.0
CC2 156.2
SC 150.4
RT & ST 153.5
TTi 23.4
TC! 130.1
TT2 10.8
TC2 119.3
CCo & SC 425.9
L.O.I.
1.03
19.88
19.16
16.43
9.67
17.65
12.61
18.10
19.13
Ignited
Residue
Cms.
395.88
125.15
121.58
128.29
21.14
107.15
9.44
97.71
344.44
Percent
CaO
29.79
32.07
30.23
22.37
13.30
24.16
14.92
25.06
29.43
Percent
Floated
31.28
30.39
32.07
5.28
26.78
2.36
24.42
86.11
Percent
CaO Rec.
33.68
30.84
24.09
2.35
21.73
1.18
20.54
85.07
Ratio
of
Enrich'
ment
1.08
1.01
0.75
0.45
0.81
0.50
0.84
0.99
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 106 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690507
690508
690509
690511
690510
A 100 PPT
B 5 Min.
C 1150 RPM
D 18 Percent
Fraction
CC2
SC
RT & ST
TTj
TC!
TT2
TC2
cc2 & sc
& TC2
Wt.
Rec.
Cms.
400.0
99.7
173.3
180.4
85.8
94.6
11.7
82.9
355.9
L.O.I.
1.03
22.15
19.35
15.66
14.63
16.60
12.59
12.16
19.63
Ignited
Residue
Cms.
395.88
77.62
139.77
152.15
73.25
78.90
10.23
68.67
286.06
Percent
CaO
29.79
38.50
30.76
22.01
17.98
25.75
16.88
27.08
31.97
Percent
Floated
19.40
34.94
38.02
18.31
19.72
2.55
17.16
71.51
Percent
CaO Rec.
25.07
36.08
28.10
11.05
17.05
1.44
15.60
76.76
Ratio
of
Enrich-
ment
1.29
1.03
0.74
0.60
0.86
0.57
0.91
1.07
I
-------
TABLE 8A (Continued)
EMULSION FLOTATION TEST NO. 107 LIMESTONE MODIFIED FLYASH PID
FACTORIAL DESIGN EXPERIMENT
Levels
Log
Number
FEED
690512
690513
690514
690516
690515
•»_•*_•»
A 60 PPT
B 5 Min.
C 1700 RPM
D 18 Percent
wt.
Rec.
Fraction Cms.
400.0
CC2 103.8
SC 107.8
RT & ST 241.4
TIi 101.1
TT-i 140 3
J. Vy | JU*tv/*J
TT2 45.3
TC0 95.0
CCn & SC 306.6
L.O.I.
1.03
23.88
21.35
14.48
9.79
17 85
.L/C U_/
13.13
20.10
21.82
Ignited
Residue
Cms.
395.88
79.01
84.78
206.46
91.20
m26
• fc VJ
39.35
75.91
239.70
Percent
CaO
29.79
40.69
32.02
23.28
17.94
27 50
fm / * tJ \J
21.08
30.84
34.50
Percent
Floated
19.75
21.19
51.61
22.80
28 81
^\J • \J JL.
9.83
18.97
59.92
Percent
CaO Rec.
26.97
22.78
40.33
13.73
9.69
19.64
69.40
Ratio
of
Enrich-
ment
1.37
1.07
0.78
0.60
0 9?
\J . y £.
0.70
1.03
1.16
-------
TABLE 9A
EMULSION FLOTATION TEST NO. 108 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20 ml 10,000 PPM FAS added, stirred for 5 minutes.
2. 400 grams of PID added, conditioned at 2400 RPM for 15 minutes, carbonated to pH 10.0, added
4.0 PPT emulsion.
3. Conditioned for 7.5 minutes at 1700 RPM, floated for four minutes, recleaned concentrate twice,
4. Scavanged cleaner tails with additional 20 PPT emulsion for 2 minutes.
5. Recleaned RT & ST twice at 1200 RPM for 2 minutes.
LOB
Number
FEED
690561
690562
690563
690564
690565
-___-. M
Wt.
Rec.
Fraction Cms.
400.0
CC2 84.0
SC 145.0
RT & ST 230.0
TT. 86.0
T^ 144.0
TT2 10.0
TC 134.0
CC & SC 363.0
L.O.I.
1.03
21.36
19.81
16.73
14.18
18.25
13.63
18.59
19.72
Ignited
Residue
Cms.
395.88
66.06
116.28
191.54
73.81
118.73
8.64
109.09
291.43
Percent
CaO
29.79
25.31
32.11
25.98
23.06
27.81
22.23
28.26
31.39
Percent
Floated
16.59
29.07
47.88
18.45
29.43
2.16
27.27
72.85
Percent
CaO Rec.
19.57
31.33
41.76
14.28
27.48
1.61
25.87
76.77
Ratio
of
Enrich-
ment
1.19
1.08
0.87
0.77
0.83
0.75
0.95
1.05
-------
TABLE 10A
EMULSION FLOTATION TEST NO. 109 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20 ml 10,000 PPM FAS added, stirred for 5 minutes.
2. 400 grams of PID added, conditioned at 2400 RPM for 15 minutes, carbonated to pH 10.0, added
4.0 PPT emulsion.
3. Conditioned for 3.5 minutes, floated for four minutes at 1621 RPM.
4. Recleaned concentrate twice, combined the CT, and CT~ fractions and added 20.0 PPT of emulsion,
floated at 1700 RPM for 2 minutes.
5. Combined the ST & RT, added 20.0 PPT emulsion, floated for 2 minutes, recleaned twice.
Log
Number
FEED
690566
690567
690568
690569
690570
Fraction
CC2
SC
t?T H QT
TCl
TT2
TC2
CC2 & SC
wt.
Rec.
Cms.
400.0
86.8
13.28
9 in f\
L JU • D
70.2
160.4
37.8
132.6
352.2
L.O.I.
1.03
24.07
20.59
USfi
12.74
11.05
14.05
16.89
20.06
Ignited
Residue
Cms.
395.88
65.91
105.46
701 QS
61.26
142.69
32.49
110.20
281.57
Percent
CaO
29.79
41.17
32.34
77 fiR
17.01
25.12
19.25
26.85
32.25
Percent
Floated
16.47
26.36
SO QR
15.31
35.67
8.12
27.55
70.39
Percent
CaO Rec.
22.77
28.62
•10 07
8.74
30.08
5.24
24.83
76.22
Ratio
of
E nrich-
raent
1.38
1.09
n 7f>
0.57
0.84
0.65
0.90
1.08
-------
TABLE 11A
EMULSION FLOTATION TEST NO. 110 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20 ml 10,000 PPM FAS added, stirred for 5 minutes.
2. 400 grams of PID added, conditioned at 2400 RPM for 15 minutes, carbonated to pH 10.0, added
4.0 PPT emulsion.
3. Conditioned for 7.5 minutes at 1700 RPM, floated for four minutes, recleaned concentrate twice.
4. Scavanged cleaner tails with additional 20 PPT emulsion for 2 minutes.
5. Recleaned RT & ST twice at 1200 RPM for 2 minutes.
Log
Number
FEED
690577
690578
690579
690580
Fraction
cc2
SC
TC1
rr« x.
-------
TABLE 12A
EMULSION FLOTATION TEST NO. Ill LIMESTONE MODIFED FLYASH PID
1. 2000 ml HO added, 20 ml 10,000 PPM added, stirred
2, 400 prams PID flyash added, conditioned for 15 minutes, carbonated to pH 10.0, added 10 PPT,
15 Percent rosin emulsion carbonated on to pH 7.0
3. Conditioned 3.5 minutes, floated for A minutes at 1700 RPM, concentrate recleaned twice.
A. CTi & CT2 combined, 5.0 PPT emulsion added, conditioned 3.5 minutes and floated 2 minutes.
5. ST & RT combined, 5.0 PPT Emulsion added, conditioned 3.5 minutes, floated 2 minutes, recleaned twice.
LOR
Number
FEED
690581
690582
690583
69058A
690585
Fraction
cc2
sc
PT X. QT
TT1
Tr
TC1
TT
TC2
& TC2
rr ~ t. <:r
Wt.
Rec.
Gms.
AOO.O
97.0
77.5
OQA 0
1A2.0
1 U") 0
60.5
81.5
oct n
i 7 A <;
L.O.I.
1.03
27.35
21.72
U1 0
8.A2
nftA
11.18
15.81
nQ7
. 7 1
o A n Q c;
Ignited
Residue
Gms.
395.88
70. A7
60.67
7s? An
130. OA
mi6
53. 7A
68.62
1 QO 7A
in i A
Percent
CaO
29.79
A9.7A
39.72
i Q ao
15. 8A
?A 06
19.82
27.39
IQ ni
/.=; in
Percent
Floated
17.61
15.16
61 1 0
32.51
in sq
13. A3
18.15
TO 77
Percent
CaO Rec.
29. Al
20.22
Al QQ
17.28
?A 7n
8.93
15.77
A1; An
n J . 'tU
AQ Al
Ratio
of
Enrich-
ment
i
*^
i
1.67
1.33
n 67
0.53
0 81
0.67
0.92
1 31
-------
TABLE 13A
EMULSION FLOTATION TEST NO. 112 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added, 20 ml of 10,000 PPM FAS added, stirred.
2. 400 grams PID added, conditioned for 15 minutes, carbonated to pH 10.0, added 10.0 PPT emulsion,
carbonated on to pH 7.0.
3. Conditioned for 3.5 minutes, floated 4 minutes at 1700 RPM, recleaned concentrate twice.
4. Combined CT & CT-, added 5 PPT emulsion, conditioned for 3.5 minutes, floated 2.0 minutes.
5. Combined ST & RT, added 5 PPT emulsion, conditioned for 3.5 minutes, floated 2 minutes,
recleaned concentrate twice.
6. Emulsion altered to 0.5% sodium alkylarylsulfonate, 23.5% tall oil, 26% fuel oil, 50.0% H-O.
Log
Number Fraction
FEED
wt.
Rec.
Cms .
400.0
L.O.I.
1.03
Ignited
Residue
Cms.
395.88
Percent
CaO
29.79
Percent
Floated
Percent
CaO Rec.
Ratio
of
Enrich-
ment
i
>j
oo
-------
TABLE 14A
EMULSION FLOTATION TEST NO. 113 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added, 20 ml of 10,000 PPM FAS added, stirred.
2. 400 grams PID added, conditioned for 15 minutes, carbonated to pH 10.0, added 10.0 PPT emulsion,
carbonated on to pll 7.0.
3. Conditioned for 3.5 minutes, floated 4 minutes at 1700 RPM, recleaned concentrate twice.
4. Combined CT^ & CT2, added 5 PPT emulsion conditioned for 3.5 minutes, floated 2.0 minutes.
5. Combined ST & RT, added 5 PPT emulsion conditioned for 3.5 minutes, floated 2 minutes, recleaned
concentrate twice.
6. Emulsive altered to 1.5% sodium alkyarylsulfonate, 23.5% tall oil, 25% fuel oil, 50% H20.
Log
Number Fraction
FEED
690623 CC2
690624 SC
t>7 c CT
690625 TTj_
690626 TT
690627 TC2
cr f nf.
Ignited
Residue
Cms.
395.88
33.70
52.09
OQA QA
156.68
1 ^ft 7f\
75.95
62.31
i /, R in
1 M f) . 1 U
Percent
CaO
29.79
52.24
45.85
73 54
19.51
OQ 1 7
24.68
32.33
A 1 A 1
^41 . Oi
Percent
Floated
8.42
13.02
7T 73
39.17
n/. c/i
18.98
15.57
17 m
Percent
CaO Rec.
14.77
20.04
64 61
25.65
TO QQ
18.74
20.14
^A Q •;
r> '< . v ->
Ratio
of
Enrich-
ment
1.75
1.54
0 79
0.65
0 Q4
0.83
1.09
i An
i
•vl
VO
1
-------
TABLE ISA
EMULSION FLOTATION TEST NO. 114 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added, 20 ml of 10,000 PPM FAS added, stirred.
2. AOO grams PID added, conditioned for 15 minutes, carbonated to pH 10.0, added 10.0 PPT emulsion,
carbonated on to pH 7.0.
3. Conditioned for 3.5 minutes, floated A minutes at 1700 RPM, recleaned concentrate twice.
A. Combined CT^ & CT2, added 5 PPT emulsion, conditioned for 3.5 minutes, floated 2.0 minutes.
5. Combined ST & RT, added 5 PPT emulsion, conditioned for 3.5 minutes, floated 2 minutes, recleaned
concentrate twice.
6. Emulsive altered to 2.0 sodium alkyarylsulfonate^.2.59% L-5 tall oil, 10.5% M-28 tall oil, 25.0% fuel
oil, 50.0% H20.
Log
Number
FEED
690628
690629
690630
690631
690632
Fraction
cc2
SC
RT & ST
TTX
TCj
TT2
TC2
CC2 & SC
wt.
Rec.
Gms.
AOO.O
6A.O
55.0
333.0
13A.O
199.0
93.0
106.0
225.0
L.O.I.
1.03
25.85
22.17
13.38
10.21
15.51
12.63
18.02
21.26
Ignited
Residue
Cms.
395.88
A7.A6
A2.81
288. A7
120.32
168.15
81.25
86.90
177.17
Percent
CaO
29.79
A9.53
A1.82
23.12
17.37
27. 2A
21.21
32.51
39.31
Percent
Floated
11.86
10.70
72.11
30.08
A2.03
20.31
21.72
AA.29
Percent
CaO Rec.
19.72
15.02
55.96
17.53
38. A3
1A.73
23.70
58. AA
Ratio
of
Enrich-
ment
1.66
l.AO
0.78
0.58
0.91
0.73
1.09
1.32
I
oo
-------
TABLE 16A
EMULSION FLOTATION TEST NO. 115 LIMESTONE MODIFIED FLYAS1I PID
1. 2000 ml H20 added, 20 ml 10,000 PPM FAS added, stirred.
2. 400 grams PID flyash added, conditioned for 1.0 hour, carbonated to pH 6.5 , added 10.0 PPT emulsion,
conditioned for 3.5 minutes, floated at 1700 RPM for 4 minutes, concentrate recleaned twice.
3. CT, & CT combined, 5 PPT emulsion added, conditioned for 3.5 minutes, floated 2 minutes.
4. ST & RT combined, 5 PPT emulsion added, conditioned for 3.5 minutes, floated 2 minutes.
5. Concentrate recleaned twice.
Log
Number
FEED
690551
690652
690653
690654
690655
Fraction
cc2
SC
DT f. CT
TT2
TC2
rc n ^c
& TC2
rr A. cr
Wt.
Rec.
Cms.
400.0
9.2
25.0
A 7Q 7
115.0
324 7
243.0
81.7
mq
1A 9
L.O.I.
1.03
35.65
29.07
i ft ?n
J.D ,£U
18.86
i c 7/:
14.27
18.16
nqi
^nB <;
Ignited
Residue
Cms .
395.88
5.92
17.73
93.31
O7C 10
208.32
66.86
qn c-i
9T A";
Percent
CaO
29.79
81.45
61.60
97 1ft
32.09
oc 71;
24.36
30.10
Percent Percent
Floated CaO Rec.
1.48 4.04
4.43 9.16
23.32 25.12
£0 7Q CQ AA
52.08 42.58
16.71 16.88
Q 01 i a ">n
Ratio
of
Enrich-
ment
2.73
2.07
OQ 1
. 7 X
1.08
Oat.
.00
0.82
1.01
i 11
i . J j
i
00
-------
TABLE 17 A
EMULSION FLOTATION TEST NO. 116 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added, 20 ml of 10,000 PPM FAS added, stirred.
2. 400 grams PID added, conditioned for 15 minutes, carbonated to pH 6.5, 10.0 PPT emulsion added,
floated 4 minutes.
3. CT^ & CT2 combined, 5.0 PPT emulsion added, conditioned 3.5 minutes, floated 2 minutes.
4. ST & RT combined, 5.0 PPT emulsion added, conditioned 3.5 minutes, floated 2 minutes, recleaned twice.
Log
Number
FEED
690659
690660
690661
690663
690662
Fraction
cc2
SC
RT & ^T
TTi
TT2
TC2
pf- t C(
& TC2
rr_ x. QI
Wt.
Rec.
Cms.
400.0
125.0
97.7
121 1
23.8
149 S
16.5
133.0
15 ri 7
999 7
L.O.I.
1.03
22.08
19.02
11 14
10.91
nso
12.08
13.66
18 10
9fl 7A
Ignited
Residue
Cms.
395.88
97.40
79.12
1 50 51
21.20
1 79 11
74.50
114.83
mis
1 76 S7
Percent
CaO
29.79
39.51
32.95
77 04
18.81
77 57
19.87
22.92
11 ia
•*£ sfi
Percent
Floated
24.35
19.78
17 fil
5.30
17 11
3.62
28.70
79 81
AA 1 1
Percent
CaO Rec.
32.29
21.87
77 81
3.34
94 49
2.41
22.08
";/, i A
Ratio
of
Enrich-
ment
I
00
1.33 ?
1.11
0 74
0.63
0 7fi
0.67
0.77
1 OS
-------
TABLE 18A
EMULSION FLOTATION TEST NO. 117 DOLOMITE MODIFIED FLYASH CI
1. 2000 ml H20 added, 20 ml of 10,000 PPM FAS, stirred.
2. 400 prams CI flyash added, conditioned for 15 minutes, carbonated to pH 7.0, 10.0 PPT
emulsion added, conditioned for 3.5 minutes, floated A minutes.
3. 10.0 PPT emulsion added to RT, conditioned for 3.5 minutes, RT refloated for 5.5 minutes.
4. Concentrate recleaned for 3 minutes.
Log
Number
FEED
690678
690679
690680
Fraction
CC
CT
1st 4 min.
ne-
wt.
Rec.
Cms .
400.0
94.0
105.0
70.0
L.O.I.
3.79
24.73
25.80
26.10
Ignited
Residue
Gms .
384.12
70.75
77.91
51.73
Percent
CaO
22.97
26.47
27. R3
30.32
Percent
Floated
18.41
20.28
13.46
Percent
CaO Rec.
21.22
24.57
17.77
Ratio
of
Enrich-
ment
1.15
1.21
1.31
CD
U>
690681
178.0
!5.23
133.09
25.95
34.64
39.14
-------
TABLE 19A
EMULSION FLOTATION TEST NO. 118 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20 ml of 10,000 PPM FAS, stirred.
2. 400 grams PID added, conditioned for 15 minutes, carbonated to pH 9.0 at 1100 RPM, added 20.0 PPT
emulsion, carbonated on to pH 6.5.
3. Continued carbonation for 15 minutes, stopped and checked slurry, continued carbonation for 15 more
minutes, floated 5 minutes.
4. Recleaned RC for 5 minutes.
Log
Number
FEED
690751
690750
690749
Fraction
RT
or
CT
CC
Wt.
Rec.
Cms
400.0
269.0
187 0
127.0
60.0
L.O.I.
1.03
14.35
71 AQ
21.79
28.07
Ignited
Residue
Cms.
395.88
230.39
1 A1 f)Q
99.33
43.76
Percent
CaO
29.79
23.36
1ft 7fi
35.66
45.81
Percent
Floated
57.59
IS 77
24.83
10.94
Percent
CaO Rec.
45.16
29.72
16.82
Ratio I
of *
Enrich-
ment
0.78
1 in
1.20
-------
TABLE 20A
EMULSION FLOTATION TEST NO. 119 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20.0 PPT 10,000 PPM FAS added, stirred.
2. AOO grains PID added, conditlned for 15 minutes, carbonated to pH 6.5, 10.0 PPT
emulsion added, conditioned for 3.5 minutes, floated 4 minutes.
3. Recleaned RC twice and each tall fraction separately.
A. RT recarbonated back to pH 6.5 before floated, emulsion split proportionately, floated and recleaned twice,
Log
Number
FEED
690757
690758
690759
__
_____
690753
690754
__-.__
690752
. —
690755
690756
wt.
Rec.
Fraction Cms.
RT
TT-i
. TCj^
TT2
TC~
RCZ
CTi
CC
CT
CCi
cc2
CT7
CC
CT
cc2
CTi
of
of CTl
of C1i
of CT2
of CT2
, CC of
, CC
CT2, TC
400.0
346.0
244.0
102.0
61.5
40.5
10.7
55.5
20.5
35.0
51.5
19.5
32.0
16.5
15.5
97.0
0
JL
L.O
1
15
12
21
16
28
25
22
28
19
28
32
25
28
22
29
.1.
.03
.16
.57
.36
.97
.01
.48
.98
.15
.93
.18
.42
.60
.58
.41
.03
Ignited
Residue
Cms.
395.88
293.55
213.33
80.22
51.06
29.16
79.74
42.75
14.73
28.02
36.99
13.18
23.81
11.78
12.03
68.85
Percent
CaO
29.79
25.42
21.53
35.79
28.48
48.61
44.83
40.29
52.37
33.95
50.07
60.03
44.55
51.45
37.72
52.10
Percent
Floated
73.38
53.33
20.05
12.76
7.29
19.93
10.68
3.68
7.00
9.24
3.29
5.95
2.94
3.00
17.21
Percent
CaO Rec.
62
38
24
12
11
29
14
6
7
15
6
8
5
3
30
.63
.54
.09
.20
.89
.37
.45
.47
.98
.52
.63
.89
.09
.80
.10
Ratio
of
Enrich-
ment
0.85
0.72
1.20
0.96
1.63
1.50
1.35
1.76
1.14
1.68
2.02
1.50
1.73
1.27
1.75
-------
TABLE 21A
AGGLOMERATE FLOTATION TEST NO. 120 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 20.0 PPT 10,000 PPM FAS added, stirred.
2. 400 grams PID added, conditioned for 15 minutes, carbonated to pH 6.5 and allowed to come back to
pH 9.0. Then 10.0 PPT emulsion added, condtioned for 3.5 minutes, floated 4 minutes.
3. Recleaned RC twice and end tail fraction separately.
4. RT recarbonated back to pH 6.5 and 5 PPT emulsion added, floated and recleaned twice.
Lop,
Number
690761
690762
690760
Fraction
Feed
RC
CT,
CC of CT.
CT of CTj
cc
690763
690764
690765
690766
690767
CT2
CC of CT2
CT of CT2
RT
TT
TC,
TT2
TC0
CC2,CC of CTj
CC of CT2,TC2
Wt.
Rec.
Cms.
400
131.0
81.0
27.0
54.0
50.0
32.0
18.0
7.0
11.0
324.0
205.0
119.0
70.0
49.0
115.0
L.O.I.
1.03
24.26
22.20
23.05
21.77
27.58
28.02
26.78
26.77
26.82
15.09
12.74
19.12
16.63
22.66
24.45
Ignited
Residue
Cms.
395.88
99.23
63.02
20.78
42.24
36.21
23.03
13.18
5.13
8.05
275.13
178.88
96.25
58.35
37.90
86.84
Percent
CaO
29.79
40.45
37.32
39.22
36.39
45.90
47.91
42.39
42.88
42.09
25.80
23.02
30.98
27.30
36.67
40.62
Percent
Floated
24.80
15.75
5.19
10.56
9.05
5.75
3.29
1.28
2.01
68.78
44.72
24.06
14.58
9.47
21.71
Percent
CaO
_____
33.65
19.72
6.83
12.89
13.93
9.25
4.68
1.84
2.84
59.57
34.55
25.02
13.36
11.66
29.58
Ratio
of
Enrich-
ment (Jo
i
____
1.36
1.25
1.32
1.22
1.54
1.61
1.42
1.44
1.41
0.86
0.77
1.04
0.92
1.23
-------
TABLE 22A
EMULSION FLOTATION TEST NO. 121 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 1.0 PPT 10,000 PPM FAS added, stirred.
2. 400 grams PID flyash added, conditioned for one hour at 1700 RPM, carbonated to pH 6.5, 5.0 PPT
emulsion added, conditioned for 3.5 minutes at 1900 RPM.
3. Rougher separation at 1900 RPM for 4 minutes, recleaned RC & CC^ for 2 minutes.
4. Combined RT, CT^ f. CT2 and repeated Step 3-3 times.
Lop,
Nttmber
FEED
Fraction
Wt.
Rec.
Cms.
400.0
L.O.I.
1.03
Ignited
Residue Percent
Oms. CaO
Percent Percent
Floated CaO Rec.
Ratio
of
Enrich-
ment
395.88
29.79
i
oo
TEST ABORTED
-------
TABLE 23A
AGGLOMERATE FLOTATION TEST NO. 122 LIMESTONE WET COLLECTED KPL
1. 2150 ml KPL slurry rfdded to flotation cell, 12 ml of FAS added, conditioned for 15 minutes.
2. Carbonated to pH 7. A at 2400 RPM, 10 PPT emulsion added, floated A minutes, RC recleaned twice.
3. CT, recleaned with additional 2.5 PPT emulsion for 2 minutes.
A. RT recleaned twice after recarbonation to pH 7.A, additional 5.0 PPT emulsion added before float.
Log
Number
690B37
690839
690838
690SAO
6908A2
6908A3
690RA1
Fraction
Feed
RC
CC,
CT2
CC of
CT of
RT
TT
TT2
TC2
CC2, TC2
CC of CT2
wt.
Rec.
Cms.
2A9.2
19.5
5.9
2.0
3.9
13.6
2.5
11.1
229.7
203.9
25.8
20. A
5. A
13.8
L.O.I.
15.03
15.60
16.62
15.10
1A.78
15. 9A
1A.A7
9.33
8.93
12. Al
11.62
15.33
15.58
Ignited
Residue
Cms.
••••••••
16.57
A. 98
1.67
3.31
11.59
2.10
9.A9
208.29
185.69
22.60
18.03
A. 57
11.65
Percent
CaO
27.13
37.25
38. A6
A0.03
37.67
36. 7A
38. A6
36.36
27.27
26.69
32.09
30.85
37.02
37.89
Percent
Floated
7.36
2.21
0.7A
1.A7
5.15
0.93
A. 22
92.63
82.58
10.05
8.01
2.03
5.18
Percent
CaO
9.12
2.83
0.98
1.8A
6.29
1.19
5.10
8A.01
73.30
10.72
8.22
2.50
6.52
Ratio
of i
Enrich- oo
ment
1.37
1.A2
1.A8
1.39
1.35
1.A2
1.3A
1.01
0.98
1.18
1.14
1.36
-------
TABLE 24A
AGGLOMERATE FLOTATION TEST NO. 123 DOLOMITE MODIFIED WET COLLECTED SLD
1. 2150 ml SLD slurry added to flotation cell, 6.35 ml FAS added, conditioned for 15 minutes.
2. Carbonated to pH 6.8 at 2400 RPM, 10 PPT emulsion added, floated 4 minutes, RC recleaned twice.
3. CT, recleaned with additional 2.5 PPT emulsion for 2 minutes.
4. RT recleaned twice after recarbonation to pH 6.8, additional 5.0 PPT emulsion added before float.
Lop,
Number
690844
690R46
690R45
690R47
690849
600850
690848
Fraction
Feed
RC
cc2
CT2
CC of CTX
CT of CT!
RT
TT1
TC1
TTi
TC2
c:r2,TC2
(/: of CT2
Wt.
Rec.
Gms.
153.8
31.3
16.0
6.2
9.R
15.3
3.4
11.9
122.5
80.?
31). 3
15.0
18.3
27.0
L.O.I.
11.25
11.57
12.20
11.09
10.92
11.54
10.74
10.45
10.04
11.54
11.02
11.07
11.08
Ignited
Residue
Gms.
27.78
14.15
5.44
8.71
13.63
3.01
10.62
109.70
80.24
29.46
13.35
16.1.1
24.56
Percent
CaO
19.60
22.19
23.14
24.20
22.49
21.21
24.07
20.39
18.61
16.08
23.05
20.82
24.0()
24.64
Percent
Floated
18.06
9.20
3.53
5.66
8.86
1.95
6.00
71.32
52.17
19.1 5
8.6R
10.47
15. Of-
Percent
CaO
««•••»
20.43
10.85
4.36
1.49
9.58
2.40
7.18
67.71
45.19
22.52
9.22
13.30
20.07
Ratio
of
Enrich-
ment
••••••^
1.13
1.13
1.23
1.14
1.03
1.22
1.04
0.95
0.86
1.17
1.06
1.27
-------
TABLE 25A
EMULSION FLOTATION TEST NO. 124 LIMESTONE MODIFIED FLYASH KPL
1. KPL Slurry added to flotation cell, 4 PPT of 10,000 PPM Na2S added.
2. 1 PPT Duomac T added, 1 drop A65 Frother added.
3. Floated 3 minutes.
4. Recleaned concentrate for 3 minutes with additional 1 PPT Duomac T and 1 drop A65 Frother.
Log
Number
FEED
700071
700072
700073
Fraction
RC
RT
Wt.
Rec.
Cms.
400.0
2.9
14.0
7.3
L.O.I.
1.03
12.45
6.18
10.15
Ignited
Residue
Cms.
395.88
2.539
13.135
6.56
Percent
CaO
29.79
47.68
32.81
28.35
Percent Percent
Floated CaO Rec.
11.38 18.43
58.90 65.65
29.42 28.33
Ratio
of
Enrich-
ment
i
vo
-------
TABLE 26A
AGGLOMERATE FLOTATION TEST NO. 125 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 1.0 PPT FAR added, then 400 grams PID
2. Preconditioned for 1.0 hour at 1700 RPM
3. Carbonated to 6.1 at 2400 RPM.
4. 5.0 PPT Emulsion added, conditioned for 3 1/2 min., rougher separation 4 min., held at 1700 RPM.
5. Recleaned RC for 2 min., remixed tail cleaner products with RT, repeated step 4 three times.
Lop,
Number Fraction
FEED
700120 CCi
700121 CC2
700122 CC3
700123 CC^
700124 CT4
700125 RT
1. 1.] , lA.T,
wt.
Rec.
Cms.
400.0
34.0
55.0
49.5
100.2
73.2
13.30
OTU T
L.O.I.
1.03
30.18
29.53
27.63
20.47
13.06
8.87.
'>*! 97
Ignited
Residue
Gms.
395.88
23.74
38.76
35.82
79.69
63.64
121.27
i 7H m
J. / o . 1 J JL
Percent
CaO
29.79
48.75
45.72
42.82
32.03
20.04
14.13
J" . **!
Percent
Floated
5.93
9.69
8.95
19.92
15.91
30.31
*•'» . .)H
Percent
CaO Rec.
9.71
14.87
12.87
21.42
10.70
14.38
JO . O /
Ratio
of i
Enrich- 7
ment
1.64
1.53
1.44
1.08
0.67
0.47
-------
TABLE 27A
AGGLOMERATE FLOTATION TEST NO. 126 LIMESTONE MODIFIED FLYASH PID
1. 2000 ml H20 added to flotation cell, 1.0 PPT FAS added, then 400 grams PID.
2. Preconditioned for 1.0 hour at 1700 RPM.
3. Carbonated to 6.1 at 2400 RPM.
4. 10 PPT Emulsion added, conditioned for 3 1/2 min., rougher separation 4 min., held at 1700 RPM.
5. Recleaned RC for 2 min., remixed cleaner tail products with RT, add 5.0 PPT emulsion and
repeated step 4 two times.
Log
Number
FEED
700140
700141
700142
700143
700144
Fraction
CC1
cc2
cc3
CT3
RT
cclf cc2,
CC3
wt.
Rec.
Cms.
400.0
27.2
21.0
23.4
50.2
319.3
71.6
L.O.I.
1.03
26.77
27.31
28.57
19.79
15.86
27.35
Ignited
Residue
Cms.
395.88
19.92
15.26
16.71
40.27
268.66
51.89
Percent
CaO
29.79
44.19
43.31
45.94
30.71
22.05
44.49
Percent
Floated
4.98
3.81
4.17
10.06
67.16
12.97
Percent
CaO Rec.
-
7.38
5.54
6.44
10.37
49.71
19.37
Ratio
of
Enrich-
ment
1.48
1.45
1.54
1.01
0.74
1.49
i
VO
Is}
1
-------
TABLE 28A
AGGLOMERATE FLOTATION TEST NO. 127 LIMESTONE MODIFIED FLYASH PID
1. 400 grams of PID flyash and 100 grams of 1^0 were attritionally scrubbed for three hours at
2000 RPM.
2. Removed to flotation cell, 1900 ml H20 added, 1 PPT FAS modifier added and conditioned for 1 hr.
3. Carbonated to pH 6.4, emulsion added at rate of 10 PPT, conditioned for 2 hrs.
4. Floated with C02 for 6 min.
5. Concentrate reconditioned for 45 minutes after addition of 5 PPT emulsion.
6. Recleaned with air for 5 min.
Lop
Number
FF.KD
700145
700146
700147
Fraction
CC
CI-
RC
PT
Wt.
Rec.
Cms.
400.0
89.2
189.3
278.:,
138.3
L.O.I.
1.03
26.13
16.70
19.72
16.00
Ignited
Residue
Gms.
395.88
65.89
157.69
223.58
116.34
Percent
CaO
29.79
36.40
24.94
28.31
24.68
Percent
Floated
16.47
39.42
55.K"
29.08
Percent
CaO Roc.
20.12
33.00
53.13
24. OQ
Ratio
of
E nrich-
mpi.t
1.22
0.84
0.95
0.33
I
-------
-94-
APPENDIX B
-------
-95-
FIGURE IB
THE CHANGE IN ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
WITH pH OF CONCENTRATED AND DILUTE SLURRIES OF MODIFIED
FLYASH SAMPLE PID (St. Clair, Mich.)
(Sample Filtered)
50
30
o 10
I
o
«
N o
-10
-20
-30
-40
-O
337. SI
1% Slu
urry PID
rrv PID
V
y
•t "
O
x
u
o
75
o
U
*
y
6.0
7.0
8.0
9.0
10.0
11.0
120
13.0
-------
-96-
FIGURE 2B
THE EFFECT OF pH ON THE ZETA POTENTIAL AND SPECIFIC CONDUCT-
ANCE OF 33 PERCENT SLURRIES OF MODIFIED FLYASH PID AND THE
COAL ASH CONSTITUENTS OF PID (UNMODIFIED FLYASH DEI) IN A
LIQUOR CONTAINING THE SOLUBLE CONSTITUENTS OF PID
C) 33% Slurry DEI
-40
10.0
11.0
12.0
13.0
-------
FIGURE 3B
THE CHANGE IN ZETA POTENTIAL AND SPECIFIC
CONDUCTANCE WITH CHANGES IN THE pH
OF CONCENTRATED AND DILUTE SLURRIES
OF UNMODIFIED FLYASH SAMPLE DEI
(St. Clalr, Mich.)
(Sample Filtered)
50
40
30
20
10
a
-10
-20
-30
-4O
6.0
O--
337. Slurry
O O 17. Slurry
7.0
8.0
9.0 10.0
pH
11.0
12.0
J.5
s
L 1
j.o «
b
1.5 S
§
2. OS
I
1.5
1.0
0.5
-------
FIGURE 4B
THE CHANGE IN ZETA POTENTIAL AND SPECIFIC
CONDUCTANCE WITH CHANGES IN THE pH
OF CONCENTRATED AND DILUTE SLURRIES
OF LIMESTONE MODIFIED FLYASH SAMPLE PID
(St. Clair, Mich.)
(Sample Filtered)
50
40
30
20
-10
-20
-30
-40
-o
-L\ 337. Slirry
7o Sluiry
8
12 .2
no s
16
14
o
^>
o
•o
o
o
V)
6.0
7.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
FIGURE 5B
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
WITH CHANGES IN pH OF LIMESTONE MODIFIED
FLYASH PID (St. Clalr, Mich.), THE COAL ASH
CONSTITUENTS OF PID AND THE LIME CONSTITUENTS
OF PID IN LIQUORS CONTAINING THE SOLUBLE
CONSTITUENTS OF PID
-40
7.0
8.0
90
IO.O
11.0
12.0
130
-------
FIGURE 6B
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
WITH CHANGES IN pH OF LIMESTONE MODIFIED
FLYASH D1D2 (TVA), THE COAL ASH CONSTITUENTS
OF D1D2 AND THE LIME CONSTITUENTS OF D1D2
IN LIQUORS CONTAINING THE SOLUBLE CONSTITUENTS
OF D1D2
50
40
-40
6.0
7.0
8.0
9.0
10.0
12.0
13.0
-------
-101-
FIGURE 7B
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
WITH CHANGES IN pH OF LIMESTONE MODIFIED FLYASH
D1D3 (TVA), THE COAL ASH CONSTITUENTS OF D1D3 AND THE
LIME CONSTITUENTS OF D1D3 IN LIQUORS CONTAINING
THE SOLUBLE CONSTITUENTS OF D1D3
-4O
-------
FIGURE 8B
THE EFFECT OF DILUTION TO OBTAIN THE TRUE VALUES FOR
THE ZETA POTENTIAL, SPECIFIC CONDUCTANCE AND pH OF 33
PERCENT SLURRIES OF MODIFIED FLYASH SAMPLE PID
o
-------
FIGURE 9B
THE EFFECT OF DILUTION TO OBTAIN THE TRUE VALUES FOR
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF
33 PERCENT SLURRIES OF MODIFIED FLYASH SAMPLE PID
(St. Clalr. Mich.)
1:512
1:256
1:128
1:64
-------
FIGURE 10B
THE EFFECT OF DILUTION TO OBTAIN THE TRUE VALUES KOR
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF
33 PERCENT SLURRIES OF MODIFIED FLYASH SAMPLE PID
30
20
at pH
10
eg
O
•i
o
u
T4
32
n
i
W
s
OK
H
u:
t-o
-10
01
u
«o
4-1
U
3
•o
o
u
-------
FIGURE IIB
30
20
10
-T 0
c
01
2 -10
41
-20
-30
-G
1:512
THE EFFECT OF DILUTION TO OBTAIN THE TRUE VALUES FOR
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF
33 PERCENT SLURRIJJj? OF^M^DIFjJ^FLYASH SAMPLE PID
t \ Zeta Pott ntlal
) Specific
3c
1:256
at pH
Conductance
1:128
1:64
1:32
1:16
1:8
i
o
H
U
en
o
c' V1
o
3
T3
'I
a.
1:2
0
-------
FIGURE 12B
30
THE EFFECT OF DILUTION TO OBTAIN THE TRUE VALUES FOR
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF
33 PERCENT SLURRIES OF MODIFIED FLYASH SAMPLE PID
<•<;«• rtm
20
at pH
10
O
•i
o
l-t
o
CO
k
X
V
y
g
JJ
u
J
o
c
01
£
N
O
a>
u
a/
a.
-20
Zeta Potential
) Specific
Conductanc
-30
1 : 512
_
1 :256 " "" 1 : f28~
1:64
1:32
1:16
1:8
1:4
1:2
-------
FIGURE 13B
THE EFFECT OF DILUTION TO OBTAIN THE TRUE VALUES FOR
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF
33 PERCENT SLURRIES OF MODIFIED FLYASH SAMPLE PID
-J— MJ.-V \
30
20
at pH
10
o
•§
o
o
*4
I
o
o
0*
-10
u
•I
V)
-20
Zeta P<
) Specif
tentlal
c Conductan
-30
1:512
1:256
1:128
1:64
1:32
1:16
1:8
1:4
1:2
-------
30
FIGURE 14B
THE EFFECT OF DILUTION TO OBTAIN THE TRUE VALUES FOR
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF
33 PERCENT SLURRIES OF MODIFIED FLYASH SAMPLE PID
(St. Clalr, Mich.)
at rtl 11
20
10
M
O
•l-l
en
i
o
c
91
O
a.
-10
o
g
u
u
•1
o
u
01
-20
Zeta Po
-O Spec Ifi
ential
Conductanc
-30
1:512
1:256
Y-
1:128
1:64
1:32
1:16
1:8
1:2
-------
-109-
FIGURE 15|
THE EFFECT ON THE ffiTA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE FID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 4 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM POTASSIUM SULFATE TO A
33 PERCENT SLURRY CONCENTRATION
-40
13.0
-------
-110-
FIGURE 16B
THE EFFECT OM THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 2 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM POTASSIUM SULFATE TO A
33 PERCENT SLURRY CONCENTRATION
20
-------
FIGURE 17B
THE EFFECT Cfl THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1 POUND PER TON OF TRIVALENT ALUMINUM AS ALUMINUM POTASSIUM SULFATE TO A
33 PERCENT SLURRY CONCENTRATION
Percent
ffl Lime
Coal Ash
-40
-------
-112-
FIGURE 18B
THE EFFECT OH THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.6 POUND PER TON OF TRIVALENT ALUMINUM AS ALUMINUM POTASSIUM SULFATE TO A
33 PERCENT SLURRY CONCENTRATION
50
40
30
e 10
-10
-20
-40
4A Percen
Lime
Modified flyash
Fraction
Coal Aih Fraction
6.0
7.0 8.0 9.0 10.0 11.0
PH
12.0
20
16
16
8
14 5
A "
b
I? o
I
o
a
•o
o
O
105
I
8
13.0
-------
-113-
FIGURE 19B
THE EFFECT OR THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.2 POUND PER TON OF TRIVALENT ALUMINUM AS ALUMINUM POTASSIUM SULFATE TO A
33 PERCENT SLURRY CONCENTRATION
50
40
10
-10
-20
-30
-40
n
o
-CD
6.0
7.0
e.o
1*
9.0
Parert Modified
Lime Fraction
-Co**
Flyash
20
18
16
14 u
b
12 §
o
§
u
o
(O
8
10.0
11.0
12.0
I3X)
-------
FIGURE 20B
THE EFFECT OF THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 4 POUNDS PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE
TO A 33 PERCENT SLURRY CONCENTRATION
Parent hodifled
Lime Fraction
-40
12.0
13.0
-------
FIGURE 2IB
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 2 POUNDS PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE
TO A 33 PERCENT SLURRY CONCENTRATION
Lime Traction
Coal ; sh Fractioi
-40
-------
-lib-
FIGURE 22B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS BY
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1 POUND PER TON OF DIVALENT SULFUR AS A SODIUM SULFIDE
-------
-117-
FIGURE 23B
THE EFFECT ON THE ZE'A POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.6 POUNDS PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE
TO A 33 PERCENT SLURRY CONCENTRATION.
20
-4O
-------
-118-
FIGURE 24B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.2 POUNDS PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE
TO A 33 PERCENT SLURRY CONCENTRATION
20
I
-------
-119-
FIGURE 25B
THE EFFECT
o
14 u
i.
M
9
o
•o
8
6.0
7.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
-120-
FIGURE 26B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF A POUNDS PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
-40
10.0
11.0
12.0
13.0
-------
-121-
FIGURE 27B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 2 POUNDS PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
50
40
30
20
e 10
-10
-20
-40
6.0
Pan nt Modifle
Coa Ash Fract
J Flyash
Ion
7.0
8.0
9.0
10.0
11.0
20
18
16
o
o
14 o
b
12 §
o
^
o
•o
§
o
105
'o
X
8
12.0
13.0
-------
-122-
FIGURE 28B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1 POUND PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
50
-40
10.0
11.0
12.0
13.0
-------
-123-
FIGURE 29B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.6 POUNDS PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
-40
-------
-124-
FIGURE 30B
THE EFFECT OB THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.2 POUNDS PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
50
30
-40
-------
-125-
FIGURE 31B
THE EFFECT ON THE 2ETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE HODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1 POUND PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATK TO A 16.6
PERCENT SLURRY CONCENTRATION
50
Modified
i Fraction
-40
12.0
J 2
13.0
-------
-IZ6-
FIGURE 32B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1 POUND PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATE TO A 8.3
PERCENT SLURRY CONCENTRATION
50
40
Modified Flj
Fraction
11.0
12.0
13.0
-------
FIGURE 33B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 4 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
50
40
Modified ;
sh Fractioi
-40
-------
-128-
FIGURE 34B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 2 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
-40
11.0
12.0
I3O
-------
-129-
FIGURE 35B
THE EFFECT ON THE 2ETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1 POUND PER TON OF TRIVALENT ALUMINUM AS ALUMINUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
50
40
30
.2 I0
-10
-20
,'-50
-40
6.0
Percent
Coal Asl
Modified F
Fraction
yash
7.0
8.0
9.0
10.0
1.0
12.0
16
f2!
20
16
8
u
SL
8
I3X)
-------
FIGURE 36B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.6 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
t Modified ?lyash
-40
7.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
-131-
FIGURE 37B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.2 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM SULFATE TO A 33
PERCENT SLURRY CONCENTRATION
50
40
e 10
I
o
N 0
-10
-20
-30
-40
6.0
Parent Modified Flyash
Coal Ash Fraction
20
IB
16
I4o
f>
b
12
u
1
u
u
»•
u
10
8
7.0
8.0
10.0
11.0
12.0
13.0
-------
-132-
FIGURE 38B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.6 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM SULFATE TO A 16.6
PERCENT SLURRY CONCENTRATION
20
16
Coal Ash Fraction
-40
10.0
11.0
12.0
13.0
-------
-133-
FIGURE 39B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.6 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM SULFATE TO A 8.3
PERCENT SLURRY CONCENTRATION
50
40
.2 I0
I
o
-10
-20
-30
-40
O Coal Ash
Parent Modified Fly ish
Fraction
9.0
10.0
11.0
12.0
20
IB
16
14 u
i.
o
x
12
O
u
^
§
U
10.H
1
—I 2
13.0
-------
-134-
FIGURE 40B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
OF THE CONSTITUENTS OF LIMESTONE MODIFIED FLYASH SAMPLE PID
AT VARIOUS LEVELS OF pH AFTER THE ADDITION OF 0.2 POUNDS PER TON
OF TRIVALENT IRON AS FERRIC CHLORIDE
TO A 33 PERCENT SLURRY CONCENTRATION
50
40
30
20
o 10
-10
-20
-30
-40
-n
Parent
Q Coal Ash
Modified Flyash
Constituents
Lime Constituents
20
ie
16
w
O
14 5
n
b
12
o
o
"o
•o
o
u
10.2
'5
£
to
8
7.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
-1J3-
FIGURE 41B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
OF THE CONSTITUENTS OF LIMESTONE MODIFIED FLYASH SAMPLE PID
AT VARIOUS LEVELS OF pH AFTER THE ADDITION OF 0.4 POUNDS PER TON
P,F TRIVALENT IRON AS FERRIC CHLORIDE
TO A 33 PERCENT SLURRY CONCENTRATION
O Coal As
(] Lime Co
-40
13.0
-------
-136-
FIGURE 42B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
OF THE CONSTITUENTS OF LIMESTONE MODIFIED FLYASH SAMPLE PID
AT VARIOUS LEVELS OF pH AFTER THE ADDITION OF 0.6 POUNDS PER TON
OF TRIVALENT IRON AS FERRIC CHLORIDE
TO A 33 PERCENT SLURRY CONCENTRATION
Parent Modified Fl
Coal As
Lime Constituents
I
-40
11.0
12.0
I3O
-------
-137-
FIGURE A3B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE
OF THE CONSTITUENTS OF LIMESTONE MODIFIED FLYASH SAMPLE PID
AT VARIOUS LEVELS OF pH AFTER THE ADDITION OF 0.8 POUNDS PER TON
OF TRIVALENT IRON AS FERRIC CHLORIDE
TO A 33 PERCENT SLURRY CONCENTRATION
50
40
30
-10
-20
-30
-40
6.0
2*-
(r
Parent
Codified Fljyash
Coal Ash Constituents
Lime Constituents
7.0
8.0
9.0
10.0
11.0
12.0
20
ie
16
14 5
n
O
12
o
o
10 ji
13.0
-------
-138-
FIGURE 4AB
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE O* THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1.0 POUND PER TON OF TRIVALENT IRON AS FfiRRIt CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
50
40
o 10
I
o
«
N 0
-10
-20
-so;
-40
-I]
-C)
Parent
Lime Frj
Coal As}
Codified Flj
ction
Fraction
ash
20
18
16
14 o
H)
b
12 «
o
o
o
o
10-S
6.0
7.0
8.0
9.0
10.0
11.0
12.0
I3X)
-------
-139-
FIGURt; 45B
THE tFFKCT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE U* THE CONSTITUENTS OF
LIMESTONE MuUlFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 2.0 POUNDS PER TON OF TRIVALENT IRON AS FERRIC CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
50
-30
-40
6.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
-140-
FIGURE 46B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 4.0 POUNDS PER TON OF TRIVALENT IRON AS FERRIC CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
' -30
-40
7.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
-141-
FIGURE A7B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 4.0.POUNDS PER TON OP TRIVALENT IRON AS PERRIC CHLORIDE TO A 16.5 PERCENT
SLURRY CONCENTRATION
50
40
10
-40
6.0
7.0
8.0
20
18
16
o
o
14 o
S.
o
o
^
§
o
•O
V)
8
9.0
10.0
12.0
13.0
-------
-142-
FIGURE 48B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 4.0 POUNDS PER TON OF TRIVALENT IRON AS FERRIC CHLORIDE TO A 8.25 PERCENT
SLURRY CONCENTRATION
50
-10
-20
'-30
-40
Asi
Parent Mbdlfied Fly^sh
•[T] Lime Fra
O Coal As
tion
Fraction
6.0
7.0
8.0
-m-
9.0
20
16
16
M
O
f.
O
14 o
5.
m
b
12
o
o
o
10
CO
8
I
10.0
11.0
12.0
13.0
-------
-143-
FIGURE 49B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 4.0 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM CHLORIDE TO A ?3 PERCENT
SLURRY CONCENTRATION
50
40
30
«
N
-10
-20
"-30
-40
Parent
-n
-o
Lime
Coal A
Modified Flyash
FJraction
sh Fraction
6.0
7.0
8.0
9.0
10.0
11.0
I2O
20
18
16
•>
o
14.5
•>
b
12
§
u
10-S
I
V)
13.0
-------
-144-
FIGURE SOB
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 2.0 POUNDS PER TON OF XRIVALENT ALUMINUM AS ALUMINUM CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
20
-------
-145-
FIGURE 5IB
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 1.0 POUND PER TON OF TRIVALENT ALUMINUM AS ALUMINUM CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
50
40
30
10
I
-10
-20
' -30
-40
6.0
{J3 Lime Fraction
Coal Ash
Parent Modified Fljash
Fraction
20
ie
16
•A
O
o
I4.o
"
12
X
«
•o
§
u
10 S
7.0
8.0
9.0 10.0
pH
11.0
12.0
-------
-146-
PIGURE 52B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.8 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
-------
-147-
FIGURE 53B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.4 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
50
40
10
o
t
N
-10
-20
-30
-40
-L\
-n
-o
Parent
Llae Fd
Modified F
action
Coal Ath Fraction
! yash
20
ie
16
12
o
*
«
o
o
o
u
&
CO
6.0
7.0
8.0
9.0 10.0
pH
11.0
12.0
-------
-148-
FIGURE 54B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS OF
LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS LEVELS OF pH AFTER THE ADDITION
OF 0.2 POUNDS PER TON OF TRIVALENT ALUMINUM AS ALUMINUM CHLORIDE TO A 33 PERCENT
SLURRY CONCENTRATION
20
Modified F
Ftaction
h Fraction
-40
7.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
-149-
PIGURE 55B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE
CONSTITUENTS OF LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS
LEVELS OF pH AFTER THE ADDITION OF 0.08 POUNDS PER TON OF
TRIVALENT ALUMINUM AS ALUMINUM CHLORIDE
TO A 33 PERCENT CONCENTRATION
Constituents
Constituents
-40
-------
-150-
FIGURE 56B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE
CONSTITUENTS OF LIMESTONE MODIFIED FLYASH SAMPLE PID AT VARIOUS
LEVELS OF pH AFTER THE ADDITION OF 0.04 POUNDS PER TON OF
TRIVALENT ALUMINUM AS ALUMINUM CHLORIDE
TO A 33 PERCENT CONCENTRATION
Lime Constituents
/ -30
-40
-------
-151-
FIGURE 57B
THE EFFECT OF pH ON THE OTA POTENTIAL AND SPECIFIC CONDUCTANCE OF 16.7 FERCBNT
SLURRIES OF UNMODIFIED CU AND DOLOMITE MODIFIED FLYASHES CI 'AND CU
50
40
30
.2 '0
o
o
»
N 0
-10
-20
-30
-40
6.0
CJ
7.0
-C3
ci
CM
CU
8.0
9.0
10.0
11.0
12.0
20
16
16
14 o
o
K
o
o
o
10 X
I
13.0
-------
-152-
FIGURE 58B
THE EFFECT OF pH ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF A 16.70 PERCENT
SLURRY OF DOLOMITE MODIFIED FLYASH CI AND THE COAL ASH CONSTITUENT OF CI
50
40
30
o 10
I
-10
-20
-50
-40
L
o
Parent
O coal Ash Fraction
Modified FLyash
6.0
7.0
8.0
9.0
10.0
11.0
12.0
20
16
16
I
o
14 o
i.
m
b
12 §
o
^
o
•o
o
o
10.S
I
CO
13.0
-------
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE CONSTITUENTS
OF DOLOMITE MODIFIED FLYASH SAMPLE CI AT VARIOHS LEVELS OF ?K AFTER HIE
ADDITION OF 1.0 POUNDS PER TON OF DIVALENT IRON AS FERBOUS AilHOKIUM SULFATE
AT A 16.7 PEF.CENT SLURRY COMCENT1--ATI011
Modified F
(h Fraction
-40
-------
-154-
FIGURE 60S
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD SAMPLE
OF WET COLLECTED LIMESTONE MODIFIED FLYASH SAMPLE KPL AT VARIOUS LEVELS OF pH
AFTER THE ADDITION OF 1.0 POUND PER TON OF DIVALENT IRON AS FERROUS
AMMONIUM SULFATE AT A 1.0 PERCENT SLURRY CONCENTRATION
50
40
30
o 10
I
o
«
M
-10
-20
-40
6.0
-O
Head KPL
Head KPL
Plus FAS
•p-
7.0
8.0
9.0
10.0
11.0
12.0
16
16
I4.S
"
12
u
•o
o
o
13.0
-------
-155-
FIGURE 6IB
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE WITH CHANGES IN pH OF WET COLLECTED
LIMESTONE MODIFIED FLYASH KPL, THE 3,000 GAUSS MAGNETIC FRACTION OF KPL AND THE
3,000 GAUSS NONMAGNETIC FRACTION OF KPL IN LIQUORS CONTAINING THE SOLUBLE
CONSTITUENTS OF KPL AT A 1.0 PERCENT SLURRY CONCENTRATION
50
,000 Gauss
.000 Gauss
-40
-------
-156-
FIGURE 62B
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE WITH CHANGES IN pH OF WET COLLECTED
LIMESTONE MODIFIED FLYASH KPL, THE 5,500 GAUSS MAGNETIC FRACTION OF KPL AND THE
5,500 GAUSS NONMAGNETIC FRACTION OF KPL IN LIQUORS CONTAINING THE SOLUBLE
CONSTITUENTS OF KPL AT A 1.0 PERCENT SLURPY CONCENTRATION
50
40
,500 Gauss
,500 Gauss
-40
12.0
13.0
I
-------
-157-
FIGURE 63B
THE EFFECT ON THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD SAMPLE
OF WET COLLECTED DOLOMITE MODIFIED FLYASH SAMPLE SLD AT VARIOUS LEVELS OF ?H
AFTER THE ADDITION OF 1.0 POUND PER TON OF DIVALENT IRON AS FERROUS
AMMONIUM SULFATE TO A 2.0 PERCENT SLURRY CONCENTRATION
50
40
-40
-------
-158-
FIGURE 64B
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE WITH CHANGES IN PH
OF WET COLLECTED DOLOMITE MODIFIED FLYASH SLD, 3,000 GAUSS
MAGNETIC FRACTION OF SLD AND THE 3,000 GAUSS NONMAGNETIC FRACTION
OF SLD AT A 2.0 PERCENT SLURRY CONCENTRATION
-40
10.0
11.0
12.0
13.0
-------
-159-
FIGURE 65B
THE ZETA POTENTIAL AND SPECIFIC CONDUCTANCE WITH CHANGES IN pH
OF VET COLLECTED DOLOMITE MODIFIED FLYASH SLD, THE 5,500 GAUSS
MAGNETIC FRACTION OF SLD AND THE 5,500 GAUSS NONMAGNETIC FRACTION
OF SLD AT A 2.0 PERCENT SLURRY CONCENTRATION
Magnetic
Nonmagnetic
-40
-------
-160-
FIGURE 66B
ZETA POTENTIAL AND SPECIFIC CONDUCTANCE WITH CHANGES IN pH OF V/ET COLLECTED
LIMESTONE MODIFIED FLYASH KPL, THE 3,000 MAGNETIC FRACTION AND THE 3,000 GAUSS
NONMAGNETIC FRACTION OF KPL AT A 1.0 PERCENT SLURRY CONCENTRATION
50
40
-40
12.0
I3X)
-------
-161-
FIGURE 67B
w:^T«r;;"T;,^X' r^*" POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, 3,000 GAUSS
MAGNETIC AND 3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED
.«, ™AS i?*™ KPL AT VARIOUS LEVELS °F PH AFTER THE ADDITION OF 2 POUNDS
PER TON OF DIVALENT IRON AS FERROUS AMMONIUM SULFATE AT A 1.0 SLURRY CONCENTRATION
DO
An
•K/
30
20
•»
| >o
1
o
•
N 0
[
(
-10
-zo
t
'' -30£
-An
J ^f
# — ^
^
(
[
> •
ii
if1----
v, J
j •"
] C
> " •
- — ^
— - • — H
^ Head KP1
) KPL Magi
j IT>T Nonr
B
etic
£U
IB
16
s
1
14.0
b
•
12 1
w
%
o
I0g
1
8
g
4
2
6.0
7.0
8.0
9.0 10.0
PH
11.0
12.0
-------
-162-
FIGURE 68B
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, 2,000 GAUSS
MAGNETIC AND 3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED
FLYASH SAMPLE KPL AT VARIOUS LEVELS OF pH AFTER THE ADDITION OF 0.5 POUNDS
PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE AT A 1.0 PERCENT SLURRY CONCENTRATION
50
40
30
20
10
I
N
-10
-20
-40
O
Head KfL
O Magnetic KPL
20
I
18
16
CO
O
I4.S
b
x
12 «
o
u
3
•o
O
u
u
&
in
6.0
7.0
8.0
9.0
10.0
11.0
12.0
13.0
-------
-163-
FIGURE 69B
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, 3,000 GAUSS
MAGNETIC AND 3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED
FLYASH SAMPLE KPL AT VARIOUS LEVELS OF pH AFTER THE ADDITION OF 1 POUND
PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE AT A 1.0 PERCENT SLURRY CONCENTRATION
90
40
30
20
e 10
-10'
-20
-30
-40
Head KP
-------
-iu4-
FIGURE 70B
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, 3,000 GAUSS
MAGNETIC AND 3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED
FLYASH SAMPLE KPL AT VARIOUS LEVELS OF PH AFTER THE ADDITION OF 2 POUNDS
PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE AT A 1.0 PERCENT SLURRY CONCENTRATION
50
40
30
20
-10
-20
-30
-40
Head KP|L
<£) KPL Magnetic
KPL Nonmagnetic
6.0
7.0
8.0
9.0
10.0
11.0
12.0
20
te
16
to
O
-C
O
14
12
o
3
•o
O
O
10
cn
13.0
-------
-165-
FIGURE 7IB
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, 3,000 GAUSS
MAGNETIC AND 3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED
FLYASH SAMPLE KPL AT VARIOUS LEVELS OF pH AFTER THE ADDITION OF 4 POUNDS
PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE AT A 1.0 PERCENT SLURRY CONCENTRATION
50
40
-40
-------
-166-
FIGURE 72B
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, 3,000 GAUSS
MAGNETIC AND 3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED
FLYASH SAMPLE KPL AT VARIOUS LEVELS OF pH AFTER THE ADDITIO*' OF 10 POUNDS
PER TON OF DIVALENT SULFUR AS SODIUM SULFIDE AT A 1.0 PERCENT SLURRY CONCENTRATION
90
40
30
20
o
•
-10
-20
-30
-40
KPL Nonmagnetic
20
16
16
8
|4.o
« "
b
,2
8
^
u
•o
8
6.0
7.0
8.0
9.0
10.0
11.0
12.0
13.0"
-------
-167-
FIGURK 7?B
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, 3,000 GAUSS MAGNETIC AND
3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED FLYASH SAMPLE KPL AT
VARIOUS LEVELS OF pH AFTER THE ADDITION OF 1 POUND PER TON TO TRIVALENT ALUMINUM
AS ALUMINUM POTASSIUM SULFATE AT A 1.0 PERCENT SLURRY CONCENTRATION
50
40
-40
12.0
130
-------
-168-
FIGURE MB
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, :,000 GAUSS MAGNETIC AND
3,000 GAUSS NONMAGNETIC SAMPLES OF WET COLLECTED LIMESTONE MODIFIED FLYASH SAMPLE KPL AT
VARIOUS LEVELS OF pH AFTER THE ADDITION OF 1 POUND PER TON OF THE PHOSPHATE RADICAL
AS PHOSPHORIC ACID AT A 1.0 PERCENT SLURRY CONCENTRATION
50
40
HPad KPL
KPL Magnetic
KPL Nonmagnetic
-40
12.0
-------
-169-
FIGURE 75B
THE EFFECT ON ZETA POTENTIAL AND SPECIFIC CONDUCTANCE OF THE HEAD, ?,000 GAUSS MAGNETIC AND
3 000 GAUSS NONMAGNETIC SAMPLES OF WFT COLLECTED LIMESTONE MODIFIED FLYASH SAMPLE KPL AT
VARIOUS LEVELS OF pH AFTER THE ADDITION OF 5 POUNDS PER TON OF STAROT
AT A 1.1 PERCENT SLURRY CONCENTRATION
!
-10
C>
-A
-()
Head
KPL I
KPL I
«
KPL
[agnetic
onmagnetic
IB
16
o
I
. o
at
K
12 °
o
u
•o
s
10.2
I
6.0
7.0
8.0
9.0
10.0
12.0
I3X)
-------
-170-
APPENDIX C
-------
FIGURE 1C
THE EFFECT OF CARBONATION ON THE pH OF 33 PERCENT
SLURRIES OF LIMESTONE MODIFIED FLYASH PID
(St. Cl«lr, Mich.)
14. OL-
-------
u.o
THE EFFECT OF CAKBONATION OH THE pH OF 33 PERCENT
SLUNIIES OF LIMESTONE MODIFIED FLY ASH D1D2
(TVA)
-------
P"
14.0
13.0
12.0
11.0
-.o.oi -
'1.0
8.0
FIGURE 3C
THE EFFECT OF CARBONATION ON THE pH OF 33 PEKCEHT
SLURRIES OF LIKE STOW MODIFIED FLTASH D1D3
(TVA)
•s.o
rj.OJ
V
Final pH 10.8
_^
OJ
7 8
Time (Hours)
10
11
12
-------
14.0
13.0
12.0 _
11.0 I I
10.o;
THE EFFECT OF CARBONATION ON THE pH OF 33 PERCENT
SLURRIES OF DOLOMITE MODIFIED FLYASH DD
(St. Clatr, Mich.)
-------
u.o
13.0
12.0 I 1
11.0
10.0 i - -
FIGURE 5C
THE EFFECT OF CARBONATION ON THE pH OF 33 PERCENT
SLURRIES OF DOLOMITE MODIFIED FLYASH CI
(St. Louis, Mo.)
-------
FIGURE 6C
THE EFFECT OF CARBOHATIOW OH THK pH OF 33 PERCENT
SLURRIES OF DOLOMITE MODIFIED FLY ASH CM
(St. Louie, Mo.)
H
6.0
5.0
il
-------
FIGURE 7C
THE CHANGE IN pH AND CARBON DIOXIDE ABSORPTION OF CI MODIFIED FLYASH.
16.6 PERCENT SLURRY
7.
0.6
o
n
o
3
O
H-
O
cr
CO
O
H
•O
O
0.2 >
0.1
0 100
-------
FIGURE 8C
THE CHANGE IN pH AND CARBON DIOXIDE ABSORPTION OP PID MODIFIED FLYASH,
12.
0.6
11.
0.5
10,
VI
4>
0.4
VI
o
X
O
0.2|
M
ra
o
0.1
20
40
60 80 100
Time, Minutes
120
-------
"r r VTGURF 9C
THE CHANGE IN pH AND CARBON DICT. -D ; . I^.^TION OP CM MODIFIED FLYASH,
- -
12
11
10
9.
„ ,
7.C
0
o
4
n
f — \
'
1 \—
1
1
1
1
1
1
-\
\
\
\
\
1
I
I
\
1
'
/
\ /
\/
(_ — — — —
_*
__ — . _.
^-^_
^^-^
0.6
n ^
U . J
r>
01
cr
o
3
O
0.4 g
Q.
1)
O"
0
H
tj
0*3 rr
• -^ !-•
O
3
H-
rr
D
0.2 >
H-
3
0.1
r,u
30
100 120
, Mlnutps
-------
FIGURK IOC
1?.
11
1C
THE CHANGE IN pH AND CARBON DIOXIDE ABSORPTION OF CM MODIFIED FLYASH,
33 PERCENT SLURRY
\
\
\
\
\
\
40
GO
80
100 120
, Minutes
140
0.6
0.5
0.4
n>
l-l
cr
o
o
H-
O
X
(-••
o.
.-9
tr
co
O
H
•o
).3 .'
oo
-------
-181-
APPENDIX D
-------
FIGURB ID
THERMALGRAVIMETRIC ANALYSIS OF CALCIUM CARBONATE
11200
1100
1000
900
800
UJ
O
700 o
01
CO
600
ui
u
500
u
UJ
DC
O
4OO
300
200
100
MILLIGRAMS
6
8
9
-------
FIGURE 2D
THERMALGRAVIMETRIC ANALYSIS OF CALCIUM SULFATE
1200
1100
1000
900
800
u
Q
700 o
600
500
M
oc
o
400
300
200
100
MILLIGRAMS
8
9
-------
FIGURK 40
TOfiRMALGHAVIMBTRIC ANALYSIS OF CALCIUM OXIDE
1200
1100
1000
900
800
o
700 5
s
600
500
400
300
200
100
a:
(9
MILLIGRAMS
-------
FIGURE 50
THEHMALGHAVIMUTRIC ANALYSIS OK WKT CGLLWJ'mJ LlMfc^'RJiic, nOOli-'itD KLYASH
KANSAS POWER AND LIGHT CONTAINING 22.84 H-JKCliNT L1MK
1
\o
CO
1
0 3
i
^
\
345678
MILLIGRAMS
s
\
\
\
\
> 1C
1200
1100
1000
900
800
Ul
Q
4
70O o
»-
z
IU
o
600 w
kl
Ul
OC
(9
500 g
400
300
200
100
-------
KlGUKJS 6i>
THERMALGRAVIMETR1C ANALYSIS OK SAMPLE 6905bl fllr.
-------
FIGURE 7D
THERMALGRAVIMBTRIC ANALYSIS OF SAMPLE 690582 THE SC OF TEST 111 CONTAINING
39.72 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
700
0
4
CO
00
600
500
z
u
u
w
UJ
Ui
c
o
400
300
200
100
MILLIGRAMS
6
8
9
-------
KICUKE 8D
THERMALCRAVIMETRIC ANAiA'Slo OF SAMPLE 6905B.» Tils. Vl^ Of iuM' ll!
15.84 PERCENT LIME FHOK A 20 1'PT El-'l-LSION Ai;UITUN :\Aft
11200
1100
1000
900
800
700 o
o\
00
MILLIGRAMS
6
9
600
500
400
300
ZOO
100
z
u
u
in
cc
o
-------
FIGURE 9D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690584 THE TT, OF TEST 111 CONTAINING
19.82 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
1000
-------
FIGURE 10D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690585 THE TC OF TKST 111 CONTAINING
27.39 PERCENT LIME FROM A 20 PPT EMULSION AUDITION RAT*
1200
1100
1000
MILLIGRAMS
6
-------
FIGURE 11D
THERMALGRAVIMBTRIC ANALYSIS OP SAMPLE 700032 THE CC, OF TEST 121 CONTAINING
47.47 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
1000
900
BOO
o
4
700 o
CM
O\
600
500
CO
u
hJ
OC
O
400
300
200
100
MILLIGRAMS
9
-------
FIGURE 120
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 700033 THE CC, OF TEST 121 CONTAINING
43.84 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
IOOO
900
800
UJ
Q
4
700 o
600
z
UJ
u
500
oc
e
400
300
200
100
MILLIGRAMS
6
8
-------
FIGURE 13D
THEKMALGRAVIMETRIC ANALYSIS OF SAMPLE 700034 THE CC6 OF TEST 121 CONTAINING
42.22 PERCENT LIME FROM A 20 PPT EMULSION ADDITION HATE
1200
1100
1000
900
800
700
o
4
u
(A
tr
o
600
500
400
300
200
100
MILLIGRAMS
-------
FIGURE 140
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE ?00035 THE CGo OF TEST 121 CONTAINUC
36.40 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
o
4
700 o
600
ui
o
500
u
UJ
or
o
400
300
200
100
MILLIGRAMS
6
8
-------
FIGURE 15D
THERMALGRAVIMETRIG ANALYSIS OF SAMPLE 700636 THE RTY OF TEST 121 CONTAINING
22.58 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1100
1000
900
800
700
tu
o
z
tu
o
oc
(9
vO
ON
400
300
200
100
MILLIGRAMS
6
8
9
-------
FIGURE 160
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 700037 TOE CT? OF TKST 121 CONTAINING
26.34 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
o
700 ©
V
600
500
400
300
200
100
z
IU
u
in
MILLIGRAMS
6
-------
FIGURE 17D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE ?00038 THE CTQ OF TEST 121 CONTAINING
29.45 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
Ui
o
<
700 5
600
z
u
o
UJ
oc
500
400
300
200
100
MILLIGRAMS
6
8
-------
FIGURE 1KD
THERMALCRAVIMETRIC ANALYSIS OF SAMPLE 690^5? THE CC,. OK TEST y6 CONTAINING
42.26 PERCENT LIME FROM A 60 PPT EMULSION ADDITION HATE
1200
1100
1000
900
800
o
4
700 e
CT>
O\
600
UJ
u
oc
e
400
300
200
100
MILLIGRAMS
8
9
-------
FIGURE 19D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690458 THE SC OF TEST 96 CONTAINING
34.04 PERCENT LIME FROM A 60 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
u
Q
4
700 5
o
o
CM
600
-------
FIGURE
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690459 THE TT, OK TEST 96 CONTAINING
14.09 PERCENT LIME FROM A 60 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
o
-------
FIGURE 2ID
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690461 THE TT? OF TEST 96 CONTAINING
14.09 PERCENT LIME FROM A 60 PPT EMULSION ADDITION RATE
11200
1100
1000
900
1800
o
4
1700 o
-------
FIGURE 22D
THERMALCRAVIMETRIC ANALYSIS OF SAMPLE 690460 THE TC,, OK TEST 96 CONTAINING
22.75 PERCENT LIME FROM A 60 PPT EMULSION ADDITION HATE
1200
1100
IOOO
900
800
o
700 o
o
CM
I
600
in
o
500
u
-------
FIGURE 23D
THERMALGRAVXMBTRIC ANALYSIS OF SAMPLE 690452 CC, OF TEST 95 CONTAINING
11.30 PERCENT LIME FROM A 60 PPT EMULSION ADDITION RATE
11200
1100
1000
900
| 800
1700 5
-a-
o
(600
1500
z
u
u
U)
Ul
Ul
e
(400
I 300
200
100
MLLIWtAMS
-------
FIGURE 24D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690453 THE SC OF TEST 95 CONTAINING
34.43 PERCENT LIME FROM A 60 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
o
700 o»
600
i
IO
o
500
oc
o
400
300
ZOO
MILLIGRAMS
6
8
-------
FIGURE 25D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 6904'34 THE TT OF TEST 95 CONTAINING
32.38 PERCENT LIME FROM A 60 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
UI
o
700 5
>£>
O
CM
I
600
z
ui
o
UI
UI
ac.
500
400
300
200
100
MILLIGRAMS
6
9
-------
THERMALGHAVIMETHIC ANALYSIS OF SAMPLE 690^56 THE TTo OF TEST 95 CONTAINING
32.72 PERCENT LIME FROM A 60 PPT EMULSION ADDITION HATE
1200
1100
1000
900
800
700
o
i
r^
O
600
o
M
500
OC
O
4OO
300
200
100
MILLIGRAMS
6
8
-------
FIGURE 27D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690455 TOE TC? OF TEST 95 CONTAINING
25.^6 PERCENT LIME FROM A 60 PPT EMULSION ADDITION RATE
1200
1100
MILLIGRAMS
6
-------
THERMAlXiKAViMJiTKlC AW Al, I bib UI- SAnrLf. OOJ.UH? inc. i^o^ ur ir.oi /j vA
48.74 PERCENT LIME FROM A 112.6 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
u
o
700 o
o\
o
CM
600
500
u
u
in
u
u
oc
o
400
300
200
100
MILLIGRAMS
6
8
-------
FIGURE 29D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 681051 THE CC3 OF TEST 73 CONTAINING
50.31 PERCENT LIME FROM A 112.6 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
UJ
Q
700 e»
600
z
ui
o
UJ
UJ
DC
500
400
300
200
100
MILLIGRAMS
8
9
-------
FIGURE 30D
THERMALGKAVIMETRIC ANALYSIS OF SAMPLE 690310 'WE CC 0*' YriST 84 CONTA.LN.LKG
51.2? PERCENT LIME FHOM A 112.6 PPT Kl'lULS.lCN AJiUii'lON HATE
1200
1100
1000
900
800
600
500
400
300
200
100
MILLIGRAMS
8
9
-------
FIGURE 3ID
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690308 THE CT, OF TEST 8A CONTAINING
26.82 PERCENT LIME FROM A 112.6 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
u
o
4
700 5
CM
CM
600
Ui
u
kl
X
O
500
400
300
200
100
MILLIGRAMS
6
6
9
-------
FIGURE 320
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690309
THE CT- OF TEST 84 CONTAINING
32.29 PERCENT LIME FROM A 112.6 PPT EMULSION ADDITION RATE
1200
1100
1000
900
BOO
o
700 o
i-
z
ui
u
600 M
ui
UI
§
500 tt
Ol
400
300
200
100
MILLIGRAMS
6
8
-------
-------
FIGURE 34D
THERMALGHAVIMETKIC ANALYSIS OF SAMPLE 6y0312 THE RT OK TEST 84 CO'U'AIHING
20.26 PERCENT LIME FROM A 112.6 PPT EMULSION ADDITION RAJE
1200
1100
1000
9OO
800
hi
O
TOO o
600
CM
I
u
4OO
300
200
100
MILLIGRAMS
-------
FIGURE 35D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690230 TOE CCj OF THE 1st 5 MINUTES
FLOTATION OF TEST 82 CONTAINING 29.93 PERCENT LIME FROM A
1
ft
CM
<
V
^
-y
\
\
\
\
\
. \
IZOO
1100
1000
900
800
UJ
o
700 5
i-
z
u
0
600 w
u
Ul
oc
o
500 g
400
300
200
100
n
I) 12 3456789 10
-------
FIGURE 36D
THERMALCRAVIMETRIC ANALYSIS OF SAMPLE 690232 THE CC OF THE 1st 5 MINUTES
FLOTATION OF TEST 82 CONTAINING 28.18 PERCENT LIME FROM A
1
i-H
«M
(
\
\
V
^\
•^.
A
\
\
\
\
\
\
i<:uu
1100
1000
900
800
U
O
700 o
z
U
U
600 M
bl
b!
oc
0
500 g
400
300
200
too
n
0 12 3456789 10
-------
FIGURE 37D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690234 THE 2nd 5 MINUTES RC FLOTATION
OF TEST 82 CONTAINING 26.30 PERCENT LIME FROM A 112.6 PPT
EMULSION ADDITION RATE
§
u
o
DC
o
»-
z
u
u
(O
u
uj
oc
o
ttt
o
§
§
§
§
MILLIGRAMS
6
8
-------
FIGURE 38D
THERMALGKAVIMETRIG ANALYSIS OF SAMPLE 690363 THE HT OK TEST 85 CONTAINING
19.69 PERCENT LIME FROM A 1*4-0.8 PPT EMULSION ADDITION HATE
1200
1100
1000
900
600
CM
I
600
500
400
300
200
100
MILLIGRAMS
6
8
-------
FIGURE 39D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690366 THE GT-1 OF TEST 85 CONTAINING
30.56 PERCENT LIME FROM A 140.8 PPT EMULSION ADDITION RATE
1
1200
1100
1000
900
800
700
u
o
o
CM
CM
600
U
O
500
UJ
lit
ac
o
400
300
200
100
MILLIGRAMS
6
8
9
-------
FIGURE 40D :
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690364 THE RC OF TEST 85 CONTAINING
51.27 PERCENT LIME PROM A 140.70 PPT EMULSION ADDITION RATE
1200
1100
7
-------
FIGURE 4ID
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690365 THK RC SECOND FRACTION OF
TEST 85 CONTAINING 44.76 PERCENT LIME FROM A 140.70 PPT
EMULSION ADDITION RATE
CM
CM
CM
1
(
-
•
1^_
—
\
\
\
\
\
\
\
~ -
I£UU
1100
1000
900
800
u
o
4
700 o
z
u
u
600 w
UJ
Ul
oe
o
500 g
400
300
200
100
n
3 12 3456769 10
-------
FIGURE 42D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690367 THE 2nd FRACTION CT, 2nd 5
MINUTES OF TEST 85 CONTAINING 26.34 PERCENT LIME FROM A
140.8 PPT EMULSION ADDITION RATE
1100
1000
900
800
O
700 0
CM
CM
600
UJ
U
MILLIGRAMS
6
-------
FIGURE 430
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690368 THE CT-2, 2nd 5 MINUTES OF
TEST 85 CONTAINING 20.44 PERCENT LIME FROM A 140.8 PPT
EMULSION ADDITION RATE
1
CM
CM
1
1
V
9 12 345678
MILLIGRAMS
^
"l
1
1
1
1
* -
IZOO
1100
1000
900
800
UJ
Q
4
700 e>
z
u
u
600 m
UJ
UJ
-------
FIGURE 440
THERMALGRAVIMBTRIC ANALYSIS OF SAMPLE 690369 THE CT,, 1st FRACTION 2nd
MINUTES RC OF TEST 85 CONTAINING 23.80 PERCENT LIME FROM A
1
-------
FIGURE 45D
THERMALGHAVIMETRIG ANALYSIS OF SAMPLE 6903?0 THE CT?, 1st FRACTION 2nd 5
MINUTES RC OF TEST 85 CONTAINING 26.4? PERCENT LIME FROM A
140.8 PPT EMULSION ADDITION RATE
V0
CM
CM
X
•-•^
^
1
"
IZUU
1100
1000
900
800
u
Q
4
700 o
z
u
u
600 M
Ui
u
oc
(9
500 g
400
200
100
n
0 12 3456789 10"
-------
OU UJf" raa'i" 05 UUnTAJ.riJ.HVj £.0*1** rc.nuiMii
140.8 PPT fcWULSION ADDITION HATE
rn\jn n.
[1200
CM
CM
1100
1000
900
800
4OO
300
200
100
MILLIGRAMS
€
8
-------
FIGURE 47D
THERMALGHAVIMETHIG ANALYSIS OF SAMPLE 6903?? Tlib) CC 'jrd, 1st FRACTION 2nd
5 MINUTES RC OF TEST 85 CONTAINING 3^.39 PERCENT LIME FROM A
140.8 PPT EMULSION ADDITION RATE
1200
liOO
1000
900
800
Q
700 o
CO
CM
CM
600
z
u
u
oc
e
500
400
300
200
100
MILLIGRAMS
6
9
-------
FIGURE 48D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690373 THE CT«, 3rd 5 MINUTES RC
OF TEST 85 CONTAINING 19.38 PERCENT LIME FROM A 140.8 PPT
Oi
CM
CM
L
0 12 345678
MILLIGRAMS
\
\
\
\
\
\
9 K
IZOO
1100
1000
900
800
u
o
700 o
i-
z
UJ
O
600 w
UJ
Ul
K
o
500 g
4OO
300
200
100
-------
FIGURE 49D
THERMALGRAVIMETRIG ANALYSIS OF SAMPLE 69037/f THE CT2, 3rd 5 MINUTES RG
OF TEST 85 CONTAINING 18.42 PERCENT LIME FROM A 140.8 PPT
EMULSION ADDITION RATE
11200
1100
1000
900
800
CM
500
400
300
ZOO
100
L
0
MILLIGRAMS
6
8
-------
OF TEST 85 CONTAINING 19.21 PERCENT LIME FROM A 140.8-PPT~
EMULSION ADDITION RATE
I20O
1100
1000
900
800
Q
700 e
u
600
u
ui
500
400
300
ZOO
100
MILLIGRAMS
6
8
-------
FIGURE 510
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690651
THE CC., OF TEST 115 CONTAINING 81.45
1
PI
CM
<
PERCE
NT LIME FRO^
ADDIT1
1 A 20 PPT E>
ON RATE
1ULSION
I
^^~
-^__
"^
-
I£UU
1100
1000
QOO
800
u
o
H1N30
> C
> (
§ 1
EOREES
~— ' Q
4OO
2OO
inn
n
3 12 3456789 10"
-------
FIGURE 52D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 690652 THE SC OF TEST 115 CONTAINING
61.60 PERCENT LIME FROM A 20 PPT EMULSION ADDITION RATE
1200
1100
1000
900
800
u
o
4
700 5
fM
600
500
tu
tu
oc
o
400
300
200
100
IMLLIORAMS
6
a
-------
. FIGURE 53D
THERMALGRAVIMETR1C ANALYSIS OF SAMPLE 6906^3 THE Tf1 OF TEST 115 CONTAINING
32.09 PERGKNT LIME FROM A 20 PPT EMULSION ADDITION KATE
1200
1100
1000
900
800
UJ
o
4
700 5
z
UJ
u
600
500
Ul
u
ff
o
MILLIGRAMS
6
8
9
400
300
200
100
-I 0
-------
FIGURE
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 69065**
THE TT2 OF TEST 115 CONTAINING 2^.35
u-l
mlL'KNT L1MK FROM A 20 WT
EMULSION ADDITION RATE
0 12 345671
MLLIWtAMS
V
X
^X
\
ilZOO
MOO
irwi
Af\f\
I 9 "J fl
i 0 0 C
5 o o C
EGREES CENTIGRADE
400
300
200
100
n
-------
FIGURE 55D
THERMALGRAVIMETKIC ANALYSIS OF SAMPLE 690655 THK TC_ OF TEST 115 CONTAINING
30.10 PERCENT LIME FiiOM A 20 PIT EMULSION ADDITION RATE
vO
0
-
V^
"N
\
-
kWg»^JCDy> — ~~K
i 8 8 8 8 8 | § i
DEGREES CENTIGRADE
\r\e\
OOQ
inn
n
12 3456789 10
-------
FIGURE 56D
THERMALGRAVIMBTRIC ANALYSIS OF SAMPLE 700071 THE RC. OF FROTH FLOTATION TEST
124 CONTAINING 47.68 PERCENT LIME AND 1 PPT OF DUOMAC T. 4 PPT
OF SODIUM SULFIDE MODIFIER AND AEROFROTH 65 FROTHER
1
l
\
\
\
V
IZUU
1100
1000
900
800
UJ
Q
700 5
z
UJ
0
600 w
UJ
u
K
e
500 ^
400
300
200
100
n
0 12 3 4 5 6 7 8 9 10"
-------
FIGURE 57D
THERMALGRAVIMETRIC ANALYSIS OF SAMPLE 700072 THE RC, OF FROTH FLOTATION TEST
124 CONTAINING 32.81 PERCENT LIME AID 1 PPT OF DUOMAC T, 4 PPT
A MODIFIER AND AEROFROTH 65
m
CM
\
\
\
\
..
IZOO
1100
1000
900
800
bJ
O
4
700 o
i-
z
bi
0
600 w
bl
U
OC
0
500 ^
400
500
200
100
n
012 3 4 5 6 7 8 9 10"
-------
FIGURE 58D
THgRMALGRAVDfKTRIC ANALYSIS OP SAMPLE 700073 THE RT OF FROTH FLOTATION TEST
124 CONTAINING 28.35 PERCENT LIME AND 1 PPT OF DUOMAC T 4 PPT,
•
\
\
1
,
\
I2UU
1100
1000
900
800
UJ
Q
4
700 5
z
UJ
u
600 OT
UJ
UJ
DC
O
500 g
400
300
200
100
n
0 1 2 3 4 5 6 7 8 9 - 10,
-------
-240-
APPENDIX E
-------
AST IE
33% WATER PULP (99 gr.) OF D,D3 AGITATED IN WARING BLENDOR FOR 1 MIN.,
ANIONIC EMULSION (50% H^O, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM
ALKYLARYLSULFONATE) ADDED AT A RATE OF 90 PPT, STIRRED FOR 5 MIN.,
POURED INTO 100 MESH SCREEN AND WASHED, H20 SAVED
Log. No.
690008
690009
690010
690011
Wt. Rec.
Cms.
1.2
4.9
68.0
10.3
Grade
Percent
CaO
18.90
19.43
16.37
16.19
Percent
CaO
Rec.
.90
3.81
44.63
6.68
Ratio
of
Enrichment
0.76
0.78
0.66
0.65
Sieve
Size
-325
-200
-100
+100
KJ
Water Analysis
Log No.
690001
690002
690003
690004
690005
Mg.CaO
in H?0
220.08
250.38
216.92
576.91
98.56
Total Cms. CaO
In Solution
1.35
-325
-200
-100
-------
AST 2E
33% WATER PULP (99 gr.) OF DjD-j AGITATED IN WARING BLENDOR FOR 1 MIN.t
ANIONIC EMULSION (50% H20, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM
ALKYLARYLSULFONATE) ADDED AT A RATE OF 90 PPT, STIRRED FOR 5 MIN.,
POURED INTO 100 MESH SCREEN AND WASHED, H20 SAVED,
RHEOSTAT USED TO SLOW STIRRING SPEED
Log No.
Wt. Rec.
Cms.
Grade
Percent
CaO
Percent
CaO
Rec.
Ratio
of
Enrichment
Sieve
Size
690019
690020
690021
7.7
7.7
76.8
16.80
16.24
17.59
5.16
5.01
54.53
0.67
0.65
0.71
+100
-100
-150
N>
I
Water Analysis
Log No.
690016
690017
690018
Mg.CaO
in H20
378.00
226.81
62.44
Total Cms. CaO
In Solution
0.67
+100
-100
-------
AST 3E
33% WATER PULP (99 gr.) OF DjD2 AGITATED IN WARING BLENDOR FOR 1 MIN.,
ANIONIC EMULSION (50% H20, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM
ALKYLARYLSULFONATE) ADDED AT A RATE OF 90 PPT, STIRRED FOR 5 MIN.,
POURED INTO 100 MESH SCREEN AND WASHED, H20 SAVED,
RHEOSTAT USED TO SLOW STIRRING SPEED
Grade Percent Ratio
Wt. Rec. Percent CaO of
Log No. Cms. CaO Rec. Enrichment
690025 4.8 23.80 5.04 1.05 +100
690026 70.7 18.90 58.68 0.83 -150
690027 7.4 17.41 5.70 0.77 -100
Water Analysis
Mg.CaO Total Cms. CaO
Log No. in ^0 In Solution
690022 540.40 +100
690023 1316.00 1.96 - 8.69% -150
-------
AST 4E
33% WATER PULP (99 gr.) OF PID AGITATED IN WARING BLENDOR FOR 2 MIN., AT 6000 RPM.
ANIONIC EMULSION (50% HoO, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM
ALKYLARYLSULFONATE) ADDED AT A RATE OF 90 PPT, STIRRED FOR 5 MIN.,
POURED INTO 100 MESH SCREEN
Log No.
690030
690031
690031
Wt. Rec.
Cms.
19.7
22.5
51.5
Grade
Percent
CaO
26.39
29.49
30.63
Percent
CaO
Rec.
17.34
22.28
52.53
Ratio
of
Enrichment
0.88
0.99
1.02
+150
-150 B.W.*
-150 A.W.*
*B.W. - Before Water Wash
-------
AST 5E
33% WATER PULP (99 gr.) OF PID AGITATED IN WARING BLENDOR FOR 2 MIN., AT 6000 RPM,
ANIONIC EMULSION (50% H20, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM
ALKYLARYLSULFONATE) ADDED AT A RATE OF 90 PPT, STIRRED FOR 5 MIN.,
POURED INTO 150 MESH SCREEN AND WASHED
Grade Percent Ratio
Wt. Rec. Percent CaO of
Log No. Cms. CaO Rec. Enrichment
690061 9.0 23.37 7.19 0.78 +150 £
690062 60.0 30.02 61.69 1.01 -150 B.W. '
-------
AST 6E
33% WATER PULP (99 gr.) OF DjD-, AGITATED IN WARING BLENDOR FOR 2 MIN., AT 6000 RPM,
ANIONIC EMULSION (50% H-0, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM
ALKYLARYLSULFONATE) ADDED AT A RATE OF 90 PPT, STIRRED FOR 5 MIN.,
POURED INTO 150 MESH SCREEN
ISJ
TEST ABORTED
-------
AST 7E
33% WATER PULP (99 gr.) OF DjD2 AGITATED IN WARING BLENDOR FOR 2 MIN., AT 6000 RPM,
ANIONIC EMULSION (50% H20, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM
ALKYLARYLSULFONATE) ADDED AT A RATE OF 90 PPT, STIRRED FOR 5 MIN.,
POURED INTO 150 MESH SCREEN
Log No.
690064
690065
690066
Wt. Rec.
Cms.
75.0
4.0
10.0
Grade
Percent
CaO
26.04
29.97
30.28
Percent
CaO
Rec.
97.31
5.97
15.09
Ratio
of
Enrichment
1.15
1.32
1.34
i
No
+150
-150 B.W.
-------
AST 8E
332 WATER PULP (99 gms.) OF D.D3 AGITATED IN A WARING BLENDOR, 10 DROPS 0.052 CALGON 2AO ADDED,
ANIONIC EMULSION (50% H20, 252 FUEL OIL, 22 1/22 TALL OIL AND 2 1/22 SODIUM ALKYLARYLSULFONATE)
ADDED AT A RATE OF 90 PPT, ROTOR SPEED BETWEEN 3000 AND 7000 RPM
Grade Percent Ratio
Wt. Rec. Percent CaO of
Log No. Cms. CaO Rec. Enrichment
690043 44.0 28.22 49.20 1.25 +150 K>
690044 32.0 32.64 41.62 1.45 -150 B.W. £
-------
AST 9E
33Z WATER PULP (99 gas.) OF DjD3 AGITATED IN A WARING BLENDOR, 10 DROPS 0.05Z CALGON 240 ADDED,
ANIONIC EMULSION (50Z H20, 25Z FUEL OIL, 22 1/2Z TALL OIL AND 2 1/2Z SODIUM ALKYLARYLSULFONATE)
ADDED AT A RATE OF 90 LBS/TON, ROTOR SPEED BETWEEN 3000 AND 7000 RPM
Grade Percent Ratio
Wt. Rec. Percent CaO of
Log No. Cms. CaO Rec. Enrichment
690046 80.0 21.26 75.43 0.94 +150
690047 3.0 23.30 3.10 1.03 -150 B.W.
690048 17.0 20.44 15.38 0.91 -150 A.W.
-------
AST IDE
33% WATER PULP (99 gns.) OF PID AGITATED IN A WARING BLENDOR, 10 DROPS 0.05% CALGON 240 ADDED,
ANIONIC EMULSION (502 H-0, 25% FUEL OIL, 22 1/2% TALL OIL AND 2 1/2% SODIUM ALKYLARYLSULFONATE)
ADDED AT A RATE OF 90 PPT, ROTOR SPEED BETWEEN 3000 AND 7000 RPM
Grade Percent Ratio
Wt. Rec. Percent CaO of
Log No. Cms. CaO Rec. Enrichment
690049 57.0 25.03 45.19 0.84 +150
690050 17.0 28.48 15.32 0.96 -150 B.W.
-------
AST HE
33% WATER PULP (99 gms.) OF PID AGITATED IN A WARING BLENDOR, 10 DROPS 0.05% CALGON 240 ADDED,
ANIONIC EMULSION (50% H20-50% FUEL OIL) ADDED AT A RATE OF 90 PPT, ROTOR SPEED BETWEEN 3000
AND 7000 RPM
Log No.
690055
690056
690057
Wt. Rec.
Cms.
7.0
85.0
15.0
Grade
Percent
CaO
18.38
28.44
27.57
Percent
CaO
Rec.
4.04
75.82
12.98
Ratio
of
Enrichment
0.62
0.95
0.93
+150
-150 B.W.
-150 A.W.
ro
-------
AST 12E
33% WATER PULP (99 gins.) OF PID AGITATED IN A WARING BLENDOR, 10 DROPS 0.05% CALGON 240 ADDED,
EMULSION (50% FUEL OIL-50% TALL OIL) ADDED AT A RATE OF 90 PPT, ROTOR SPEED BETWEEN
3000 and 7000 RPM
Log. No.
690052
690053
690054
Wt. Rec.
Cms.
50.0
6.0
47.0
Grade
Percent
CaO
23.76
30.72
26.03
Percent
CaO
Rec.
38.71
5.99
39.85
Ratio
of
Enrichment
0.80
1.03
0.87
+150
-150 B.W.
-150 A.W.
ro
K>
-------
AST 13E
33% WATER PULP (99 gr.) of PID AGITATED IN A WARING BLENDOR, 10 DROPS OF CONCENTRATED HC1 ADDED,
EMULSION (50% FUEL OIL-50% TALL OIL) ADDED AT A RATE OF 90 PPT, ROTOR SPEED BETWEEN 3000 and 7000 RPM
Grade Percent Ratio
Wt. Rec. Percent CaO of Screen
Log No. Cms. CaO Rec. Enrichment Size
690069 2.0 16.54 0.95 0.56 +150
690070 104.0 28.31 85.19 0.95 -150 B.W. ^
-------
AST 14E
33% WATER PULP (100 gr.) D^- AGITATED IN A WARING BLENDOR, ADDED 10 DROPS OF CONCENTRATED HC1,
ADDED 50% FUEL OIL, 50% TALL OIL EMULSION AT 90 PPT, ROTOR SPEED 6000 RPM
Log No.
690067
690068
690058
Wt. Rec,
Cms.
75.0
5.0
23.0
Grade
Percent
CaO
26.95
34.56
29.27
Percent
CaO
Rec.
87.01
7.44
28.97
Ratio
of
Enrichment
1.20
1.53
1.30
Screen
Size
+150
-150 B.W.
-150 A.W.
i
-------
AST 15E
33% WATER PULP (100 gr.) DjD-, AGITATED IN WARING BLENDOR, ADDED 10 DROPS OF CONCENTRATED HC1,
ADDED 50% FUEL OIL, 50% TALL OIL EMULSION, ROTOR SPEED 6000 RPM
Test Aborted
-------
AST 16E
33% WATER PULP (100 gr.) PID AGITATED IN WARING BLENDOR, ADDED 10 DROPS OF SODIUM SILICATE,
ADDED 50% FUEL OIL, 50% TALL OIL EMULSION, ROTOR SPEED 6000 RPM
Log No.
690091
690092
690093
Wt. Rec.
Cms.
2.0
98.0
12.0
Grade
Percent
CaO
21.84
28.04
27.44
Percent
CaO
Rec.
1.58
97.40
11.24
Ratio
of
Enrichment
0.73
0.94
0.92
+150
-150 B.W.
-------
AST 17E
33% WATER PULP (150 gr.) DjJD, AGITATED IN WARING BLENDOR, 10 DROPS OF SODIUM SILICATE ADDED,
ADDED 50% FUEL OIL, 50% TALL OIL EMULSION, ROTOR SPEED 6000 RPM FOR 3 MIN.
Log No.
690128
690127
Wt. Rec.
Cms.
12.0
141.0
Grade Percent Ratio
Percent CaO of
CaO Rec. Enrichment
Not Submitted for Chemical Analysis
Screen
Size
-f-150
-150 B.W
-------
AST 18E
150 GR. PID AND 50 GR. TALL OIL GROUND IN A BALL MILL, AGITATED IN WARING BLENDOR
AND TAKEN AS MATERIAL FLOATING, STUCK TO SIDES AND THAT IN THE WATER
Grade Percent Ratio
Wt. Rec. Percent CaO of Screen
Log No. Cms. CaO Rec. Enrichment Size ,
to
Oi
690131 0.9 Test Aborted Not Submitted For Chemical Water °°
-------
AST 19E
150 GR. OF PID GROUND IN BALL MILL WITH 1.0 GR. TALL OIL,
TRANSFERRED TO WARING BLENDOR AND AGITATED, FRACTIONS TAKEN WERE THOSE FLOATING,
STUCK ON SIDES OF BALL AND THOSE IN WATER
Grade Percent Ratio
Wt. Rec. Percent CaO of Screen
Log No. Cms. CaO Rec. Enrichment Size
• —— _______ ____
690133 9.1 Test Aborted Not Submitted For Chemical Sides
690134 1.6 Analysis Water
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AST 20E
33Z WATER SLURRY, 100 GR. PID AGITATED IN WARING BLENDOR WITH 3 DROPS TALL OIL,
6000 RPM FOR 3 MIN.
Log No.
690136
690137
690138
Wt. Rec,
Cms.
24.7
3.0
1.7
Grade
Percent
CaO
28.95
70.21
Percent
CaO
Rec.
Ratio
of
Enrichment
0.97
2.35
Screen
Size
Sides
Float
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AST 21E
33Z WATER SLURRY, 100 GR. PID AGITATED IN WARING BLENDOR WITH 6 DROPS TALL OIL,
6000 RPM FOR 3 MIN.
Log No.
690139
690140
Wt. Rec.
Cms.
39.7
1.3
Grade
Percent
CaO
27.35
27.74
Percent
CaO
Rec.
Ratio
of
Enrichment
0.91
0.93
Screen
Size
AST 21 Sides
AST 21 Float
I
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