EPA-650/2-74-025-a
September 1975
APPLICABILITY OF THE MEYERS
PROCESS FOR CHEMICAL
DESULFURIZATION OF COAL:
SURVEY OF THIRTY-FIVE COALS
U.S. Environmental Protection Agency
Office of Research and Development
Washington. O.C. 20460
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EPA-650/2-74-025-0
APPLICABILITY OF THE MEYERS
PROCESS FOR CHEMICAL
DESULFURIZATION OF COAL:
SURVEY OF THIRTY-FIVE COALS
by
J.W. Hamersma andM.L. Kraft
Systems Group of TRW, Inc.
One Space Park
Redondo Beach, California 90278
Contract No. 68-02-0647
ROAP No. 21ADD-096
Program Element No. 1AB013
EPA Project Officer: L. Lorenzi,. Jr.
Industrial Environmental Research Laboratory
Office of Energy, Minerals, and Industry
Research Triangle Park, North Carolina 27711
Prepared for
U.S. ENVIRONMENTAL PROTECTION AGENCY
Office of Research and Development
Washington, D. C. 20460
September 1975
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EPA REVIEW NOTICE
This report has been reviewed by the National Environmental Research Center,
Research Triangle Park, Office of Research and Development, EPA, and ap-
proved for publication. Approval does not signify that the contents neces-
sarily reflect the views and policies of the Environmental Protection Agency,
nor does mention of trade names or commercial products constitute endorse-
ment or recommendation for use.
RESEARCH REPORTING SERIES
Research reports of the Office of Research and Development, U.S. Environ-
mental Protection Agency, have been grouped into series. These broad cate-
gories were established to facilitate further development and application
of environmental technology. Elimination of traditional grouping was con-
sciously planned to foster technology transfer and maximum interface in re-
lated fields. These series are:
1. ENVIRONMENTAL HEALTH EFFECTS RESEARCH
2. ENVIRONMENTAL PROTECTION TECHNOLOGY
3. ECOLOGICAL RESEARCH
4. ENVIRONMENTAL MONITORING
5. SOCIOECONOMIC ENVIRONMENTAL STUDIES
6. SCIENTIFIC AND TECHNICAL ASSESSMENT REPORTS
7. MISCELLANEOUS
This report has been assigned to the ENVIRONMENTAL PROTECTION TECHNOLOGY
series. This series describes research performed to develop and demonstrate
instrumentation, equipment and methodology to repair or prevent environmental
degradation from point and non-point sources of pollution. This work pro-
vides the new or improved technology required for the control and treatment
of pollution sources to meet environmental quality standards.
This document is available to the public for sale through the National
Technical Information Service, Springfield, Virginia 22161.
Publication No. EPA-650/2-74-025-a
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ABSTRACT
Run-of-mine coal samples were collected from each of 35 U.S. mines
located in 13 states from New Mexico and Montana to West Virginia and
Pennsylvania. Each coal was treated separately by the Meyers Process
(ferric sulfate extraction) and float-sink fractionation (physical clean-
ing). The Meyers Process removed 90-99% of the pyritic sulfur (23-80% of
the total sulfur) from all of the coals which contained sufficient pyritic
sulfur for accurate sulfur determination (i.e., greater than 0.25% w/w).
Fourteen of the coals were reduced to less than 1% total sulfur by the
Meyers Process, while five of the coals were reduced to less than 1%
total sulfur by physical cleaning (1.90 float material, 14 mesh x 0).
With the exception of two mines, the Meyers Process removed significant to
very large increments of sulfur above that quantity which was separable
by physical cleaning. Significant amounts of Ag, As, Cd, Cr, Cu, Mn, Ni,
Sb, and Zn were removed along with the pyrite by the Meyers Process, while
float-sink procedures removed significant amounts of Ag, As, Cr, Cu, F,
Li, Mn, and Zn.
This report was submitted in fulfillment of Contract Modification No. 1
of Contract 68-02-0647 under the sponsorship of the Office of Research and
Development, Environmental Protection Agency.
m
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TABLE OF CONTENTS
Section Page
1.0 CONCLUSIONS 1
2.0 RECOMMENDATIONS 4
3.0 INTRODUCTION 5
4.0 PROGRAM RESULTS 10
4.1 Summary . . > 10
4.2 Selection, Sampling and Preparation of Coals 13
4.2.1 Selection of Coals 15
4.2.2 Sampling of Coals 18
4.2.3 Coal and Sample Preparation at TRW 20
4.3 Chemical Removal of Pyritic Sulfur 20
4.3.1 Experimental Method 21
4.3.1.1 Extraction Procedure 23
4.3.1.2 Coal Sampling from Reaction Vessel 24
4.3.1.3 Precision of Sulfur Analysis 25
4.3.1.4 Atomic Absorption Method for
Pyritic Sulfur Determination 26
4,3.2 Pyritic Sulfur Removal Results 29
4.3.3 Rate of Pyritic Sulfur Removal 35
4.3.4 Heat Content Changes and Ferric Ion Consumption. . . 39
4.3.5 Ferric Ion Consumption as a Function of Time .... 42
4.3.6 Removal of Residual Sulfate . 45
4.3.7 Summary of Ash Changes 50
4.3.8 Organic Sulfur Changes 53
4.3.9 Miscellaneous Data 62
IV
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TABLE OF CONTENTS (Continued)
Section Page
4.4 Float-Sink Testing 64
4.4.1 Procedures 64
4.4.2 Results and Discussions 64
4.5 Removal of Trace Elements 68
4.5.1 Analysis Procedures and Results 68
4.5.2 Removal Efficiencies 74
4.5.3 Summary and Conclusions 76
5.0 ACKNOWLEDGMENTS 79
6.0 REFERENCES 80
7.0 GLOSSARY OF ABBREVIATIONS AND SYMBOLS 82
8.0 UNIT CONVERSION TABLE 83
9.0 APPENDICES 84
Table of Contents 84
Tables 85
Figures 88
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TABLES
Page
1. Summary of Pyrite Removal Results 11
2. Initial Coal Selection 14
3. Present Coal Selection 15
4. Coal Analysis Summary - Initial Fifteen Coals 16
5. Coal Analysis Summary - Present (Final) Twenty Coals 17
6. Precision of Sulfur Forms Analysis 26
7. Determination of Pyritic Sulfur Using Atomic
Absorption Techniques 28
8. Summary of Pyritic Sulfur Removal Data 30
9. Pyritic Sulfur Removal as a Function of Time in Percent. . ... 36
10. Pyritic Sulfur Removal as a Function of Time -
% W/W Pyritic Sulfur 37
11. Summary of Heat Content Changes and Excess Ferric Ion
Consumption 40
12. Average Heat Content Losses and Ferric Ion Consumption .... 42
13. Ferric Ion Consumption as a Function of Time 44
14. Sulfate Content of Treated Coals 46
15. Special Sulfate Removal Experiments - Camp Nos. 1 & 2 Coal . . 47
16. Special Sulfate Removal Experiments - Orient No. 6 Coal. ... 48
17. Summary of Treated Coal Sulfate Content 49
18. Summary of Ash Changes (% W/W) .... 51
19. Average Excess Ash Removal (% W/W) 52
20. Organic Sulfur Data 54
21. Summary of Organic Sulfur Increments 56
22. Sulfate Determination on Whole Coal and Plasma Ash 59
23. Organic Sulfur Changes with Ferric Chloride 59
v1
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TABLES (Continued) p
24. Analysis of Leached and Toluene Extracted Coals Before
Vaporization Treatment 61
25. Analysis of Extracted Coals from Survey Program After
Vaporization Treatment 61
26. Miscellaneous Data 63
27. Summary of Float-Sink Tests, 14 mesh x 0 Coal, Comparison
to Meyers Process-, 100 Mesh x 0 Coal 65
28. Comparative Trace Element Analysis Results (PPM in
Moisture-Free Coal) 70
29. Trace Element Composition of Untreated Coals (PPM) 72
30. Trace Element Analytical Precision 73
31. Trace Element Removals (% W/W) 75
VII
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FIGURES
1. Pyritic Sulfur Removal Process Chemistry 5
2. U. S. Bureau of Mines Sampling, Handling System (Amended) 19
3. Pyrite Removal as a Function of Time 39
vi 11
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1.0 CONCLUSIONS
1. Only one of the thirty-five run-of-mine (ROM) coals investigated
in this survey met the Clean Air Act sulfur oxide emission standard of
0.6 Ibs* of sulfur/106 btu for new stationary combustion sources.
2. The process for chemical removal of pyritic sulfur from coal
(Meyers Process) was demonstrated to remove (operating at 100°C):
a) 90 to 99% of the pyritic sulfur (23 to 80% of the total
sulfur) from the twenty-three Appalachian Basin coals experimentally
investigated in the survey program. An additional coal obtained
from the Walker Mine, contained insufficient pyritic sulfur, 0.07%
w/w, for measurable evaluation in this program.
b) 91 to 99% of the pyritic sulfur (43 to 57% of the total
sulfur) from the six Eastern Interior Basin coals investigated.
c) 98% of the pyritic sulfur (64% of the total sulfur) from
the single Western Interior Basin coal investigated.
d) 59 to 89% of the pyritic sulfur from the four Western coals
investigated. Of these four samples, only coal from the Colstrip and
Navajo Mines contained sufficient pyritic sulfur to give reasonably
accurate results.
e) significant amounts of Ag, As, Cd, Cr, Cu, Mn, Ni, Sb, and
Zn.
3. Seven potentially hazardous trace elements - Ag, Be, Cd, Hg, Sb,
Se and Sn -were generally present in the coals studied in amounts that
may be only of minimal environmental significance ( <5 ppm) for effluents
from coal combustion facilities.
4. The Meyers Process reduced the total sulfur content of 14 coals
under investigation to below 1.0% (eight of these were reduced to 0.75%
or less).
*EPA policy is to express all data in Agency documents in metric
units. Because implementing this practice will result in undue cost,
NERC/RTP is providing conversion factors for the particular non-metric
units used in this document. These factors are located on page 83.
1
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5. The major factor determining the ultimate amount of pyrite
removal in ROM Eastern coals was the top size of the coal. While 40-50%
of the coals gave 90-99% removal with a 149y (100 mesh) top size, the
remaining coals had to be reduced to 105y (150 mesh) top size and some to
74y (200 mesh) top size. The size reduction also resulted in a substantial
increase in the rate of pyrite removal so that in most cases, the reaction
time could be reduced from 23 hours to 13 hours or less.
6. The rate of pyrite removal was measured as a function of time for
twenty coals, and it was found that the median percentages of removal were
as follows: 68% in 1 hour, 78% in 3 hours, 87% in 6 hours, 90% in 13 hours,
and 94% in 23 hours.
7. Most coals showed an increase in heat content after Meyers Process
treatment. For the Appalachian and some of the Eastern Interior Basin coals,
this heat content rise amounted to 1-11% of the initial heating value.
When calculated on a dry mineral matter free basis, which takes into account
the ash reduction due to pyrite removal, an average heat content loss of
7 ±2.1% was found for Western coals, Interior Basin coals lost 4 ±1.5%,
and Appalachian coals lost an insignificant 1 ±1.2%.
8. Sulfate retention, although variable, was least for Appalachian
coals, averaging 0.09%; intermediate for Interior Basin coals, averaging
0.26%; and high for Western coals. Reduction of leaching time to
12-14 hours for the Western and Interior Basin coals reduced retention
significantly.
9. Ash removal, in addition to that accounted for by pyrite removal,
was observed in varying degrees for all coals and increased with increas-
ing ash content in the coal. Excess ash removal was minimal for Appalachian
coals, intermediate for Interior Basin coals, and greatest for Western
coals.
10. A single-stage toluene extraction for elemental sulfur was found
to be inadequate and in some cases resulted in apparent increases in
organic sulfur.
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11. A vaporization technique at 375°C has been shown to be effective
in removing residual sulfur in those cases where a single stage toluene
extraction has been found to be inadequate.
12. Filtration rates were proportional to the amount of ash present
in the coals. High ash coals filtered significantly slower than low ash
coals.
13. Float-sink testing showed that conventional coal cleaning could
reduce the sulfur content of only two of the coals tested to the level
obtainable by the Meyers Process.
14. Varying amounts of 18 selected trace metals (see Section 4.5) were
removed by the Meyers Process and by conventional coal cleaning. The
Meyers Process removed significant amounts (>50%) of Ag, As, Cd, Cr, Mn,
Ni, Sb and Zn, while float-sink procedures removed substantial amounts
(>50%) of Ag, As, Cr, F, Li, Mn, and Zn in the majority of the coals.
Substantial differences were found for Mn and Pb for which the removal
was found to be significantly higher using the Meyers Process, and for
F and Li, where float-sink methods removed significantly greater amounts.
15. An atomic absorption method for the analysis of pyritic sulfur
was developed which has precision and accuracy equivalent to the ASTM
procedure.
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2.0 RECOMMENDATIONS
1. The Meyers Process should continue to be tested on additional
coals from all parts of the U.S. in order to further define the appli-
cability of the process for meeting legislated sulfur oxide pollution
control standards.
2. Future studies should include rate studies concerned with the
removal of pyritic sulfur from various coal size and density fractions
which are typical of the output of coal preparation units, for the pur-
pose of establishing optimum combinations of the Meyers Process with cur-
rent coal handling and treatment practices.
3. In order to further define process economics on a wide variety
of coals, the raw rate data obtained and partially treated in Section 4.3.3
should be reduced to kinetic rate expressions and evaluated in greater
detail.
4. Process parameters necessary to achieve optimum residual ele-
mental sulfur and sulfate removal, as well as the fate of major acid
soluble ash constituents such as calcium, magnesium and non-pyritic iron,
should be studied.
5. Near term emphasis should be placed on Appalachian coals since
the process applicability, as defined by the results from the first coals
leached in this survey, appears to be greatest for this region of the
county, and since 60% of current coal production in the U.S. is mined
in this region.
6. Further trace metal analysis should be conducted in order to
determine the conditions of optimum trace metal removal by the combina-
tion of float-sink separation with the Meyers Process.
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3.0 INTRODUCTION
The Meyers Process utilizes a regenerable aqueous ferric sulfate
leaching unit to chemically convert and remove the pyritic sulfur content
of coal as elemental sulfur and iron sulfate. In addition, the ash content
of the coal is decreased by 10 to 40% and the heat content per unit weight
increases by as much as 11%. The process chemistry for both leaching and
regeneration is outlined in Figure 1.
CRUSHED COAL IS TREATED WITH FERRIC SULFATE SOLUTION
Fe$? + 4.6
• 4.8^0 -10.2 FeSC>4
0.85
GENERATED SULFUR IS REMOVED BY VAPORIZATION OR SOLVENT EXTRACTION
FERRIC SULFATE SOLUTION IS REGENERATED WITH OXYGEN AND EXCESS
FERRIC AND FERROUS SULFATES ARE REMOVED
9.6 FeSO4 ' 4.8H25O4 + 2.4 Oj- 4.8 Fe2 (SO^ * 4.8
IRON
SULFATES
RECYCLE
SOLUTION
OVERALL REACTION:
FeS2 + 2.402- 0.8 S + 0.2
0.6 FeSO
Figure 1. Pyritic Sulfur Removal Process Chemistry
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The detailed chemistry, reaction kinetics, and engineering and
economic viability of the process were established under an Environmental
Protection Agency sponsored bench-scale program (Contract No. EHSD 71-7)
for evaluation of the Meyers Process^'. Because of the success of the
bench-scale program and the national need for sulfur oxide control tech-
nology, the process is now in a pilot plant design phase.
Other major methods which offer promise for the control of sulfur
oxides from coal burning stationary sources include: flue gas scrubbing,
coal liquefaction, and physical cleaning. These alternative methods are
compared to the Meyers Process in the following discussion.
Chemical desulfurization has some inherent advantages over flue gas
scrubbing for sulfur oxide control in that: a) application of this proc-
ess requires no major modification of existing or new power plant facil-
ities or of power plant operation, b) sulfur is removed from coal directly
as elemental sulfur and iron sulfate, and in relatively small amounts (e.g.,
approximately 230,000 tons/yr of these by-products from reducing
3.2 x 106 tons/yr of a 4% sulfur coal to 0.8% sulfur, versus 1,000,000 tons/
yr of a gypsum sludge throwaway material for comparable sulfur oxide
removal using non-regenerable lime-scrubbing). This second advantage does
not apply, of course, when comparing the Meyers Process to the regenerable
flue gas scrubbing processes now under investigation. The iron sulfates
from the Meyers Process may be converted to an insoluble basic iron sulfate
form by calcining, may be used to start up additional process plants, or
may possibly be sold as a chemical product in some locations.
The Meyers Process has advantages over coal liquefaction in that:
(a) operation under conditions of 100°C to 130°C, ambient to 100 psig is
possible, while coal liquefaction requires temperatures of 400-500°C and
pressures in excess of 1,000 psi; (b) a thermal efficiency of greater than
90% is obtained, compared with a thermal efficiency for coal liquefaction
of approximately 60-70% (this is an important factor in the conservation
of the overall U.S. energy base); and (c) only air or oxygen is required
as a consumable chemical, while liquefaction requires at least 1 to 2% by
weight hydrogen or synthesis gas and for catalytic liquefaction, a signi-
ficant amount of catalyst is found to be unrecoverable. However, coal
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liquefaction is capable of reducing a broader range of coals to meet air
quality standards.
The Meyers Process has advantages over physical cleaning (or separa-
tion by physical methods of coal into rock-rich and rock-lean portions) in
that: (a) large quantities of waste products are not generated (e.g., for
typical physical cleaning of coal, which is basically conducted to remove
non-combustible rock, 5-10% of the carbon content of the coal is discarded
along with the rock-rich fraction, giving rise to a secondary pollution
problem of acid drainage from tailings. For deep cleaning of coal, whose
purpose is to remove a large quantity of the pyritic sulfur, up to 30% or
40% by weight of the coal may be discarded, giving rise not only to an acid
drainage problem but to physical and combustion hazards due to the mass of
reject); (b) pollutants are converted into small amounts of potentially
useful chemicals (e.g., elemental sulfur and iron sulfate); and (c) con-
sistent and greater reduction in overall pyritic sulfur content can be
achieved.
Because of the widespread application of physical cleaning techniques
for removal of non-combustible rock from coal (which includes some pyrite),
the physical cleaning process deserves to be compared directly to the
Meyers Process for applicability in meeting the emission standards for
sulfur oxides. Indeed, in actual practice simple coal washing may well
be used prior to the Meyers Process to provide an improved coal product
containing both minimum ash and minimum sulfur, as well as optimum heating
value.
Therefore, an EPA sponsored program for a survey of the "Applicability
of the Meyers Process for Chemical Desulfurization of U.S. Coal" (Contract
No. 68-02-0647) was established to determine the potential of the Meyers
Process to desulfurize U.S. coals and to establish a comparison with
physical cleaning of coal. It is significant to note that both processes
are amenable to simple laboratory testing: the Meyers Process, through
chemical leaching with ferric sulfate solution as described in Figure 1;
and physical cleaning, through utilization of float-sink testing in dense
media. In addition, it was a further objective of the program to deter-
mine the fate of minor elements commonly found in domestic coals during
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chemical leaching. The detailed results of that initial survey program
to)
were complete in April 1974 and presented in a reportv '. This present
report covers the results of both the above-mentioned initial program and
a contract modification which extended the program scope to include addi-
tional coal mines. The detailed data obtained in the first program are
not repeated here.
The potential of the Meyers Process to provide a means to meet federal
standards of performance for new stationary sources is high. The Appala-
chian Coal Basin is an illustrative example. This coal region has partic-
ular importance as it provides 60% of current U.S. coal production, with
22 billion tons of identified and recoverable reserves, and is also the
major single area of U.S. sulfur oxide air pollution. Currently, approxi-
mately 90% of the coal mined for utility use in the Appalachian Basin
exceeds the sulfur content required to meet the sulfur dioxide emission
standard of no greater than 1.2 Ibs of SO emitted per million btu of
A
input energy. However, predictions made on the basis of available sulfur
forms data show that application of the chemical removal process can
increase the quantity of Appalachian coal which is capable of meeting
the performance standard by a factor of four, to nearly 40%, at 95%
pyritic sulfur removal. (Indeed, the results of the survey program to
date show that eleven of the twenty-three Appalachian coals evaluated
(48%) were reduced to 0.6-0.9% w/w sulfur and were consistent with the
federal standard.) In addition, many of the Appalachian coals could
meet state standards for existing sources using the Meyers Process.
There are 23 major coal mining districts in the United States having
several hundred.identifiable coals, all of which vary significantly in
composition; i.e., ash content, carbon content, sulfur content, pyrite
distribution, etc. Thus, in order to establish the applicability of
chemical removal of pyritic sulfur from coal process technology for sul-
fur oxide pollution control in the United States, the amount of sulfur
which may be removed from representatives of the widest possible variety
of coals must be determined. Consequently, this survey program evaluates
20 U.S. additional coals from mines in the Appalachian and Eastern Interior
coal basins of the United States.
8
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This report of the survey program contains data on over 115 coal
extractions and 540 sets of coal float-sink determinations, necessitating
more than 6,000 separate chemical and spectroscopic analyses. Therefore,
the following guide is provided for the readers who wish to focus their
attention in a specific area. Program results are presented in four major
areas:
• Selection, sampling and preparation of coals
• Chemical removal of pyritic sulfur
• Float-sink studies
• Evaluation of trace element changes
These sections are followed by references, a glossary, and appendices.
Those readers desiring to review the experimental data obtained for removal
of pyritic sulfur from coal are directed to Sections 4.1, 4.3 and 4.4
(p. 10, 20, and 64, respectively), as well as to the appendix tables cited
in these sections. Those readers desiring the selection criteria of coals
for the survey are directed to Section 4.2, while those readers interested
in experimental methods and sample techniques and preparation are directed
to Sections 4.2 and 4.3 (p. 13 and 20, respectively). Float-sink (wash-
ability) studies are reported in Section 4.4 (p. 64) and the trace element
studies are presented in Section 4.5 (p. 68).
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4.0 PROGRAM RESULTS
The program results are presented in the five sections to follow:
(1) Summary, (2) Selection, Sampling and Preparation, (3) Chemical Removal
of Pyritic Sulfur, (4) Float-Sink Testing, and (5) Removal of Trace Ele-
ments in Coal.
4.1 SUMMARY
The Meyers Process is operable over a wide range of conditions (e.g.,
100°C-130°C, coal top sizes of 1/4" to 200 mesh x 0, pressures from ambient
to 100 psig, and both with and without concurrent regeneration of leach
solution). Detailed discussions of the data obtained utilizing these
variations are presented in separate reports covering the bench-scale
fl 3}
programsv ' '.
A set of reaction conditions amenable to laboratory testing which are
within the above range of variables was selected for this survey program.
More specifically, testing was conducted at approximately 100°C and ambient
pressure, and the leach solution was periodically changed in order to main-
tain reasonable reaction rates. Each coal was found to require specific
conditions for maximum pyrite removal and total sulfur content reduction
relative to one or more of the following factors: reaction time, coal
particle size, degree and type of washing for sulfate removal, and excess
utilization of ferric ion. More than one reaction trial was often neces-
sary for identification of the conditions for high pyrite removal.
A summary of the best results to date for chemical removal of pyritic
sulfur and the optimal results for conventional coal washing (float-sink
evaluation) are shown in Table 1 in terms of total sulfur changes. The
table describes the results obtained on coals which contained sufficient
pyritic sulfur for accurate sulfur removal determination (i.e. >0.25% w/w).
The Edna, Belle Ayr, and Walker mines were below this limit and therefore do
not appear in the table. Actual total sulfur values before and after chem-
ical removal are shown in Columns 4 and 5. These may be compared with
Column 6, which shows sulfur values which could be obtained for full proc-
ess optimization (at 95% pyrite removal with no increase in starting
10
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Table 1
SUMMARY OF PYRITIC SULFUR REMOVAL RESULTS
Mine
Navajo
Seam
Nos. 6, 7 & 8
Kopperston No. 2 Campbell Creek
Harris Nos. 1 &
Colstrlp
Warwick
Marion
Matnies
Isabella
Orient No. 6
Lucas
Jane
Marti nka
North River
Humphrey No. 7
NO. 1
Bird No. 3
Williams
Siioemaker
Meigs
Fox
Dean
Powhattan No. '
Eagle Wo. 2
Star
Robinson Run
Homestead
2 Eagle & No. 2 Gas
Rosebud
Sewickley
Upper Freeport
Pittsburgh
Pittsburgh
Herri n No. 6
Middle Kittanning
Lower Freeport
Lower Ki ttanni ng
Corona
Pittsburgh
Mason
Lower Kittanning
Pittsburgh
Pittsburgh
Clarion 4A
Lower Kittanning
Dean
Pittsburgh No. 8
Illinois No. 5
No. 9
Pittsburgh
No. 11
Camp Hos. 1X2 No. 9 (W. Ky. )
Ken
Delirant
Muskingurn
Weldon Ho. 11
Eqypt Valley
No. 21
No. 9
Upper Freeport
Meigs Creek
Des Moines ho. 1
Pittsburgh Ho. 8
State
N. Mexico
W. Virginia
W. Virginia
Montana
Pennsylvania
Pennsylvania
Pennsylvania
Pennsylvania
' Illinois
Pennsyl vani a
Pennsylvania
W. Virginia
Alabama
W. Virginia
E. Kentucky
Pennsylvania
W. Virginia
W. Virginia
Ohio
Pennsylvania
Tennessee
Ohio
Illinois
W. Kentucky
W. Virginia
W. Kentucky
W. Kentucky
W. Kentucky
Pennsylvania
Ohio
Iowa
Ohio
I Total Sulfur w/w in Coala
Initial
0.8
0.9
1.0
1.0
1.4
1.4
1.5
1.6
1.7
1.8
1.8
2.0
2.1
2.6
3.1
3.1
3.5
3.5
3.7
3.8
4.1
4.1
4.3
4.3
4.4
4.5
4.5
4.8
4.9
6.1
6.4
6.6
After Meyers Process
Current Results
0.6
0.6
0.8
0.6
0.7
0.7
0.9
0.7
0.9
0.6
0.7
0.6
0.9
1.5
1.6
0.8
1.7
1.7
1.9
1.6
2.1
1.9
. 2.0
2.5
2.2
2.4
2.0
2.8
1.0
3.2
2.2
2.7
95% Removal
0.5
0.5
0.5
0.7
0.3
0.5
0.5
0.6
0.4
0.4
0.5
0.7
0.7
1.1
1.2
0.4
1.4
1.4
1.6
0.8
1.6
1.7
1.8
1.9
1.6
1.5
1.8
2.1
0.6
2.6
1.4
1.7
Meyers Process
PyrUe
Conversion
% w/w
90
92
94
83
92
96
95
96
96
94
91
92
91
91
90
96
96
96
93
93
94
99
94
91
97
93
99
91
96
"4
92
93
Meyers Process
Total Sulfur
Decrease
% w/w
25
33
23
30
54
50
36
54
44
64
63
70
55
42
48
75
50
51
48
57
49
53
54
43
50
47
55
42
80
47
65
59
% Sulfur (n Coalb
After Float-
Sink
0.8
0.9
...
1.0
1.2
1.7
1.5
1.4
0.7
0.8
0.8
2.2
1.9
2.3
1.6
2.3
3.6
2.8
2.0
3.0
3.3
2.9
3.0
3.0
3.2
2.9
3.5
2.1
4.4
3.9
4.6
Dry, moisture-free basis.
1.90 Float material, 14 mesh x 0, is defined here as
the limit of conventional coal
°Sulfur content of coal at 95% pyrite removal and no increase in sulfate or measured
cleaning (See Section 4.4)
organic sulfur content.
-------
sulfate or measured organic sulfur content). Thus, for example, although
99% pyrite conversion was obtained for the Camp Nos. 1 and 2 mines, the
total sulfur was reduced to 2.0%, not the theoretical 1.8%, due to a slight
measured increase in other sulfur forms.
Because of the widespread application of physical cleaning techniques
for removal of non-combustible rock (which includes varying amounts of
pyrite) from coal (along with some carbon), float-sink fractionation was
performed in order to define the relative utility of washing and chemical
desulfurization for each coal. The results which are shown in Table 1,
indicate that: a) the Meyers Process, at its current state of development,
removed 83-99% of the pyritic sulfur content of the 32 coals studied,
resulting in total sulfur content reductions of 25 to 80%, b) eleven (34%)
of the coals were reduced in sulfur content to the 0.6 - 0.8% sulfur levels
generally consistent with the federal standard for new stationary sources
and many state standards, c) in all cases, the Meyers Process removed sig-
nificant to very large increments of sulfur over that separable by physical
cleaning, and d) in one case, the Mathies mine, coal cleaning resulted in
a sulfur content increase.
State emission regulations for discharge of sulfur oxides from utility
and large industrial power plants can also be met by application of the
Meyers Process. For example, the Pennsylvania state standard for eight
air basins is approximately 1.1% sulfur, for coal of 25 x 106 btu/ton.
Several of the tested Pennsylvania coal mines (Marion, Mathies, Isabella,
Bird No. 3 and Delmont) meet this standard after chemical desulfurization
but do not meet the standard after efficient physical cleaning. These
coals could also be transported to Michigan, New Jersey or New York to
meet their state standards of approximately 1.0% and 1.8% and 2.4% sulfur,
respectively. Two of the Ohio coal mines (Meigs and Powhattan No. 4) would
meet the "28 county standards" of approximately 2% sulfur for the state of
Ohio after treatment by the Meyers Process, whereas efficient cleaning of
these coals reduces their sulfur content to only 2.8% and 3.3%,
respectively.
The Orient No. 6 mine of Illinois meets the Chicago area standard of
1.29% sulfur after chemical desulfurization but does not meet the standard
12
-------
after physical cleaning. The Camp Nos. 1 and 2 mines in Western Kentucky
meet the state standard for "Priority 3" regions of less than 2.3% sulfur
after treatment by the Meyers Process, whereas physical cleaning reduces
the total content of this coal to 2.5%. The Humphrey No. 7 mine is
reduced to 1.5% sulfur, which meets the West Virginia standards for
"Regions 2 and 3" of 1.7 and 2%,respectively, whereas physical cleaning
reduces the sulfur content to 1.9%. The Wei don mine in Iowa is reduced
to 2.3% sulfur by the Meyers Process which meets the state requirement of
approximately 3.1% sulfur. Physical cleaning does not meet the standard,
reducing the sulfur content to 3.8%.
Process improvements, such as more efficient residual sulfur and sul-
fate removal, will cause most coals to be further reduced in sulfur content
to the "95% removal" level shown in Column 6 of Table 1.
In the production of clean fuel using commercial practices, it is
very likely that an optimum process cost and product will be obtained by
physically cleaning coal prior to ferric sulfate leaching, in order to
remove rock and some of the larger pyrite particles. There are prelimi-
nary indications that the efficiency of the Meyers Process may be enhanced
by utilization of physically cleaned coal, resulting in faster rates,
greater total removal, and reduced ash dissolution.
Results from this chemical desulfurizaton survey also showed that
silver, arsenic, cadmium, chromium, copper, manganese, nickel, antimony,
and zinc could be substantially removed from many of the coals during
the Meyers Process treatment.
The detailed results are presented in the following five sections
and in the cited Appendix divisions.
4.2 METHODOLOGY OF SELECTION, SAMPLING AND PREPARATION OF COALS
TRW selected thirty-five coal mines which were sampled in two groups.
The data obtained for the first group of fifteen mines has already been
reported^ ', but will be included in summary form in this report, in order
to substantiate correlations and conclusions drawn from the data for all
the coals. The data obtained in the second group of twenty mines is new
13
-------
and is completely reported herein. The mine selections were made on the
basis of the following criteria:
a) Representation of the widest possible variety of coal beds,
coal regions, and coal rank;
b) High production and reserves;
c) Sulfur content in coal sufficiently high to require control
of sulfur oxide emissions from combustion.
(4)
The selected mines, the annual production of each mine in 1972V ,
and the analysis summary of each group of coal samples are given in
Tables 2, 3, 4, and 5. The following sections present a summary of the
Table 2
GROUP 1
INITIAL COAL SELECTION
CATEGORY
c;
*n
~(S
0 •—
U 10
o
in (_>
o c
c *o
E -c
3 0
CD 0> C
V) C t/l
3 — . ID
IE"
E 0) "0
3 *-> O
i-
<— 0
O k-
c_> &> C
3 •— a) wi
3 *J •—
0 ••- *J
ceo
^ — 1 C
-•- «0 HJ
CO *J
1 f— I/>
3 O 3
t/1
-------
Table 3
GROUP 2
PRESENT COAL SELECTION
CATEGORY
••-
CO
o
o
c
n
.c
« -t-> CO
••- O C
CO (_}•—•
STATE
Ohio
East Ohio
Pennsylvania
Pennsylvania
West Virginia
West Virginia
West Virginia
Pennsyl vani a
Pennsylvania
Ohio
Pennsylvania
West Virginia
Ohio
Tennessee
West Virginia
West Virginia
Alabama
West Kentucky
West Kentucky
West Kentucky
COUNTY
Meigs
Monroe
Fayette
Washington
Marion
Harrison
Marshall
Westmoreland
Indiana
Columbi ana
Somerset
Logan
Meigs
Scott
Wyoming
Boone
Jefferson
Ohio
Ohio
Hopkins
MINE
Muski ngum
Powhattan No. 4
Isabella
Mathies
Williams
Robinson Run
Shoemaker
Delmont
Mari on
Lucas
Bird No. 3
Marti nka
Meigs
Dean
Kopperston No. 2
Harris Nos. 1 i 2
North River
Homestead
Ken
Star
SEAM
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Middle Kittanning
Lower Kittanning
Lower Kittanning
Clarion 4A
Dean
Campbell Creek
Eagle 8 No. 2 Gas
No. 11
No. 9
No. 9
1972 Production
000 Tons
4,310
691
722
2,205
1,045
n.a.*
1,643
426
436
n.a.
955
n.a.
n.a.
60
1,332
1,718
2,469
1,536
1,494
COMPANY
Central Ohio Coal Company
Quarto Mining Company, Sub-
sidiary of North American
Coal Company
National Mines Corporation
Mathies Coal Company
Consolidation Coal Company
Consolidation Coal Company
Consolidation Coal Company
Eastern Associated Coal
Corporation
Tunnel ton Mining Company
Buckeye Coal Mining Company
Island Creek Coal Company
American Electric Power Company
American Electric Power Company
Royal Dean Coal Company
Eastern Associated Coal
Corporation
Eastern Associated Coal
Corporation
Peabody Coal Company
Peabody Coal Company
Peabody Coal Company
*Not currently available.
rationale for selection, a description of the sampling of the coals, and a
discussion of sample preparation for testing at TRW. A detailed discussion
of the coals and mines selected and maps showing the geographic distribu-
tion of the mines and seams are given in Appendix A.
4.2.1 Selection of Coals
Using the above criteria, a total of twenty-four of the mines was
selected from the Appalachian Coal Basin. This large number was chosen
since nearly 70% of current U.S. production comes from this region, and
272 x 109 metric tons (300 x 10 tons) of reserves (800 years supply at
current production) still exist, although only 10-15% of the coal now
mined can meet the federal standards for new stationary sources. Further-
more, much of the coal is high in pyritic sulfur, thus making it amenable
to treatment. This coal is also closest to the major markets. The mines
(Tables 2, 3, 4, and 5) were selected to represent a wide geographic
15
-------
Table 4
COAL ANALYSIS SUMMARY
INITIAL FIFTEEN COALS^
Mine
Warwick
Egypt Vallej
No. 21
Humphrey
No. 7
Fox
Walker
Jane
Nos. 1 S2
No. 1
Eagle No. 2
Camp Nos. 1
and 2
Orient No. 6
Wei don
Edna
Navajo
Belle Ayr
Colstrip
Seam
Sewickley
Pittsburgh
No. 8
Pittsburgh
Lower
Ki ttanning
Upper
Ki ttanning
Lower
Freeport
Mason
Illinois No. 5
Seam No. 9
Herrin No. 6
Des Hoines
No. 1
Wadge
Nos. 6,7,8
Roland-Smith
Rosebud
As Received
Ba 1s
Rank
hvAb
hvAb
hvAb
hvAb
Ivb
hvAb
hvAb
hvAb
hvBb
hvAb
hvCb
hvCb
hvCb
sub A
subB
Moisture
X w/w
1.50
2.07
1.63
1.83
2.07
1.17
2.22
3.31
3.99
3.51
13 29
8.41
11.07
19.14
20.41
Dry Forms of Sulfur, % w/w
Total
1.37
6.55
2.58
3.83
0.71
1.85
3.12
4.29
4.51
1.66
6.39
0.75
0.81
0.76
1.01
Pyritic
1.09
5.07
1.59
3.09
0.07
1.44
1.98
2.64
2.80
1.30
5.24
0.14
0.28
0.22
0.34
Sulfate
0.01
0.14
0.01
0.05
0.00
0.00
0.08
0.04
0.06
0.01
0.15
0.00
0.03
0.03
0.00
Organic
0.27
1.34
0.98
0.69
0.64
0.41
1.06
1.61
1.65
0.36
1.00
0.61
0.50
0.54
0.67
Dry Proximate Analysis, % w/w
Ash
40.47
25.29
9.88
13.55
16.67
21.75
11.39
26.53
21.13
22.51
15.74
9.13
25.29
7.55
10.38
Volatiles
27.77
36.12
37.66
38.33
18.89
30.07
38.91
34.30
35.86
31.67
40.62
40.65
35.51
47.11
43.09
Fixed
Carbon
31.76
38.59
52.46
48.12
64.44
48.18
49.70
39.17
43.01
45.82
43.64
50. qq
39.20
45.34
46.53
Heat
Content
btu
8612
10594
13631
12973
12602
11932
13054
10566
11105
11163
11760
11246
10050
12034
11591
For a complete set of data, see Reference 2.
distribution of the seams and those having large reserves and high produc-
tion (Kittanning, Pittsburgh, and Freeport), with a lesser effort being
made to get a wide selection of stratigraphic groups. From a stratigraphic
standpoint, these mine selections range from the Sewickley Seam, which is
relatively young, to the Eagle and No. 2 Gas Seams, which are relatively
old.
A group of six coals was selected from the Eastern Interior Coal
Basin representing the Illinois No. 5 (Kentucky No. 9), and the Illinois
(Herrin) No. 6 (Kentucky No. 11) seams. Less emphasis was placed on this
region due to its smaller production and the fact that the generally higher
organic sulfur contents (1.5-2.5%) of these coals make them less able to
meet pollution control standards by pyritic sulfur removal alone.
16
-------
Table 5
COAL ANALYSIS SUMMARY9
PRESENT (FINAL) TWENTY COALS
Mine
Muskingum
Powhattan
No. 4
Isabella
Mathies
Williams
Robinson
Run
Shoemaker
Delmont
Lucas
Bird No. 3
Marti nka
Meigs
Dean
Kopperston
No. 2
Harris
Nos. U2
Homestead
Ken
Star
Seam
Meigs Creek
No. 9
Pittsburgh
No. 8
"ittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Middle
Ki ttanning
Lower
Ki ttanning
Lower
Ki ttanning
Clarion 4A
Dean
Campbell Creek
Eagle & No. 2
Gas
No. 11
No. 9
No. 9
As Rec
Bas
Rank
hvAb
hvAb
hvAb
hvAb :'
hvAb
hvAb
hvAb
hvAb
hvAb
Ivb
hvAb
hvBb
hvAb
hvAb
hvAb
hvAb
hvBb
hvBb
hvBb
elved
Moisture
X w/w
3.36
2.10
1.57
2.15
1.28
0.96
1.51
0.77
1.84
3.88
0.84
1.84
4.77
1.06
1.38
1.72
1.57
5.41
4.76
6.13
Dry Forms of Sulfur, % w/w
Total
6.08
4.12
1.57
1.46
3.48
4.38
3.51
4.89
1.37
1.79
3.14
1.96
3.73
4.09
0.91
1.00
2.06
4.46
4.83
4.32
Pyr1 ti c
3.65
2.57
1.07
1.05
2.23
2.89
2.19
4.56
0.90
1.42
2.87
1.61
2.19
2.62
0.47
0.49
1.42
3.11
2.85
2.60
ulfate
0.06
0.19
0.04
0.04
0.04
0.06
0.05
0.08
0.02
0.05
0.05
0.09
0.06
0.15
0.03
0.03
0.07
0.10
0.26
0.24
Organic
2.37
1.36
0.46
0.37
1.21
1.43
1.27
0.25
0.45
0.32
0.22
0.26
1.48
1.32
0.41
0.48
0.57
1.25
1.72
1.50
Dry Proximate Analysis, % w/w
Ash
21.68
37.17
42.22
41.01
13.18
13.36
33.48
27.18
26.40
30.23
49.64
26.53
17.28
30.15
18.63
49.25
16.56
15.08
13.90
olatiles
36.36
29.01
24.69
24.53
38.64
38.88
31.13
28.33
24.45
35.30
16.18
21.60
34.92
36.91
23.89
26.86
23.19
33.14
35.26
33.94
Fixed
Carbon
41.96
33.82
33.09
34.46
48.18
47.76
35.39
44.49
49.15
56.02
53.59
28.76
38.55
45.81
45.96
54.51
27.56
49.66
52.16
Heat
ontent
btu
11014
8603
8216
8154
13013
12962
9495
11012
11046
13451
10550
7552
10246
12107
10957
12414
7693
12099
12308
For a complete set of data, see Appendix C.
A single sample from the Weldon Mine, Des Moines No. 1 Seam, was
chosen from the Western Interior Basin.
A group of four coals was selected from the remaining coal basins in
the western half of the United States. Even though this area contains
more than half of all U.S. reserves, the selections were deliberately
limited because of present low production, sulfur contents generally
less than 1.0%, and pyritic sulfur contents so low (<0.25%) that the
results of chemical extraction would be difficult to measure.
17
-------
4.2.2 Sampling of Coals
Samples containing 908 kg (one ton) of raw run-of-mine (ROM) coal
were collected from each mine. The samples were taken in increments that
represented at least a half day's production. Samples were collected in
accordance with ASTM Standard D2234* ' with the following preferences:
automatic samples, stopped belt increments, and, if necessary, full fall-
ing stream intercepts. Auger sampling of unit trains in certain instances
was also utilized in cases where it could be shown that the trains con-
tained only ROM coal from a single seam and mine.
The samples were sealed in plastic-lined drums (six per mine) for
shipment to Commercial Testing and Engineering Laboratory (CT&E) where
each 908 kg (one ton) gross sample was crushed to 38.1 mm x 0 (1-1/2" x 0)
by a jaw crusher, divided into four parts and treated as follows:
• A 38.1 mm x 0 (1-1/2" x 0) fraction was taken for float-sink
fractionalion,
• A second part was crushed to 9.51 mm x 0 (3/8" x 0) for float-
sink fractionation,
• A third part was crushed to 1.41 mm x 0 (14 mesh x 0) for float-
sink fractionation. An 11 kg sample of this material was also
sent to TRW for chemical processing to remove pyritic sulfur.
• The remaining part was held in reserve.
Float-sink fractionation of portions 1, 2 and 3 above was performed
with organic liquids at 1.30, 1.40, 1.60 and 1.90 specific gravities. The
resulting fractions were analyzed for ash, total sulfur, and pyritic sul-
fur on a dry basis. The results were then used to calculate washability
tables in order to determine cumulative recoveries and rejects at the
various specific gravities. Figure 2 illustrates the sequence of sampling
and testing.
The procedures used to collect each of the current twenty 908 kg
samples are described in Appendix A, while the procedures used for the
initial fifteen coals have been reported previously
18
-------
R.O.M.
SAMPLE - 908 KG. (2000 LBS)
LINED 200 L (55 GAL) DRUMS
SHIPPED TO C.T.&E. LAB.
CRUSHED TO 38.1 MM (1-1/2") TOP SIZE
JAW CRUSHER
1/4 OF SAMPLE
OVERSIZE SCREEN
9.51 MM (3/8")
1/4 OF SAMPLE
1/4 OF SAMPLE
FINES
CRUSHED TO 9.51 MM (3/8") TOP SIZE
IMPACT CRUSHER
OVERSJZE SCREEN OVERSIZE
~" 1.41 MM (14 MESH)
FINES
OVERSIZE SCREEN OVERSIZE
149M (100 MESH)
FINES
CHEM. ANAL.
T.S.,PY. S., ASH
FLOAT-SINK ANAL.
SP.GR. 1.3
1.4
1.6
1.9
140 KG. USED
SCREEN
1.41 MM (14 MESH)
FINES
SCREEN
149M (100 MESH)
FINES
CHEM. ANAL.
T.S., PY.S.,ASH
FLOAT-SINK ANAL.
SP.GR. 1.3
1.4
1.6
1.9
70 KG, USED
CRUSHED TO-1.41 MM (-14
MESH) HAMMER MILL
1.41 MM (-14 MESH)
TRW
SAMPLE
FLOAT-SINK ANAL.
SP. GR. 1.3
1.4
1.6
1.9
3 KG. USED
1/4 OF SAMPLE
(RESERVE)
Figure 2. U.S. Bureau of Mines Sampling, Handling System
Amended
19
-------
4.2.3 Coal and Sample Preparation at TRW
An 11 kg (25 1b) sample of coal ground to 1.41 mm x 0 (14 mesh x 0)
was shipped from CT&E to TRW in a sealed polyethylene bag inside a
5-gallon can. If any surface moisture was observed upon receipt at TRW,
the coal was spread on a polyethylene sheet in a fume hood and allowed to
air dry from 4 to 6 hours. This gross sample was then reduced by riffling
to obtain 1600-2000g portions. One sample was stored under nitrogen or
argon in a glass container as a reserve, and another was ground in a dis-
integrator with a 0.58. mm screen. After several passes, the entire lot
was sieved using a 149y (100 mesh) screen. All oversize material was then
passed through the grinder several more times and resieved; this process
was repeated until more than 99% of the material passed through a 149y
(100 mesh) screen. The remaining fraction of 1%, which was composed of
slate and other rock-like material, was discarded. The entire lot of
149y x 0 (100 mesh x 0) coal was then thoroughly mixed by conventional
cone and quartering techniques on a polyethylene sheet. The coal was
then bottled as 100.0 g samples in containers that had been flushed with
nitrogen or argon. In order to guarantee relatively uniform samples, the
coal was periodically mixed during this process. It was found that when
the coal was 100% 149y x 0 (100 x 0 mesh), in most cases 91% would pass a
105y (150 mesh) screen and 70% would pass a 74y (200 mesh) screen.
If finer coal was needed, the required amount of coal (200-300g) was
quantitatively ground in a ball mill to pass a 105y (150 mesh) or 74y
(200 mesh) screen.
4.3 CHEMICAL REMOVAL OF PYRITIC SULFUR
This section presents descriptions of the experimental methods and
summarizes results from the studies involving chemical removal of pyritic
sulfur from the surveyed coals. The removal of trace elements from coals
as a result of the Meyers Process is described in Section 4.5, together
with a discussion of the experimental methods used to determine the trace
element composition.
Also included in this section are discussions of: (a) total pyritic
sulfur removal and its removal as a function of time, (b) ferric ion
20
-------
consumption and its relationship to pyrite removal and the final heat
content of coal, (c) ash changes, (d) sulfate retention, (e) changes
in the organic sulfur content, and (f) miscellaneous findings.
4.3.1 Experimental Method
The reaction conditions for pyritic sulfur removal have been adapted
(1 3)
from the previous bench scale studies (Contract EHSD 71-7)v ' ' and the
(2\
previously completed Part Iv ' of the survey program, for the purposes of:
(a) obtaining 90-100% pyritic sulfur removal, (b) simulating process design
as nearly as possible, and (c) obtaining as much quantitative data as pos-
sible. The general procedure is discussed below.
Mesh Size — Coal ground to 100 mesh x 0 was found to give the maximum
extraction rates and to be most satisfactory for laboratory scale sampling.
Coal ground to a finer mesh was used only if conditions warranted.
Ferric Ion Concentration - Ferric sulfate solution IN in ferric ion
appears to be optimum, although differences due to concentration changes
(1 3)
do not appear to be greatv ' .
Reaction Temperature — The reaction temperature was held at the
reflux of 1 N ferric sulfate solution, which is approximately 102°C.
This allows a reasonably high reaction rate and yet did not require
pressure equipment.
A trial experiment was run for each coal (due to the high variance
in the behavior of individual coals) in order to select the reaction time,
mesh size, and number of leach solution changes needed for maximum pyrite
removal.
Reaction Time - Each coal was leached a total of six or more hours,
depending on the characteristics of the individual coal being treated.
Ferric Ion to Total Iron Ratio - Since the rate of pyrite removal is
slowed substantially by ferrous ion accumulation, each coal was treated
under conditions designed to keep this ratio >0.80 by one of the following
methods:
• Increasing the solvent to coal ratio (w/v) from a nominal 3 to 8
used in the bench scale work to 25.
21
-------
• Changing the leach solution after 3 to 6 hours of reaction or
more often, if required.
0 A combination of the above.
Post Sample Treatment — After treatment, the samples were thoroughly
washed to remove any residual leach solution. The wet coal was extracted
with toluene to remove elemental sulfur, and then dried. All sample cal-
culations were done on a dry basis in order to eliminate variables due to
wetness of the coal. Sulfur forms and proximate analysis were obtained
for each treated coal sample.
In addition to the characterization of the initial and treated coal,
further evaluations were performed on the 20 additional coal mines sampled
for this part of the survey, in order to determine in greater detail the
kinetic behavior of pyritic sulfur extraction and at the same time, to
investigate potential problem areas that may arise when the Meyers Process
is applied to a large variety of coals. This included an evaluation of the
following items for all coal samples processed:
Rate of Pyrite Removal - Coal samples were taken periodically and
analyzed for pyritic sulfur. In order to simplify rate calculations, the
ratio of coal to leaching solution was kept constant by always withdrawing
an equivalent amount of leach solution.
Rate of Ferric Ion Consumption — The leach solution withdrawn from
the above samples was analyzed for ferrous as well as total iron in order
to determine the rate of ferric ion consumption and iron balance. Addi-
tional samples were withdrawn and analyzed as necessary in order to get
precise results.
Retention of Leach Solution on the Coal - Retention of the leach solu-
tion on the coal was determined by weighing the coal after filtration under
a set of standardized conditions and subtracting the dry weight of the
treated coal.
Retention of Sulfur Solvent — Retention of the sulfur solvent on the
coal was determined by weighing the coal after filtration under a set of
standardized conditions and subtracting the weight of the treated coal.
22
-------
4.3.1.1 Extraction Procedure
The exact procedure used in this survey is described below:
One hundred grams of 100 mesh x 0 coal are added to 2 £
refluxing IN ferric sulfate solution contained in a 4-necked,
3 I glass cylindrical reaction vessel equipped with a mechanical
stirrer, reflux condenser and a thermocouple attached to a
recorder. Each vessel also has a stopcock at the bottom for
taking samples and is heated by a specially constructed heating
mantle. After the coal addition, an additional 0.5&1N ferric
sulfate solution is used to wash down the sides of the vessel.
At this point, the to solution sample is taken and the leaching
process is considered started. Then, the reaction mixture,
which is at 88 ±4QC, is rapidly brought to reflux, a process
that takes 8-12 minutes. Leach solution samples for each
analysis are collected by taking a 35 ml aliquot of the reaction
mixture (the sampling procedures are discussed below) and cooling
it immediately to 0°C. After cooling, the aliquot is centrifuged
to remove all suspended solids and 30 ml of this is used for iron
analysis. The remaining coal is washed, dried and saved for
pyritic sulfur analysis.
After 4-6 hours, the heating is stopped and the reaction
mixture is drained from the flask, filtered and dewatered under
vacuum conditions. The final reaction volume and solution reten-
tion on the coal are determined at this time. The wet, unwashed
coal is slurried with 200 ml fresh ferric sulfate solution at
30°C and added to 2 ifresh IN ferric sulfate solution at reflux.
Another 300 ml ferric sulfate is then used to wash any residual
coal into the flask. A to leach solution sample is taken imme-
diately and the entire reaction mixture is brought to reflux in
8-12 minutes. Leach solution samples are taken at regular
intervals; and after a total elapsed reacton time of 10 to
24 hours, the reaction mixture is drained from the reaction
flask, filtered and washed clear with 0.5 - l.OHwater.
The extracted coal is then slurried with 2£0.2N H2S04 at
*• 80°C. This is followed by slurrying in 2iwater. If schedul-
ing does not permit the coal to be extracted with toluene imme-
diately, it is stirred at^50°C in water for an extended period
until it can be filtered and extracted.
After the extraction of residual sulfate and iron, the wet
coal is transferred into a 1«, round bottom flask equipped with a
mechanical stirrer and Dean-Stark trap. Toluene, 400 ml, is
added and the mixture is brought to reflux. This is continued
until all the water is azeotroped off (approximately 0.75 -
1.25 hour and 50 - 75 ml) plus another 15 minutes. The hot
solution is then filtered, washed with 50 - 75 ml toluene, and
dried in a vacuum oven at 100 - 12QOC. The coal is then weighed
and analyzed.
23
-------
4.3.1.2 Coal Sampling from Reaction Vessel
In order to determine the rate of pyrite removed from the coal, it is
necessary to periodically take coal samples from the reactor for pyrite
analysis. This is because the accumulation of ferrous ion in solution
reflects not only the oxidation of pyrite but also a small and variable
reaction with the organic matter in coar ' * '.
Initially, it was thought that, since 100 mesh x 0 or finer coal was
being used, the coal distribution within the rapidly stirred and boiling
reactor would be uniform in all directions. It soon became apparent, how-
ever, that even with all the turbulence in the reactor, a float-sink sep-
aration was taking place with the heavier particles settling in a small
dead space (ca Ig) where the stopcock is attached to the bottom of the
reaction vessel. This results in poor or erratic pyrite analysis in the
first six hours of reaction when pyrite concentrations are high. The
pyrite composition of the segregated material was found to be over 10% w/w
after 1 hour of reaction for coal which initially had only 4.9% w/w pyritic
sulfur. Removing this material with 200 ml leach solution, quickly adding
it back through the top of the reactor, and then taking a sample before
any settling took place was not successful because the heavy particles
rapidly, but unevenly, sand toward the bottom of the reaction vessel.
This resulted in erratic pyritic sulfur values with differences of up to
1%. In some cases, the sampling of pyrite-rich areas resulted in apparent
pyritic sulfur gains of 1-3% after 1 hr of reaction. The problem was fin-
ally solved by using a "thief" technique in which an aluminum tube,
designed to take a 30-40 ml sample along the entire vertical axis of the
reactor, was rapidly inserted into the vessel and then closed off when it
reached the bottom. In order to guarantee that the high pyrite material
which collected in the bottom of the reactor was in suspension at the
time the sample was taken, several 200 ml aliquots were taken out of the
bottom of the reactor and poured into the top just before the sample was
taken. This procedure was used on the final five coals that were treated,
and good reactor-to-reactor precision and pyritic sulfur values consistent
with ferrous ion accumulation were obtained.
24
-------
It is also postulated that sampling problems would be substantially
reduced by removal of high density material by float-sink methods. The
specifics of four different methods of reaction vessel sampling, as well
as the coals sampled by each method, are briefly summarized below:
Method A: Lucas, Marion. Meigs, Mathies, Powhattan Coals. A
35 ml sample was taken from the bottom of the reactor after first
removing the coal plug in the valve with 200 ml of solution.
Samples from all of the coals taken during the first 5-6 hrs
were low in pyrite. Precision for the Lucas, Marion and Mathies
coals which had low initial pyrite (-1%) was good; precision for
the Meigs and Powhattan coals was poor. Only samples taken after
5-6 hours, when most of the pyrite is removed by chemical reaction,
were considered reliable.
Method B: Muskingum, Isabella, Robinson Run, Delmont, Bird No. 3,
Star and Ken Coals. In this procedure the coal plug was withdrawn
with 200 ml of solution and added back to the reactor just before
sampling. This resulted in very poor precision between reactors
and apparent increases in pyrite content during the first 3 hrs
in several cases. Samples taken during these runs were consid-
ered reliable only after 8 hrs. Reasonable results were obtained
for the low ash Star and Ken coals.
Method C: Shoemaker and Williams Coals. An aluminum tube with an
open bottom that holds 30-40 ml within the vertical axis of the
reaction vessel was rapidly inserted to the bottom of the reactor;
then the bottom was closed off and the tube withdrawn. This
method gave good precision but may have given slightly low results,
as with Method A.
Method D: Martinka, Kopperstone, Harris Nos. 1 and 2, North River,
Homestead and all additional (No. 3) runs on the Powhattan No. 4,
Williams and Lucas Mines. Method C was modified by withdrawing
the plug from the bottom of the reactor with 200 ml of solution
and pouring it back into the top of the reactor. This method
gave good precision and the results were considered accurate.
4.3.1.3 Precision of Sulfur Analysis
During the course of these studies, a substantial amount of sulfur
analyses data was collected which included 35 sets of sulfur forms analyses
on untreated coals and an additional 34 sets on the treated coals. It was
the practice during this research program to process multiple samples for
individual analysis rather than to perform a duplicate analysis on a single
sample. In this way, all sampling and handling errors were included in
each analysis, and the results would not appear artificially precise. The
25
-------
standard deviation for each set of these analyses was used to calculate a
pooled standard deviation for each type of analysis both before and after
extraction. The results of these calculations (tabulated in Table 6) show
that, in all cases, precision is excellent. In addition, the precision of
the analysis on the treated coals is only slightly less than that of the
untreated coals, indicating that the leaching and work-up procedures were
carried out in a very uniform way.
Table 6
PRECISION OF SULFUR FORMS ANALYSIS
POOLED STANDARD DEVIATIONS, % W/W ABSOLUTE
Samples (Sn)
Initial (35)
Treated (34)
All (69)
SULFUR FORMS
Total
0.063
0.066
0.064
Pyrite
0.074
0.071
0.072
Sulfate
0.010
0.019
0.016
Organic
0.085
0.090
0.090
4.3.1.4 Atomic Absorption Method for Pyritic Sulfur Determination
The analysis for pyritic sulfur normally requires approximately 1-5 g
of coal and substantial labor for the ASTM analysis'6'. Because as many as
six to ten samples would be withdrawn from the chemical reactor containing
100 g coal during the course of a run, it was apparent that the method of
analysis should be examined for modification that would allow a reduction
in both sample size and analysis time. The following criteria were
considered:
t The methods of chemical extraction of sulfate and pyritic sulfur
would not be changed because they have been accepted as effec-
tive and because change would require a development effort out
of scope of this contract.
• Only methods requiring 0.25-1.0 g of total sample would be
considered.
• Since new methods which are characterized by both speed and
accuracy for determining iron have been developed in recent
years, these methods would be examined for applicability.
26
-------
• The iron analysis (pyritic sulfur) should have the same
accuracy and precision as the old method.
The method of sulfur extraction used was identical to the ASTM proce-
dure^ ' in which both pyritic and sulfate sulfur determinations are per-
formed on the same sample, with the exception that a 0.7-1.0 g sample is
used. Iron oxide and ferrous sulfate are first extracted with refluxingSN
HC1 for 0.75 hr. The filtered and washed residue is then extracted with
refluxing 5N HNO- for 0.5 hr to remove iron pyrite. The extract solutions
are then brought up to volume for an iron analysis by the procedure
described below. Sulfur is not determined directly because a small
amount of organic sulfur is usually extracted by the nitric acid.
Atomic absorption spectrophotometry (AAS) was selected for pyritic
iron determination for the following reasons:
a) The extraction of small amounts of organic material does not
affect the determination. Hence, several steps in the ASTM
procedure, which are designed to destroy organic material in
order to prevent is reaction with the strong oxidizing agent
used in the subsequent titrimetric determination of iron,
can be eliminated.
b) The atomic absorption method for determining iron is normally
free of interelement interferences.
c) Matrix effects can be eliminated by use of a dual channel
atomic absorption spectrometer, such as the Fisher Jarrell-
Ash instrument.
d) Extracted color does not interfere with the determination
as is the case for the ASTM procedure, which has a color-
imetric endpoint.
e) The method is precise, accurate, fast, and inexpensive.
The results of analysis performed by the atomic absorption and ASTM
methods are summarized in Table 7. Note that in those cases where multiple
analyses were performed, the precision of the AAS method is excellent. In
fact, the precision obtained is that expected from a good Eschka (total)
27
-------
Table 7
SULFUR FORMS ANALYSIS9'b'c
ATOMIC ABSORPTION VS. ASTM PROCEDURES
Sample
Muskingum
Powhattan No. 4
Isabella
Mathies
Wi 1 1 i ams
Robinson Run
Shoemaker
Delmont
Marion
Lucas
Bird' No. 3
Marti nka
Meigs
Dean
Kopperston No. 2
Harris No. 1 and 2
North River
Homestead
Ken
Star
Eagle No. 2
Lower Kittanningf
Lucas
% w/w Pyritic Sulfur
AAS
0.22 ± .028
0.46 ± .064
0.06 ± .007
0.08 ± .000
0.28'± .049
0.08 ± .014
0.44 ± .148
0.22 ± .078
0.04 ± .007
0.22 ± .049
0.11 ± .014
0.12 ± .007
0.18 ± .035
0.20 ± .007
0.02 ± .000
0.02 ± .000
0.17 ± .028
0.22 ± .028
0.24 ± .050
0.04 ± .021
0.25 ± .004d
0.48 ± .038d
0.12 ± .007
ASTM
0.26 ± .007
0.43 ± .057
0.07 .007
0.02 .000
0.30 .035
0.08 .014
0.46 .120
0.20 .134
0.05 ± .014
0.20 ± .007
0.16 ± .035
0.12 ± .007
0.16 ± .035
0.16 ± .035
0.06 ± .035
0.07 ± .042
0.12 ± .021
0.22 t .092
0.30 ± .050
0.08 ± .028
0.19
0.33 ± .035
0.21 ± .034
Sample
Marion
Mathies
Meigs
Powhattan
Eagle No. 2
Jane
Fox
MeigsC
Powhattan No. 4
Muskingume
Mathiesc
Marion
Powhattan No. 4
Robinson Run
Lucas
Williams
Isabel la
Shoemaker
Meigs
Bird No. 3
Delmont
Eagle No. 2
Egypt Valley
% w/w Pyritic Sulfur
AAS
0.06 ± .021
0.02 ± .000
0.18 ± .035
0.46 ± .064
0.18
0.62
0.50
0.43
0.64
0.60
0,98 ± .007
0.34 ± .007
2.53 ± .000
2.72 ± .014
1.24 ± .007
1.94 ± .000
1.05 ± .042
2.18 ± .007
1.88 ± .191
2.64 ± .021
4.27 ± .014
2.66 ± .03dH
4.70 ± .004°
ASTM
0.05 ± .022
0.08 ± .000
0.16 ± .035
0.11
0.63
0.47
0.43
0.54
0.48
1.05 ± .065
0.90 ± .017
2.57 ± .060
2.89 ± .190
1.42 ± .082
2.23 ± .062
1.07 ± .070
2.19 ± .100
2.19 ± .030
2.87 ± .062
4.56 ± .044
2.67 ± .15d
5.07 ± .02°
I\J
co
Unless otherwise noted, all analysis have been performed on two samples of treated coal.
Values without standard deviation are single determinations.
CA11 values greater than 1% are untreated coal.
Average of 3 determinations.
eAnalysis from trial runs.
Sample from previous bench-scale program (Ref. 3).
-------
sulfur analysis rather than a sulfur forms analysis. The results are also
substantiated by the pyritic sulfur analysis of the final 23 hr samples
(see p. 32 for details of reaction conditions, including reaction times)
which were determined both by the AAS method and by the standard ASTM
procedure performed by an outside commercial laboratory (CT&E). The
pooled standard deviation for all 20 sets of analyses was 0.032 for the
AAS method but was 0.060 for the ASTM method. In addition, the number of
analyses which were rechecked and found to be wrong was much greater when
the ASTM procedure was used. These "outliers" are not included in the
above calculations. Thus, it appears that the AAS determination of iron
for the pyritic sulfur analysis gives a substantial improvement in preci-
sion over the ASTM procedure.
In all cases, the agreement with the values determined by the ASTM
method is excellent, although the AAS results tend to be slightly low in
certain cases. Because treatment by the Meyers Process tends to increase
the amount of color extractable by nitric acid, it is possible that these
small differences may partly be due to difficulty in determining the end
point of the ASTM titration. In general, however, the average values as
determined by both methods were statistically interchangeable, giving
further indication of the validity of the accuracy of the AAS method.
The AAS and ASTM determined values of the final pyritic sulfur content
of the treated coals are therefore reported without differentiation in
Appendix D and the two sets of duplicates were used to calculate the
pyritic sulfur removal for the 20 additional coals treated in this report.
4.3.2 Pyritic Sulfur Removal Results
Table 8 summarizes the results of the pyritic sulfur removal experi-
ments. The percentage removal may be calculated by dividing the differ-
ence between the initial and final weight percent pyritic sulfur by the
initial weight percent pyritic sulfur. However, because of the ash (both
pyritic and excess) that is removed, the remaining pyritic sulfur in the
treated coal is slightly concentrated, and calculation of removal on a
percent basis results in a value lower than is actually the case. For
this reason, a corrected value was also calculated which compares the
29
-------
Table 8
SUMMARY OF PYRITIC SULFUR REMOVAL DATA3
u>
Q
Mine
Warwick
MusMngum
Egypt Valley No. 2)
'owhattan No. 4
sabella
Mathles
Wi 1 1 i ams
Huiiphrey No. 7
Robinson Run
Shoemaker
Delff'Ont
Marion
Jafie
Lucas
jird iJo. 3
Fox
Martinka
Meiggs
Seam
Sewickley
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh Ho. 8
Pi ttsLiurgh
Pittsburgh
'Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Lower Freeport
lidOle Kittanning
4_rwpr Kittanni^o
Lower Ki ttarming
Lower Ki ttanning
Clarion lio. 1-A
Rank
hvAB
nvAb
nvAb
hvAb
hvAb
hvAb
twAb
hvAb
hvAb
hvftb
hvAb
nwb
hvAb
hvAb
1-,/h
fwAb
hvAb
hvBb
(tin
No.
1-3
4
-2
1-3
4
1-2
3
1-2
1-2
1-2
3
1-3
1-2
3
1-2
1-2
1-2
1-2
3
1-2
3
1-?
1-3
4
1-2
1-2
xn.
1me
23
13
23
13-226
13
23
23
23
23
23
23
23
23.5
23
23
23
23
11-236
23
23
23
?i
23
14
23
23
.each
hanqes
1
1
1
1
1
1
1
0
0
1
1
1
1
1
1
0
1
1
0
0
1
1
1
0
1
l*sbb
00
100
50
100
200
100
200
100
150
100
150
100
150
150
100
200
100
100
100
100
150
150
100
200
100
100
Wf mK pVfttTlC SULFUR I
.086
.65
.010
1.07
.025
2.75
-0.60
1.07
1.070
1.05
'.065
2.23
i . 062
1.59
1.114
2.89
'.190
2.19
^.100
4.56
t.044
0.90
'.017
1.44
±.098
i.087
?.82
-.062
3.09
'.017
1.42
'.010
2.19
'.030
LttlS. ft
FW
',043
0.06
0.24
.'.031
0.62
±.178 ,
0.38
0.44
-.051
0.04
0.04
'.0.00
0.05
-.035
0.29
-.086
0.10
0.14
'.055
0.08
•..012
0.08
0.46
f.lll
0.21
-.090
0.04
'.013
0.14
'..007
0.63
-.034
0.03
n. 13
'.034
0.37
-.163
n.26
0.12
-.006
0.17
'.029
/N
IM
+ .096
1.03
3.41
i.033
4.45
'.ISO
4.69
2.3!
^.079
2.71
1.03
1.070
1.00
±.074
1.94
'.072
2.13
1.45
».127
2.81
+ .190
2.11
1.73
'.149
4.35
'.100
0.86
'.021
1.30
i.098
0.81
>,.093
1.34
2.74
'.071
2.72
'.164
2.83
1.30
'.021
2.02
'.042
WRITE ftEMflWL 1
92
94
93
88
93
84
99
96
95
87
96
91
97
96
79
95
96
90
56
85
94
96
88
92
92
92
! "/M
92
95
94
89
93
85
99
96
95
88
96
91
97
96
80
96
96
91
60
35
94
96
89
93
92
93
4.0
0.9
3.5
...
1.9
—
0.3
3.3
1.7
—
3.5
0.5
5.1
2.0
1.5
0.8
—
2.6
1.2
5.3
—
0.4
1.3
-------
Table 8 (Cont'd)
Dean
No. 1
Kopperston No. 2
Harris No. 1&2
North River
Orient No. 6
Homestead
Eagle No. 2
Camp Nos. 142
Ken
Star
Wei don
Edna
Navajo
Belle Ayr
Colstrip
Lean
Mason
Campbell Creek
Eagle & No. 2 Gas
Corona
Herri n No. 6
Ho. 11
Illinois No. 5
No. 9 (W. Kentucky)
Ho. 9
No. 9
Des Moines No. 1
Wadge
Hos. 6,7,8
Roland-Smi th
Rosebud
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvBb
hvAb
hvBb
hvBb
hvBb
iivCb
hvCb
hvCb
subA
subA
1-2
1-3
1-2
1-2
1-2
1-3
4
5
1-2
1
2
3
4
1-3
4
5
6
1-2
1-2
1-3
4
1-3
1-3
4
1-3
1-3
23
23
13
23
23
23
23
13
23
13
14
14
23
13
23
23
13
23
23
23
13
23
23
6
6-10e
12-136
0
1
0
0
0
1
1
1
1
2
1
1
1
1
1
2
1
1
2
2
1
1
2
0
1
1-2
150
100
100
100
100
100
200
200
100
100
100
100
100
100
100
200
200
100
150
100
200
100
100
100
100
100
2.62
i.087
1.98
+ .062
0.47
±.026
0.49
+ .036
1.42
+ .026
1.30
+ .084
3.11
±.049
2.64
+ .154
2.80
±.120
2.85
+ .038
2.60
+ .100
5.2«
±.038
0.14
+ .015
0.28
, r\A A
± . U^H
0.22
+ .017
0.34
+ .015
0.17
+ .029
0.21
+ .045
0.04
±.029
0.03
+ .00
0.14
±.038
0.32
±.076
0.12
0.06
0.22
+ .056
0.36
0.11
0.33
0.19
0.62
+ .210
0.33
0.02
0.14
0.28
+ .021
0.24
±.029
0.47
±.099
0.15
0.06
±.020
0.04
±.040
0.03
0.03
+ .012
0.06
+ .006
2.45
±.092
1.77
' +.077
0.43
+ .039
0.46
+ .036
0.28
+ .046
0.98
±.113
1.18
1.24
2.89
±.074
2.28
2.53
2.31
2.45
2.18
+ .242
2.47
2.78
2.66
2.57
1.043
2.36
+ .104
4.77
+ .106
5.19
0.08
+ .025
0.24
+ .059
0.25
0.19
+ .021
0.28
+ .016
94
89
92
94
90
75
91 -
95
93
86
96
88
93
78
88
99
95
90
91
91
97
57
86
89
86
82
94
90
92
94
91
76
92
96
93
94
98
94
94
80
89
99
96
91
91
92
98
59
87
90
89
83
1.1
2.3
6.2
0.5
2.7
6.1
1.8
7.6
0.7
1.2
1.9
15
14
5.6
1.9
aWalker mine omitted due to low pyritic sulfur content (0.07%). b!00 mesh x 0 and 200 mesh x 0 coal is symbolized as 100 and 200, respectively.
This value is calculated by dividing the pyritic sulfur loss in £ w/w by the initial » w/w pyritic sulfur. This value is calculated by dividing
the number of millimoles of sulfur loss by the initial number of millimoles of pyritic sulfur. Indicates different reaction times with no
significant differences in results.
-------
weight of the pyrite in the treated coal to the weight of pyrite in the
untreated coal. The latter value, though harder to calculate because it
requires a material balance, is more nearly accurate than the former;
consequently, this value is used in the following discussions.
The results of the pyritic sulfur removal are very encouraging in
that, with the exception of the very low pyrite western coals, 90-99% w/w
pyritic sulfur removal was achieved for all the coals treated. The
western coals were reduced to a measured 0.09-0.06% w/w pyritic sulfur,
which were among the lowest values observed in the program. However, the
low initial pyritic sulfur content of these coals (0.14-0.34% w/w) obscures
this fact in the percentage removal calculations, where removal of only
59-89% was obtained.
The standard set of reaction conditions included a reaction time of
23 hours, one change of leach solution during the 4 to 6 hour time period,
and the use of 100 mesh x 0 coal. Although high removal was achieved with
the low pyritic sulfur Belle Ayr, Colstrip, Navajo and Kopperston coals
using reaction times of only 6-14 hours, these conditions were insufficient
for high removal from many of the other coals. Samples of the other coals
were further ground to 150 or 200 mesh x 0 to expose more finely divided
pyrite encapsulated in the coal and at the same time allow faster extrac-
tion, since the smaller size particles would thus present a greater sur-
face area for reaction. The 200 mesh x 0 Camp Nos. 1 & 2 coal was run for
23 hours (Run No. 5), which resulted in 99% pyrite removal compared to
80-89% removal (Run Nos. 1-4) for 100 mesh x 0 coal. The remaining pyrite
was reduced from 0.62% to 0.02% w/w. Since Run No. 5 indicated a much
increased rate of removal, an additional experiment (Run No. 6) was per-
formed with a total reaction time of 13 hours. This run resulted in 96%
pyrite removal with a final pyrite content of 0.14 w/w. Another set of
experiments, using 200 mesh x 0 Orient No. 6 (Run Nos. 4-5) coal, gave
much better removals than obtained with 100 mesh x 0 coal. In the 23-hour
run, the removal was increased from 76% to 92%, and the final pyrite con-
tent was reduced from 0.32% to 0.12% w/w. Reducing the reaction time to
13 hours gave an apparent increase in removal to 96%, with a final pyrite
content of 0.06% w/w. The small discrepancy is probably the result of
accumulated experimental errors.
32
-------
Because of this observed increased removal during reduced reaction
time, a series of 13 and 14 hour runs using 200 mesh x 0 coal was also
conducted with the Egypt Valle No. 21, Powhattan No. 4, Fox, Warwick, and
Wei don coals in order to check the generality of this phenomenon. These
runs resulted in increased pyrite removals from 89 to 93% for the Egypt
Valley coal; 85 to 99% for the Powhattan No. 4 coal; 92 to 95% for the
Warwick coal; 92 to 98% for the Wei don coal; and 89 to 93% for the Fox
coal. The corresponding final pyrite changes were 0.62% to 0.38%, 0.44%
to 0.04%, 0.09% to 0.06%, 0.47% to 0.15%, and 0.37% to 0.26%, respectively.
In a similar manner, grinding the Lucas coal to 150 mesh x 0 increased
removal by 9% to 94% and reduced the final pyritic sulfur content from
0.21% to 0.08%. Thus, grinding the coals to 150 or 200 mesh x 0 allows
a much faster rate of reaction, and equal or increased pyrite removal is
observed in all cases.
Since kinetic data were being generated with the final 20 coals treated
in this survey, the reaction times were held at 23 hours except in special
cases. However, based on the final pyritic sulfur content obtained after
13 hrs in the trial runs, the coal was further ground to either 150 or
200 mesh x 0 in order to ensure greater than 90% pyritic sulfur removal.
Using this technique, nine of the 20 coals were ground to 150 mesh x 0 and
six of the coals to 200 mesh x 0 in order to achieve this goal. In addi-
tion, it was found on the basis of samples taken from the reactor after
13 hours, that pyritic sulfur removal was greater than 90% for eleven
coals, greater than 80% for seven coals, and indeterminate for two other
coals (due to poor samples).
The data were examined by geographic region for the amount of fine-
ness required in order to achieve greater than 90% pyrite removal. It
was determined that, while it was not necessary to grind any Western coal
finer than the standard 100 mesh x 0 to obtain a low final pyritic content,
50-60% of the coals from both the Interior and Appalachian coal basins
needed to be ground finer than the standard 100 mesh x 0. Because of the
limited number of samples from the Interior Basin, no further correlation
could be made. However, for coals from the Appalachian Basin, it was
found that 75% of the samples from both the Pittsburgh (8 samples) and
Kittanning (4 samples) seams, 33% of the three Freeport samples, and 50%
33
-------
of the two Sewickley samples needed size reduction. Examination of the
Appalachian coal by stratigraphic groups showed that 70% of the 10 samples
from the oldest Monongahela series including the Sewickley (Meigs Creek
No. 9) and Pittsburgh seams required further grinding. In the Allegheny
Series including the Freeport and Kittanning seams, 60% of the 7 coals
needed further size reduction while only 20% (1 sample) of the remaining
6 different seam samples from the youngest Kanawha Group needed to be
reduced further. Thus, it appears that in order to obtain 90-100% pyrite
removal, 50-60% of the coals from the Eastern part of the U.S. must be
ground finer than 100 mesh (149y). For Appalachian coals this requirement
increases for the older stratigraphic groups. Furthermore, it was found
that additional comminution of the coal increased the rate of pyrite
removal substantially, so that in all but two cases the target of 90%
removal was achieved in 13 hrs or less instead of 23 hours.
The effect of coal particle size on the ultimate amount and rate of
pyrite removal has emerged as a very important process variable. Because
the present program was oriented toward complete pyrite removal, a detailed
study of particle size was not made. Thus, while it appears that 50-60% of
the Eastern coals must be ground finer than 100 mesh (149y) for complete
removal (under the standard set of conditions utilized here), it is not
known whether or not >90% removal could be obtained in certain cases if
the coal was reduced to only 80 mesh, 50 mesh or larger sizes. In addi-
tion, the exact effect of coal fineness on the rate of pyrite removal has
not been established. It is thus recommended that further work include
substantial studies on the effect of coal particle size on the extent and
rate of pyrite removal.
Although the precision of the results of this survey has been excel-
lent, Run No. 2 on the Eagle No. 2 coal and Run No. 3 on the Jane coal are
exceptions; the former shows lower than expected final pyrite, and the
latter shows higher than expected final pyrite. The data and circumstances
surrounding these experiments have been carefully examined and checked and
no systematic reasons can be found for these discrepancies. The high
standard deviation for Runs 1 and 3 on the Camp Nos. 1 and 2 coal led to
the discovery that the temperature controls were maintaining all the leach
34
-------
solutions 2-6 C below reflux; the spread in pyrite removals appears to
parallel these differences. Run No. 4, carefully held at reflux, resulted
in much higher removal. Although the results of the second set of 20 coals
are much more precise than the initial set, a close examination of the
results listed in Appendices C and D also shows that the spread between
triplicate pyritic sulfur values is often of the order of 0.1-0.2% w/w.
Thus, duplicate or triplicate runs or determinations are necessary in
order to obtain results that can be treated with a relatively high degree
of confidence.
4.3.3 Rate of Pyritic Sulfur Removal
The rate of pyrite removal was also followed for the 20 coals sampled
for this part of the survey by withdrawing slurry samples periodically
from the reactor. As discussed in Section 4.3.1.2, some difficulty was
encountered in obtaining representative samples from the reactor. The
principal problem was that the boiling and stirred leach solution still
acted as a float-sink medium for the coals. This was especially true for
the high ash ROM samples used in this survey. Thus, 15 coals were leached
with varying degrees of success before a satisfactory method of sampling
was developed. The metnod (Section 4.3.1.2 and Method D in Table 9) con-
sisted of using an aluminum tube that was rapidly inserted along the verti-
cal axis of the reactor and was closed off when it reached the bottom.
Assuming a uniform horizontal distribution, a representative slice was
therefore taken along the non-uniform vertical axis. When interpreting
the data in Tables 9 and 10, the data obtained by Methods A, B and C from
samples taken during the first six hours of leaching should be regarded
with some suspicion.
The rate data are summarized in Table 9 in terms of % pyritic sulfur
removal, and in Table 10 in terms of pyritic sulfur content. The data
indicate that for all coals tested, the major portion of the pyrite is
removed in six to seven hours with the average removal being 85 ±6%
(median 86%). After six to seven hours, pyrite removal slows down sub-
stantially; 90-95% removal is attained in 10-23 hours. Although signifi-
cant reaction amounting to more than 10% occurred for the Isabella, Bird
No. 3, and Meigs mines during the 12-23 hour interval, eleven mines had
35
-------
Table
u>
PYRITIC SULFUR REMOVAL AS A FUNCTION OF TIME IN PERCENT3 >b'c
Mine
lusklngum
Powhattan No. 4
Isabella
MatMes
Williams
Robinson Run
Shoemaker
Jelmont
larlon
Lucas
Bird No. 3
Fox
Marti nka
Meiggs
Dean
Kopperston No. 2
Harris Nos. 1&2
North River
Homestead
Ken
Star
Seam
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Middle Kittanning '
Lower Kittanning
Lower Kittanning
Lower Kittanning
Clarion 4A
Dean
Campbell Creek
Eagle & No. 2 Gas
Corona
No. 11
No. 9
No. 9
Methodd
B
A
Df
B
A
C
Df
B
C
Df
B
A
A
Df
B
D
D
A
D
D
D
D
D
B&C
B
Mesh6
100
100
200
100
150
100
150
150
100
150
200
100
100
150
150
200
100
100
150
100
100
100
100
100
150
Initial %
Pyritic
Sulfur
3.65
2.75
1.07
1.05
2.23
2.89
2.19
4.56
0.90
1.42
2.87
3.09
1.42
2.19
2.62
0.47
0.49
1.42
3.11
2.85
2.66
Median
Range
Time, Hours
0.5
(51 )a
_c
58
--
(67)
(58)
55
—
54
51
--
(57)
(74)
--
42*
42*
12
66
51
58
4.9
--
43
53
12-74
1.0
(57)a
i.-
68
..
(72)
68
--
69
66
--
46
--
51
45*
58*
34
74
73
74
71
--
68
34-74
2.0
76
77
76
70
77
83
67
76
57-8
3.0
34
—
-
(68)
(87)
37
-
81
-
80
85
80
-
77
63
77*
59
87
84
77
88
78
34-8
5.0
73*b
--
82
54*
74
(92)
87
42*
85
87
-
88
85
63*
68
74
69
83
80
83
88
84
82
42-88
6.0
75*b
85
90
-
--
87
--
83
89
81
88
89
87
75-90
7.0
-
88
--
77
75
90
83
91
91
87
77-91
8.0
80
64
77
94
89
90
92
87
81
87
73
91
85
87
64-94
9.0
.-
74)
79
10.0
69
95
87
82
93
87
69-95
12 0
72
90
92
83
92
87
93
90
72-9
3 0
86
92
79
90
94
--
95
—
96
94
99
82
91
84
84
91
85
90
79-9
23 0
93
84
97
96
95
87
96
97
89
98
95
96
85
N.A.
95
N.A.
92
92
94
94
90
93
90
91
94
84-97
aValues in parenthesies are suspected of being high due to lack of ferrous ion accumulation and known deficiencies in the method of sampling.
bThe precision of the starred values is poor.
CA dash indicates that the value was not included due to extremely poor precision or illogical analysis (e.g., gain).
dSee Section 4.3.1.2, p. 24 for exact details. The slurry sample was withdrawn from the bottom of the reactor in Methods A & B. In Methods C & D, a
thief technique was used.
eTop size of coal.
fResults are from a single repeat experiment.
-------
Table 10
PYRITIC SULFUR REMOVAL AS A FUNCTION OF TIME-% W/W PYRITIC SULFUR*>b>C
Mine
Muskingum
Powhattan No. 4
Isabella
Mathies
Williams
Robinson Run
Shoemaker
Oelmont
Marion
Lucas
Bird No. 3
Fox
Martinka
Meiggs
Dean
Kopperston No. 2
Harris No. 1 & 2
North River
Homestead
Ken
Star
Seam
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Middle Kittanning
Lower Kittanning
Lower Kittanning
Lower Kittanning
Clarion 4A
Dean
Campbell Creek
Eagle & No. 2 Gas
Corona
No. 11
No. 9
No. 9
Methodd
B
A
Df
B
A
C
Df
B
C
Df
B
A
A
Df
B
D
D
A
D
D
D
D
D
B&C
B
Mesh6
100
100
200
100
150
100
150
150
100
150
200
100
100
150
150
200
100
100
150
100
100
100
100
100
150
Initial %
Dv/yi fir
ryn 1 1 c
Sulfur
3.65
2.75
1.07
1.05
2.23
2.89
2.19
4.56
0.90
1.42
2.87
3.09
1.42
2.19
2.62
0.47
0.49
1.42
-rn —
2.85
2.60
Time, Hours
0.5
(1
(1
1
(0
(0
1
1
1
(0
(0
.80)d
.20)
.16
--
.41)
.93)
.00
—
.01
.08
—
.39)
.37)
--
0.83*
1
2
.26*
.30
0.16
0.24
0.60
1
.-
.47
1.0
(1.58)a
(1.10)
0.87
--
(0.63)
0.72
--
0.67
0.75
0.76
--
1.51
0.78*
0.92*
1.74
0.12
0.13
0.37
--
0.87
2.0
0.67
0.52
0.52
0.92
•OT
0.48
3.0
1.24
__b
--
(0.34)
(0.30)
0.30
--
0.42
--
0.18
0.21
0.29
--
0.70
0.53
0.72*
1.08
0.06
0.08
0.33
0.56
5.0
0.99*D
_b
0.50
0.49*
0.27
(0.18)
0.28
1.67*
0.33
0.29
—
0.11
0.21
1.07*
0.46
0.56
0.82
0.06
0.29
0.33
0.42
6.0
0.90*°
0.41
0.26
--
0.27
-
0.18
--
0.53
0.05
0.35
0.29
7.0
--
0.27
--
0.67
0.66
0.05
0.27
0.24
8.0
0.72
0.39
0.24
0.14
0.24
0.09
0.12
0.19
0.54
0.40
0.39
0.04
0.22
9.0
__b
0.72
0.47
10.0
0.86
0.12
0.28
0.40
0.18
12.0
0.78
0.22
0.18
0.24
0.04
0.18
0.18
13.0
0.52
0.23
0.23
0.10
0.14
—
0.12
—
0.04
0.08
0.02
0.51
0.28
0.34
0.42
0.04
23.0
0.24
0.44
0.08
0.04
0.05
0.29
0.10
0.08
0.46
0.04
0.21
0.04
0.21
N.A.
0.13
N.A.
0.12
0.17
0.17
N.A.
0.03
0.14
0.28
0.24
a) Values in parenthesis are suspected of being high due to lack of ferrous In accumulation and known deficiencies in the method of sampling.
b) The precision of the starred values is poor:
c) A dash indicates that the value was not included due to extremely poor precision or illogical analysis (e.g., gain).
d) See Section 4.3.1.2, page 24 for exact details. The slurry sample was withdrawn from the bottom of the reactor in Methods A & B.
In Methods C and D, a thief technique was used.
d) Top size of coal in mesh.
f) Results are from a single repeat experiment.
-------
insignificant removals of 5% or less and six of these mines showed zero or
negative removal in at least one set of runs. In respect to the remaining
mines, one was leached for only 13 hours, and no 13-hour samples were taken
in two cases. Thus, it appears that a 23-hour reaction time should be
considered an upper limit for leaching and that, depending on the coal,
85-95% removal can be achieved in 6-13 hours.
The data for leaching times below six hours is not nearly as easy to
interpret because of individual coal variations and because the problems
with sampling are most evident when the pyrite content is high. This can
readily be seen for the Muskingum, Powhattan No. 4, Mathies, Williams,
Shoemaker, Marion, Lucas and Fox coals, for which as long as 13 hours was
necessary for the ferrous ion build-up in solution to account for the
apparent pyrite decrease, assuming a sulfate/sulfur ratio of 1:5 (Fig-
ure 1). These values, which are in parentheses in Tables 9 and 10, were
identified by checking the ratio of total ferrous ion present to the
amount of ferrous ion expected for the measured pyritic sulfur decrease
(see Section 4.3.4 and Table 13 for details). A value less than one indi-
cates that the measured pyritic sulfur removal obviously is in error on
the low side. However, a value greater than one may also be in error due
to a low measured pyritic sulfur coupled with a high degree of ferric ion
reactivity with the coal. Since this reactivity with the coal appears to
be nonlinear with time, there is no known adequate way to determine the
extent of this error.
In spite of these problems, a substantial amount of information about
the pyrite removal in the early stages of the leaching has been obtained.
Median removal values have been determined from the data in Table 9 and
were found to be 53% in 0.5 hours, 68% in 1.0 hour, 78% in 3.0 hours, and
87% in 6.0 hours. The range of values was substantial: 12-74% at
0.5 hour, decreasing to 34-74% at 1.0 hour and closing further to 75-90%
in 6.0 hours. Although the main reason for these variations may be due to
sampling problems, it is likely that they represent significant individual
differences between coals.
The median pyritic sulfur removal values in Table 9 are plotted as a
function of time in Figure 3. Note that, except for a small amount of
38
-------
10 12 14
Leach Time, Hrs.
Figure 3. Pyrite Removal as a Function of Time
scatter in the 4-8 hour region, a smooth line can be drawn through all the
points. This is an indication that, despite the wide range of removal
rates, the kinetic expression is the same order in pyrite, ferrous, and
ferric ion concentration in all cases. The peculiar characteristics of
the coal, such as pore structure, size distribution of pyrite, etc., may
thus be primary factors affecting the rate constant, causing the removal
curve for a particular coal to fall either above or below that of Fig-
ure 3. Since this is potentially a very significant area in terms of
predictions of the applicability of the Meyers Process, it is important
that these data be thoroughly examined at a future date for the purpose
of fitting a rate expression to these results.
4.3.4 Heat Content Changes and Ferric Ion Consumption
The data in Table 11 presents the results of ferric sulfate extraction
of pyritic sulfur from coals in terms of changes in heat content of the
coals, and suggests a relationship between this effect and excess ferric
39
-------
Table 11
SUMMARY OF HEAT CONTENT CHANGES AND EXCESS FERRIC ION CONSUMPTION*
Coal Mine
Warwick
Muskingum
Egypt Valley No. 21
Powhattan No. 4
Isabella
Mathies
Williams
Humphrey No. 7
Robinson Run
Delmont
Marion
Jane
Lucas
Bird No. 3
Fox
Martinka
Meigs
Dean
No. 1
Kopperston No. 2
Harris NOS. 1 8 2
Orient No. 6
Homestead
Eagle No. 2
Camp Nos. 1 8 2
Ken
Star
Edna
Havajo6
Belle Ayr
Col strip
Seam
Sewickley
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pi ttsburqh
Upper Freeport
Upper Freeport
Lower Freeport
Middle Kittanning
Lower Kittanning
Lower Kittanning
Lower Kittanning
Clarion 4fl
Dean
Mason
Campbell Creek
Eagle 4 No. 2 Gas
Herrin No. 6
No. 11
Illinois No. 5
No. 9 (U. Kentucky
No. 9
No. 9
Wadge
Nos. 6, 7, 8
Roland-Smith
Rosebud
Dry Basis, btu/lb
Initial
8612
110H
10594
8603
8216
8154
13013
13631
12962
9495
11012
11046
11932
13451
10551
12973
7552
10246
12107
13054
10957
12414
11163
11935
10566
11103
12099
12308
12246
10050
12034
11591
Final
9365
11578
11506
9480
9312
9024
13587
13949
13764
10156
12108
11720
12392
13884
11500
13174
8138
11063
12663
13341
11340
12556
11034
12266
11401
11740
13689
12650
12201
10353
11520
11321
Chan
btu/lb
* 753
+ 564
+ 912
+ 877
+1096
+ 870
+ 574
+ 318
+ 802
+ 661
+1096
+ 674
+ 460
+ 433
< 949
+ 201
+ 586
+ 317
« 556
* 287
+ 383
+ 142
- 129
« 331
+ 835
+ 635
+ 590
+ 342
- 45
+ 303
- 514
- 270
£&
", w/w
+ 8.7
+ 5.1
+ 8.6
+10.2
+13.3
+10.7
+ 4.4
+ 2.3
+ 6.2
+ 7.0
+ 10.0
+ 6.1
+ 3.9
+ 3.2
+ 9.0
+ 1.5
* 7.8
+ 8.0
+ 4.6
+ 2.2
* 3.5
+ 1.1
» 2.8
« 7.9
t 5.7
+ 4.9
» 2.8
- 0.4
+ 3.0
- 4.3
- 2.3
Dry Mineral Matter
Free Basis,
Initial
153S1
14608
14851
14573
15197
14715
15309
15356
15321
15049
15842
15517
15682
14902
15835
15347
(16447)d
14503
15047
14997
(16300)
15585
14686
14994
14552
14614
14620
13602
13849
13111
13065
Final
15184
14106
14554
14607
15199
14925
15142
15137
15078
14841
15582
15533
15440
14930
15601
14775
15373
14250
14932
14743
15687
15302
14072
14579
14238
14209
14006
13467
13186
12908
11958
11993
btu/lb
Chana
btu/lb
- 197
- 502
- 297
+ 34
+ 2
+ 210
- 1F-7
- 219
- 243
- 208
- 260
+ 21
- 242
+ 28
- 234
- 572
-1074
- 253
- 115
- 254
- 613
- 283
-1063
- 614
- 415
- 314
- 405
- 614
- 864
- 416
- 638
-1153
-1072
5
% w/w
-1.3
-3.4
-2.0
+0.2
0
+1.4
-1.1
-1.4
-1.6
-1.4
-1.6
+0.1
-1.5
+0.2
-1.5
-3.7
(-6.5)
-1.7
-0.8
-1.7
(-3.8)
-1.8
(-6.4)
-4.2
-2.8
-2.2
-2.8
-4.2
-6.0
-3.1
-4.8
-3.8
-8.2
ntt
Excess
erric Ion
134
242
86
121
105
179
124
98
120
194
93
47
61
143
92
76
98
295
198
165
67
112
97
570
177
116
392
785
981
515
659
974
1520
mM/g
Excess
-erric Ion
1.36
2.42
0.88
1.21
1.05
1.79
1.24
1.00
1.20
1.94
0.93
0.47
0.62
1.43
0.92
0.72
0.98
2.95
1.98
1.69
0.67
1.12
0.97
5.70
1.83
1.20
3.92
7.85
11.31
5.33
6.66
12.04
19.09
++
Total Fe Expt.
Total Fe+* Calc!>
1.45
1.20
.33
1.79
3.04
1.40
1.43
.27
.71
.35
.79
.74
.21
0.89
1.48
1.92
1.51
1.90
1.97
2.53
1.48
2.24
1.47
.34
.96
3.09
1.56.
--c
--C
--C
-- c
a) These values are the average of replicate 23-nour runs, except where noted.
b) The calculated values are based on a sulfatetsulfur ratio of 1:5.
c) These values have not been calculated because the low initial pyrite makes them uie
d) Values in parenthesis are questionable due to high correction factors.
e) Run No. 4.
ion consumption. Because pyrite removal is in effect the removal of low
btu "ash" (2995 btu/lb), its removal in most cases has more than compen-
sated for any oxidation of the coal matrix. Thus, with the exception of
the Western coals and one Western Interior Basin coal, heat content
increases of 1.1-13.3% were observed. The Western coals, with low
initial pyrite (0.14-0.34% w/w) and a high order of reactivity with
ferric ion, had heat content changes of +3.0 to -4.3%.
Although dry btu determinations are useful for those interested in
shipping and using coal, a true picture of the effect of ferric ion
40
-------
oxidation of the organic coal matrix and its relationship to excess ferric
ion consumption can only be obtained by examining the dry mineral matter
free heat contents. These values (also listed in Table 11) show a heat
content loss of 3.1 to 8.8% for the Western coals, 2.0 to 6.0% loss for
the Eastern and Western Interior Basin coals, and a +1.4 to -3.7% change
for the Appalachian Basin coals.
The heat content changes for the Martinka, Kopperston and North River
mines are anomalous in that all three have abnormally high untreated dry-
mineral-matter-free heat contents of 16,300-16,600 btu/lb which dropped
substantially after treatment to the area normal for other coals, resulting
in calculated heat content losses of 600-1100 btu/lb. The excess ferric
ion that reacted with 100 g of these coals was only 67-98 mM, which is
entirely inconsistent with the 1000-1500 mM ferric ion required for a
similar loss for the Belle Ayr and Col strip coals. Because these coals
have an exceptionally high ash content, these errors may be due to the
assumption used in the dry-mineral-matter-free calculation. In addition,
sample calculations have shown that the dry ash free (daf) heat content
becomes very sensitive to small changes in analytical values when the ash
content of the coal is >40%. For these reasons, these results are con-
sidered suspect and are indicated by parentheses in Table 11. These data
are therefore not included in the following calculations.
The differences in dry-mineral-matter-free heat content loss were
averaged for all three groups of coals (Table 12). The Appalachian coals
averaged a loss of 172 ±185 btu/lb or 1 ±1.2%; the Eastern Interior Basin
coals, 592 ±237 btu/lb or 4 ±1.5%; and the Western coals, 896 ±331 btu/lb
or 7 ±2.6%. These values were found to be mathematically significant by
the t test at the 99% level in all three cases, assuming that the method
— (78)
of calculation did not introduce any systematic errorv ' '. Thus, in view
of experimental uncertainties and calculation assumptions, heat content
loss for the Appalachian coals must be considered nil; for the Interior
Basin coals, small; and for the Western coals, significant.
The extent of reaction of the ferric ion with the coal matrix is
illustrated by examining excess ferric ion consumption. Ferric ion
41
-------
consumption was calculated by subtracting from the total ferrous ion pro-
duced the amount of ferrous ion that should have been produced by pyrite
removal, assuming the reaction chemistry of Figure 1 and dividing by the
actual amount of coal present (since the ferric ion can attack both the
organic and ash contents of the coal). When the values are calculated on
a dry-mineral-matter-free basis, the scatter increases substantially.
Table 12
AVERAGE HEAT CONTENT LOSSES AND FERRIC ION CONSUMPTION
Coal Basin
Appalachian
Interior
Western
Dry Mineral Matter Free Heat Content, btu/lb
Average
Initial
15166+426
14658+208
13406+382
Average
Loss
172+185
592+232
896+331
Heat Content Loss
Per % Loss
172
148
128
1 49+22a
Excess Ferric Ion Consumption
Average
mM/g
1.3+0.6
5.2+3.5
10.8+6.3
mM/g Per %
Heat Content Loss
1.3
1.3
1.5
1.4+0.13
aAveraqe value for all three coal basins
These calculations show that the coals fall into three distinct
classes, with the Appalachian Coal Basin coal consuming 0.47-2.95 mM/g
excess ferric ion, the Interior Coal Basin coal 1.20-11.31 mM/g excess
ferric ion and the Western coals 5.33-19.09 mM/g excess ferric ion. The
corresponding averages are 1.3, 5.2 and 10.8 mM/g, respectively. In gen-
eral, the results follow the degree of metamorphism of these coals. The
Western coals have low rank and an open pore structure, which provides an
abundance of active sites for reaction. The Eastern Interior Basin coals
have a higher rank but still have an open pore structure that allows sub-
stantial reaction, while the Appalachian Basin coals, though of similar
rank, have the most closed pore structure and as a result show very little
reaction with the ferric ion.
The data were examined further to establish a relationship between
heat content loss and excess ferric ion consumption. These results, tabu-
lated in Table 12, indicate that 0.94 ±0.12 mM/g ferric ion is consumed
for every 100 btu/lb loss in heat content.
4.3.5 Ferric Ion Consumption as a Function of Time
The rate of ferric ion consumption was also followed as a function of
time, both as an independent check on the pyrite removal values and to
42
-------
determine whether the ferric ion reactivity with coal is linear as a
(1 23^
function of time. Previous workv ' * ' has shown that ferric ion reacts
with pyrite according to Eq. 1:
FeS2 + 4.6 Fe2 (S04)3 + 4.8 H20 -> 10.2 FeS04 + 4.8 H2$04 + 0.8S (1)
to produce 10.2 mM ferrous ion per mM of pyrite (or 5.1 mM ferrous ion per
mM pyritic sulfur) and a sul fate/sulfur ratio of 1.5. Assuming this
stoichiometry, the mM/g coal excess ferric ion consumption (i.e., the
amount of reaction of ferric ion with the coal) can be calculated at any
time, t , if the actual pyrite and ferrous ion concentrations are known
A
at that time. The calculation is shown in Eq. 2 and values of excess
ferric ion are listed as mM/g in Table 13.
mM/g Coal Excess Ferric _ Total Reaction of
Ion Consumption Ferric Ion with Coal
mM/g Coal Ferrous Ion - mM/g Coal Ferrous Ion Generated
by Pyritic Sulfur Removal (2)
These values can then be used to calculate the ratio shown in Eq. 3 and
tabulated in Column 5 of Table 13.
Ratio = Actual Ferrous Ion / Ferrous Ion Generated by Pyrite
Present in mM/g Coal / Removal in mM/g Coal (3)
The value for Eq. 2 must be positive, and the value for Eq. 3 must be 1.0
or greater by definition. It should be noted, however, from the data
shown in Table 13, that several negative values for Eq. 2 were obtained,
indicating that the input data for either ferrous ion or pyrite concentra-
tion were incorrect. As a result of this finding, both the means of
sampling and the analysis of both leach solution and coal were examined
for possible error. This examination indicated that sampling error was
clearly the cause, since all other methods were standard and tested proce-
dures. This problem and its solution is documented in Sections 4.3.1.2
and 4.3.3 and will not be further discussed in this section.
43
-------
Table 13
FERRIC ION CONSUMPTION AS A FUNCTION OF TIME*
Mine
Muskingum
Powhattan
No. 4
Isabella
Mathies
Williams
Robinson Run
Shoemaker
Delmont
Marion
Lucas
Bird No. 3
OX
Martinka
Meigs
Dean
KODperston
Ho. 2
Harris No.
1 I 2
North River
Hoaestead
Cen
Star
Seam
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Middle Kittanning
Lower Kittanning
Lower Kittanning
Lower Kittanning
"larion 4A
Dean
Campbell Creek
Eagle « No. 2 Gas
Corona
No. 11
No. 9
No. 9
Sampl ing
Method
A
D
B
A
c
0
B
C
0
B
A
A
D
B
D
D
A
D
D
D
0
0
BtC
B
Meshc
100
200
100
150
100
150
150
100
150
200
100
100
150
150
200
100
100
150
100
100
100
100
100
150
Excess
Ferric
lond.e
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
•H/9
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
T*/(I
Ratio
mM/g
Ratio
mM/g
Ratio
mM/g
Ratio
Time, Hours
0.5
0.81
-0.94
0.62
0.56
-1.22
1.58
-1.32
-0.14
0.86
-0.77
0.63
0.88
1.45
2.93
-2.61
-0.08
0.96
0.87
1.49
3.74
-1.04
-0.13
0.84
-0.76
0.55
--
--
2.15
-3.67
_„
--
0.24
1.26
0.43
1.29
1.71
4.36
0.25
1.50
0.51
2.33
0.07
1.05
0.59
1.24
1.51
1.!I4
1.0
0.96
-0.68
0.74
1.03
1.34
1.44
-4.02
0.45
1.40
-0.75
0.70
1.25
1.52
5.97
-0.93
-0.33
0.86
0.93
1.41
5.52
-1.04
0.11
1.09
-0.30
0.84
1.35
2.29
2.61
-8.11
-1.84
0.49
0.65
1.64
0.44
1.22
1.51
2.08
0.50
1.90
0.52
1.90
0.12
1.0'
0.35
1.10
_.
--
1.30
1.47
2.0
1.33
1.40
1.69
1.62
1.00
1.38
-2.02
0.56
1.00
1.26
3.0
1.14
-0.25
0.91
0.95
2.57
0.58
1.47
-0.49
0.84
3.21
5.12
0.09
1.03
3.13
3.94
0.12
1.10
0.04
1.02
2.35
2.31
2.78
6.83
-2.04
0.58
0.80
1.57
1.04
1.45
1.45
1.59
0.77
2. IB
0.76
2.16
0.56
1.32
0.56
1.15
2.22
1.68
5.0
1.09
•0.05
0.98
2.56
1.71
0.82
1.89
0.75
1.58
-0.20
0.94
2.36
1.76
2.20
2.13
0.34
1.12
1.77
1.59
2.90
2.50
0.22
1.17
0.23
1.11
0.86
1.30
1.07
1.70
1.30
1.50
1.64
1.57
0.94
2.41
0.92
2.34
O.S2
1.46
1.91
1.46
0.88
1.2?
2.81
1.81
6.0
1.29
2.14
1.99
•0.36
0.94
2.91
2.48
1.72
1.82
1.96
0.62
3.39
1.84
1.89
1.47
3.70
2.01
7.0
1.32
1.15
1.33
0.63
1.21
1.40
1.33
0.56
1.16
2.10
1.68
1.07
2.53
3.85
1.94
2.20
1.54
4.17
2.11
8.0
0.83
1.77
-0.05
0.98
1.07
1.34
3.57
2.83
0.47
1.13
-2.01
0.62
1.28
1.78
0.88
2.28
0.88
1.46
9.0
-0.32
0.92
1.89
1.69
10.0
0.88
1.29
0.15
1.04
12.0
0.75
1.24
1.32
1.41
1.20
1 .04
2.17
1.76
1.16
2.63
0.89
1.45
5.25
2.36
13.0
1.94
1.39
1.17
1.37
0.82
1.54
1.21
1.31
0.67
1 .11
0.29
1.21
0.59
1.28
3.69
2.66
0.72
1.19
-2.19
0.61
0.98
1.48
2.58
1.88
1.72
1.49
0.67
1 .97
5.00
2.20
6.12
2.5?
23.0
2.42
1.45
1.21
1.33
3.65
1.84
1.05
1.79
1.79
3.04
1.24
1.40
3.11
1.92
1.20
1.27
1.94
1.71
2.60
1.76
0.93
1.16
0.47
1.35
1.43
1.74
..
--
0.92
1.21
2.95
1.92
1.98
1.51
--
--
1.12
2.53
0.97
1.48
5.32
2.15
3.92
1 .96
7.85
3.09
aThese values correlate with those in 7flh1e<> 9 .ind IT.
^Sec Section 4.3.1.2, p. 24 for exact details. The slurry sa^-ole v.is w
a "thief" technique was used.
Top size of coal
^irtl/g * calculated irnllimolcs of ferric ion tnrtt re
-------
to conclusively show whether or not the effect is linear. Since the rate
(1 3)
of removal of pyriteisa nonlinear reactionv ', the variation of the ratio
in Eq. 3 was closely examined. A constant ratio would indicate coal reac-
tivity paralleling the rate of pyrite removal. The results indicate that
for the Powhattan No. 4, Williams, and Homestead mines the ratio increased;
for the Shoemaker, Lucas, Harris No. 1 & 2 and North River mines, there
was a slight increase; the Martinka and Kopperston mines showed small
changes and the Dean mine showed a drop. Thus, it appears that reactivity
with the coal matrix depends to a large extent on the nature of the coal
and that this phenomenon should be examined in detail in the future,
4.3.6 Removal of Residual Sulfate
The data presented in Table 14 indicate that substantial sulfate is
retained on some coals when a minimal coal wash procedure is used after
extraction of pyritic sulfur. The wash procedure consists of three 500 ml
hot water rinses of the coal on the filter funnel after filtration of the
reaction mixture. This procedure, which was used on many trial runs and
the final triplicate runs for Camp Nos. 1 & 2 and Orient No. 6 coals,
resulted in sulfate values (sulfur as sulfate, but referred to only as
sulfate in the following discussion) ranging from a very acceptable
0.06-0.10% (Jane, Humphrey No. 7 and Col strip) to a very high 0.45-0.85%
(Mathies, Orient No. 6, Eagle No. 2, Belle Ayr, and Edna) with the majority
of coals falling in the range of 0.2-0.4% (see Table 14).
It is currently believed that sulfate retained on the treated coals
can be reduced or eliminated by one or more of the following methods:
(a) control of acidity and iron concentration or form during extraction,
(b) selection of optimum filtration temperature, (c) equilibration of the
leach solution with the coal as in the thickener section of a process plant,
or (d) selection of the appropriate washing parameters. Because detailed
evaluation of these processing techniques was not practical during this
program, only those approaches involving washing techniques were investi-
gated. Several of these methods have been evaluated under a separate EPA
program for bench-scale experimentation (Contract No. 68-02-1336, Refer-
ence 3) and have been found to be effective.
45
-------
Table 14
SULFATE CONTENT OF TREATED COALS*
(% w/w)
Mine
Warwick
Muskingum
Egypt Valley No. 2
Powhattan No. 4
Isabella
Mathies
Wi 1 11 ams
Humphrey No. 7
Robinson Run
Shoemaker
Delmont
Marion
Jane
Lucas
Bird No. 3
Fox
Martinka
Meigs
Dean
No. 1
Kopperston No. 2
Harris Nos. 1&2
North River
Orient No. 6
Homestead
Eagle No. 2
Camp Nos. 1&2
Ken
Star
Wei don
Edna
Navajo
Belle Ayr
Col strip
Seam
Sewickley
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Lower Freeport
Middle Kittanning
Lower Kittanning
Lower Kittanning
Lower Kittanning
Clarion 4A
Dean
Mason
Campbell Creek
Eagle & No. 2 Gas
Corona
Herri n No. 6
No. 11
Illinois No. 5
No. 9 (W. Kentucky)
No. 9
No. 9
Des Moines No. 1
Madge
Nos. 6,7,8
Roland-Smith
Rosebud
Mesh
100
150
100
100
100
150
100
100
150
100
200
100
100
100
150
100
100
100
150
100
100
TOO
100
200
100
100
100
100
150
100
100
100
100
100
% W/W SULFATE
nitial
0.01
0.06
0.14
0.19
0.04
0.04
0.04
0.01
0.06
0.05
0.08
0.02
0.00
0.05
0.05
0.05
0.07
0.06
0.15
0.08
0.03
0.03
0.07
0.01
0.10
0.04
0.06
0.26
0.24
0.15
0.00
0.03
0.00
0.00
Regulara'b
12-14 Mrs.
...
0.11
0.08
0.04
0.02
0.06
0.04
0.05
0.05
0.08
0.13
0.07
0.08
0.17
0.18
0.12
0.15
0.12e
0.14
0.06
Minimala'b
12-14 Hrs.
0.35
0.25
0.65
0.10
0.40
0.06
0.23
0.31
0.22
0.26
0.30
0.45d
0.40
0.85d
0.42d
0.38
0.42
0.31
0.68
0.54
0.64
0.06
Regular3'0
21-23 Hrs.
0.14
0.17
0.11
0.12
0.01
0.10
0.06
0.10
0.00
0.08
0.06
0.06
0.06
0.13
0.11
0.09
0.08
0.14
0.16
0.09
0.08
0.06
0.09
0.22
0.30
0.23
0.28
0.26
0.34
0.18
0.49
0.85
aSee text for explanation of procedure.
Most of the data in this column is derived from single analysis trial runs.
cThe data in this column are derived from the average of the analysis of two
or three runs.
d23-hr. run.
e6-hr. run.
46
-------
Table 15 summarizes sulfate extraction experiments performed on the
treated Camp Nos. 1 and 2 coal. Note that both methanol and aqueous
methanol are much less effective than water in reducing the sulfate con-
tent of the coal, but that the addition of 1% v/v sulfuric acid to aqueous
methanol reduces the sulfate to 0.24% w/w. In addition, basic solutions
such as 5% w/v sodium carbonate and 10% v/v concentrated ammonium hydroxide
in aqueous methanol, and chelating agents such as 3% w/w ethylenediamine
tetraacetic acid and 10% w/w tetraethylene tetraamine, are apparently
slightly more effective than water in reducing the sulfate level.
Table 16 summarizes a second set of sulfate extraction experiments
performed on treated Orient No. 6 coal. With this coal, an additional wash
with either water, 0.1-3N sulfuric acid, or IN oxalic acid for one hour at
elevated temperature was effective in reducing the sulfate level from 0.62
to 0.25% w/w or less. Washing with IN sulfuric acid at 30°C (Expt. 6) was
Table 15
SPECIAL SULFATE REMOVAL EXPERIMENTS
CAMP NOS. 1 AND 2 COALa.b
Experiment
1
2
3
4
5
6
7
8
Reagent
H20
CH3OH
aq.CH3OHc
1% H2S04 in aq. CH3OHC
5% Na2C03 in aq.CH3OHc
10% NH4OH in aq.CH3OHc
3% EDTA in aq. CH3OHC
10% Tetraethylene
tetraamine in aq. CH3OH
Temp.,°C
Reflux
Ref 1 ux
Ref 1 ux
Reflux
Reflux
Reflux
Reflux
Reflux
Final % S04> w/w
0.19
0.33
0.49
0.24
0.13
0.20
0.13
0.11
alnitia1 sulfate retention 0.42% w/w, the ratio of coal to extraction
solution was 1:60 w/v
^Extraction time of four hours followed by thorough water wash
cMethanol:water ratio of 7.3
47
-------
Table 16
SPECIAL SULFATE REMOVAL EXPERIMENTS, ORIENT NO. 6 COALa'b
Experiment
1
2
3
4
5
6
7
Reagent
H20
0.1N H0SQ.
2 4
0.5N H2S04
l.ON H2S04
3. ON H9SOA
2 4
l.ON H2S04
IN Oxalic Acid
Temp . , °C
^90
^80
^80
^80
*v80
^30
-V60
Final % S04> w/w
0.25
0.21
0.23
0.19
0.23
0.36
0.16
Initial sulfate retention 0.62% w/w, the ratio of coal to extraction solu-
tion was 1:20 w/v
Extraction time of one hour followed by thorough hot water wash
not as effective, giving a final sulfate value of 0.36% w/w and indicating
that elevated temperature is necessary for more effective sulfate removal.
However, since the results of all 7 experiments are from single trials and
since the values, with the exception of Experiment 6, are grouped so
closely, the remaining six methods (Methods 1, 2, 3, 4, 5 and 7) in Table 16
can be considered equally effective at this point.
Based on the above experimentation, water washing as well as washing
with dilute sulfuric acid is capable of removing residual sulfate. Dilute
sulfuric acid should be advantageous in those cases where basic iron sul-
fates are present. Basic solutions or chelating agents, though effective,
would introduce unnecessary process expense and should not be considered if
the above methods are effective. Therefore, the following standard proce-
dure was adopted for the survey studies in order to ensure, without opti-
mization, a low level of sulfate in the treated coals.
The extracted coal is slurried with 2 Jl of IN sulfuric acid at
MJOOC for 2 hours, filtered and stirred with another 2 I IN sul-
furic acid at ^800C for an additional two hours. After
48
-------
filtration, this procedure is repeated with 2 £ water at ^80 C.
If scheduling does not permit the coal to be extracted with
toluene immediately, stirring is continued at ^50°C for an
extended period until filtration and extraction can be
performed.
The results listed in Table 14 are summarized in Table 17 and show
that the final sulfate content can be reduced to 0.06-0.17% w/w for the
Appalachian Basin coals, 0.17-0.35% w/w for the Eastern and Western Interior
Basin coals, and 0.06-0.85% w/w for the Western coals using this method.
The median final sulfate values for 23 hr runs involving the Appalachian
and Interior Basin coals were 0.09% and 0.28%, respectively, indicating
that sulfate retention is much more pronounced for the Interior Basin coals.
Data for 12-14 hr reaction times indicate that reaction time did not sig-
nificantly affect the final median sulfate content of the Appalachian
coals, while the median for the Interior Basin coals is reduced 0.11% to
0.17%. With the Western coals, reaction times of 6-14 hrs were necessary
in order to prevent excessive sulfate retention. Thus, given a standard
set of working conditions, it can be concluded that sulfate retention
depends both on the coal basin in which it is mined and to a certain extent
on the coal leaching time.
Table 17
SUMMARY OF TREATED COAL SULFATE CONTENT
(% w/w)
Appalachian
a) 23 hrs.
b) 12-14 hrs.
Interior
a) 23 hrs.
b) 12-14 hrs.
Western
a) 23 hrs.
b) 6-14 hrs.
Initial"
0.05
0.09
0.00
Treated
0.09
0.06
0.28
0.17°
d
0.13
0.06
0.12
0.01
Treated
0.09
0.07
0.26r
0.16C
>0.50d
0.12
Low
initial
0.00
0.01
0.00
Treated
0.00
0.02
0.18r
0.17C
0.49
0.06
Hiah
initial
0.19
0.26
0.03
Treated
0.17
0.13
0.34.
0.18
0.85
0.15
^MBHM^^^H
aROM unleached coal.
treated coal washed by procedure on page 48to remove sulfate.
cInsufficient data-two runs only..
runs only.
49
-------
In addition to the above conclusions, it should also be kept in mind
that, as indicated in Table 14, the amount of sulfate retained appears to
depend somewhat on the individual characteristics of the coal. Also, the
washing procedure used here, while conforming to the general constraints
of the Meyers Process, has not been optimized. In particular, the use of
a continuous countercurrent wash or multiple washes may be as effective as
the prolonged washes used above. Moreover, a sulfuric acid wash may not
be necessary. Thus, for a complete understanding of the problem, several
coals should be further investigated in detail in order to determine the
minimum conditions necessary for sulfate removal.
4.3.7 Summary of Ash Changes
Table 18 summarizes the ash changes which occurred upon extraction of
the coals with ferric sulfate. The expected ash change or loss can be
computed from the relative molecular weights and the assumptions that all
the pyritic sulfur FeS,,, is converted to iron oxide (Fe?0 ) in the ashing
o
process at 800 C:
FeS2 + 2.75 02 0.5 Fe203 + 2 S02
M.W. 119.85 M.W. 159.70
Thus, 64.00 g of sulfur from FeSp is converted to 159.70 x 0.5 or 79.85 g
of ferric oxide during the ashing process, which results in 1.25% ash
(79.85/64.00) production for every 1.00% pyritic sulfur present. The
calculated ash loss can then be computed by multiplying the absolute per-
cent pyritic sulfur removal by 1.25. In all cases, more ash was removed
than can be accounted for by pyrite removal alone. In general, excess
removal was greatest for the Western coals which averaged 3.9% excess
removal, while coals from the Appalachian and Interior Coal Basins had
similar excess removals, averaging 2.4 and 2.6%, respectively.
The various coal mines were also examined for correlations by seams
and ash content (Table 19). In the Appalachian region, there were no
significant differences between the coal seams. In the Interior coal
basins, differences occurred between seams; however, these results are not
considered significant because of the small number of mines considered.
When the coals are examined by ash content, it is clear that excess removal
50
-------
Table 18
SUMMARY OF ASH CHANGES
(% W/Wa)
Mine
Warwick
luskingum
igypt Valley
No. 21
Powhattan No. 4
Isabella
Mathies
Wi lliams
Humphrey No. 7
Robinson Run
Shoemaker
Delmont
Marion
Jane
Lucas
Bird No. 3
Fox
Marti nka
Meigs
Dean
No. 1
Kopperston No. 2
Harris Nos. 1&2
North River
Orient No. 6
Homestead
Eagle No. 2
Camp Nos. 1&2
Ken
Star
Wei don
Edna
Navajo
Belle Ayr
Colstrip
Seam
Sewickley
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Lower Freeport
Middle Kittanning
Lower Kittanning
Lower Kittanning
Lower Kittanning
Clarion 4A
Dean
Mason
Campbell Creek
Eagle & No. 2 Gas
Corona
Herri n No. 6
No. 11
Illinois No. 5
No. 9 (W. Kentucky)
No. 9
No. 9
Des Moines No. 1
Wadge
Nos. 6,7,8
Roland-Smith
Rosebud
Initial
40.47
21.68
25.29
37.17
42.22
41.01
13.18
9.88
13.36
33.48
27.18
26.40
21.75
8.68
30.23
13.55
49.25
26.53
17.28
11.39
30.15
18.63
49.28
22.51
16.56
26.53
21.13
15.08
13.90
15.74
9.13
25.29
7.55
10.38
xtracted
35.32
16.05
18.86
32.13
35.72
36.43
9.16
6.97
7.63
28.87
20.44
22.61
17.99
6.32
24.17
9.72
43.46
20.38
13.66
8.50
25.53
16.46
42.84
18.85
11.50
19.80
15.77
9.44
8.58
6.43
6.77
20.53
3.37
5.17
C
Change
-5.15
-5.63
-6.43
-5.04
-6.50
-4.58
-4.02
-2.91
-5.73
-4.61
-6.74
-3.79
-3.76
-2.31
-6.06
-3.83
-5.79
-6.15
. -3.62
-2.89
-4.62
-2.17
-6.44
-3.66
-5.06
-6.73
-5.36
-5.64
-5.32
-9.31
-2.36
-4.76
-4.18
-5.21
al culated
Change"
-1.25
-4.26
-5.56
-2.89
-1.29
-1.25
-2.43
-1.81
-2.43
-2.16
-5.44
-1.08
-1.63
-1.51
-3.43
-3.40
-1.63
-2.53
-3.06
-2.21
-0.54
-0.58
-1.60
-1.23
-3.61
-2.96
-2.73
-3.21
-2.95
-5.96
-0.10
-0.30
-0.24
-0.35
ixcess
-3.90
-1.37
-0.87
-2.15
-5.21
-3.33
-1.59
-1.10
-3.31
-2.45
-1.30
-2.72
-2.13
-0.80
-2.63
-0.43
-4.17
-3.63
-0.56
-0.68
-4.08
-1.60
-4.84
-2.43
-1.45
-3.77
-2.63
-2.43
-2.37
-3.35
-2.26
-4.46
-3.94
-4.86
aAll values in the Table are in % W/W and are an average of two or more values based on
Runs 1 and 2 in Appendix D and Runs 1, 2 and 3 in Reference 2.
bBased on the removal of pyrite, FeS2-
51
-------
Table 19
AVERAGE EXCESS ASH REMOVALS
(% W/W)
Region
r d
Appalachian (23)c - 2.4
Eastern &
Western
Interior (7) - 2.6
Western (4) - 3.9
Seam3
Sewickley (2)c
Pittsburgh (7)
Freeport (3)
Kittanning (5)
Others (5)
Herrin No. 6 (2)
Illinois No. 5 (4)
Des Mgines No. 1 (1)
2.6d
2.7
2.4
2.3
2.4
1.9
2.8
3.3
Ash Content
Low (7)c
Medium (8)
High (8)
Low (4)
Medium (3)
High (0)
Low (3)
Medium (1)
High (0)
1.2d
2.1
3.7
2.4
2.9
—
3.7
4.5
—
aSeam correlations: 1) Sewickley = Meigs Creek No. 9; 2) Herrin No. 6 = No. 11; 3) Illinois
No. 5 = No. 9.
bLow Ash, 0-15%; Medium Ash, 15-25%; High Ash, >25':.
cNumber of mines in sample.
Average ash loss in weight %.
increases with increasing ash content. This is most apparent with the
Appalachian coals, where high ash coals (>25% w/w) have more than three
times the excess removal of low ash coals (0-15% w/w).
Since the aqueous extraction solution is both acidic and oxidizing,
inorganic materials in the ash could be brought into solution by either
an acidic or oxidizing attack. However, the most likely mechanism of sol-
ution probably is dissolution of basic inorganic compounds by the sulfuric
acid that is present in solution (Figure 1). Since acid soluble compounds
of sodium, potassium, magnesium and iron, such as oxides and carbonates,
can be major constituents of coal ash, they could easily account for the
excess ash removal. However, since research has thus far not accurately
resolved these questions, additional experimentation should be performed
in order to establish purification requirements for recycled ferric sul-
fate streams. In addition, the use of "cleaned" coal which normally has
40-70% less ash than ROM coal would substantially reduce any purification
requirements. Operation of a continuous large-scale (pilot) facility may
be required to completely clarify potential problems in this area.
52
-------
4.3.8 Organic Sulfur Changes
After several coals had been extracted, the results seemed to indicate
that the treated coal apparently had a higher organic sulfur content than
the starting coal. Although organic sulfur increases of 0.01-0.14% w/w were
attributable to ash removal, these did not account for all of the apparent
increases. However, the organic sulfur value is the least accurate of all
sulfur analyses because it is not determined directly, but by subtracting the
amount of pyritic and sulfate sulfur from the total sulfur. For this reason,
the organic sulfur value contains resultant errors from all three analyses.
Thus, according to ASTM Standards^ , duplicate organic sulfur values with
spreads of up to 0.4-0.6% w/w can be considered acceptable for analyses done
by different operators in different laboratories. The problem is made even
more complicated due to the possibility that treating the coal with ferric
sulfate solution can introduce a systematic error in the results. Therefore,
a thorough statistical analysis was made in order to assess the validity of
the indicated results.
All the data were tested for significance by applying the t test, in
which the value of £ was calculated according to the equation:
t = (B - A) N/h
°d
where
A = average starting organic sulfur,
F = the average final organic sulfur,
n = the number of values in each set, and
a. = the standard deviation of the difference B - A.
d
The value of t is then used to determine the level of significance by con-
sulting a standard table of values used for the t distribution^ .
These data, which are summarized in Tables 20 and 21, show that,
although no increases are found for Western coals, significant average
increases of 0.23 and 0.31% w/w are found for the Appalachian and Interior
coals, respectively. Differences between various seams in each region and
between these regions themselves were tested and not found to be signifi-
cant. The chances that the organic sulfur increases for coals in these
regions are real were found to be significant at the 99% confidence level.
53
-------
Table 20
ORGANIC SULFUR DATA
tn
Mine
Warwick
Huskingun-
tgypt Valley no. 21
(•owhattan i-lo. 4
Isabel 1*
Mathles
Williams
Humpnrey No. 7
Robinson Run
Shoemaker
Delmont
Marlon
Jane
Lucas
Dird no. 3
Fox
Martinka
Nelgs
Seam
Sewlckley
Melgs Creek No. 9
Pitttburgn i.o. E
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Lower Freeport
Middle Kittannlng
Lower Kittannir.g
Lower Kittanning
.oxer Kittanniiig
Clarion 4A
Run
1-3
1-2
1-3
1-2
1-2
1-2
1-2
1-3
1-2
1-2
1-2
1-2
1-2
1-2
1-2
1-3
1-2
1-2
Total
Kxn.
Time
23
23
13-23
23
23
23
23
23
23
23
23
23
12-23
23
23
23
23
23
Mesh*
100
150
100
100
100
150
100
100
150
100
200
100
100
100
150
100
100
100
ORGANIC SULFUR (X M/H)
Initial
0.27
1.088
2.37
-.113
1.34 •
.' . 026
1.36
= .097
0.46
•.074
0.37
1.068
1.21
-.063
0.98
;.120
1.43
-.193
1.27
i.lOO
0.25
-.051
o.«
-.035
0.41
•.051
0.32
:.147
0.22
-.080
0.69
-.044
0.57
i.025
1.48
-. . 046
Final
0.59
1.061
2.81
s.044
2.16
1.182
1.48
-.053
0.65
1.014
0.79
t.041
1.39
'.046
1.25
-.066
2.12
-.014
1.34
-.169
0.69
;.125
0.58
r.103
0.49
1.035
0.55
-.095
0.56
1.080
1.18
= .206
0.38
1.021
1.63
-.061
Difference
+0.32
'.107
+0.44
t.121
+0.82
1.184
+0.12
t.lll
+0.19
i.07«
+0.42
1.079
+0.18
1.079
+0.27
?.148
+0.69
1.194
+0.07
1.196
+0.44
:.135
+0.13
1.109
+0.08
1.062
+0.23
-.175
• 0.34
:.113
+0.49
1.211
-0.19
1.033
+0.15
1.076
calculated
Increase
0.02
0.14
0.09
0.07
0.03
0.02
0.05
0.03
0.09
0.06
0.02
0.02
0.02
0.01
0.01
0.03
0.04
0.10
corrected _
Dlfference
+0.30
1.107
+0.30
1.121
+0.73
1.185
+0.05
i.lll
+0.16
1.075
+0.40
1.079
+0.13
1.078
+0.24
-.148
+0.60
1.194
+0.01
t.196
+0.42
1.135
+0.11
1.109
+0.06
1.062
+0.22
1.175
+0.33
•-.113
+0.46
1.211
-0.23
1.033
+0.05
1.076
Significance Level
fnr Inr routed
>0.0
95
80
95
None
80
90
70
90
80
'lone
80
Hone
.'ione
None
80
90
90
None
>0.1
90
None
95
..
None
90
None
70
80
-
80
--
-
--
70
90
80
--
>0.2
70
-
95
__
-
80
-
None
70
-
70
-
-
-
None
80
Hone
-
>0.4
--
90
..
--
none
-
--
None
--
Hone
--
--
--
-
None
-
-
-------
Table 20 (Cont'd)
Ol
en
Dean
,io. 1
Kopperston No. 2
Harris Nos. 1S2
north River
Orient ,iO. 6
homes teat
Eagle ,,o. 2
Camp Dos. U2
i(en
Star
He 1 don
Edna
liavajo
Belle Ayr
Coistrip
a
Dean
Mas on
Campbell Creek
eagle S No. 2 Gas
Corona
iierrin ..o. 6
i,o. 11
I llinois no. 5
,,o. 9 (;•;. Kentucky)
,,o. 9
No. 9
Des Hoines Ho. 1
«adge
,.o. 6.7,8
Roland-Smith
flosebuc.
1-2
1-3
1-2
1-2
1-2
1-3
1-2
1-3
1-3
1-2
1-2
1-3
1-3
1-3
1-3
1-3
23
23
13
23
23
23
23
13-14
13
23
23
23
23
23
6-10
12-13
fin -~,J -5
150
100
100
100
100
100
100
100
100
100
150
100
IOC
100
100
100
1.32
-.091
1.C6
*.126
0.41
-.055
0.48
±.036
0.57
:.025
0.36
-.100
1.25
*.051
1.61
1.156
1.65
•.130
1.72
-.053
1.50
-.075
1.00
i.069
0.61
'.038
0.50
±.044
0.54
-.035
0.67
±.019
1.75
±.033
1.32
-.133
0.49
+ .041
0.67
-.039
0.70
±.040
0.46
-.095
1.86
±.116
1.68
-.065
1.73
'.066
2.24
i.043
2.06
-.097
1.69
±.161
0.59
±.043
0.57
-.077
0.65
±.030
0.57
±.056
+0.43
+0.26
-.183
+0.08
+0.19
+0.13
+0.10
±.145
+0.61
+ 0.07
•.169
+0.08
'.146
+0.52
+0.56
+0.69
±.175
-0.02
±.057
+0.07
±.089
+0.11
±.046
-0.10
±.059
0.05
0.03
0.02
0.01
0.04
0.01
0.01
0.12
0.09
0.07
0.08
0.10
0.02
0.03
0.02
0.04
+ 0.37
±.097
+0.23
±.183
+0.06
±.069
+0.18
±.053
+ 0.09
±.047
+0.09 "
+ .U5
+0.60
±.127
-0.05
±.16"
-0.01
±.146
+0.45
±.071
+0.48
±.123
+0.59
±.175
-0.04
±.057
+0.04
±.089
+0.09
i . Qt.6
-0.14
±.059
80
70
None
80
70
done
90
None
Hone
90
80
80
Hone
^one
ijone
None
80
None
-
70
None
--
80
-
-
90
80
95
-
-
--
-
70
--
-
None
--
-
80
-
-
80
80
90
-
-
-
-
Hone
-
--
-
-
-
None
-
--
None
None
80
-
-
-
-
a!00 mesli x 0 ano 200 mesh x 0 is symbolized as 100 and 200, respectively.
Increase cue to ash removal; see Tables 18 and 19.
Corrected to reduction in ash.
dTested ty using £ test; results with a significance of less than 70:; (where o =• i organic sulfur)
were not considered statistically important.
-------
Table 21
SUMMARY OF ORGANIC SULFUR INCREMENTS*
Coal Basin
All Samples (34)b
Appalachian (23)
Interior (7)
Western (4)
Medi an
0.16
0.22
0.45
0.04
Average
0.22 ± .124C
0.23 ± .127
0.31 ± .286
0.01 ± .100
Low
-0.23
-0.23
-0.05
-0.14
High
+0.73
+0.73
+0.60
+0.09
Increase in organic sulfur after leaching and after correction for reduc-
tion in ash content.
lumber of mine samples
'Pooled standard deviations
From an analytical point of view, a systematic error of 0.1% is easily
possible and from a practical perspective, differences less than 0.1% are
not important; therefore, the data were tested for statistical significance
for differences of >0.1% w/w. Using this criterion, six coals had a
>0.1% w/w organic sulfur increase with a significance of 90 or more per-
cent, six were significant at the 80% level, and three at the 70% level.
For a difference of >0.2% w/w, two were significant at the 90% level, five
at the 80% level, and three at the 70% level. When tests were made for
significance for differences >0.4% w/w, only the Weldon and Egypt Valley
No. 21 coals had 80% or more significance.
These organic sulfur increases could result from three possible
sources: (a) actual organic sulfur increases caused by either sulfonation
or sulfation reactions, (b) apparent organic sulfur increases caused by
formation of unextractable inorganic sulfur species during coal leaching,
and (c) incomplete removal of elemental sulfur in the toluene extraction
step. Partially oxidized coals, coals with many phenolic groups or other
active sites, or highly porous coals with a large internal surface area
should be prime candidates for sulfonation or sulfation. Coals of this
type included in the survey are the Western and the Interior Basin coals.
56
-------
In fact, these two groups of coals in general had a higher ferric ion
consumption (see Table 12) than the Appalachian coals. Ferric ion oxida-
tion of coal should typically produce phenols, alcohols and other reactive
sites which could easily react with the sulfuric acid present in any extrac-
tion. Since both of these groups of coals did not show organic sulfur
increases significantly different from Appalachian coals, the possibility
of sulfonation or sulfation reactions does not seem likely.
Apparent organic sulfur increases could result from insoluble inor-
ganic compounds, such as CaS04 or Fe(OH)S04, precipitating in the pores
of tightly structured coal, as is the case for most Appalachian coals.
Coals with high pyritic sulfur contents, such as Egypt Valley No. 21,
Weldon, and Fox coals, could produce significant amounts of sulfate inter-
nally which could precipitate as CaSO^ in the coal pores by reacting with
CaO or CaCCL present in all coal ash, or could form insoluble Fe(OH)S04
under appropriate conditions. Even though the analytical procedure for
hydrochloric acid extraction of sulfate sulfur was designed specifically
to remove sulfate formed by oxidation or weathering and thus could easily
miss deeply imbedded inorganic material, it seems unlikely that more than
0.1% sulfate sulfur could be missed in the analysis, even in the Appa-
lachian coals.
The third possibility is the incomplete removal of the elemental
sulfur in the toluene extraction step. Elemental sulfur would raise the
total sulfur value but would not result in erroneously high pyritic or
sulfate sulfur values. Because organic sulfur is calculated by differ-
ence, this additional sulfur would then result in a higher organic sulfur
value. Since the extraction step has not been optimized and is presently
performed only once, this source of error should be considered an excel-
lent possibility. In addition, this residual elemental sulfur would be
expected to be the greatest in the highly structured and small-pored
Appalachian coals, and less in the more porous Internal Basin and Western
coals. Because actual results follow these trends, this is considered
the probable source of the organic sulfur increase. Additional experi-
mentation is required to confirm this possibility and to establish tenta-
tive solutions.
57
-------
In order to distinguish between these three possibilities, a series
of experiments was run using the Warwick, Fox, Weldon, Egypt Valley
No. 21, Delmont, and Homestead coals, which showed organic sulfur increases
of 0.32, 0.49, 0.69, 0.82, 0.44, and 0.61% w/w, respectively, and repre-
senting both Appalachian and Interior Basin coals.
The first group of experiments was designed to determine whether or
not unextractable inorganic species were being formed in the pores of these
coals. Sulfate was first determined by the usual 5N HC1 extraction on the
whole coal in order to establish the amount of extractable sulfur. In a
separate set of experiments, the organic matter was removed by a low tem-
perature oxygen plasma technique at 150 C, which oxidizes the coal matrix
without significant oxidation of pyrite to sulfate. A sulfate determina-
tion was then performed on the ash using standard procedures. The results
summarized in Table 22 show that there is no significant difference between
the sulfate found by either procedure. Thus, it can be concluded that the
organic sulfur increases are not due to the formation of the unextractable
inorganic species in the coal pores.
If the increases were due to sulfonation or sulfation reactions of
the ferric sulfate leach solution, the use of ferric chloride to remove
pyrite should result in np_ organic sulfur increase. Since this differ-
ence would be most striking for the Egypt Valley and Weldon coals which
had organic sulfur increases of 0.82 and 0.69% w/w, these coals were
extracted in duplicate with ferric chloride, and the organic sulfur con-
tent was followed as a function of time. The results of these experi-
ments, listed in Table 23, show a steady increase in organic sulfur con-
tent in both cases as the pyrite was extracted. In addition, samples taken
at intermediate times which were not extracted with toluene had much higher
organic sulfur increases than those that were extracted once with toluene.
When compared to ferric sulfate leaching, both coals had slightly
smaller organic sulfur increases (Table 23). These differences, which
were 0.16% w/w for the Weldon coal and 0.30% w/w for the Egypt Valley
coal, could be an indication of a small amount of reaction of the ferric
sulfate leaching reagent with the coal; but given both experimental and
analysis variables, this cannot be established using the present data.
58
-------
Table 22
SULFATE DETERMINATION ON WHOLE COAL AND PLASMA ASH£
Coal Mine
Warwick
Egypt Valley
Fox
Weldon
% W/W SULFATE
Whole Coal
0.14
0.12
0.09
0.18
Plasma Ashed
0.12
0.22
0.07
0.11
Determination in both cases by the standard ASTM
method and based on whole coal weight.
Table 23
ORGANIC SULFUR CHANGES WITH FERRIC CHLORIDE6
Coal
Egypt Valley
Ferric
Sulfate
Weldon
Ferric
Sulfate
Time (hr)
0.0
2.0
5.5
23.0
23.0
0.0
1.5
4.0
10.0
23.0
23.0
Sulfur Content, % w/w
Pyritic Organic
5.07b
1.01
0.34
0.00
0.38
5.24b
1.73
0.66
0.20
0.00
0.47
1.34b
2.48
1.70C
1.86C
2.16C
1.00b
1.89
2.23
2.26,,
1.53C
1.69C
All extractions used the same procedure as
the ferric sulfate runs; each coal was ex-
tracted in duplicate and the results averaged.
Initial value for ROM coal.
'Extracted with toluene before analysis.
59
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Thus, it is felt that the observed increases are not due to reaction of
the leaching reagent with the coal, but rather are due to incomplete
removal of elemental sulfur from coal in the toluene extraction step.
Incomplete removal of elemental sulfur is a logical result of the
experimental method also because no attempt was made to optimize sulfur
removal and only a single toluene extraction was made. A check for sulfur
recovery on all 34 toluene extracts showed that sulfur recovery averaged
55 ± 15%, compared to 85-97% that is routinely obtained in our bench scale
work* ' ' where a double toluene extraction and careful sulfur mass bal-
ance is made. Since a single toluene extraction is sufficient to remove
elemental sulfur from some coals and is obviously inadequate in other
cases, it is important that experimentation be conducted in order to deter-
mine the degree and severity of extraction that are necessary to remove the
elemental sulfur from a wide range of coals.
Favorable results obtained in vaporization of residual elemental sulfur
and sulfate in earlier work on the Meyers Process indicated that similar
treatment of coals which had apparent incomplete elemental sulfur and/or
sulfate removal could lead to significant additional sulfur reductions and
could further verify the source of the organic sulfur increases. Thus, two
examples — the Delmont and Warwick coals —were chosen in which reduction
of the organic sulfur (i.e., removal of remaining elemental sulfur) would
allow the treated coal to meet EPA's most stringent new source standards.
An additional coal from the Homestead Mine representative of the Interior
Basin, which could be reduced below most Priority 2 and 3 state standards,
was chosen as the third example. Analyses of these coals before vapori-
zation treatment are shown in Table 24.
Each of the coals was treated in duplicate in ceramic boats for 3 hrs
at 370°C in a tube furnace under a 1-liter/minute flow of argon or argon/
hydrogen. The results based on total sulfur analysis listed in Table 25
show that substantial amounts of additional sulfur were removed in all
three cases. The Delmont and Warwick coals were reduced enough to meet
EPA's new source standards. The Homestead coal was reduced by a substan-
tial 0.83% indicating that not only all the residual sulfur was removed,
but also most of the residual sulfate. Note also that the presence of
60
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Table 24
ANALYSIS OF LEACHED AND TOLUENE EXTRACTED COALS
BEFORE VAPORIZATION TREATMENT
Mine
Delmont Mine,
Upper Freeport
Seam
Warwick Mine,
Sewickley Seam
Homestead Mine,
No. 11 Seam
% W/W Sulfur
Total
0.96
0.82
2.38
Pyritic
0.21
0.09
0.22
Sulfate
0.06
0.14
0.30
Organic
0.69
0.59
1.86
Initial
Organic3
(0.25)
(0.27)
(1.25)
aOrganic sulfur content of run-of-mine coal before ferric sulfate
leaching.
Table 25
ANALYSIS OF EXTRACTED COALS FROM SURVEY PROGRAM
AFTER VAPORIZATION TREATMENT9
Mine
Delmont Mine,
Upper Freeport Seam
Warwick Mine,
Sewickley Seam
Homestead Mine,
No. 11 Seam
% W/W Total Sulfur
Starting6
0.96
AS (loss)
0.82
AS (loss)
2.38
AS (loss)
Ar(370°C)
0.80
0.16
0.61
0.21
1.71
0.68
Ar/H2(370°C)
0.64
0.32
0.56
0.26
1.55
0.83
aAverage of duplicate runs.
bFrom Table 24
61
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hydrogen in the vaporization gas increased sulfur removal significantly in
all cases. These results essentially prove the hypothesis that organic
sulfur increases in treated coals are the result of incomplete toluene
extraction.
These very promising results indicate that treatment of additional
survey coals by this technique could result in significantly lower sulfur
values of treated coals by removing sulfate in those cases where it was
high and elemental sulfur in those cases where its removal was incomplete.
An examination of the data indicates that approximately 20 out of a total
of 35 coals could benefit from this treatment. In addition, it is pos-
sible that vaporization could be developed into a viable alternative to
toluene extraction in the overall process. This alternative must be
explored in any future research.
4.3.9 Miscellaneous Data
Table 26 contains miscellaneous data which were accumulated during
this survey and which are treated briefly in the paragraphs below:
The Filtration Rates of the various coals are qualitatively
shown in Table 26. These observations are based on the amount
of time required to obtain a dewatered filter cake. A label
of fast (F) indicates no problem in filtration, with the rate
proceeding near the maximum rate of the funnel; medium (M)
indicates a slower, but still acceptable rate; and slow (S)
indicates that unacceptably long times were required for fil-
tration. It was found that the rate of filtration closely fol-
lows the ash content of the treated coals, with high ash coals
filtering much slower than low ash coals. In the case of
200 mesh x 0 coal from the Camp Nos. 1 & 2 mine (No. 11 seam)
which filters very slowly, the removal of excess ash by density
fractionation at 1.90 specific gravity changes its filtration
rate from slow to very fast. Thus, the use of cleaned coal
could substantially reduce filtration requirements in any com-
mercial plant.
Liquid Retention in the form of leach solution and toluene was
also determined under a set of standard, but not optimum, con-
ditions and is expressed as g liquid retained per 100 g coal.
In both cases, the vacuum filtration was continued 3 minutes
after no more liquid was visible on top of the filter cake.
Table 26 indicates that in both cases coal to coal variations
were within experimental error and toluene is retained to a
lesser extent than the leach solution. These results are
consistent with the postulate that the liquid is being held
62
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Table 26
MISCELLANEOUS DATA
Mine
Warwick
Muskimjum
Egypt Valley
No. 21
Powhattan No. 4
Isabella
Mathies
Wi 11 i ams
Humphrey No. 7
Robinson Run
Shoemaker
Delmont
Marion
Jane
Lucas
Bird No. 3
Fox
Marti nka
Meigs
Dean
No. 1
Kopperston No. 2
Harris Nos. U2
North River
Orient No. 6
Homestead
Eagle No. 2
Camp Nos. 1&2
Ken
Star
del don
Edna-
Navajo
Belle Ayr
Colstrip
Seam
Sewickley
Meigs Creek No. 9
Pittsburgh No. 8
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pi ttsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Lower Freeport
Middle Kittanning
Lower Kittanning
Lower Kittanning
Lower Ki ttanning
Clarion 4A
Dean
Mason
Campbell Creek
Eagle & No. 2 Gas
Corona
Herri n Mo. 6
No. 11
Illinois Mo. 5
No. 9 (W. Ky.)
Ho. 9
No. 9
Des Moines Mo. 1
Madge
Nos. 6,7,8
Roland-Smi th
Rosebud
tfesh
100
150
100
:oo
100
150
100
100
150
100
200
100
100
100
150
100
100
100
150
100
100
100
100
100
100
100
100
100
150
100
100
100
100
100
Free Sv
T .In.de
4-1/2
4
8
6-1/2
6
1-1/2
5-1/2
7
7
4-1/2
6
5
1
0.5
0
0
0
vel 1 i ng
<
4
8-1/2
5
7
0
3-1/2
5-1/2
7
0
2-1/2
0
0
0
0
0
0
0
Rank
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
mvb
hvAb
hvAb
Ivb
hvAb
hvAb
hvBb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvBb
hvAb
hvBb
hvBb
hvBb
hvCb
hvCb
hvCb
subA
subB
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvAb
hvA'
hvAb
mvb
hvAb
hvAb
Ivb
hvAb
hvAb
hvBb
hvAb
hvAb
hvAb
hvAb
hvAb
hvBb
hvBb
hvAb
hvBb
hvBb
hvBb
hvCb
hvCb
subA
subB
subB
Liquid Retention
in q/lOOq Coal
25
38
41
43
49
41
40
45
37
43
39
46
38
35
37
29
39
53
30
35
39
30
33
32
33
40
30
30
24
30
27
38
32
33
37
31
27
43
31
27
Fi 1 tration
Rat p
M
F
F
S
S
S
F
M
F
S
M
H
F
F
F
F
S
S
F
M
F
F
i
S
H
M
S
M
M
M
M
F
F
F
Ash
r-.-.t- ^a
H
L
M
H
H
H
L
L
L
H
M
M
M
L
M
L
H
M
L
L
M
L
H
M
I
M
M
L
L
L
L
M
L
L
Low, 0-17%; Medium, 17-27',:; High >27"f; see text for details.
in the spaces between the coal particles, and that the differ-
ences between the leach solution and toluene merely reflect
the fact that toluene is less dense than the leach solution.
The Free-Swelling Index (FSI) is an indication of the caking
qualities of a coal and therefore has some importance in
evaluation of a coal for coking and for use in certain types
of steam boilers. The data show that, for coals that have
high excess reactivity with ferric ion (such as the Eastern
Interior Basin coals), the FSI is substantially reduced.
Coals having little excess reactivity with ferric sulfate
(such as the Appalachian Basin coals) have little or no change
upon treatment. This is consistent with the generally
accepted idea that slight oxidation of a coal reduces its FSI.
The Rank of the treated and untreated coals is the same in all
instances except for the Orient No. 6, Belle Ayr and Navajo
coals. Because rank is determined only by heat content for
hvAb and lower ranked coals, and because rank is quite insen-
sitive to small btu changes, only minor differences in rank
should be expected.
63
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4.4 FLOAT-SINK TESTING
Float-sink testing (washability studies) were run on thirty-one of the
thirty-five coals by the Commercial Testing and Engineering Company in
order to determine how conventional float-sink procedures compare to the
Meyers Process in efficiency of pyrite removal, heat content change, and
ash loss. In addition, information was obtained that can be used to eval-
uate a combined two-step process, involving coal washing followed by the
Meyers Process, that would produce coal containing minimum amounts of
pyrite and ash and a maximum heating value.
4.4.1 Procedures
The mine samples, representing 20 mines and coal seams, were selected,
sampled and prepared according to the procedures described in Section 4.2
and Appendix A of this report. No tests were run on the four samples from
the Edna, Navajo, Belle Ayr and Col strip mines, since they contained less
than 0.3% w/w pyritic sulfur and 1.0% total sulfur and were judged eco-
nomically unfeasible for removal of pyritic sulfur by washing.
Five hundred pounds each of the 1-1/2" x 100 mesh, 3/8" x 100 mesh
and 14 mesh x 0 portions prepared from the initial samples of the coals
were fractionated according to standard float-sink procedures using
organic liquids of 1.30, 1.40, 1.60 and 1.90 specific gravities. Samples
of each size (head sample), of each gravity portion, and of the two
100 mesh x 0 samples, were analyzed on a dry basis for % w/w ash, total
sulfur and pyritic sulfur.
The raw data were then used to calculate washability data showing
cumulative recovery and cumulative reject at the various specific gravities
for each of the size portions. A complete set of tables showing all new
data is included in Appendix E. The remaining data have been reported
(2)
previouslyv .
4.4.2 Results and Discussion
Table 27 shows the summary of the results for the 14 mesh x 0 por-
tions of 1.90 and 1.60 specific gravities and how they compare to the
Meyers Process (100 mesh x 0 coal) for the total sulfur and pyritic sulfur
reductions and ash removal. The 14 mesh x 0 float-sink material was
64
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Table 27
SUMMARY OF FLOAT-SINK TESTS
14 MESH x 0 COAL
COMPARISON TO MEYERS PROCESS
100 MESH x 0 COAL
Mine Seam
Warwick
Muskingum
Egyot Valley
No. 21
Powhattan No. 4
Isabella
Mathies
Mi 1 1 i ams
lumphrey No . 7
(obinson Run
Shoemaker
Jelmont
torion
Jane
telker
Lucas
3ird No- 3
Fox
Marti nka
Meigs
Dean
NO. 1
Kopperston No. 2
Harris Nos.
1 & 2
North River
Orient No. 6
Homestead
Eagle No. 2
Camp Nos. 1 & 2
Ken
Star
Sewickley
Meigs Creek
No. 9
Pittsburgh No. 8
Pittsburgh No, 8
Mttsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Lower Freeport
Upper Kittanning
Middle Kittanninq
Lower Kittanning
Lower Kittanning
Lower Kittanning
Clarion 4A
Dean
Mason
Campbel 1 Creek
Eagle No. 2 Gas
Corona
Herri n No. 6
No. 11
Illinois No. 5
No. 9 (W. Ky)
No. 9
No. 9
Des Moines No 1
Ini tial Analysis
% w/w
otal Pyritic
Sulfur Sulfur ? Ash
1.37 1.09 40.47
6.08 3.65 21.68
6.55 5.07 25.29
4,12 2.57 37.17
1.57 1.07 42.22
1.46 1.05 41.01
3.48 2.23 13.18
2.53 1.59 9.88
4.38 2.89 13.36
3.51 2.19 33.48
4.89 4.56 27.18
1.37 0.90 26.40
1.85 1.44 21.75
0.71 0.07 16.67
1.79 1.42 8.68
3.14 2.87 30.23
3.83 3.09 13.55
1.96 1.61 49.64
3.73 2.19 26.53
4.09 2.62 17.28
3.12 1.98 11.39
0.91 0.47 30.15
1.00 0.49 18.63
2.06 1.42 49.25
4.46 3.11 16.56
4.29 2.64 26.53
4.51 2.30 21.13
4.83 2.85 15.08
4.32 2.60 13.90
6.39 5.24 15.74
Washed Coal Analys s, % w/w
1.90 Float Material
BTU Total Pyritic
Recya Sulfur Sulfur % Ash
93 1.02 0.54 17.02
96 4.36 1.99 19.18
96 4.63 3.42 11.86
93 3.27 1.89 17.40
95 1.48 0.59 14.93
95 1.67 1.02 14.89
98 2.32 0.88 7.87
99 1.90 0.90 6.97
97 3.01 1.24 7.95
96 3.62 2.07 12.23
92 2.13 1.38 10.29
95 1.17 0.58 10.04
97 0.78 0.40 11.15
98 0.66 0.07 12.17
98 0.67 0.32 5.80
93 1.52 0.39 8.80
98 2.00 1.32 8.78
91 0.84 0.46 21.53
95 2.83 1.07 14.10
96 3.05 1.26 12.65
97 2.29 1.03 6.77
95 0.33 0.34 11.31
96 0.92 0.36 13.14
95 2.13 1.08 19.87
97 3.25 1.71 10.61
97 2.92 1.53 12.52
96 2.90 1.22 10.21
97 3.47 1.55 10.02
9C 3.01 1.67 10.47
97 3.91 2.72 8.81
1.60 Float Material
BTU Total Pyritic
ecya Sulfur Sulfur % Ash
89 0.92 0.41 12.96
89 4.17 1.69 16.82
92 4.27 3.03 10.25
88 3.04 1.51 12.37
89 1.40 0.41 9.39
90 1.62 0.93 11.94
97 2.15 0.69 7.09
97 1.S2 0.81 6.45
95 2.81 1.02 7.21
92 3.22 1.60 8.62
90 1 .84 1 .09 8. 72
91 1.10 0.50 7.98
95 0.70 0.31 9.40
93 0.66 0.07 9.59
97 0.62 0.27 5.04
91 1.40 0.75 7.25
95 1.90 1.21 7.44
85 0.75 0.30 14.69
91 2.67 0.84 11.00
92 2.98 1.20 11.69
96 2.15 0.88 6.3
92 0.79 0.28 9.12
89 0.87 0.30 =>.5
91 2.07 0.93 11.8
95 3.07 1.50 9.!
94 T.77 1.35 10.4
91 2.75 1.01 8.4
96 3.37 1.44 9.46
97 2.92 1.57 10.0
95 3.81 2.60 8.2
b
Final Analysis , % w/w
BTU Total Py-ntic
Recya Sulfur Sulfur S Ash
99 0.66 0.06 35.32
97 3.22 0.24 16.05
93 :.71 0.33 18.69
100 1.94 0.04 32.13
100 0.72 0.06 35.72
'r'0 0.94 0.05 36.43
99 1.74 0.29 9.16
99 1.49 0.14 66.97
98 2.20 0.08 7.63
99 1.73 0.08 28.87
98 0.96 0.21 20.44
100 0.68 0.04 22.61
98 0.69 0.14 17.99
c c c c
100 0.63 0.07 6.32
98 0.80 0.13 24.17
9C 1.64 0.26 9.72
(93) 0.58 0.12 43.46
98 1.94 0.17 20.38
99 • 2.08 0.17 13.66
9S ,.r-2 0.21 3.50
;%) 1.61 0.04 25.53
9° .77 0.04 16.46
(04) 0.93 0.14 42.84
96 :.3S 0.22 11.50
97 1.97 0.11 19.49
98 2.02 0.14 15.77
97 2.78 0.28 9.44
96 2.46 0.06 8.58
94 2.25 0.15 5.94
aSee text for method of calculation of recovery (Recy)
Best run
cNot run due to low pyritic sulfur
chosen even though it may be too fine to be used in a commercial installa-
tion, because in most instances the best results were obtained with this
top size. A series of telephone contacts was made with all the mine
operators in this study in order to verify this assumption. These con-
tacts indicated that, of those mines which also clean coal before ship-
ment, that the resulting sulfur and ash contents obtained from the
1.90 float 14 mesh x 0 material are roughly equal to the sulfur and ash
65
-------
contents of the coal presently being shipped from the corresponding prepa-
ration plants. The 1.60 float data are included to illustrate what can be
produced from a coal preparation plant with a sharply increased reject
fraction. In addition, the current trend as the result of the current
coal (and energy) shortage has been to decrease rejects, with concomitant
increasing of the sulfur and ash content, in order to increase production.
For these reasons, it is felt that the 1.90 float 14 mesh x 0 fraction
represents a conservative basis for comparing the efficiency of coal
cleaning to the Meyers Process.
In several cases, including the Humphrey No. 7, Marion, Dean, Eagle
No. 2, Ken and Star mines, the 38.1 mM x 149y (1-1/2" x 100 mesh) portions
gave similar or slightly better results than the 1.41 mm x 0 (14 mesh x 0)
portions, while better results were observed with the coarse fraction for
the Shoemaker, Meigs, Homestead and Weldon coals. With all other coals,
coal cleaning potential decreased when coarser material was washed.
The percent float-sink btu/lb loss (see Table 27 for tabulation of
results) was calculated from the percent w/w and ash content of the cumu-
lative material which.was rejected at the specific gravity of interest.
This value was assumed to represent the total heat content loss and was
subtracted from 100% to give the btu recovery. Complete organic material
recovery was assumed for the Meyers Process because no evidence has been
found to date that indicates material other than ash is dissolved in the
leaching process. The percent recovery was then calculated using the
before and after dry-mineral-matter-free heat content of the coal.
The analysis of the 1.90 float material shows that 0.0-1.9% w/w more
total sulfur is removed from the coal by the Meyers Process than by the
float-sink method, with a median value of 0.7% w/w. For the 1.60 float
material, the corresponding figures are 0.0-1.6% w/w with a median value
of 0.6% w/w. The majority of the remaining total sulfur values obtained
for both specific gravities were between 0.4 and 1.0% higher by the float-
sink method than by the Meyers Process.
The advantages of chemical leaching are even more apparent in the
final pyritic sulfur values where, for all but one coal, the final values
are between 0.0 and 0.3% w/w. Float-sink separation at a specific gravity
66
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of 1.90 resulted in final pyritic sulfur values of 0.3 to 3.4%, which drop
to 0.3 to 3.0% at a specific gravity of 1.60. The corresponding median
values are 1.1 and 1.0% w/w, respectively. The 1.90 float material of the
low sulfur Harris Nos. 1 and 2 and Kopperston No. 2 mines as well as the
Warwick, Jane, Lucas and Martinka mines had final pyritic sulfur values of
0.3-0.5%, making them possibly competitive with the Meyers Process. Note,
however, that 90% pyrite removal is not always reflected in the total sul-
fur values due to slight increases in other sulfur forms. Although for
approximately one-half of the coals the Meyers processing results are
already near optimum (see Table 1), additional processing improvements will
be necessary to reach near optimum values for the others. However, in all
cases the Meyers Process reduced the total sulfur content of the coals
lower than that obtainable by conventional coal cleaning. In most cases,
the differences were substantial.
The heat content recovery for the 1.90 float material is 96 ±2% and
for the 1.60 float material, it is 93 ±3%. In contrast, chemical leach-
ing results in 99 ±1% recovery for the Appalachian coals and 96 ±3% for
the Eastern and Western Interior basin coals. Thus, chemical leaching and
washing the Interior Basin coals at a specific gravity of 1.90 result in
comparable heat losses, while in all other categories the Meyers Process
is superior with respect to heat content recovery. In addition, oxidation
of the coal during the leaching process results in an in situ generation
of heat which can be used to supply process heat requirements for the
Meyers Process, while losses due to washing are discarded with the refuse
and in some cases may even present a fire hazard. Thus, for almost every
coal, the Meyers Process is more efficient than physical separations with
respect to energy recovery.
Table 27 also summarizes ash changes as the result of both processes.
Note that in most cases, especially the Warwick, Isabella, Mathies, Shoe-
maker, Bird No. 3, Martinka, Kopperston No. 2 and North River mines, sub-
stantially more ash is removed by physical cleaning compared to the Meyers
Process (in which only ash corresponding to pyrite is removed). Only in
low ash cases, such as the Fox, Williams, Humphrey No. 7, Robinson Run,
Lucas, Fox, Dean, No. 1, Homestead, Ken, Star, and Weldon coals, are both
67
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processes comparable. With the Walker coal, which has essentially zero
pyritic sulfur, only ash reduction was achieved. However, ash reduction
in itself is valuable in that reduced shipping costs, reduced load on
electrostatic precipitators and enhanced heating values are realized. In
addition, a certain part of the ash is soluble in the leach solution of
the Meyers Process and any initial ash reduction should reduce both puri-
fication requirements on this solution and, depending upon pyrite reduc-
tion, on operating costs of the Meyers Process. Thus, depending on the
situation, a simple cleaning procedure on most coals, and especially those
containing >15% w/w ash, would be advantageous prior to treatment with the
Meyers Process.
4.5 REMOVAL OF TRACE ELEMENTS
In the last few years, the potential environmental hazards of trace
elements emitted in the flue gas from coal combustion has become a matter
(9-14)
of concern . In view of this interest, it seemed appropriate to per-
form a survey of trace element concentrations in the coals selected for
this project, and to examine removal efficiencies by both the Meyers Process
and physical cleaning. This has been accomplished for 20 coals representa-
tive of the Appalachian, Eastern Interior and Western coal basins for the
elements Ag, As, B, Be, Cd, Cr, Cu, F, Hg, Li, Mn, Ni, Pb, Sb, Se, Sn, V,
and Zn.
4.5.1 Analysis,.Procedures, and Results
In selecting procedures for the elements of interest, three major
factors were considered. First, a sensitivity of 1 ppm (dry weight of
whole coal) was selected as the lowest possible level of interest with
the exception of Hg, where 0.1 ppm was used. This value was selected on
the basis that if 100% of the element were emitted from the stack, 1 ppm
in the feed coal would result in an emission of only 45 g/hr (0.1 Ib/hr)
from a 100 MW utility which, by all available information, seemed to be a
conservatively safe emission level. Secondly, the analytical method
chosen should have an overall accuracy of ±10% so that removal efficien-
cies could be accurately determined. The third factor considered was cost.
On the basis of the survey nature of this task and the uncertain environ-
mental hazards associated with the selected trace elements, it was decided
68
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that extensive methods development studies were not warranted and that
relatively inexpensive procedures should be used. In several cases, the
first two requirements were relaxed where added costs of meeting the
requirements seemed excessive for the added value. Based on these cri-
teria, all the trace analyses except those for As, B and F were performed
using atomic absorption spectroscopy. The elements As and B were deter-
mined spectrophotometrically, while F was determined using a specific ion
electrode technique. Details of the procedures and all of the raw data
from the analyses are presented in Appendix F, In the case of Se, the
method chosen appeared to perform well only on occasion and the results
are so mixed that all of the data presented is highly suspect. Several
studies are currently being conducted on a reliable Se method for coal.
The aforementioned procedures have been checked by comparing TRW
analysis results of NBS Sample 1632 with NBS reported values and are sum-
marized in Table 28. Recently, a large scale interlaboratory comparison
of trace element results for coal using SRM 1632 was completed by the
U.S. Environmental Protection Agency and the National Bureau of Standards' '
The mean values obtained from all other participating laboratories for the
trace element concentrations are also included in Table 28.
Referring to Table 28, it can be seen that analyses for elements As,
Be, Cu, Hg, Mn, Ni, Pb and Zn all show fair to excellent agreement with
the certified NBS values both in accuracy and precision. The value
obtained for vanadium is in good agreement with the reported NBS value;
however, the precision between replicate samples is poor. This poor pre-
cision is not indicative of the precision normally obtained with coal
samples, which is typically ±24% relative deviation. The value obtained
for Cr is approximately 18 ppm higher than the NBS reported value, which
might be attributed to contamination or incorrect background correction.
The cadmium value reported by TRW is 2 ppm higher than the NBS reported
value. However, the range of values reported is approaching the lower
limit of detectability for this element by AAS and for this reason will
show a large degree of scatter and inaccuracy. The difficulty with the
Cd analysis is not limited to the TRW results, since all laboratories had
difficulty with this analysis; this is apparent when the mean value of
0.9 is compared with the NBS certified value of 0.19. No fluoride values
69
-------
Table 28
COMPARATIVE TRACE ELEMENT ANALYSIS RESULTS'
(PPM IN MOISTURE-FREE COAL)
As
Ag
Cd
Cr
Cu
Hg
Li
Mn
Ni
Pb
Se
Sb
Sn
Tl
Th
U
V
Zn
fe
Be
F
B
NBS 1632
Certified
Values
5.9 + 0.6
0.19 + 0.03
20.2 +0.5
18 + 2
0.12 + 0.02
40 +_ 3
15 + 1
30 + 9
2.9 +_ 0.3
0.59 +_0.3
(3)e
1.4 + 0.1
35 +_ 3
37 +_4
8700 + 300
(1.5)e
EPA-A11 Labs
Grand Mean
6.24
0.9d
22.7
0.22
41.3
19.0
30.4
4.6
1.7
34.9
29.5d
1.75
83. 5d
TRW
5.0 +_0.64
1 +.0.7
2.4 +_0.14
38 +2.8
15 + 1.4
0.10 +. 0.0
28 +_ 0.0
39 i 1.4
18 +_0.7
30 +_ 1.4
4.8 +^ 3.2
4 +_ 5.2
32 +_ 20
33+1.4
2.0 +.0.1
73 +_7
32 + 11
Illinois State Geological Survey
Neutron
Activatior
5.7
0.18
39
2.8
Atomic Absorption
LTA
<0.4
24
18
16
22
40
HTA
<0.4
22
23
16
32
38
Optical
umssion
22
28
26
24
0.2C
2C
54
1.72
43C
X-Ray
Fluor.
22
22
26
49
1.12
Ion
Elec.
80.4
aTable taken from Reference 8; TRy values added.
Average of at least four or more determinations.
cValues reported separately in Reference 8.
Oruestionable mean; wide scatter or limited data.
elnformation value only. Not certified by NBS.
are reported by NBS; however, several spiked samples were analyzed to
check the procedure employed for recovery of added fluoride. The percent
recovery obtained was 85%, suggesting that TRW reported values might be
slightly lower than the true value. Analysis results which have recently
been reported by the Illinois Geological Survey (IGS) for SRM 1632 have
included additional results for F, B, Sn, and Sb. TRW results are in
good agreement for F, B, and Sn but are in poor agreement for Sb. There
are no comparative analyses available for the elements Ag and Li, so no
comment can be made as to the relative accuracy of the procedures
employed.
70
-------
The results of trace element analyses for 18 elements in 10 coals
before and after treatment by the Meyers Process and by deep cleaning are
presented in Appendix F, Tables F-2 through F-ll. The first group of
10 coals was reported in the final report^ ' of the preceding coal survey
program and are included only in summary here. A summary of the trace
element levels in the untreated coals appears in Table 29. The analyses
were run in triplicate for the first survey program and in duplicate on
both untreated and treated coals for the present survey program. The
change from triplicate to duplicate analyses was a cost saving step but
resulted in slightly less precision for the second phase of the program.
Up to 22 sets of calculated standard deviations (a) for each element
in the untreated coal were used to calculate a pooled standard deviation
(S) for each element. The same was done for coal extracted by the Meyers
Process and for the washed coal. The pooled standard deviation is calcu-
lated as follows:
2
s = ..... Vn
where
a = standard deviation for a given set of analyses
-------
Table 29
TRACE ELEMENT COMPOSITION OF UNTREATED COALS (PPM)
Ag
As
B
Be
Cd
Cr
Cu
F
Hq
L1
Mn
N1
Pb
Sb
Se
Sn
V
Zn
Appalachian Coal Basin
Egypt
Bird Valley Humphrey
Musklnaum Mathles Robinson Powhattan Delmont Mai*1on Lucas 13 Mefgs 121 Jane Fox Warwick 17
2.3 1.8 1.6 0.8 2.6 1.5 2.0 2.9 0.6 4 2 <0.1 4 0.5
2.0 6,1 5.9 4.3 40 98 74 16 2.6 22 29 24 13 9
54 54 60 62 18 10 20 30 115 34 27 16 20 26
2.0 2,7 0.6 3.3 4.2 2.2 3.8 3.6 1.4 0.7 0.8 2.0 1.0 0.4
1.6 0.8 1.8 1.2 1.8 1.5 1.4 1.4 0.8 <0.5 <0.5 <0.5 <0.5 <0.5
110 110 100 141 144 76 52 149 100 55 55 94 81 26
15 29 10 25 20 38 13 26 23 26 35 25 24 16
117 210 100 282 131 155 65 105 222 168 122 94 251 78
0.09 0.09 0.14 0.07 <.02 0.06 <0.2 0.10 0.05 0.31 0.11 0.07 0.14 0.06
55 64 12 52 24 76 8 54 22 26 38 4 76 13
25 66 42 57 94 25 15 45 44 41 46 24 31 31
29 34 26 37 68 23 35 36 22 41 33 147 44 17
12 19 12 20 31 15 18 23 12 15 25 5 16 7
<5 <5 19 <5 16 <5 <5 <5 9 <5 <5 <5 <5 <5
59 74 49 54 25 8 63 <5 <5 17 <5 <5
15 12 8 <5 20 <5 10 15 15 <5 <5 <5 <5 <5
33 60 28 60 40 54 12 60 50 102 147 94 78 77
30 41 30 40 76 34 50 80 38 31 34 105 55 18
Eastern Interior Basin
Eagle Orient Camp Nos.
Ken #2 16 142
1.4 <0.1 <0.1 8
6.5 6.6 15.2 5.7
6.0 30 43 272
2.0 0.5 6 1.5
1.7 0.5 0.7 0.8
76 126 74 122
16 18 36 17
124 151 105 215
<0.2 0.16 0.12 0.16
9 4 23 10
60 86 57 98
30 136 53 27
16 29 0.5 25
24 <5 <5 <5
15 <5 <5 <5
12 <5 <5 <5
35 64 69 105
40 215 25 97
Western Coals
Belle
<0.1 <0.1
0.4
-------
Table 30
TRACE ELEMENT ANALYTICAL PRECISION
Element
Ag
As
B
Be
Cd
Cr
Cu
F
Hg
Li
Mn
Ni
Pb
Sb
Se
Sn
V
Zn
Average
Concentration
(ppm)
2.5
11.4
48.1
2.0
1.3
71.3
20.4
125.2
0.13
25.1
39.7
43.5
23.0
12.0
18.3
26.0
58.0
51.4
Pooled Standard Deviation (ppm)
Untreated
Coal
1.32(15)*
1.78(21)
3.85(22)
0.39(19)
0.26(21)
4.26(20)
2.18(22)
11.18(21)
0.03(18)
3.77(21)
4.74(22)
6.16(22)
3.51(21)
5.77(8)
5.91(5)
9.91(7)
15.81(22)
5.25(22)
Meyers Process
1.91(12)
1.22(12)
5.49(19)
0.20(19)
0.42(9)
4.10(20)
3.08(19)
18.50(19)
0.054(9)
3.65(20)
2.44(20)
6.15(19)
7.19(19)
3.96(4)
1.15(2)
9.14(8)
14.98(19)
4.73(20)
Float Sink
0.16(5)
1.80(8)
1.96(10)
0.52(9)
0.63(10)
1.83(10)
1.76(10)
8.57(9)
1.11(10)
1.74(10)
7.94(10)
4.38(10)
7.17(10)
9.94(10)
4.98(10)
3.02(10)
All
Samples
1.48
1.64
4.59
0.36
0.42
3.83
2.49
14.13
0.04
3.36
3.52
6.54
5.35
6.19
5.03
9.68
14.01
4.69
% Relative
Standard
Deviation for
All Samples
59
14
10
18
32
5
12
11
31
13
9
15
23
52
27
37
24
9
*Values in parenthesis are numbers of sets of data used in the calculations.
In keeping with the low levels at which these elements were present, the
percent relative deviations of these analyses were generally high:
Ag, ±59%, Be, ±18%, Cd, ±32%, Hg, ±31%.
Seven of the remaining elements (As, Cu, Li, Pb, Sb, Se and Sn) were
generally present in the range of 3-30 ppm, while the remaining seven
(B, Cr, F, Mn, Ni, V and Zn) were generally above 30 ppm. The analytical
precision of these fourteen elements, while not as good as had been hoped,
was generally acceptable: As, ±14%, B, ±10%, Cr, ±5%, Cu, ±12%, F, ±11%,
Li, ±13%, Mn, ±9%, Ni, ±15%, Pb, ±23%, Sb, ±48%, Se, ±32%, Sn, ±38%,
V, ±24%, Zn, ±9%.
73
-------
4.5.2 Removal Efficiencies
The removal efficiencies for trace elements from coal treated by the
Meyers Process and by physical cleaning are summarized in Table 31. A dis-
cussion of the results on an element-by-element basis is presented in this
section.
Ag - Due to the low values of Ag present in coal and the poor pre-
cision of the results, the data for Ag are somewhat inconclusive.
However, in over half of the cases where there is a decided
difference after treatment, 50% or more of the Ag has been
removed.
As - Arsenic is easily and effectively removed by both treatments
in almost every case. The Meyers Process is slightly more
effective and removed at least 80% of the As in every case.
B - Boron is not appreciably removed from coal by either process
except in isolated cases.
Be - Beryllium is not appreciably removed by either process except
in isolated cases.
Cd - Due to the low values of Cd present in coal and the poor pre-
cision of the results, the data for Cd are somewhat inconclusive.
The data suggest that Cd is removed by the Meyers Process,
— (9)
which is consistent with the reportedv ' presence of Cd in the
ZnS phase, since Zn is easily removed. The values for washed
coals are inconclusive.
Cr - Chromium is removed by both treatments in almost every case
by 50% or greater.
Cu - Copper is only moderately removed by either process.
F - There is only limited evidence of fluoride removal by the
Meyers Process. Washing, however, shows 30-60% removal in
nearly every case.
Hg - Due to the very low (0.1 ppm) levels of Hg in all coals exam-
ined, no data on removal are available.
74
-------
Table 31
TRACE ELEMENT REMOVALS (% W/W)
Element
Ag
As
6
Be
Cd
0
Cu
F
Hg
U
Mn
N1
Pb
Sh
Se
Sn
V
In
Condition
M'b
Fsb
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
M
Fs
K
Fs
M
Fs
M
Fs
M
Fs
Appalachian Coal Basin
Robinson Powhattan Bird Egypt Humphrey
Muskinaum Mathies Run M Oelmont Marion Lucas »3 Meigs Valley Jane Fox Warwick *7
83+17 89+3 NDC Gaind NO >33 ND NO Inde 50+15 ND NO NO NO
>57+?0 44+16 3315 ND 62+8 -33 :-50 66+24 Ind
84+1 ^'95+1 98+1 97+4 81+1 98+1 85+6 81+7 94+5 -.100 91 + 1
97+3 88+_l 73+2 18+8 81+1 75*3
NO NO NO Gain ND ND ND 50+1.3 13+5 HO 70+2 19+9 ND 38+9
44+_7 ND ND 19+;5 72+5 ND ND 92+1 15+6
ND 33+8 ND 30+9 17+5 ND ND 28+1 NO 43+16 38 70+14 ND NO
Gain ND ND fiD 52+2 54+3 21*4 Gain 29+18
67+J4 >38*24 ND ND 33*41 .57 ND 36+20 >38 Ind Ind Ind Ind Ind
Gain Gain Gain G.iin Gain • ND ND ~ND ND
53*8 49+4 63+1 40+2 44+fi 50*5 48+3 59+3 52+1 ND 60+14 58+5 41+4 ND
45*8 56+3 70+.2 56*1 64+1 37£3 48+3 62+1 50+1
ND 24+8 Gain ND ND 50+1 Gain 58+9 39+5 35+9 11+4 44+6 ND ND
dain 34J7 Gain 20+.15 45*2 42+6 38+5 38+TO 52+/1
Gain ND ND 23+1 NO ND 11+5 ND ND 21+9 ND 12+2 33*6 ND
26+7.2 58+5 ND 59*_1 59*3 48+3 36+6 54+6 6S+2
NO ND Gain 43+23 Gain
ND 38*7 33*23 10*4 NO 18-1 25*9 NO NO NO 92*2 Sain 21-6 NO
72*18 59+6 58*"15 67+3 58»3 64*1 50+9 70+7 5 HZ
75+9 90+4 83+3 72+1 S8+1 70+3 56+14 80+3 64+85 Ind Ind
~
ND .'58*10 Ind Gain N0 Gain ND :8+22
ND ND Ind
67+36 Ind Ind Ind
Ga i n
4ira ND ND ND
20+14
58+7 84+1 82*4 55+J8
10+3
Western Coals
Belle
Ayr Colstrip
!nd Ind
NO Ind
NO 86+E
Ind Ind
Ind Ind
Gain Gain
19+.7 ^a'"
44+9 ND
41+7 NB
Gain Gain
92+25 93^.3
89+6 58*5
Gain 93+^11
Ind Ind
ND Ind
Ind Ind
Gain 98+11
95+_l ND
tn
aM«100 mesh x Ot a finer ROM coal treated by the Meyers Process
bFs=1.90 float fraction of 14 mesh x 0 coal treated by float-sink methods
cND=no statistically significant difference between initial and final values.
Gain-treated coal showed increase in trace metal content.
elnd»both initial and final values near or below level of detectability.
-------
Li - Lithium is removed in only a few cases by the Meyers Process
but shows 50-70% removal by washing in nearly every case.
Mn - Manganese is easily and effectively removed by the Meyers
Process by 60-90% in most cases. Washing is nearly as effec-
tive but seems to remove slightly less than 40-70%.
Ni - Nickel is removed by the Meyers Process by 30-70% in most coals.
Washing does not appear to be effective.
Pb - In several cases Pb shows excellent removal (70-90%) by the
Meyers Process. For cases where both processes are analyzed,
neither appears to be effective.
Sb - Due to the low values of Sb present in coal and the poor pre-
cision of the results, the data for Sb are inconclusive. How-
ever, in those cases where there is a high Sb concentration
in the starting coal, Sb is effectively removed by the Meyers
Process and to a lesser extent, by washing.
Se - No conclusion can be drawn due to the difficulties with the
analyses.
Sn - Tin shows little signs of being removed by either process.
V - Vanadium shows moderate removal by either process, with
slightly better results by washing.
Zn - Zinc is easily and effectively removed by either process in
almost every case. The Meyers Process appears more effective
(70-90%) than washing (30-40%).
4.5.3 Summary and Conclusions
Analyses of 50 coal samples, consisting of 20 as-received, 20 chemically
extracted using the Meyers Process, and 10 undergoing float-sink separation
have shown that both float-sink procedures and the Meyers Process are able
to remove significant amounts of several trace elements. Although results
vary from coal to coal as to elements extracted and the degree of extrac-
tion, some general conclusions can be reached.
• Elements commonly found in nature as sulfides are the calco-
phile elements, which include As, Co, Cu, Ni, Pb and Sb. The
76
-------
Meyers Process appears to be more efficient than float-sink
procedures in removing these elements. The Meyers Process
has demonstrated removal of As, Cu, Ni, Pb, and Sb, whereas
float-sink procedures removed only As, Cu, and Sb.
A positive correlation has been demonstrated between Zn and
(9)
Cd in Illinois coals by the IGSV '. These two elements are
believed to be present in the host phase ZnS. Both Zn and
Cd are removed with the Meyers Process, but only Zn removal
was demonstrated by float-sink. Coals extracted by the
Meyers Process generally exhibited a much higher rate of Zn
removal than float-sink samples which could account for the
accompanying increased number of samples exhibiting Cd
removal. Because Cd is present in all of the tested coals
in amounts less than 2 ppm, it is statistically difficult
to observe the smaller changes in concentration that would
be expected as the result of float-sink separation.
Float-sink procedures were found to extract significant
amounts of Li and F which were not removed to any signifi-
cant degree by the Meyers Process.
The elements As, Cr, Mn, Ni, and Zn were found amenable to
removal by the Meyers Process in over 65% of the coals
tested. The degree of extraction was found to vary from
coal to coal, however, with As registering removals varying
from 81-100%; Cr, 23-71%; Mn, 44-93%; Ni, 27-89%; and
Zn, 47-95%. Ag, Cd, and Sb also appear to be effectively
removed by the Meyers Process; but due to their low con-
centrations, the data are inconclusive.
Float-sink procedures accounted for a larger number of ele-
ments being significantly removed. Again, the results
were variable from coal to coal. Ag was found to be
removed in the range 28-66%; As, 18-97%; Cr, 37-70%;
Cu, 20-88%; F, 28-69%; Li, 33-72%; Mn, 20-96%; and Zn,
10-70%.
77
-------
• The elements Pb and Cd were not removed from the coals using
float-sink procedures. Sn also registered no losses. How-
ever, because of the large gains in Sn concentration found in
the washed coals, it is suspected that contamination occurred
during washing. This could be a result of Sn extracted from
the soldered joints in the metal containers used in these
separations by HC1 present due to slight hydrolysis of the
chlorinated float-sink solvents.
• Three mines (Mathies, Ken, and Delmont) showed the largest
number of elements removed (14, 15 and 14, respectively).
In conclusion, the Meyers Process as well as float-sink procedures
are potentially viable techniques for the removal of a number of poten-
tially hazardous trace elements. This study indicates that Ag, As, Cd,
Cr, Mn, Ni, Zn and Sb are removed by the Meyers Process in significant
amounts for the majority of the coals tested. Float-sink procedures have
been shown to also be useful for the reduction of Ag, As, Cr, Cu, F, Li,
Mn and Zn in the majority of the coals tested. The effective removal of
As, Cd, Cr, Sb, Ni, and Zn from coal is especially noteworthy, as these
compounds are reportedly concentrated (along with Pb and Se) in the fine
(9-12)
particulate emitted from coal-fired power plantsv '. This fine par-
ticulate has been demonstrated to pass through conventional particulate
control devices.
78
-------
5.0 ACKNOWLEDGMENTS
The following TRW personnel deserve acknowledgement: W.P. Kendrick
and D. Kilday for experimental assistance; E.A. Burns and R.J. Ottinger
for technical assistance; J.L. Blumenthal and B. Dubrow for managerial
assistance; and S. Quinlivan for report editing and coordination.
The Program Manager for this study at the Systems Group of TRW Inc.,
was Robert A. Meyers, and the monitoring Project Officer for this Environ-
mental Protection Agency contract was Lloyd Lorenzi, Jr. Appreciation is
expressed to Mr. Lorenzi for his guidance and encouragement. Messrs.
I. Foster and R. Kaplan of the Commercial Testing and Engineering Company
(Chicago, Illinois) deserve special recognition for their cooperation in
expediting coal sampling and analyses for TRW at CT&E.
79
-------
6.0 REFERENCES
1. Hamersma, J.W., E.P. Koutsoukos, M.L. Kraft, R.A. Meyers, G.J. Ogle,
and L.J. Van Nice, "Chemical Desulfurization of Coal: Report of
Bench-Scale Developments," EPA R2-73-173, prepared for the Office
of Research and Monitoring of the Environmental Protection Agency,
Research Triangle Park, N.C., February 1973.
2. Hamersma, J.W., M.L. Kraft, C.A. Flegal, A.A. Lee, and R.A. Meyers,
"Applicability of the Meyers Process for Chemical Desulfurization of
Coal: Initial Survey of Fifteen Coals," EPA-650/2-74-025, prepared
for the Office of Research and Monitoring of the Environmental Pro-
tection Agency, Research Triangle Park, N.C., April 1974.
3. Koutsoukos, E.P., M.L. Kraft, R.A. Orsini, R.A. Meyers, M.J. Santy,
and L.J. Van Nice, "Program for Bench-Scale Development of Processes
for the Chemical Extraction of Sulfur from Coal," EPA Contract
No. 68-02-1336, prepared for the Office of Research and Monitoring
of the Environmental Protection Agency, Research Triangle Park, N.C.,
in press.
4. "1973 Keystone Coal Industry Manual," Mining Information Services,
McGraw-Hill Mining Publication, McGraw-Hill, Inc., New York, 1973.
5. Averitt, Paul, "Coal Resources of the United States," Bulletin 1275,
Bureau of Mines, U.S. Department of the Interior, 1969.
6. "1971 Book of ASTM Standards, Gaseous Fuels; Coal and Coke," Part 19,
American Society of Testing and Materials, Philadelphia, Pa., 1971.
7. Youden, W.J., "Statistical Methods for Chemists," John Wiley & Sons,
New York, p. 119, 1951.
8. Bauer, E.L., "A Statistical Manual for Chemists," Academic Press,
New York, p. 61, 1971.
9. Final report, "Occurrence and Distribution of Potentially Volatile
Trace Elements in Coal," R.R. Ruch, H.J. Gluskoter and N.F. Shimp,
EPA-650/2-74-054.
80
-------
10. J.W. Kaakinen, R.M. Jorden, and R.E. West, "Trace Element Study in a
Pulverized Coal Fired Power Plant," Paper No. 74-8 presented at the
67th APCA Annual Meeting, Denver, Colorado, 1974.
11. A. Lohr, A.H. Miguel, D.F.S. Natusch, and J.R. Wallace, "Preferential
Concentration of Toxic Species on Small Airborne Particulates," Paper
No. 74-201 presented at the 67th Annual APCA Meeting, June, 1974.
12. R.E. Lee, Jr.,. and D.J. von Lehmden, "Trace Metal Pollution in the
Environment," J. Air Pollution Control Assoc. 23 (10): 853, 1973.
13. D.F.S. Natusch, J.R. Wallace and C.A. Evans, Jr., "Toxic Trace
Elements: Preferential Concentration in Respirable Particles,"
Science 183 (4121): 202, 1974.
14. C.E. Billings, A.M. Sacco, W.R. Matson, R.M. Griffin, W.R. Coniglio
and R.A. Harley, "Mercury Balance on a Large Pulverized Coal-Fired
Furnace," J. Air Pollution Control Assoc. 23(9): 773, 1973.
81
-------
7.0 GLOSSARY OF ABBREVIATIONS AND SYMBOLS
Abbreviations
Abs
ASTM
btu
cal
eq
Exp.
Kcal
ml
ppm
Rxn.
wt
Symbols
C
A
u
M
mM
N.
P
R
S
S°
S_
o
T
t
V
W
absolute
American Society for Testing and Materials
British Thermal Unit
calories
equation
experiment
kilocalories
milliliter
parts per million
reaction
weight
concentration
difference in quantity following delta
micron
molarity
millimole
normality
total pressure, atmospheres
gas constant, cal/mole, K
sulfur
elemental sulfur
organic sulfur
pyritic sulfur
total sulfur
sulfate
standard deviation
absolute temperature, K
time, hours (leaching)-minutes (regeneration)
volume
pyrite concentration in coal, wt%
ferric ion to total iron ratio
82
-------
8.0 UNIT CONVERSION TABLE
To Convert From
btu
feet (ft)
gallons (gal)
inches (in.)
miles (mi)
ounces (oz)
pounds (Ibs)
pounds (Ibs)
square miles (sq.mi)
temp (°F -32)
tons
calories (cal)
meters (m)
liters
centimeters (cm)
kilometers (km)
grams (g)
grams (g)
kilograms (kg)
square kilometers (sq.km)
temp (°C)
kilograms (kg)
Multiply By
252.0
0.3048
3.785
2.540
1.609
28.35
453.6
0.4536
2.590
0.5556
907.200
83
-------
9.0 APPENDICES
TABLE OF CONTENTS
APPENDIX A Seam Extent and Sample Location
APPENDIX B Ranking of Treated and Untreated Coals
APPENDIX C Untreated Coal Analysis Data
APPENDIX D Pyritic Sulfur Removal Data
APPENDIX E Washability Tables
APPENDIX F Methods Development and Trace Element Analysis Data.
References for Appendix F
P_age_
90
134
142
148
155
176
203
84
-------
APPENDICES
TABLES
Page
A-l to A-2 Sulfur Content Data
A-l Average Sulfur Content of U.S. Coal 91
A-2 Average Sulfur Content of Coals by State 94
B-l to B-5 Coal Ranking Data
B-l Untreated Coal, Final Twenty Coals 135
B-2 Untreated Coal, Initial Fifteen Coals 136
B-3 Pyritic Sulfur Extractions, Final Twenty Coals 137
B-4 Pyritic Sulfur Extractions, Initial Fifteen Coals 138
B-5 Computer Program for Determining the Rank of Coal 139
C-l to C-5 Untreated Coal Analyses
C-l Muskingum, Powhattan No. 4, Isabella and 143
Mathies Mines
C-2 Williams, Robinson Run, Shoemaker and Delmont 144
Mines
C-3 Marion, Lucas, Bird No. 3, and Martinka Mines 145
C-4 Meigs, Dean, Kopperston No. 2 and Harris Nos. 1 146
and 2 Mines
C-5 North River, Homestead, Ken and Star Mines 147
D-l to D-5 Pyritic Sulfur Removal Data
D-l Muskingum, Powhattan No. 4, Isabella and 149
Mathies Mines
D-2 Williams, Robinson Run, Shoemaker and Delmont 150
Mines
D-3 Marion, Lucas, Bird No. 3, and Martinka Mines 151
D-4 Meigs, Dean, Kopperston no. 2 and Harris Nos. 1 152
and 2 Mines
D-5 North River, Homestead, Ken, and Star Mines 153
D-6 Pyritic Sulfur Removal Data
E-l to E-60 Washability Tables
Muskingum Mine
E-l 38.1 mm x 149y (1-1/2"x 100 mesh) 156
E-2 9.51 mm x 149u (3/8" x 100 mesh) 156
E-3 1.41 mm x 0 (14 mesh x 0) 156
Powhattan No. 4 Mine
E-4 38.1 mm x 149y (1-1/2" x 100 mesh) 157
E-5 9.51 mm x 149n (3/8" x 100 mesh) 157
E-6 1.41 mm x 0 (14 mesh x 0) 157
Isabella Mine
£-7 38.1 mm x 149u (1-1/2" x 100 mesh) 158
E-8 9.51 mm x 149u (3/8" x 100 mesh) 158
E-9 1.41 mm x 0 (14 mesh x 0) 158
85
-------
Mathies Mine
E-10 38.1 mm x 149y (1-1/2" x 100 mesh) 159
E-ll 9.51 mm x 149y (3/8" x 100 mesh) 15g
E-12 1.41 mm x 0 (14 mesh x 0) 159
Williams Mine
E-13 38.1 mm x 149y (1-1/2" x 100 mesh) 160
E-14 9.51 mm x 149y (3/8" x 100 mesh) 160
E-15 1.41 im x 0 (14 mesh x 0) 160
Robinson Run Mine
E-16 38.1 mm x 149y (1-1/2" x 100 mesh) 161
E-17 9.51 mm x 149y (3/8" x 100 mesh) 161
E-18 1.41 mm x 0 (14 mesh x 0} 161
Shoemaker Mine
E-19 38.1 mm x 149y (1-1/2" x 100 mesh) 162
E-20 9.51 mm x 149y (3/8" x 100 mesh) 162
E-21 1.41 rrni x 0 (14 mesh x 0) 162
Delmont Mine
E-22 38.1 mm x 149y (1-1/2" x 100 mesh) 163
E-23 9.51 mm x 149y (3/8" x 100 mesh) 163
E-24 1.41 mm x 0 (14 mesh x 0) 163
Marion Mine
E-25 38.1 mm x 149y (1-1/2" x 100 mesh) 164
E-26 9.51 mm x 149y (3/8" x 100 mesh) 164
E-27 1.41 mm x 0 (14 mesh x 0) 164
Lucas Mine
E-28 38.1 mm x 149y (1-1/2" x 100 mesh) 165
E-29 9.51 mm x 149u (3/8" x 100 mesh) 165
E-30 1.41 mm x 0 (14 mesh x 0) 165
Bird No. 3 Mine
E-31 38.1 mm x 149y (1-1/2" x 100 mesh) 166
E-32 9.51 mm x 149y (3/8" x 100 mesh) 166
E-33 1.41 mm x 0 (14 mesh x 0) 166
Martinka Mine
E-34 38.1 mm x 149y (1-1/2" x 100 mesh) 167
E-35 9.51 mm x 149y (3/8" x 100 mesh) 167
E-36 1.41 mm x 0 (14 mesh x 0) 167
ftfi
-------
Meigs Mine
E-37 38.1 mm x 149y (1-1/2" x 100 mesh) 168
E-38 9.51 mm x 149y (3/8" x 100 mesh) 168
E-39 1.41 mm x 0 (14'mesh x 0) 168
Dean Mine
E-40 38.1 mm x 149y (1-1/2" x 100 mesh) 169
E-41 9.51 mm x 149y (3/8" x 100 mesh) 169
E-42 1.41 mm x 0 (14 mesh x 0) 169
Kopperston No. 2 Mine
E-43 38.1 mm x 149y (1-1/2" x 100 mesh) 170
E-44 9.51 mm x 149y (3/8" x 100 mesh) 170
E-45 1.41 mm x 0 (14 mesh x 0) 170
Harris Nos. 1 & 2 Mines
E-46 38.1 mm x 149y (1-1/2" x 100 mesh) 171
E-47 9.51 mm x 149u (3/8" x 100 mesh) 171
E-48 1.41 mm x 0 (14 mesh x 0) 171
North River Mine
E-49 38.1 mm x 149y (1-1/2" x 100 mesh) 172
E-50 9.51 mm x 149y (3/8" x 100 mesh) 172
E-51 1.41 mm x 0 (14 mesh x 0) 172
Homestead Mine
E-52 38.1 mm x 149y (1-1/2" x 100 mesh) 173
E-53 9.51 mm x 149y (3/8" x 100 niesh) 173
E-54 1.41 mm x 0 (14 mesh x 0) 173
Ken Mine
E-55 38.1 mm x 149y (1-1/2" x 100 mesh) 174
E-56 9.51 mm x 149y (3/8" x 100 mesh) 174
E-57 1.41 mm x 0 (14 mesh x 0) 174
Star Mine
E-58 38.1 mm x 149y (1-1/2" x 100 mesh) 175
E-59 9.51 mm x 149y (3/8" x 100 mesh) 175
E-60 1.41 mm x 0 (14 mesh x 0) 175
F-l Atomic Absorption Analytical Parameters -j82
F-2 to F-ll Trace Element Analyses Data
F-2 Muskingum Mine 193
F-3 Mathies Mine 194
F-4 Robinson Run Mine 195
F-5 Powhattan No. 4 Mine 196
F-6 Delmont Mine 197
F-7 Marion Mine 198
F-8 Lucas Mine 199
F-9 Bird No. 3 Mine 200
F-10 Meigs Mine 201
F-ll Ken Mine 202
-------
APPENDICES
FIGURES
Page
Maps - Seam Extent and Sample Location
A-l Percentage Distribution of Cumulative Coal Production of the 92
United States to 1 January 1967
A-2 Coal Fields of the Conterminous United States 92
A-3 Coal Resources of the United States 93
A-4 Pennsylvania - Sewickley Seam 105
A-5 West Virginia - Sewickley Seam 106
A-6 Ohio - Sewickley Seam 107
A-7 Pennsylvania - Pittsburgh Seam 108
A-8 West Virginia - Pittsburgh Seam 109
A-9 Ohio - Pittsburgh Seam 110
A-10 Pennsylvania - Upper Freeport (No. 7) Seam 111
A-11 West Virginia - Upper Freeport (No. 7) Seam 112
A-12 Ohio - Upper Freeport (Ho. 7) Seam 113
A-13 Pennsylvania - Lower Freeport (No. 6A) Seam 114
A-14 West Virginia - Lower Freeport (No. 6A) Seam 115
A-15 Ohio - Lower Freeport (No. 6A) Seam 116
A-16 Pennsylvania - Upper Kittanning Seam 117
A-17 West Virginia - Upper Kittanning Seam 118
A-18 Ohio - Upper Kittanning Seam 119
A-19 Pennsylvania - Middle Kittanning (No. 6) Seam 12°
A-20 West Virginia - Middle Kittanning (No. 6) Seam 121
A-21 Ohio - Middle Kittanning Seam I22
A-22 Pennsylvania - Lower Kittanning Seam I23
A-23 West Virginia - Lower Kittanning Seam 124
A-24 Ohio - Lower Kittanning Seam I25
A-25 Ohio - Clarion 4A Seam 126
A-26 Eastern Kentucky - Mason Seam I2?
A-27 Illinois - No. 5 - Harrisburg-Springfield Seam 128
A-28 Indiana - Springfield - No. V Seam 129
88
-------
A-29 Western Kentucky - No. 9 Seam 130
A-30 Illinois - Herrin No. 6 Seam 131
A-31 Western Kentucky - No. 11 Seam 132
A-32 Indiana - Hymera No. VI Seam 133
89
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APPENDIX A
SEAM EXTENT AND SAMPLE LOCATION
90
-------
A.I Selection of Coals
Some of the background information which was utilized to aid in the
selection of the twenty coals for this study is presented below in three
paragraphs: Previous Production by State, Distribution of Coal Reserves
and Distribution of Sulfur Content(4»5)-
Previous Production by State - Figure A-l shows the percentage
distribution of the cumulative production of coal in the United
States up to January 1, 1967. In descending order of production,
the six most productive states were: Pennsylvania, West Virginia,
Illinois, Kentucky, Ohio and Indiana. These states have produced
slightly over 84% of the coal consumed to date.
Distribution of Coal Reserves in the United States - The
distribution of the coal reserves in the United States is shown
by Figure A-2, which gives aerial distribution and Fiqure A-3,
which quantitatively describes the total resources remaining.
From an examination of Figure A-3, it is apparent that coal from i
the following seven states would represent the vast majority of
the remaining resources of bituminous coal in the United States:
Illinois, West Virginia, Colorado, Pennsylvania, Kentucky, Ohio
and Indiana.
Distribution of Sulfur Content in Coal
general distribution
and average
This distribution shows that the
sulfur coal are east of the Mississippi
- Table A-l shows the
sulfur content of U.S. coals.
major areas containing high
River.
TABLE A-l
AVERAGE SULFUR CONTENT OF U.S. COAL*
Coal Resources Determined
by Mapping and Exploration
Total bituminous coal, subbituminous
coal, and lignite
Bituminous coal east of the
Mississippi River
Low Sulfur
(1.02 or
Less)
652
20%
Medium
Sul fur
f].l-3.03rt
15%
37%
High
Sulfur
(>32H
20%
43%
*Dry basis.
91
-------
STATES WEST
OF THE
MISSISSIPPI
RIVER
WESTERN INTERIOR BASIN 3.6
ROCKY MOUNTAIN STATES 4.4
WEST COAST AND ALASKA 0.5
ALABAMA 2.7
TENNESSEE 1.1
VIRGINIA 2.6
OTHER STATES 0.9
A 3.3
Figure A-l
Percentage Distribution of Cumulative Coal
Production of the United States to 1 January 1967
Figure A-2
Coal Fields of the Conterminous United States
92
-------
Figure A-3
COAL RESOURCES OF THE UNITED STATES
100
BILLIONS OF SHORT TONS
200
300
UD
co
NORTH DAKOTA
MONTANA
ILLINOIS
ALASKA ]
WYOMING1
WEST VIRGINIA
COLORADO2
PENNSYLVANIA
KENTUCKY
NEW MEXICO2
OHIO
INDIANA
UTAH
MISSOURI
KANSAS
ALABAMA
TEXAS
VIRGINIA2
'//////////////////// R™;.: \nZZMMS
*^^i ////s/////// s / { / j
J^t'JiQ^CCC^^C^^vS^C'^CCf / / t
J^Q«^^J«^Qs^^^^^^iJi^C^^^^^B
^^^^^^^^^^^XVviviv^I
"^^vl/ / / / / / / £\
•^^o^^^^^y^^^
5?SSi^^
s^^^^^^^3
^^^^y^3
SS3
EXF
:-:.:•:•:.;•: ::!^-;-:v.:-l
1ANATION
ES5SS BITUMINOUS C
f^^i SUBB1TUMINOU
FP»1 LIGNITE
i^ ANTHRACITE At
SEMlANTHRAd
3AL
S COAL
vID
[E
NOTES:
1 SMALL RESOURCES OF LIGNITE INCLUDED WITH SUBBITUMINOUS COAL
2 INCLUDES ANTHRACITE IN QUANTITIES TOO SMALL TO SHOW ON SCALE
OF DIAGRAM
-------
A review of the average sulfur content of the states previously
demonstrated to be of interest from a reserve or production point of view
are listed below in Table A-r2.
TABLE A-2
AVERAGE SULFUR CONTENT OF COALS BY STATE*
*Dry basis.
A. 1.1 Coal Sample Selection
State
Colorado
West Virginia
Illinois
Kentucky
Ohio
Indiana
Pennsylvania
%S
0.56
1.40
2.95
2.22
3.52
3.00
1.96
(4,5)
APPALACHIAN COALS
Coals sampled, as noted in the following sections, are given in their
descending strati graphic order in the Monongahela, Conemaugh, and Allegheny
stratigraphic groups, as defined in Pennsylvania and correlated with other
beds of the Appalachian Region.
t Sewickley Seam - The Sewickley seam, most recent in geologic
age of the coal beds investigated, is present in Pennsylvania
(Greene, Butler, Clarion, Armstrong, Washington, Fayette,
Westmoreland and Allegheny Counties), West Virginia (Marion,
Monongalia, Wetzel, Marshall and Ohio Counties, where an
estimated 2 billion tons remain), and Ohio, where the Sewickley
correlates with the Metgs Creek (or No. 9) seam which is found
in Monroe, Belmont, Harrison and Jefferson Counties. The Meigs
Creek seam ranks third in production in Ohio. This initial
survey initiated the examination of this coal with a sample
from the Warwick mine in Greene County, Pennsylvania. Sub-
sequently, a sample of this coal was taken at the Muskigum
mine in Morgan County, Ohio. State maps showing the extent
of this bed and the locations of the two mines are shown as
Figures A-4, A-5 and A-6.
94
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Pittsburgh Seam - The Pittsburgh bed has been described as the
most valuable individual mineral deposit in the United States.
It is of minable thickness over an area of about 15,000 sq. km
(6,000 sq. mi) in Pennsylvania (Washington, Greene, Indiana,
Somerset, Allegheny, Armstrong, Westmoreland and Fayette Counties
where approximately 7 billion tons remain), West Virginia (parts
of Brooke, Ohio, Marshall, Wetzel, Monongalia, Marion, Doddridge,
Harrison, Taylor, Preston, Mineral, Barbour, Upshur, Lewis,
Gilmer, Braxton, Calhoun, Clay, Roane, Kanawha, Putnam, Mason,
Cabell and Wayne Counties with approximately 10 billion tons
of minable reserves), and eastern Ohio (primarily Belmont,
Harrison, Jefferson, Carroll, Columbiana, Mahoning and Monroe
Counties which contain some 10 billion tons of reserve).
Pittsburgh coal is also found in the Georgis Creek basin
(Garrett and Allegheny Counties, Maryland) where only about
2 million tons remain. A Pittsburgh coal from Greene County,
Pennsylvania was examined in the previous bench-scale program^1'.
This program expanded the coverage of the Pittsburgh bed by
sampling coals from: the Humphrey No. 7, Williams, Robinson
Run, and Shoemaker mines in West Virginia; the Mathies and
Isabella mines in Pennsylvania; and the Egypt Valley No. 21
andPowhattan No. 4 mines in Ohio. State maps showing the
counties containing minable Pittsburgh coal and the locations
of the mines sampled are shown in Figures A-7, A-8 and A-9.
In this case, where the remaining reserves are rather clearly
defined, the yearly production of the mines sampled represent
approximately one two-thousandths of the seam reserve.
Upper Freeport Seam - The Upper Freeport bed is less uniform
in thickness than the overlying Pittsburgh bed or the underlying
Lower Kittanning bed because it was subjected to local uplift
and erosion before deposition of the overlying rocks. Neverthe-
less, it is a persistent bed throughout large areas in Pennsylvania,
West Virginia, and Ohio, and is the third most important bed in
the northern part of the Appalachian bituminous coal basin, both
in production and in contained resources. In Pennsylvania, the
Upper Freeport bed is thick and continuous in the counties around
Pittsburgh and in the southwestern part of the state, where it
ranges in thickness from 0.6 to 3 m (2 to 10 ft), and is 1 to 2 m
(4 to 6 ft) thick over considerable areas. In West Virginia, the
Upper Freeport bed is considered to be of minable thickness and
purity over an area of 3,030 sq. km (1,165 sq. mi) in a belt
running north-south through the central part of the state. In
the northern part of the belt it ranges in thickness from 0.9 to
4 m (3 to 12 ft) and is 1 to 1.5 m (4 to 5 ft) thick over large
areas. It thins to the south and is generally less than 0.6 m
(2 ft) thick in Clay and Braxton Counties. In Ohio, the Upper
Freeport bed is very irregular in thickness. It is locally as
much as 2 m (8 ft) thick, but typically thins within a few miles,
or tens of miles, to less than 35 cm (14 in.). Nevertheless, its
wide distribution makes it the fourth most important bed in Ohio
in known resources. The Marion and Delmont mines in Westmoreland
95
-------
and Indiana Counties in Pennsylvania were sampled. State maps
showing the location of these mines and the counties containing
minable coal are shown in Figures A-10, A-11 and A-12.
Lower Freeport (No. 6A) Seam - The Lower Freeport seam is also
present in Pennsylvania, West Virginia, Ohio and Maryland. In
Pennsylvania it is present in Lawrence, Beaver, Washington,
Greene, Butler, Allegheny, Fayette, Westmoreland, Armstrong,
Indiana, Somerset, Cambria, Bedford and Fulton Counties. In
teest Virginia, it is minable in parts of Nicholas, Roane,
Braxton, Preston, Ohio, Brooke and Hancock Counties. Of the
original 700 million tons minable in West Virginia, compara-
tively little has been removed. In Ohio the Lower Freeport
is present and of importance in Jefferson, Athens, and Perry
Counties where some 3 billion tons remain. In Maryland the
Lower Freeport is mined in Garrett and Allegheny Counties in
the northwest corner of the state bordering on West Virginia
and Pennsylvania. For this program, a sample was taken from
the Jane Mine in Pennsylvania. State maps showing the counties
with minable Lower Freeport coal as well as the location of
the mine sampled are shown in Figures A-13, A-14 and A-15.
Since only two counties in Maryland are of concern, they are
not mapped.
Upper Kittanning Seam - The Upper Kittanning coal is strati-
graphical ly the uppermost of the three Kittanning coals originally
named at Kittanning, Pennsylvania. In Pennsylvania {Lawrence,
Beaver, Washington, Greene, Fayette, Westmoreland, Armstrong,
Clarion, Jefferson, Indiana, Somerset, Cambria and Clearfield
Counties) the seam is thin and thus infrequently deep-mined. In
West Virginia, the coal is of sufficient thickness for mining
in parts of Kanawha, Nicholas, Clay, Braxton, Webster, Upshur,
Lewis, Randoph, Barbour, Harrison, Taylor, Marion, Monongalia and
Preston Counties over an area of some 3,600 sq. km (1400 sq. mi).
The original reserves in West Virginia were estimated at 4
billion tons; and since this bed has not been a major producer
for the state, the majority of the coal remains.
The Upper Kittanning seam is not a major coal bed in Ohio but geo-
logically it follows the Lower Kittanning in its persistence from
northeast to southwest in the Ohio coal fields. In Maryland, the
Upper Kittanning seam is mined in both Garrett and Allegany
Counties where it forms parts of the 1 billion tons of remaining
coal reserves.
One sample for this program was taken from the Walker Mine in
Maryland. State maps showing the extent of this bed are shown
in Figures A-16, A-17, and A-18. (Maryland, where the sample
was taken, is again not shown because of the two county repre-
sentations.)
Qfi
-------
Middle Kittanninq or No. 6 Seam - This bed of coal is remarkably
uniform and persistent and for many years was the most important
coal bed in Ohio from the standpoint of quality and production.
It is now outranked in production by the Pittsburgh (No. 8) bed,
but is mined in every county along its outcrop from the Ohio-
Pennsylvania state line and in Columbiana County on the north
to Lawrence County on the south. This great coal bed is also
important in Pennsylvania and West Virginia, and is tentatively
correlated with the important Herrin (No. 6) coal of Illinois.
Conservative estimates indicate well over 7 billion tons of No.
6 coal is over 0.9 m (28 in.) thick in Ohio.
The coal is exceptionally firm and stands shipping well which,
coupled with low ash often having high fusion temperature and a
very low "free swelling index" (free burning), makes it an
exceptional coal for the retail market. When it is mechanically
cleaned and sized, it is an outstanding domestic stoker coal,
free from troublesome "coke trees" and other operating difficulties.
It is extensively used in the ceramic and cement industries owing
to its superior performance under difficult operating conditions.
For steam generation, it gives unusually good performance on
chain or traveling grate stokers. Owing to its favorable ash
softening temperature and burning characteristics it performs
well in both multiple and single retort underfeed stokers.
A single sample from this seam was taken from the Lucas Mine in
Columbiana County, Ohio. State maps showing the location of
this mine and the extent of the same are shown in Figures A-19,
A-20, and A-21.
Lower Kittanning Seam - The Lower Kittanning bed is most pervasive
throughout the northern part of the Appalachian basin throughout
portions of Pennsylvania, West Virginia, Ohio and Maryland. In
Pennsylvania (Lawrence, Beaver, Washington, Greene, Fayette,
Westmoreland, Butler, Clarion, Armstrong, Somerset, Indiana,
Jefferson, Clearfield, Cambria, Bedford and Fulton Counties) it
is widely strip mined. In West Virginia the Lower Kittanning
(also called the No.5 Block) is minable in parts of Mingo, Logan,
Boone, Wayne, Lincoln, Kanawha, Nicholas, Fayette, Clay, Roane,
Braxton, Webster, Randolph, Upshur, Lewis, Barbour, Taylor, Marion,
Mononqalia, Preston and Mineral Counties. It covers an area
greater than 6,700 sq. km (2600 sq. mi) and is estimated to have
originally contained over 10 billion tons. Though one of the
most mined beds of West Virginia, much of this reserve remains.
This coal is present in most of the counties comprising the coal
fields of eastern Ohio, extending from Mahoning County in the
northeast through Lawrence and Scioto Counties in the southeast.
In Ohio, the estimated minable reserves total three billion tons.
The coal is also present in the two coal counties of Maryland
(unmapped), though this is not of major commercial importance.
97
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The previous bench scale progranr examined a Lower Kittanning
coal from Indiana County, Pennsylvania. For this program,
samples were obtained from the Fox and Bird No. 3 mines in
Pennsylvania and the Martinka mine in West Virginia. State
maps showing the extent of this bed and the mine locations are
given in Figures A-22, A-23, and A-24.
Clarion or No. 4A Seam - The Clarion coal can be traced from the
Ohio-Pennsylvania line southwest to the Ohio River. However,
along most of this line of outcrop the bed is too thin to be
worked. The one deposit of importance lies in the southern
part of the state and includes northern Lawrence, eastern Scioto,
eastern Jackson, northwestern Gallia, and southern Vinton
Counties. In places the coal lies directly below the Vanport
lime but elsewhere is separated by two partings of clay. This
varies, however, and especially so along the margin of the field.
The thickness of the bed in Southern Ohio is 10.9 to 1.2 m
(3 to 4 ft) thick. The Clarion coal is moderate in heating
value, high in sulfur and ash.
Clarion coal when washed is a very suitable industrial coal for
steam generation utilizing underfed stokers, pulverized fuel
furnaces, chain or traveling grate stokers, and spreader stokers.
The most desirable feature of this coal for steam use is the
wide ash fusion range, as the fusion starts at an initial 2150°F,
with the softening temperature 2280°F and the ash fluid temper-
ature at 2560°F. This fusion range makes it a relatively safe
coal to use on stokers.
A sample from this seam was taken from the Meigs mine in Meigs
County, Ohio. A state map showing the location of this mine is
shown in Figure A-25.
Dean Seam - The Dean seam, more commonly known as Big Mary seam,
has its most important development in the New River area of
Anderson, Campbell, and Morgan Counties in Tennessee. Mining
thicknesses in this area range from 0.9 to 3 m (36 in. to 10 ft)
or more. The roof is a strong gray shale unusually subject to
air slacking, while the bottom is a soft shale or clay. The
Big Mary seam commonly occurs in two benches; and in the thinner
seam areas, only the upper bench is evident. The lower bench
may vary from 0.2 to 0.7 m (10 in. to 30 in.) in thickness and
occurs below the top bench with an interval of from several
inches to 1.5 m (5 ft) or more. Occasionally, the two benches
join to form a thick seam. The coal from the Big Mary vein is
coarse and blocky. It is suitable for general steam and domestic
use and was formerly a favorite railroad fuel. A single sample
was taken from the Dean mine in Scott County, Tennessee.
98
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Mason Seam - To provide an example of an Eastern Kentucky coal,
a sample was taken from the Dixie Fuel Company's No. 1 mine in
Harlan County, Kentucky. A state map showing the location of
the sampling point in the Upper Cumberland reserve district is
shown in Figure A-26.
Campbel1 Creek Seam - A domestic steam, gas, by-product, and
metallurgical coal named for its occurrence along Campbell Creek,
Kanawha County, West Virginia. It is minable in parts of Wayne,
Mingo, Wyoming, McDowell, Logan, Lincoln, Boone, Raleigh, Fayette,
Kanawha, Nicholas, Clay, and Calhoun Counties in West Virginia
over an area of about 5,400 sq. km (2,100 sq. mi); it is the
most important seam of the entire Pottsville Group, the original
minable tonnage estimated as having been about 8 billion tons.
The coal is generally a multiple-bedded gas and splint type coal;
it is 0.6 to 3 m (2 to 10 ft) thick, averaging perhaps 1.5 m
(5 ft). It occurs 11 to 29 m (37 to 95 ft) above the Powellton
coal. A sample of this seam was taken from the Kopperston No. 2
mine in Wyoming County, West Virginia.
Eagle Coal Seam - A domestic steam, by-product and coking coal
named for Eagle, West Virginia, where it was first mined. It
is minable in parts of McDowell, Mingo, Wyoming, Boone, Kaleigh,
Kanawha, Fayette, Nicholas, Clay, Webster, Braxton, Upshur, and
Randolph Counties in West Virginia over an area of 3,500 sq. km
(1,360 sq. mi); the original minable tonnage is estimated to have
been nearly 4.2 billion tons. The coal is double-to-multiple-
bedded and splinty and ranges from 0.6 to 3 m (2 to 10 ft) thick,
averaging perhaps 1.2 m (4 ft). A sample of this bed was taken
from the Harris Nos. 1 and 2 mines in Boone County, West Virginia.
Corona Seam - In Alabama the Pratt Coal Group ranks second only
to the Mary Lee Group from a tonnage standpoint and includes the
American (Nickel Plate), Curry, Gillespie and Pratt (Corona).
beds mined in Jefferson and Walker Counties. The principal
beds in this group are the Pratt (known in the western part of
the basin as the Nickel Plate). Thickness of the Pratt bed
varies from 0.9 to 1.7 m (2 ft 10 in. to 5-1/2 ft); an average
of 26 sections of this bed shows 1.7 m (5-1/2 in.) of coal,
63 cm 12-1/2 in.) of parting and 0.9 m (34 in.) of coal. Roof
and floor of the Pratt bed usually are sandstone. This bed is
one of the major sources of coking coal in Alabama. The Corona,
which ranges from 0.8 to 1.2 m (30 to 52 in.) in thickness,
probably is the western extension of the Pratt bed. A single
sample was taken from the North River mine in Jefferson County,
Alabama.
99
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EASTERN INTERIOR REGION
No. 5 Bed (I11J, or No. 9 ^Ky.) Seam - The No. 5 bed is the
most widespread and commercially valuable coal bed in the
Eastern Interior coal basin. It is known in Illinois as the
No. 5 Harrisburg or Springfield bed; in Indiana as the Spring-
field or No. V bed; and in western Kentucky as the No. 9 bed.
It is of minable thickness over an area of about 52,000 sq. km
(20,000 sq. mi) in the three states and it is recognizable
as a lithologic unit over an area of about 78,000 sq. km
(30,000 sq. mi). In southeastern Illinois, it is 1 to 1.5 m
(4 to 5 ft) thick over large areas; in Indiana it has an
average thickness of 1.5 m (5 ft) and locally is as much as
3 m (11 ft) thick throughout its area of occurrence. From
the standpoint of resources, it is the most important bed in
Indiana and western Kentucky, and it is second only to the
Herrin No. 6 bed in Illinois.
In Illinois the No. 5 bed is present in strippable quantities in
some fifty counties having more than forty-one billion tons of
reserves. In Indiana,the Springfield (No. V) bed is present in
Sullivan, Vigo, Knox, Greene, Daviess, Pike, Gibson, Posey,
Vanderburgh and Warrick Counties, which contain twenty-six
billion tons of reserve.
The correlating coal seam in western Kentucky (the No. 9 bed)
is commonly found throughout the entire reserve district and
presently may be mined in Butler, Daviess, Henderson, Hopkins,
Muhlenberg, Ohio, Union, or Webster Counties.
A previous prograrrr ' utilized a No. 5 coal from Fulton
County, Illinois. This survey program has obtained samples
from the Eagle No. 2 mine in Gal latin County, Illinois. In
Kentucky, samples were taken from the Camp Nos. 1 and 2 mines
in Union County, the Ken mine in Ohio County and the Star mine
in Hopkins County. State maps showing the extent of these beds
are shown in Figures A-27, A-28, and A-29.
Herrin No. 6 Bed (IllJ, No. 11 (Ky.) Seam - The Herrin No. 6
bed is recognizable over an area of about 29,000 sq. km (15,000
sq. mi) in the Eastern Interior coal basin, where it is second
in commercial importance only to the No. 5 bed. It is known in
western Kentucky as the No. 11 bed and in Indiana as the Hymera
or No. VI bed. This coal attains maximum thickness in southern
Illinois, where it is locally as much as 4 m (14 ft) thick. In
central Illinois and in western Kentucky, the Herrin (No. 6) bed
is 1.5 to 2 m (5 to 7 ft) thick over large areas. It thins
eastward and is relatelv unimportant in Indiana. It also thins
toward the northwest edge of the basin. From the standpoint
of resources and production, it is the most important coal in
Illinois. In Illinois, the No. 6 bed has reserves in fifty-six
counties, totalling approximately sixty-six billion tons.
In Kentucky, the No. 11 bed is presently being
100
-------
mined in Hopkins, Ohio and Muhlenberg Counties. Indiana's
equivalent Hymera (No. VI) bed is of lesser importance but
it occurs in minable thickness in Sullivan, Knox, Pike, Gibson,
Warrick, Vanderburgh and Posey Counties.
The previous bench-scale prograrrr ' utilized a No. 6 coal from
Randolph County, Illinois and the present program examined
samples of No. 6 coal from the Orient No. 6 mine in Jefferson
County, Illinois and from the Homestead mine in Ohio County,
Kentucky. State maps showing the extent of minable beds and
the mine locations are shown in Figures A-30, A-31, and A-32.
WESTERN INTERIOR REGION
Des Moines No. 1 Seam - To provide a sample of coal from the Western
Interior Region, an Iowa coal from Marion County (the Des Moines
No. 1) seam was selected. Iowa's total reserves are an estimated
7 billion tons.
WESTERN COAL REGION
Wadge Seam - The Wadge seam of the Yampa field in the Green River
region is an example of coals from the northwestern part of
Colorado. The Edna mine in Routt County was sampled. The Wadge
seam in Colorado correlates with other coals of the Green River
region mined in the Rock Springs area in southwestern Wyoming.
In Colorado, the reserves are estimated at some one and one-half
billion tons.
No. 6, 7 and 8 Seams (Fruitland Formation) - The No. 6, 7 and 8
seams of the Fruitland Formation are presently being mined by
one of the largest stripping operations in the nation at the
Navajo mine in San Juan County, New Mexico. The coal resources
of New Mexico are estimated at 62 billion tons, 80% of which are
subbituminous coals which include the coal mined at the Navajo
mi ne.
Roland-Smith Seam - The Roland-Smith seam of the Powder River
Region represents one of the largest strippable reserve areas
of subbituminous coal in the U.S. For this program a sample
of the seam was taken from the Belle Ayr mine in Campbell County
(center of the Powder River Region), Wyoming.
Rosebud Seam - The Rosebud seam of subbituminous coal is repre-
sentative of the vast reserves (20 billion tons) of strippable
coal available in the Fort Union Region of Eastern Montana. This
region is represented in northeastern Wyoming by the coals of the
Powder River Region and translates into the lignites of eastern
Montana and western North Dakota. For the survey program, a sample
was taken from a large mine in the area, the Col strip mine in
Rosebud County, Montana.
101
-------
A.1.2 Mine Sample Procedures
The following tabulation describes in detail the specific sampling
procedures used in the twenty additional mines sampled in this part of
the program. The procedures for the initial fifteen coals were documented
(3)
previously .
• Muskingum Mine, Meigs Creek No. 9 Seam, Morgan County, Ohio,
Central Ohio Coal Company. The raw run of the mine coal was
collected over a 4 hour period on September 17, 1973. One
hundred and forty-four increments totaling 908 kg (2000 Ibs)
were taken by stopped belt sampling as the coal was going to
the preparation plant.
t Powhattan No. 4 Mine, Pittsburgh No. 8 Seam, Monroe County, Ohio,
Quarto Mining Company., The raw run of the mine coal sample was
collected over a 3-3/4 hour period of September 18, 1973. One
hundred and forty-eight increments totaling 908 kg (2000 Ibs) were
taken from a stopped belt leading from the stock pile to the
tipple.
• Isabella Mine, Pittsburgh Seam, Fayette County. Pennsylvania,
National Mines Corporation. The raw run of mine sample was
collected over a 3-1/2 hour period on November 21, 1973.
One hundred and forty-eight increments totaling 908 kg (2000 Ibs)
were taken from a stopped belt leading from the mine to the
preparation plant.
t Mathies Mine, Pittsburgh Seam. Washington County, Pennsylvania,
Mathies Coal Company. The raw run of mine sample was
collected over a 4 hour period on July 23, 1973. Ninety
increments totaling 908 kg (2000 Ibs) were taken from a stopped
belt leading from the mine to the coal preparation plant.
t Robinson Run Mine, Pittsburgh Seam, Harrison County, West
Virginia, Consolidation Coal Company. The raw run of the mine
coal sample was collected over a 4 hour period on
September 19, 1973. One hundred and forty-four increments totaling
908 kg (2000 Ibs) were taken from a stopped belt leading to the
preparation plant.
• Williams Mine. Pittsburgh Seam, Marion County, West Virginia,
Consolidated Coal Company, Mountaineer Coal Company Division.
The raw run of mine coal sample was collected over a 6-3/4
hour period on September 20, 1973. Sixty-six 30 Ib increments
totaling 908 kg (2000 Ibs) were taken from a stopped belt
leading to the preparation plant.
• Shoemaker Mine, Pittsburgh Seam, Marshall County, West Virginia,
Consolidation Coal Company, Mountaineer Coal Company Division.
The raw run of mine sample was collected over a 4 hour period
on September 19, 1973. One hundred and forty-eight increments
totaling 908 kg (2000 Ibs) were taken from a stopped belt
leading from the mine to the preparation plant.
102
-------
Marion Mine, Upper Freeport Seam, Indiana County, Pennsylvania.
Tunnel ton Mining Company. The raw run of mine coal was collected
over a 4-1/2 hour period on July 23, 1973, Sixty increments
totaling 908 kg (2000 Ibs) were taken by stopped belt sampling
as the coal was going into the silo.
Delmont Mine, Upper Freeport Seam, Westmoreland County,
Pennsylvania, Eastern Associated Coal Corporation. The raw run
of mine coal sample was collected over a 5 hour period on
September 21, 1973. One hundred and sixty increments totaling
908 kg (2000 Ibs) were taken from a stopped belt leading to
the preparation plant.
Lucas Mine, Middle Kittanning Seam, Columbiana County, Ohio,
Buckeye Coal Mining Company. The raw run of mine sample was
collected over a 5 hour period on July 24, 1973. Sixty
increments totaling 908 kg (2000 Ibs) were collected from
fifteen locations in the raw coal pit.
Martinka Mine, Lower Kittanning Seam, Logan County, West
Virginia, American Electric Power Company"! The raw run of
mine sample was taken during a 3-1/2 hour period on May 2, 1974.
One hundred and forty-seven increments totaling 908 kg
(2000 Ibs) were taken from a stopped belt.
Bird No. 3 Mine, Lower Kittanning Seam, Somerset County,
Pennsylvania, Island Creek Coal Company. The raw run of mine
sample was taken over a 3-1/2 hour period on September 21, 1973.
One hundred and sixty-six Increments totaling 908 kg (2000 Ibs)
were taken from a stopped belt leading to the tipple and
before the coal from the No. 2 and No. 3 mines were blended.
Meng«L Mine, Clarion 4A Seam, Meigs County, Ohio, American
Electric Power Company. The raw run of mine sample was
collected over a 3-1/2 hour period on September 17, 1973. One
hundred and forty increments totaling 908 kg (2000 Ibs) were
taken from a stopped belt leading to the stockpile.
Dean Mine, Dean Seam, Scott County, Tennessee, Royal Dean Coal
Company. The raw run of mine sample was collected over a
4 hour period on January 17, 1974. Approximately 55 increments
totaling 908 kg (2000 Ibs) were taken from a stopped belt
leading from the mine to the stockpile.
Kopperston No. 2 Mine, Campbell Creek Seam, Wyoming County,
West Virginia, Eastern Associated Coal Corporation.The raw
run of mine sample was collected over a 4 hour period on
November 26, 1973. One hundred sixty increments totaling
908 kg (2000 Ibs) were taken from a moving belt leading from
the mine to the preparation plant.
103
-------
0 Harris Nos. 1 and 2 Mines, Eagle and No. 2 Gas Seams, Poone
County, West Virginia. Eastern Associated Coal Corporation.
The raw run of mine sample was collected over a 4 hour
period on November 26, 1973. One hundred and forty increments
totaling 908 kg (2000 Ibs) were taken from mine cars coming
directly from the mine.
t North River Mine, Corona Seam. Jefferson County, Alabama.
Republic Steel Corporation. The raw run of mine sample was
taken on May 23, 1974. Fifty 40 Ib increments totaling
908 kg (2000 Ibs) were taken from various locations in the
stockpile.
• Homestead Mine, No. 11 Seam. Ohio County. Kentucky. Peabody
Coal Company.The raw run of mine sample was collected over
a 4 hour period on December 11, 1973. An automatic sampler was
used to take 30 increments totaling 908 kg (2000 Ibs).
• Ken Mine, No. 9 Seam. Ohio County, Kentucky, Peabody Coal
Company. The raw run of mine sample was collected over a
4-1/4 hour period on December 12, 1973. An automatic sampler
was used to take 30 increments totaling 908 kg (2000 Ibs).
• Star Mine. No. 9 Seam. Hopkins County, Kentucky. Peabody Coal
Company.The raw run of mine sample was collected over a
4 hour period on December 13, 1973. Approximately 30 increments
totaling 908 kg (2000 Ibs) were taken at the primary cut of an
automatic sampler.
104
-------
ERIE
CRAWFORD'
WARREN
O
cn
MERCER
FOREST
MC KEAN
POTTER
ELK
CAMERON
VENANGQ
CLINTON
LAWRENCE
BEAVER
'
BUTLER
CLARION
JEFFERSON
ARMSTRONG
CLEARFIELD
CENTRE
INDIANA
ALLESHENY
CAMBRIA / BLAIR
HUNTINGDON
WESTMORELAND
ARV/ICK
WASrilN
SOMERSET
FAVETTE
BEDFORD
FULTON / FRANKLIN
TIOGA
BRADFORD
SUSQUEHANNA
WAYNE
SULLIVAN
LYCOMING
WYOMING
LUZERNE
LACKAWANNA
PIKE
COLUMBIA
UNION
CARBON
MONROE
NORTHAMPTON
5CHUYLKILL
LEHIGH
PERRY
CUMBERLAND
ADAMS
DAUPHIN
BERKS
LEBANON
BUCKS
LANCASTER
CHESTER
MONTGOMERY
DELAWARE
YORK
PENNSYLVANIA
SEWICKLEYSEAM
FIGURE A-4
-------
I 1
en
WESTVIRGINIA
SEWICKLEY SEAM
FIGURE A-5
-------
OHIO
SEWICKLEYSEAM
FIGURE A-6
107
-------
ORIGINAL
PROGRAM
SAMPLE
PENNSYLVANIA
PITTSBURGH SEAM
FIGURE A-7
-------
WEST VIRGINIA
PITTSBURGH SEAM
FIGURE A-8
-------
OHIO
PIHSBURGH SEAM
FIGURE A-9
110
-------
PENNSYLVANIA
UPPER FREEPORT (NO 7))SEAM
FIGURE A-10
-------
! •
WEST VIRGINIA
UPPER FREE PORT (NO 7) SEAM
FIGURE A-ll
-------
HOLMES
/ JEFFERSON
OHIO
UPPER FREEPORT (NO 7) SEMI
FIGURE A-12
113
-------
MC KEAN
POTTER
c.M-11 I'lill
TIOGA
BRADFORD
SUSQUEHANNA
WYOMING
SULLIVAN / /LACKAWANNA
LYCOMING
CLINTON
WAYNE
PIKE
LUZERNE
11 i M'\ inn
i I till'
UNION
SNYDER
INDIANA
O
0 _
4
*
COLUMBIA
CARBON
MONROE
NORTHAMPTON .
SCHUYLKILL
LEHI6H
MIFFLIN
JUNIATA
CAMBRIA / BLAH
RELAND
HUNTINGDON
WASH I';
BEDFORD
m FRANKLIN
PERRY
CUMBERLAND
ADAMS
DAUPHIN
BERKS
LEBANON
BUCKS
LANCASTER
MONTGOMERY
CHESTER y "I •*•'
DELAWARE
YORK
PENNSYLVANIA
LOWER FREEPORT (NO 6A) SEAM
FIGURE A-13
-------
' I
WEST VIRGINIA
LOWER FREEPORT (NO 6A) SEAM
FIGURE A-14
-------
•\J
OHIO
LOWER FREEPORT (NO 6A) SEAM
FIGURE A-15
116
-------
PENNSYLVANIA
UPPER KITTANNING SEAM
FIGURE A-16
-------
WEST VIRGINIA
UPPER KITTANNING SEAM
FIGURE A-17
-------
HOLMES
OHIO
UPPER KITTANNING SEAM
FIGURE A-18
119
-------
PENNSYLVANIA
MIDDLE KITTANNING (NO 6) SEAM
FIGURE A-19
-------
WEST VIRGINIA
MIDDLE KITTANNING (NO 6) SEAM
FIGURE A-20
-------
OHIO
MIDDLE KITTANNING (N061SEAM
FIGURE A-21
122
-------
PENNSYLVANIA
LOWER KITTANNING SEAM
FIGURE A-22
-------
I '
! •
WEST VIRGINIA
LOWER KITTANNINGSEAM
FIGURE A-23
-------
OHIO
LOWER KIHANNING SEAM
FIGURE A-24
125
-------
OHIO
CLARION 4A SEAM
FIGURE A-25
126
-------
i '
1
EASTERN KENTUCKY
MASON SEAM
FIGURE A-26
-------
ILLINOIS
5RISBURG - SI
128
-------
INDIANA
SPRINGFIELD - NO.I SEAM
FIGURE A-28
129
-------
WESTERN KENTUCKY
NO. 9 SEAM
FIGURE A-29
-------
ILLINOIS
131
-------
, o
I I
WESTERN KENTUCKY
NO. 11 SEAM
FIGURE A-31
-------
INDIANA
HYMERA - NO.ST SEAM
FIGURE NO. A-32
133
-------
APPENDIX B
RANKING OF TREATED AND UNTREATED COALS
NOTE: The values used for the calculations
in this appendix are the average of
the triplicate determinations detailed
in Appendices C and D.
The EPA standard % sulfur will yield
1.2 Ibs S02/106 btu.
134
-------
Table B-l
COAL RANKING DATA-UNTREATED COAL
FINAL TWENTY COALS
Mine
Muskinaum
Powhattan No. 4
Isabella
Mathies
Williams
Robinson Run
Shoemaker
Delmont
Marion
Lucas
Bird No. 3
Martinka
Meigs
Dean
Kopperston
Harris Nos. 1&2
North River
Homestead
Ken
Star
Seam
Meigs Creek
No. 9
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Middle
Kittanning
Lower
Kittanning
Lower
Kittanning
Clarion 4A
Dean
Campbell Creek
Eagle & No. 2
Gas
Corona
No. 11
No. 9
No. 9
Moisture
%
3.36
2.10
1.57
2.15
1.28
0.96
1.51
0.77
1.84
3.88
0.84
1 .84
4.77
1.06
1.38
1.72
1.57
5.41
4.76
6.13
Sulfur
%
6.08
4.12
1.57
1.46
3.48
4.38
3.51
4.89
1.37
1.79
3.14
1.96
3.73
4.09
0.91
1.00
2.06
4.46
4.83
4.32
Ash
%
21.68
37.17
42.22
41.01
13.18
13.36
33.48
27.18
26.40
8.68
30.23
49.64
26.53
17.28
30.15
18.63
49.25
16.56
15.08
13.90
BTU
Moist
10644
8422
8087
7979
12846
12838
9352
10927
10843
12929
10461
7413
9757
11979
10806
12200
7572
11289
11523
11554
Dry
11014
8603
8216
8154
13013
12962
9495
11012
11046
13451
10550
7552
10246
12107
10957
12414
7693
11935
12099
12308
Moist
Mineral
Matter
Free
14118
14267
14958
14399
15113
15173
14821
15720
15232
14323
15702
16144
13811
14887
16075
15316
16352
13892
13918
13724
Dry
Mineral
Matter
Free
14608
14573
15197
14715
15309
15321
15049
15842
15517
14902
1 5835
16447
14503
15047
16300
15585
16613
14686
14614
14620
Fixed
Dry
41.96
33.82
33.09
34.46
48.18
47.76
35.39
44.49
49.15
56.02
53.59
28.76
38.55
45.81
45.96
54.51
27.56
50.30
49.66
52.16
Carbon
Dry
Mineral
Matter
Free
56.04
57.65
61.37
62.36
56.84
56.64
56.31
64.39
69.19
62.19
80.94
62.82
54.82
57.15
68.46
68.52
59.66
62.30
60.37
62.35
Volatile Matter
Dry
36.36
29.01
24.69
24.53
38.64
38.88
31.13
28.33
24.45
35.30
16.18
21.60
34.92
36.91
23.89
26.86
23.19
33.14
35.26
33.94
Dry
Mineral
Matter
Free
43.96
42.35
38.63
37. 6*
43.16
43-. 36
43.69
35.61
30.81
37.81
19.06
37.18
45.18
42.85
31.54
31.48
40.34
37.70
39.63
37.65
EPA
Standard
% Sulfur
0.66
0.52
0.49
0.49
0.78
0.78
0.57
0.66
0.66
0.81
0.63
0.45
0.61
0.73
0.66
0.74
0.46
0.72
0.73
0.74
Class
II-3
II-3
II-3
II-3
II-3
II-3
II-3
II-3
II-2
II-3
II-l
II-3
II-4
II-3
II-3
II-3
II-3
II-4
II-4
II-4
GO
en
Class: H-1, Bituminous - Low Volatile (Ivb)
II-2, Bituminous - Medium Volatile (mvb)
II-3, Bituminous - High Volatile A (hvAb)
II-4, Bituminous - High Volatile B (hvBb)
-------
Table B-2
COAL RANKING DATA - UNTREATED COAL
INITIAL FIFTEEN COALS
Mine
Edna
Navajo
Belle Ayr
Colstrip
Me 1 don
Eagle No. 2
Orient No. 6
Camp Nos. 1 & 2
Walker
Egypt Valley
No. 21
No. 1
Jane Nos. 1 & 2
Fox
Warwick
Humphrey No. 7
Seam
Wadge
Nos. 6, 7, 8
Roland-Smith
Rosebud
Des Moines No. 1
Illinois No. 5
Herri n No. 6
Seam No. 9
Upper
Kittanning
Pittsburgh No. 8
Mason
Lower Freeport
Lower
Kittanning
Sewickley
Pittsburgh No. 8
Moisture
8.41
11.07
19.14
20.41
13.29
3.31
3.51
3.99
2.07
2.07
2.22
1.17
1.83
1.50
1.63
Sulfur
0.75
0.81
0.76
1.01
6.39
4.29
1.66
4.51
0.71
6.55
3.12
1.85
3.83
1.37
2.58
Ash
*
9.13
25.29
7.55
10.38
15.74
26.53
22.51
21.13
16.67
25.29
11.39
21.75
13.55
40.47
9.88
Bl 1
Moist
11216
8937
9731
9225
10197
10216
10771
10662
12341
10375
12764
11792
12736
8483
13409
Dry
12246
10050
12034
11591
11760
10566
11163
11105
12602
10594
13054
11932
12973
8612
13631
Mineral
Matter
Free
12458
12316
10601
10398
12427
14498
14294
13971
15079
14543
14664
15498
15066
15150
15106
Dry "
Mineral
Matter
Free
13602
13849
13111
13065
14331
14994
14814
14552
15398
14851
14997
15682
15347
15381
15356
Dry
50.22
39.20
45.34
46.53
43.64
39.17
45.82
43.01
64.44
38.59
49.70
48.18
48.12
31.76
52.46
Dry
Minera
Matter
Free
55.84
54.09
49.47
52.56
53.70
55.85
60.94
56.67
78.83
54.44
57.26
63.45
57.11
56.82
59.23
Class: II-l, Bituminous - Low Volatile III-l, Subbi luminous A
II-2, Bituminous - Medium Volatile III-2, Subbltuminous B
II-3, Bituminous - High Volatile A
II-4, Bituminous - High Volatile B
II-5, Bituminous - High Volatile C
Dry
40.65
35.51
47.11
43.09
40.62
34.30
31.67
35.86
18.89
36.12
38.91
30.07
38.33
27.77
37.66
Dry "
Mineral
Matter
Free
44.16
45.91
50.53
47.44
46.30
44.15
39.06
43.33
21.17
45.56
42.74
36.55
42.89
43.18
40.77
EPA
Standard
% Sulfur
0.73
0.60
0.72
0.70
0.71
0.63
0.67
0.67
0.76
0.64
0.78
0.72
0.78
0.52
0.82
Class
II-5
II-5
II-5/
III-2
II-5
II-3
II-3
II-4
II-l
II-3
II-3
II-3
II-3
II-3
II-3
CO
cr>
-------
Table B-3
COAL RANKING DATA - PYRITIC SULFUR EXTRACTIONS
FINAL TWENTY COALS
Mine
Muskingum
Powhattan No. 4
Isabella
Mathies
Williams
Robinson Run
Shoemaker
Delmont
Marion
Lucas
Bird No. 3
Martinka
Meigs
Dean
Kopperston
Harris Nos. 1&2
North River
Homestead
Ken
Star
Seam
Meiqs Creek
No. '9
Pittsburgh No. 8
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Pittsburgh
Upper Freeport
Upper Freeport
Middle
Kittanning
Lower
Kittanning
Lower
Ki ttanninq
Clarion 4A
Dean
Campbell Creek
Eagle & No. 2
Gas
Corona
No. 11
No. 9
No. 9
Moisture
%
3.36
2.10
1.57
2.15
1.28
0.96
1.51
0.77
1.84
3.88
0.84
1 .84
4.77
1.06
1.38
1.72
1.57
5.41
4.76
6.13
Sulfur
%
3.22
2.04
0.72
0.94
1.74
2.20
1.87
0.96
0.68
0.89
0.80
0.58
1.94
2.08
0.61
0.77
0.93
2.38
2.78
2.46
Ash
%
16.05
32.12
35.72
36.43
9.16
7.63
28.87
20.44
22.61
6.32
24.17
43.46
20.38
13.66
25.53
16.46
42.84
11.50
9.44
8.58
BTU
Moist
11189
9281
9166
8830
13413
13632
10003
12015
11504
13345
11403
7988
10535
12529
11184
12340
8192
11602
12085
11875
Dry
11578
9480
9312
9024
13587
13764
10156
12108
11720
13884
11500
8138
11063
12663
11340
12556
8323
12266
12689
12650
Moist
Mineral
Matter
Free
13632
14300
14960
14605
14948
14933
14617
15462
15252
14351
15470
15090
13570
14773
15470
15039
15306
13311
13533
13148
Dry
Mineral
Matter
Free
14106
14607
15199
14925
15142
15078
14841
15582
15538
14930
15601
15373
14250
14932
15687
15302
15550
14072
14209
14006
Fixed Carbon
Dry
47.00
38.60
40.27
38.06
52.06
57.16
41.33
49.75
52.08
58.53
58.26
34.41
44.35
52.08
46.78
52.76
33.42
52.58
54.26
56.43
Dry
Minera'
Matter
Free
57.50
59.66
65.81
63.05
58.10
62.76
60.55
64.09
69.11
63.01
79.15
65.07
57.28
61.55
64.76
64.36
62.53
60.53
60.99
62.72
Volatile Matter
Dry
36.95
29.28
24.01
25.51
38.78
35.21
29.80
29.81
25.31
35.15
17.57
22.13
35.27
34.26
27.69
30.78
23.74
35.92
36.30
34.99
Dry
Minera
Matter
Free
42.50
40.34
34.19
36^95
41.90
37.24
39.45
35.91
30.89
36.99
20.85
34.93
42.72
38.45
35.24
35.64
37.47
39.47
39.01
37.28
EPA
Standard
% Sulfur
0.69
0.57
0.56
0.54
0.82
0.83
0.61
0.73
0.70
0.83
0.69
0.49
0.66
0.76
0.68
0.75
0.50
0.74
0.76
0.76
Class
II-4
II-3
II-3
II-3
II-3
II-3
II-3
II-3
11-2
II-3
II-l
II-3
II-4
II-3
II-3
II-3
II-3
II-4
II-4
II-4
CO
Class:
II-l, Bituminous
II-2, Bituminous
11-3, Bituminous
II-4, Bituminous
Low Volatile
Medium Volatile
High Volatile A
Hiqh Volatile B
-------
Table B-4
COAL RANKING DATA - PYRITIC SULFUR EXTRACTIONS
INITIAL FIFTEEN COALS
Mine
Edna
Navajo
Belle Ayr
Colstrip
Wei don
Eagle No. 2
Orient No. 6
Camp Nos. 1 and 2
Egypt Valley
No. 21
No. 1
Jane Nos. 1 and 2
Fox
Warwick
Humphrey No. 7
Seam
Wadge
Nos. 6,7,8
Roland-
Smith
Rosebud
Des Moines
No. 1
111 inois
No. 5
Herrin
No. 6
Seam No. 9
Pittsburgh
No. 8
Mason
Lower
Free port
Lower Kit-
tanning
Sewickley
Pittsburgh
No. 8
Moisture
%
8.41
11.07
19.14
20.41
13.29
3.31
3.51
3.99
2.07
2.22
1.17
1.83
1.50
1.63
Sulfur
%
1.14
0.76
0.82
0.69
2,34
2.12
1.40
2.77
2.09
1,62
0.67
1.64
0.82
1.49
Ash
6.77
20.53
3.37
5.17
5.43
19.80
18.85
15.77
18.86
8.50
17.99
9.72
35.32
6.97
Moist
11175
8924
9315
9010
10833
11024
10G47
11272
11268
13045
12272
12933
9225
13722
Dry
12201
10035
11520
11321
12493
11401
11034
11740
11506
13341
12417
13174
9365
13949
BTU
Moist
Mineral
Matter
Free
12077
11479
9670
9545
11677
14096
13410
13669
14253
14416
15259
14504
14956
14890
Dry
Mineral
Matter
Free
13186
12908
11958
11993
13467
14579
13898
14238
14554
14743
15440
14775
15184
15137
Fixed Carbon
Dry
50.88
43.65
49.61
52.38
54.96
45.70
49.23
47.78
43.06
53.87
51.65
51.97
38.07
55.99
Dry
Mineral
Matter
Free
55.08
56.24
51.60
55.59
59.51
58.60
62.15
58.16
54.62
59.63
64.27
58.38
61.80
60.85
Volatile Matter
Dry
42.35
35.82
47.02
42.45
38.61
34.50
31.92
36.45
38.08
37.63
30.36
33.31
26.61
37.04
Dry
Mineral
Matter
Free
44.92
43.76
48.40
44.41
40.49
41.40
37.85
41.84
45.38
40.37
35.73
41.62
38.20
39.15
EPA
Standard
y. Sulfur
0.73
0.60
0.69
0.68
0.75
0.68
0.66
0.70
0.69
0.80
0.75
0.79
0.56
0.84
Class
II-5
II-5/
III-l
III-2
III-2
II-5
II-3
II-4
II-4
II-3
II-3
II-3
II-3
II-3
II-3
Class:
II-l , Bituminous-Low Volatile (Ivb)
II-2, Bituminous-Medium Volatile (mvb)
II-3, Bituminous-High Volatile A (hvAb)
II-4, Bituminous-High Volatile B (hvBb)
I II-l , Subbituminous A
CO
oo
III-2, Subbituminous B
-------
Table B-5
COMPUTER PROGRAM FOR DETERMINING
THE RANK OF COAL
PROGRAM RANK
-------
7 FORMAT (*EFA STANDARD-% SULFUF.=** F4. 2* *%* )
55 PRINT 5
5 FORMAT <*RANK=*>
RANK SORTING
IF (DRYFC-98.) 11*10*10
11 IF (BRYFC-92.) 12*20*20
12 IF CDBYFC-86. ) 13*30,30
13 IF (DRYKO78.) 14*40*40
14 IF (DBYFC-69.) 15*50*50
15 IF (WETBTU-I4000-) 16*60*60
16 IF (WETBTU-13000.> 17*70*70
17 IF (WETBTU-11500.) 18*80*80
18 IF (WETBTU-10500. > 19*90*90
19 IF
-------
110
120
130
1111
21
31
41
51
61
71
81
91
101
111
121
131
1000
700
68
PRINT
WRITE
GO TO
PRINT
WRITE
GO TO
111
( 6, 1 11 )
1000
121
(6, 121)
1000
PRINT 131
WRITE <6* 131)
FORMAT
FORMAT
FORMAT
FORMAT
FORMAT
FORMAT
FORMAT
FORMAT
FORMAT
C*CLASS
(*CLASS
<*CLASS
(*CLASS
C*CLASS
(*CLASS
(*CLASS
C+CLASS
(*CLASS
1-1* META-ANTHRACITE*)
1-2* ANTHRACITE*)
1-3* SEMI ANTHRACITE*)
II-l* BITUMINOUS-LOW VOLATILE*)
11-2* BITUMINOUS-MEDIUM VOLATILE*)
11-3* BITUMINOUS-HIGH VOLATILE A*)
11-4, BITUMINOUS-HIGH VOLATILE B*)
11-5* BITUMINOUS-HIGH VOLATILE C* )
II-5* BITUMINOUS-HIGH VOLATILE C* *
1*AGGLOMERATING*/*CLASS 111-1*SUBBITUMINOUS A*NONAGGLOMERATING*)
FORMAT (*CLASS III-2* SUBBITUMINOUS B*)
111-3* SUBBITUMINOUS C*)
IV-1* LIGNITE A*)
IV-2* LIGNITE B*)
69
FORMAT (*CLASS
FORMAT <*CLASS
FORMAT <* CLASS
PRINT 700
FORMAT
-------
APPENDIX C
UNTREATED COAL ANALYSES DATA
142
-------
Table C-l
UNTREATED COAL ANALYSES
MUSKINGUM, POWHATTAN NO. 4, ISABELLA AND MATHIES MINES
Mine, Seam, and
Location
Muskingum Mine
Meigs Creek No. 9
Morgan County
Ohio
Powhattan No. 4
Pittsburgh No. 8
Monroe County
East Ohio
Isabel la Mine
Pittsburgh Seam
Fayette County
Pennsy Ivan ia
Mathies Mine
Pittsburgh Seam
Washington County
Pennsy Ivan i a
C antnl a
Oaulp 1 6
A
B
C
Average
Std. Dev,
A
B
C
Average
Std. Dev.
A
B
C
Average
Std. Dev.
A
B
C
Average
Std. Dev
As Received
Basis
Moisture
% w/w
3.32
3.40
3.35
3.36
±.040
2.16
1.85
2.29
2.10
±.225
1.66
1.56
1.50
1.57
+ .081
2.31
2.18
2.15
2.15
+ .025
Dry Forms of Sulfur, % w/w
Total
5.96
6.10
6.18
6.08
±0.111
4.08
4.08
4.21
4.12
±.075
1.54
1.58
1.58
1.57
+ .023
1.45
1.44
1.48
1.46
±.021
Pyritic
3.64
3.66
3.65
3.65
±0.010
2.51
2.57
2.63
2.57
+.060
1.14
1.06
1.00
1.07
±.070
0.98
1.05
1.11
1.05
±.065
Sulfate
0.08
0.05
0.04
0.06
±.021
0.18
0.21
0.19
0. 19
±.015
0.04
0.04
0.04
0.04
+ .00
0.04
0.04
0.04
0.04
±.00
Organic
2.24
2.39
2.4?
2.37
t.113
1.39
1.30
1.39
1.36
±.097
0.36
0.48
0.54
0.46
+ .074
0.43
0.35
0.33
0.37
±.068
Dry Proximate Analysis, % w/w
Ash
21.58
21.75
21 .72
21.68
±.091
37.07
37.67
36.77
37.17
±.458
42.37
42.18
42.12
42.22
+ .131
41.03
4i.03
40.96
41.01
±.040
Volatiles
•' 37.49
35.97
35.63
36.36
±.990
28.66
29.03
29.35
29.01
±.345
24.71
24.62
24.74
24.69
+ .062
24.41
24.43
24.75
24.53
±.191
Fixed
Carbon
' 40.93
42.28
42.65
41.96
±.994
34.27
33.30
33.88
33.82
±.573
32.92
33.20
33.14
33.09
+ .145
34.56
34.54
34.29
34.46
+ .150
Heat
Content
btu
11030
10981
11033
11014
±29.2
8522
8520
8769
8603
±143.2
8223
8197
8227
8216
±16.2
8289
8028
8146
8154
±130.6
oo
-------
Table C-2
UNTREATED COAL ANALYSES
WILLIAMS, ROBINSON RUN, SHOEMAKER AND DELMONT MINES
Mine, Seam, and
Location
Wi 1 1 iams Mine
Pittsburgh Seam
Marion County
West V i rgin ia
Robi nson Run Mine
Pittsburgh Seam
Harrison County
West V i rgini a
Shoemaker Mine
Pittsburgh Seam
Marshal 1 County
West Vi rginia
Delmont Mine
Upper Freeport
Westmoreland County
Pennsy 1 vania
Sample
A
8
c
Average
Std. Dev.
A
B
C
Average
Std. Dev.
A
B
C
Average
Std. Dev.
A
B
C
Average
Std. Dev.
As Received
Basis
Moisture
% w/w
1.33
1.25
1.25
1.28
±.046
0.93
0.94
1 .00
0.96
±.038
1.49
1.54
1.50
1.51
±.025
0.81
0.77
0.7*4
0.77
±.035
Dry Forms of Sulfur, % w/w
Total
3.49
3.48
3.47
3.48
±.010
4.36
4.42
4.37
4.38
±.032
3.51
3.52
3.50
3.51
±.010
it. 86
4.91
4.90
4.89
±.025
Pyritic
2.18
2.21
2.30
2.23
±.062
2.88
2.70
3.08
2.89
±.190
2.09
2.29
2.20
2.19
±.100
4.61
4.53
4.54
4.56
±.044
Sulfate
0.04
0.05
0.04
0.04
±.006
0.06
0.06
0.06
0.06
±.00
0.05
0.05
0.05
0.05
±.00
0.08
0.08
0.08
0.08
±.00
Organic
1.27
1.22
1.13
1.21
'.063
1.42
1.66
1.23
1.43
±.193
1.37
1.18
1.25
1.27
±. 100
0.17
0.30
0.28
0.25
±.051
Dry Proximate Analysis, % w/w
Ash
13.19
13.11
13.25
13.18
±.070
13.43
13.20
13.45
13.36
±.139
33.61
33.48
33.36
33.48
±.125
27.40
26.92
27.22
27.18
±.242
Volatiles
38.50
38.47
38.94
38.64
+ .263
39.01
39.15
38.49
38.88
±.348
30.94
31.10
31.35
31.13
+ .207
28.45
28.08
28.47
28.33
+ .220
Fixed
Carbon
48.31
48.42
47.81
48.18
±.272
47.56
47.65
48.06
47.76
±.375
35.45
35.42
35.29
35.39
±.242
44.15
45.00
44.31
44.49
±.327
Heat
Content
btu
12947
13069
13025
13013
±61.6
12912
13022
12951
12962
+ 56.8
9512
9486
9488
9495
±14.5
11044
10981
1101 1
11012
±31.5
-------
Table C-3
UNTREATED COAL ANALYSES
MARION, LUCAS, BIRD NO. 3, AND MARTINKA MINES
Mine, Seam, and
Location
Marion Mine
Upper Freeport Seam
Indiana County
Pennsylvania
Lucas Mine
Middle Ki ttanning
Columbiana County
Ohio
Bi rd No. 3 Mine
Lower Ki ttanni ng
Sommerset County
Pennsy 1 van ia
Martinka Mine
Lower Kittanning
Logan or Mingo
West Vi rginia
Sample
A
D
c
Average
Std. Dev.
A
B
C
Average
Std. Dev.
A
B
C
Average
Std. Dev.
A
B
C
Average
Std. Dev.
As Received
Basis
Moisture
% w/w
1.71
1.69
2.13
1.84
±.248
3.89
3.88
3.86
3.88
±.015
0.88
0.82
0.83
0.84
±.032
1.50
2.30
1.70
1.84
±.428
Dry Forms of Sulfur, % w/w
Total
1.37
1.34
1.39
1.37
±.025
1.93
1.73
1.71
1.79
±. 122
3.09
3.19
3.15
3.14
±.050
1.93
1.96
1 .98
1.96
±.025
Pyritic
0.92
0.89
0.8g
0.90
±.017
1.51
1.35
1 .40
1.42
±.082
2.82
2.94
2.85
2.87
±.062
1.59
1.62
1.63
1.61
±.021
Sulfate
0.00
0.03
0.03
0.02
±.017
0.05
0.05
0.05
0.05
±.00
0.05
0.05
0.05
0.05
±.00
0.10
0.09
0.09
0.09
±.006
Organic
0.45
0.42
0.47
0.45
±.035
0.37
0.33
0.26
0.32
±.147
0.22
0.20
0.25
0.22
±.080
0.24
0.25
0.26
0.26
±.033
Dry Proximate Analysis, % w/w
Ash
26.46
26.44
26.31
26.40
+ .081
fi.66
8.78
8.61
8.68
±.087
30.12
30.58
29.99
30.23
±.310
49.60
49.65
49.68
49.64
+ .040
Volatiles
"24.70
24.59
24.06
24.45
±.342
35.48
35.30
35.12
35.30
±. 180
16.19
16.09
16.25
16.18
+ .081
21.94
21.66
21.54
21.60
±.085
Fixed
Carbon
48.84
48.97
49.63
49.15
±.423
55.86
55.92
56.27
56.02
+ .221
53.69
53.33
53.76
53.59
+ .320
28.46
28.69
28,78
28.76
+ .094
Heat
Content
btu
1 1076
11039
1 1024
1 1046
+ 26.8
13520
13443
13390
13451
+65.4
10554
10495
10600
10550
±52.6
7548
7550
7559
7552
+5.9
en
-------
Table C-4
UNTREATED COAL ANALYSES
MEIGS, DEAN, KOPPERSTON NO. 2, AND HARRIS NOS. 1 & 2 MINES
Mine, Seam, and
Location
Mei gs M i ne
Clarion 4A Seam
Meigs County
Ohio
Dean Mine
Dean Seam
Scott County
Tennessee
Kopperston Mine
Campbell Creek Sea
Wyoming County
West Virginia
Harris Nos. 1 & 2
Mines
Eagle and No. 2 Gas
Seams
Boone County ,
West Virginia
Sample
A
B
C
Average
Std. Dev.
A
B
C
Average
Std. Dev.
A
B
C
Average
. Std. Dev.
A
B
C
Average
As Received
Basis
Moisture
% w/w
it. 77
4.79
4.74
4. 77
±.025
1.13
1.08
.96
1.06
..087
1.40
1.40
1.34
1.38 •
-.035
1.74
1.72
1.71
1.72
±.015
Dry Forms of Sulfur, % w/w
Total
3.69
3.73
3.76
3.73
±.035
4.11
4.10
4.06
4.09
±.026
0.95
0.86
0.93
0.91
'.047
1.01
1.00
1.00
1.00
±.006
Pyritic
2.22
2. 19
2.16
2.19
±.030
2.64
2.69
2.52
2.62
' .087
0.49
0.44
0.48
0.47
±.026
0.52
0.45
0.50
0.49
±.036
Sulfate
0.06
0.06
0.05
0.06
±.006
0.15
0.15
0.15
0.15
±0.00
0.04
0.04
0.02
0.03
'.012
0.03
0.03
0.03
0.03
±.00
Organic
i .41
1.48
1.55
1.48
±.046
1.32
1.26
1.39
1.32
'.091
0.42
0.38
0.43
0.41
-.055
0.46
0.52
0.47
0.48
±.036
Dry Proximate Analysis, % w/w
Ash
26.49
26.39
26.71
26.53
±.164
17.42
1 6 . 9.7
17.46
17.28
•0.272
30.10
30.15
30.20
30.15
'0.050
18.62
18.69
18.58
18.63
±0.056
Volatiles
35.46
34.61
34.70
34.92
±.467
39.09
3e.5?
35.13
36.91
-2.01
23.99
23.69
23.99
23.89
^0.173
26.76
26.71
27.12
26.86
±0.224
Fixed
Carbon
38.05
39.00
38.59
38.55
±.495
45.49
46.51
47.41
45.81
-2.03
45.91
46.16
45.81
45.96
±0.180
54.62
54.60
54.30
54.51
±0.231
Heat
Content
htu/lb
10240
10255
10243
10246
±7.9
12153
12088
12080
12107
•40.0
10941
10986
10945
10957
•24.9
1237
12434
12439
12414
±38.5
-------
Table C-5
UNTREATED COAL ANALYSES
NORTH RIVER, HOMESTEAD, KEN AND STAR MINES
Mine, Seam, and
Location
:iortn River Mine
Corona Seam
Jefferson County
Alabama
Homestead Mine
:io. 11 Seam
On'o County
west Kentucky
Ken Mine
No. 9 Seam
Ohic County
West Kentucky
Star Mine
No. 9 Seam
'.iopkins County
Vest Kentucky
Sample
n
C
Average
Std. Dev.
A
L
r
^-
Average
Std. Dev.
A
•i
r
"verage
Std. ::ev.
r.
F
C
Average
Std. Jev.
As Received
Basis
Moisture
% w/w
1.51
1 .57
1.54
l.:7
i . 035
5.47
5.39
5.38
5.41
:.C49
4.77
4.79
4.71
4.76
+ .042
6.16
6.14
6.00
6.13
±.038
Dry Forms of Sulfur, % w/w
Total
2.r:7
2.06
2.C4
2 . Of.
t .Olb
4.47
4.45
4.46
4.46
+ .010
4.^6
4.79
.'..84
4.83
-.336
4.30
4.32
4.35
4.32
±.025
Pyritic
1.42
1.44
1.40
1.42
± .020
3.12
3.17
3.05
3.11
t.049
2.83
2.83
2.89
2.85
* .038
2.50
2.60
2.70
2.60
±.100
Sulfate
0/7
' . 07
O.T7
0.07
i . "'O
0.10
O.io
0.11
0.11
* ,00f
. 0.26
0.25
0.2*
0.26
•.oor
0.27
0.22
0.22
0.24
±.029
Organic
o.58
0.55
O.F7
0.57
+ .°25
1.2^
1,21
1.30
1.25
T.n31
1.72
1.72
1.69
1.72
±.053
1.58
' 1.50
1.43
1.50
±.075
Dry Proximate Analysis, % w/w
Ash
19.21
4^ . ?5
A° . 30
4^.25
:' .04E
16.54
16.56
16.57
16.56
+ .150
15.06
15.03
15.14
15. OR
±.057
13.89
1 3 . 84
13.98
13.90
±.071
Volatiles
23.26
23. IS
23. T;
23.1"
+ .058
32.77
33.80
32.85
33.14
+ .573
34.30
35 . 63
35.85
35.26
+ .839
35.14
33.56
33.12
33.94
±1.062
Fixed
Carbon
27.53
' 27.5°
27.5° .
27.56
±.073
50.69
49.64
50.58
50.30
+ .592
50.64
49.34
49.01
49.66
±.841
56.97
52,60
52,90
52.16
±1.064
Heat
Content
btu/lb
771 r
7692
1-1J,
7?93
±21.
11966
11962
11878
11935
±49.7
12127
12063
12107
12099
±32.7
12275
12309
12340
12308
±35.5
-------
APPENDIX D
PYRITIC SULFUR REMOVAL DATA
NOTE: The complete general procedure used
to treat the coals is contained in
Section 4.3 of this report. Variables
such as mesh, reaction time, and leach
numbers and times are listed in the
tables. Numbers in parentheses are
not considered valid for various
reasons but are included for
completeness. Averages are included
only where appropriate.
148
-------
Table D-l
PYRITIC SULFUR REMOVAL DATA
MUSKINGUM, POWHATTAN NO. 4, ISABELLA AND MATHIES MINES
line, Seam,
and Location
Muskingum Mine
Melgs Creek No. 9
Morgan County
Ohio
Powhattan No. 4
Pittsburgh No. 8
Monroe County
East Ohio
Isabella Mine
Pittsburgh Seam
Fayette County
Pennsylvania
Mathies Mine
Pittsburgh Seam
Washington County
Pennsylvania
Mesh
150
150
100
100
200
100
100
150
150
Total
Rxn.
Time
23
23
23
23
23
23
23
23
23
Leach Changes
Number Time (hrs)
1 5.0
1 5.0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 9.0
1 9.0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 4.5
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
Run
Number
1
2
1-2
A-C
1
2
1-2
A-C
3
1
2
1-2
A-C
1
2
1-2
A-C
Total
Sulfur
3.24
3.20
3.22
+ .028
6.08
± . 1 1 1
2.04
2.03
2.04
1.007
4.12
±.075
1 .94
0.71
0.72
0.72
±.007
1.57
±.023
0.95
0.92
0.94
±.021
1.46
±.021
)ry Forms of Sulfur. % w/w
Pyritic
0.24
0.27
0.20
0.26
0.24
±.031
3.65
±.010
n.41
0.39
0.50
0.47
0.44
±.051
2.57
±.060
0.04
0.05
0.07
0.06
0.07
0.06
±.010
1.07
±.070
0.08
0.02
0.08
0,02
0.05
±.035
1.05
±.065
Sulfate
0.18
0.16
0.17
±.014
0.06
±.021
0.11
0.13
0.12
±.014
0.19
±.015
0.10
0.00
0.01
0.01
±.007
0.04
±0.00
0.10
0.10
0.10
±.00
0.04
±.00
Organic
2.80
2.81
2.81
±044
2.37
±.113
1.53
1.42
1.48
±.053
1.36
±.097
1.80
0.51
0.41
0.65
±.014
0.46
±.074
0.80
0.87
0.79
±.041
0.37
±.068
Dry Proximate Analysis, % w/w
Ash
16.11
15.99
16.05
•±.085
21.68
±.990
31.76
32.48
32.13
±.509
37.17
±.458
35.61
35.83
35.72
±.156
42.22
±.131
36.16
36.70
36.43
±.382
41.01
±.040
Volatile
Matter
36.96
36.94
36.95
+ .014
36.36
±.990
29.26
29.29
29.28
±.021
29.01
±.345
24.35
23.67
24.01
±.481
24.69
±.062
26.11
24.91
25.51
±.849
24.53
±.191
Fixed
Carbon
46.93
47.07
47.00
±.086
41.96
±.994
38.98
38.23
38.60
±.509
33.82
±.573
40.04
40.50
40.27
±.506
33.09
±.145
37.73
38.39
38.06
±.931
34.66
±.150
btu/lb
11546
11611
11578
±46.0
11014
±29.2
9529
9431
9480
±69.3
8603
±143.2
9321
9302
9312
±13.4
8216
±130.6
9071
8978
9024
±65.8
8154
±130.6
-------
01
o
Table D-2
PYRITIC SULFUR REMOVAL DATA
WILLIAMS, ROBINSON RUN, SHOEMAKER AND DELMONT MINES
Mine, Seam,
and Location
Williams Mine
Pittsburgh Seam
Marlon County
West Virginia
Robinson Run Mine
Pittsburgh Seam
Harrison County
West Virginia
Shoemaker Mine
Pittsburgh Seam
Marshall County
West Virginia
Delmont Mine
Upper Freeport
Westmoreland County
Pennsylvania
Mesh
100
100
150
150
150
100
100
150
200
200
Total
Rxn.
Time
23
23
23
23.5
23.5
23
23
23
23
23
Leach Changes
Number Time (hrs)
1 10
1 10
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 6
1 6
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 7
1 7
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 4.5
1 6
1 6
Treated Average
Std. Dev.
Initial Average
Std. Dev.
Run
Number
1
2
1-2
A-C
3
1
1
1-2
A-C
1
2
1-2
A-C
3
1
2
1-2
A-C
Dry Forms of Sulfur, % w/w
Sulfu
1.76
1.72
1.74
±.028
3.48
+ .010
1.80
2.20
2.19
2.20
+ .007
4.38
±.032
1.78
1.96
1.87
+ .127
3.51
+ .010
1.73
0.90
1.02
0.96
-.085
4.89
+ .025
Pyrltlc
0.25
0.32
0.32
0.27
0.29
+ .036
2.23
+ .062
0.10
0.09
0.09
0.07
0.07
0.08
±.012
2.89
±.190
0.34
0.38
0.55
0.55
0.46
+ .111
2.19
±.100
0.08
0.16
n. 11
0.27
0.30
0.21
+ .090
4.56
+ .044
Sulfate
0.06
0.06
0.06
+ .00
0.04
+.006 .
0.09
0.00
0.00
0.00
+ .00
0.06
+ .00
0.07
0.08
0.08
±.007
0.05
±.00
0.11
0.05
0.07
0.06
+ .014
0.08
+ .000
Organic
1.42
1.36
1.39
+ .046
1.21
+ .063
1.55
2.11
2.12
2.12
+ .014
1.43
'±.193
1.35
1.33
1.34
±.169
1.27
+ .100
1.7C
0.71
0.67
0.69
+ .125
0.25
1.051
Ash
9.19
9.12
9.16
+ .049
13.18
+ .070
8.58
7.47
7.79
7.63
±.226
13.36
+ .139
28.50
29.24
28.87
±.523
33.48
+ .125
27.24
20.14
20.74
20.44
+ . 424
27.18
±.242
Volatile
Matter
39.35
38.22
38.78
±.779
38.64
+ .263
36.26
35.31
35.11
35.21
+ .141
38.88
±.348
29.95
29.66
29.80
+ .205
31.13
+ .207
31.5C
29.95
29.67
29.81
+ .198
28.33
+ .220
FTxe3
51.46
52.66
52.06
±.801
48.18
+ .272
55.16
57.22
57.10
57.16
+ .266
47.76
+ .375
41.55
41.10
41.33
+ .562
35.39
+ .242
41.18
49.91
49.59
49.75
i.468
44.49
+ .327
btu/lb
13610
13564
13587
±32.5
13013
±61.6
13377
13793
13736
13764
+40.3
12962
±55.8
10131
10180
10156
±34.6
9495
+ 14.5
10195
12150
12067
12108
t58.7
11012
+ 31.5
-------
cn
Table D-3
PYRITIC SULFUR REMOVAL DATA
MARION, LUCAS, BIRD NO. 3, AND MARTINKA MINES
Mine, Seam,
and Location
Marion Mine
Upper Freeport Seam
Indiana County
Pennsylvania
Lucas Mine
Middle Kittanning
Columbia County
Ohio
Bird No. 3 Mine
Lower Kittanning
Sommerset County
Pennsylvania
Marti nka Mine
Lower Kittanning
Logan or Mingo
West Virginia
Mesh
100
TOO
100
100
150
150
150
IOC
100
Total
Rxn.
Time
23
23
23
23
23
23
23
23
23
Leach Changes
Number Time (hrs)
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 6
1 6
Treated Average
Std. Oev.
Initial Average
Std. Dev.
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
Run
Number
1
2
1-2
A-C
1
2
1-2
A-C
3
1
2
1-2
A-C
1
2
1-2
A-C
Drv Forms
Total
Sulfur
0.77
0.76
0.57
0.62
0.68
±.100
1.37
±.0?F
0.83
0.95
0.89
±.085
1.79
1.122
0.63
0.78
0.83
0.80
±.035
3.14
±.050
0.59
0.57
0.58
±.01A
2.06
±.015
Pyritic
0.04
0.06
0.03
0.04
0.04
±.013
0.90
* m 7
0.19
0.19
0.26
0.20
0.21
±.C34
1.42
+ .087
0.07
0.10
0.13
0.12
0.18
0.13
±.034
2.87
±.062
0.13
0.13
0.12
0.12
0.12
±.006
1.42
±.020
f Sulfur. % w/w
Sulfate
0.04
0.05
0.05
0.09
O.OP
:..C?2
0.02
-.017
0.13
0.14
0.09
0.15
0.13
±.026
0.05
±.00
0.15
0.11
0.11
0.11
±.00
0.05
±.00
0.09
0.07
0.08
±.014
0.07
±.00
Organic
0.69
0.65
0.49
0.49
0.58
±.103
0.45
+ .035
0.50
0.69
0.55
±.095
0.32
+ .147
0.41
0.55
0.57
0.56
±.049
0.22
±.080
0.37
0.38
0.38
±.021
0.57
±.025
Drv Proximate Analysis, % w/w
Ash
22.59
22.63
22.61
±.028
26.40
1 +.081
6.25
6.39
6.32
±.099
8.68
i.087
23.85
24.49
24.17
±.453
30.23
±.310
43.44
43.47
43.46
±.021
49.25
±.045
Volatile
Matter
25.17
25.45
25.31
±.198
24.45
±.342
35.49
34.81
35.15
+ .481
35.30
±.180
17.35
17.79
17.57
+ .311
16.18
±.081
22.20
22.06
22.13
±.099
23.19
±.058
Fixed
Carbon
52.24
51.92
52.08
± . 200
49.15
±.423
58.26
58.80
58.53
+ .491
56.02
±.221
58.80
57.72
58.26
±.549
53.59
±.320
34.36
34.47
34.41
+ .101
27.56
±.073
utu/lh
11739
11701
11720
±26.9
11041
±26.8
13922
13845
13884
+54.4
13451
±65.4
11532
11468
11500
±45.3
10550
±52.6
8137
8138
8138
±0.7
7693
±21.0
-------
01
ro
Table D-4
PYRITIC SULFUR REMOVAL DATA
MEIGS, DEAN, KOPPERSTON, AND HARRIS NOS. 1 & 2 MINES
Mine, Seam,
and Location
Melgs Mine
Clarion 4A Seam
Melgs County
Ohio
Dean Mine
Dean Seam
Scott County
Tennessee
Kopperston Mine
Campbell Creek Seam
Wyoming County
West Virginia
Harris Nos. 1 & 2
Mines
Eagle and No. 2 Gas
Seams
Boone County
West Virginia
Mesh
100
100
150
150
100
100
100
100
Total
Rxn.
Time
23
23
23
23
13
13
23
23
Leach Changes
Number Time (hrs)
1 9
1 9
Treated Average
Std. Dev.
Initial Average
Std. Dev.
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
Run
Number
1
2
1-2
A-C
1
2
1-2
A-C
1
2
1-2
A-C
1
2
1-2
A-C
Total
Sulfur
1.97
1.90
1.94
±.049
3.73
±.035
2.08
2.07
2.08
±.007
4.09
±.026
0.63
0.59
0.61
±.028
0.91
±.047
0.77
0.77
0.77
±.00
1.00
±.006
Dry Forms
Pvrltlc
0.20
0.19
0.15
0.14
0.17
±.029
2.19
±.030
0.20
0.13
0.19
0.18
0.17
±.029
2.62
±.087
0.02
0.03
0.02
0.08
0.04
±.029
0.47
t.026
0.02
0.04
0.02
0.10
0.04
±.038
0.49
±.036
if Sulfur. %
Sulfate
0.16
0.13
0.14
±.021
0.06
±.006
0.17
0,15
0.16
±.014
0.15
±.00
0.07
0.08
0.08
±.007
0.03
±.012
0.06
0.07
0.06
± 007
0.03
±.00
w/w
Organic
1.61
1.63
1.63
±.061
1.48
±.046
1.75
1.74
1.75
+ .033
1.32
±.091
0.54
0.46
0.49
±.041
0.41
«.055
0.68
0.64
0.67
+ .039
0.48
+ .036
Dry 1
Ash
20.61
20.16
20.38
+ .318
26.53
±.164
13.72
13.59
13.66
±.092
17.28
+ .272
25.56
25.50
25.53
+ .042
30.15
+ .050
16.33
16.59
16.46
±.184
18.63
+ .056
volatile
Matter
35.03
35.51
35.27
+ .339
34.92
±.467
33.66
34.85
34.26
±.841
36.91
±2.01
27.42
27.96
27.69
±.382
23.89
+ .173
31.60
29.96
30.78
±1.16
26.86
±.224
Fixed
44.36
44.33
44.35
±.465
38.55
±.495
52.62
51.56
52.08
+ .846
48.81
±.2.03
47.02
46.54
46.78
+ .384
45.96
t.180
52.07
53.45
52.76
±1.18
54.51
±.231
btu/lb
11022
11104
11063
±58.0
10246
±7.9
12674
12652
12663
±15.6
12107
±40.0
11339
11341
11340
±1.4
10957
±24.9
12551
12561
12556
±7.1
12414
±38.5
-------
Table D-5
PYRITIC SULFUR REMOVAL DATA
NORTH RIVER, HOMESTEAD, KEN, AND STAR MINES
Mine, Sean,
and Location
North River Mine
Corona Seam
Jefferson County
Alabama
Homestead Mine
No. 11 Seam
Ohio County
West Kentucky
Ken 'line
No. 9 Seam
Ohio County
West Kentucky
Star Mine
No. 9 Seam
Hopkins County
West Kentucky
Mesh
100
100
100
100
100
100
150
150
Total
Rxn.
Time
23
23
23
23
23
23
23
23
Leach Changes
Nuraber Time (hrs)
0
0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 5.0
1 5.0
Treated Average
Std. Dev.
Initial Average
Std. Dev.
1 5
1 5
Treated Average
Std. Dev.
Initial Average
Std. Dev.
2 5 S 10
2 5 & 10
Treated Average
Std. Dev.
Initial Average
Std. Dev.
Run
Number
1
2
1-2
A-C
1
2
1-2
A-C
1
2
1-2
A-C
1
2
1-2
A-C
Dry Forms of Sulfur, % w/w
Total
Sulfur
0.92
0.94
0.93
'.014
2.06
'.015
2.31
2.45
2.38
.099
4.46
• .oin
2.82
2.75
2.78
-.059
4.83
'.036
2.52
2.39
2.46
-'.092
4.32
'.025
Pyri tic
0.19
0.13
0.15
0.10
0. 14
'.038
1.42
'.026
0.20
0.15
0.24
0.28
0.22
• .056
3.11
• .049
0.28
0.34
0.21
0.27
0.28
1.021
2.85
-.038
0.06
0. 10
0.03
0.06
0.06
.'.029
2.60
-.100
Sulfate
0.09
0.09
0.09
i.OO
0.07
'.00
0.29
0.32
0.30
-.021
0. 10
• .011
0.27
0.24
0.26
'.021
0.26
'.006
0.35
0.33
0.34
-'.014
0.24
'.029
Organic
0.67
0.73
0.70
+ .040
0.57
t.025
1.84
1.87
1.86
'.116
1.25
• .051
2.24
2.27
2.24
^•043
1.72
'.053
2.09
2.02
2.06
±.097
1.50
-'.075
Dry Proximate Analysis, % w/w
Ash
42.68
43.00
42.84
1.226
49.28
' .045
11.40
11.59
11.50
'.134
16.56
'.150
9.46
9.42
9.44
1.028
15.08
'.057
8.68
8.47
8.58
±.148
13.90
Volatile
Matter
23.85
23.62
23.74
i.163
23.19
t.058
36.77
35.08
35.92
* 1 . 20
33.14
'.573
36.62
35.97
36.30
±.460
35.26
'.839
34.92
35.06
34.99
i.099
33.94
Fixed
Carbon
33.47
33.38
33.42
' .279
27.56
±.073
51.83
53.33
52.58
'1.21
50.30
'.592
53.92
54.61
54.26
±.461
49.66
±.841
56.40
56.47
56.43
±.178
52.16
btu/lu
8399
8247
8323
1107.5
7693
•-21.0
12301
12231
12266
'49.5
11935
"19.7
12695
12683
12689
±8.5
12099
132.7
12646
12655
12650
6.4
2308
-------
TABLE D-6
PYRITIC SULFUR REMOVAL DATA
NAVAJO MINE
Mine, Seam
and Location
Navajo Mine
Nos. 6,7,8 Seam
San Juan County
New Mexico
Mesh
100
100
Total
Rxn.
Time
23
6
Leach Changes
Number Time (hrs)
2 5.0, 13.5
1 3
Initial Average
Run
Number
1-3
4
-
Dry .Forms c
Total
Sulfur
0.76
0.61
0.81
Pyr1t1c
0.04
0.03
0.28
F Sulfur. % w/w
Sulfate
0.15
0.12
0.03
Organic
0.57
0.46
0.50
Dry Proximate Analysis. % w/w
Ash
20.53
19.70
25.29
Volatile
Matter
35.82
35.77
35.51
Mxed
Carbon
43.60
44.53
39.40
btu/lb
10033
10353
10050
Includes Supplemental Run Data and Summary of Initial Data from Ref. 2.
tn
•Pk
-------
APPENDIX E
WASHABILITY TABLES
NOTE: Coal washability results have been
performed through standard flat and
sink testing, discussed in Section 4.4
155
-------
Central Ohio Coal Co.
Muskingum Mine - Meigs Creek #9 Seam
Morgan County, Ohio
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-1. 38.1 mm X 149y (1V2" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
head Sample
Fine"
FRACTION ANALYSIS
"Sulfur
tut. *Ash Total PyHtlc
1.1 3.98 3.49 .68
38.5 9.81 4.23 1.49
43.5 21.19 4.61 2.41
8.4 37.88 6.59 5.48
8.5 61.75 15.12 14.26
CUMULATIVE RECOVERY FLOAT
•Sulfur
*Wt. Msh Total Pyrltle
1.1 3.98 3.49 .68
39.6 9.65 4.21 1.47
83.1 15.69 4.42 1.96
91.5 17.73 4.62 2.28
00.0 21.47 5.51 3.30
22.23 5.49 3.41
27.40 5.27 3.04
CUMULATIVE REJECT SINK
SSSulfur
tut. JAsh Total PyHtlc
100.0 21.47 5.51 3.30
98.9 21.66 6.53 3.33
60.4 29.22 6.36 4.50
16.9 49.89 in. 88 9.90
8.5 61.75 15.12 14.26
a) 38.1 mm x 149M (1-1/2" x 100 mesn) = 99.0" of Raw Run of Mine Coal Crushed to ?R.l mm.
b) 149n x 0 (100 mesii x 0) = 1.0' of Raw Run of Mine Coal Crushed to 3R.1 n«r.
TABLE E-2. 9.51 mm X 149y {3/8" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1 . 30 1 . 40
1.40. 1.60
1.60 1.90
1.90
Head Sample
Fineb
FRACTION ANALYSIS
iSulfur
»t. JAjh Total Pyrltle
4.8 8.51 4.19 1.92
48.5 15.13 4.89 2.78
34.6 26.90 5.25 3.25
6.3 36.61 6.11 5.25
5.8 61.00 13.72 13.24
CUMULATIVE RECOVERY FLOAT
'Sulfur
«tt. Msh Total Pyrltle
4.8 8.51 4.19 1.92
53.3 14.53 4.83 2.70
R7.9 19.40 4.99 2.92
94.2 20.55 5.07 3.07
100.0 22.90 5.57 3.66
22.39 5.61 3.41
22.96 5.56 3.28
CUMULATIVE REJECT SINK
"Sulfur
IWt. lAsh Total PyHtlc
100.0 22.90 5.57 3.66
"5.2 23.62 5.64 3.75
46.7 32.45 6.42 4.76
12.1 48.30 9.76 9.08
5.8 61.00 13.72 13.24
a) 9.51 mm x 149« (3/8" x 100 mesn) = 94.2" nf R,iw Run of nine Coal Crushpd to 1.51 m
b) 149n x 0 (100 rcesn x 0) = 5.8 of Raw Run of (line Coal Crushed to 9.51 pm.
TABLE E-3. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample
FRACTION ANALYSIS
'Sulfur
»t. lAsh Total PyHtlc
11.5 9. 18 3.46 .82
35.5 12.46 4.38 1.64
32.1 24.39 4.20 2.05
11.5 35.42 5.64 4.04
9.4 57.90 16.74 16.06
CUMULATIVE RECOVERY FLOAT
Sulfur
tut. Msh Total PyHtlc
11.5 9.18 3.46 .82
47.0 11.66 4.15 1.44
79 . 1 1 6 . 82 4.17 1 . 69
90.6 19.18 4.36 1.99
100.0 22.82 5.52 3.31
22.52 5.60 3.40
CUMULATIVE REJECT SINK
'Sulfur
twt. JAsh Total Pyrltle
100.0 22.82 5.52 3.31
R8.5 24.60 5.7" 3.63
53.0 32.73 6.74 4.97
20.9 45.53 10.63 9.45
9.4 57.90 16.74 16.06
a) 1.41 mm x 0 (14 mesh x 0) = 100.0'. of Mine Coal Crushed to 1.41 run.
156
-------
Quarto Mining Company
Powhattan No. 4 Mine - Pittsburgh No. 8 Seam
Monroe County, Ohio
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-4. 38.1 mm X 149y C\l/2" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1 . JO
1 . JO 1 .10
1.40 I. o()
1 .00 1 . vo
1 . VO
Head Sample3
F1neb
FRACTION ANALYSIS
JSulfur
JWt. JAsh Tottl Pyrltlc
b.5 5.33 2. OH .59
34.9 It). 04 J.Ob 1 .3-j
lo.O 22.10 4.90 3.9b
7.9 34. 3 / -3.99 4.2.0j 3.91 3.02
CUMULATIVE RECOVERY FLOAT
JSulfur
JWt. JAsh Total Pyrltlc
a. 5 -j.33 2. ob .T)
43.4 9.oO 3.OO I .2'.)
09. 4 1 2.9ri 3.5 1 1.95
6/.J 15.49 J.rso 2.25
IOO.O 37.26 . J.o4 2. 70
38.13 3.69 3.65
58.79 3.52 1.46
CUMULATIVE REJECT SINK
JSulfur
JWt. JAsh Total Pyrltlc
100.0 J/.20 3.04 2. 70
"1.5 40.22 3.9-j 2. '19
00.0 5o.4o ->.4n 3.1')
40.6 72.77 4.JI J./v
32. / ;J2.Oo 3.91 3.62
a) 38.1 mm x I49u (IV x 100 mesh) « 98.3* of Raw run of Mine Coal Crushed to 38.1
b) 149p x 0 (100 mesh x 0) - 1.7* of Raw Run of Mine Coal Crushed to 38.1 mm.
SPECIFIC GRAVITY
Sink Float
1 .30
1 . 30 1 . 40
1.40 1.60
1 .00 1 .90
1 .90
Head Sample8
Fine11
TABLE E-5. 9
FRACTION ANALYSIS
tSul fur
JWt. JAsh Total Pyrltlc
22.3 4.33 2.45 .39
25.0 13.H 1 94
100.0 3/9o 3. /'3 2 49
37.33 3.61 2.64
47.33 3.53 2.33
100 mesh)
CUMULATIVE REJECT SINK
JSulfur
JWt. JAsh Total Pyrltlc
100.0 37.95 J./5 2.49
77.7 4/.00 4.12 3.09
52. 1 03. oo 4.45 3.11
39.7 77. IB 4.23 3.^5
33.4 63.06 J.fl-J 3.59
a) 9.51 mm x U9ii_{|'< x 100 mesh) - 94.3* of Raw Run of Mine Coal Crushed to 9.51 am.
b) H.9V x 0 (100 mesh x 0) = 5.7% of Raw Run of Mine Coal Crushed to 9.51 mm.
TABLE E-6. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1 .40 1 .60
1.60 1.90
1 .90
Head Sample*
FRACTION ANALYSIS
JSulfur
JWt. JAsh Total Pyrltlc
14.6 5./0 .2.35 .47
2ti. 7 9.54 2.63 1 .05
15.4 23.91 4.36 j.3/
8.6 51 .71 4.87 4.4rt
32.7 77.41 4.01 3. 96
CUMULATIVE RECOVERY FLOAT
JSulfur
IWt. JAsh Total Pyrltlc
14.0 5.76 2.35 47
43. j tt.27 2.5/ i tVj
53.7 12.J/ 3.04 1 51
O/. S 1 7.4O 3.27 1 89
100. 0 3/.O3 3.71 2 57
37.18 3.90 2.72
CUMULATIVE REJECT SINK
JSulfur
JWt. JAsh Total Pyrltlc
100 O 3/.OJ 3 71 2.57
35 -I 42.37 3 94 2. PJ
56 7 58.99 .1 5ti i.yG
41 3 72.;'/ 4
-------
National Mines Corporation
Isabella Mine, Pittsburgh Seam
Fayette County, Pennsylvania
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-7. 38.1 m X 149y OVz" X 100 mesh)
SPECIFIC GRAVITY
Sink "eat
1.30
1.30 1.40
1.1(0 1.60
1.60 1.90
1.90
Head Sample3
Fine*
FRACTION ANALYSIS
(Sulfur
XHt. XAsh Total Pyrltlc
15.7 5.64 -94 .30
26.3 9.75 1.40 -69
10.5 17.87 2. 46 1.41
7.2 34.54 2.24 1.52
40.3 82.74 1.44 1.42
CUMULATIVE RECOVERY FLOAT
XSulfur
IHt. XAsh Total • Pyrltlc
15.7 5.64 .94 .30
42.0 8.21 .23 .54
52.5 10.14 .47 .72
59.7 13.09 -57 .81
100.0 41.16 .52 1.06
40.17 .48 0.95
45.06 2.08 1.44
CUMULATIVE REJECT SINK
XSulfur
XUt. XAsh Total PyHtlc
100.0 41.16 .52 .06
84.3 47.77 .62 .20
58.0 65.01 .72 .43
47.5 75.43 .56 .44
40.3 82.74 .44 .42
a) 38.1 mm x 149p (1-1/2" x 100 mesh) - 99.6S of Raw Run of Mine Coal Crushed to 38.1 mm
b) 149ll " 0 (100 mesh x 0) - 0.44 of Raw Run of Mine Crushed to 38.1 mm
TABLE E-8. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fine*-
FRACTION ANALYSIS
(Sulfur
JWt. XA§h Total Pyrltlc
18.6 5.03 .92 .25
24.9 10.02 1.27 .33
10.1 17.85 2.04 1.26
6.9 45.92 2.62 1.80
39.5 82.35 1.63 1.61
CUMULATIVE RECOVERY FLOAT
ISulfur
ttlt. XAsh Total Pyrltlc
18.6 5.03 -92 .25
43.5 7.89 .12 .30
53-6 9.76 .29 .48
60.5 13.89 .44 .63
100.0 40.93 -52 1.02
41.81 .58 1.09
48.27 .55 1.23
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total Pyrltlc
100.0 40.93 1.52 1.02
81.4 49.13 1.65 1.19
56.5 66.37 1.82 1.57
46.4 76.93 1.78 1.64
39.5 82.35 1.63 1.61
a) 9.51 mm x I49u (3/8" x 100 mesh) - 97-5* of Raw Run of Mine Coal Crushed to 9.51 mm
b) I49u x 0 (100 mesh x 0 ) - 2.5t of Raw Run of Mine Coal Crushed to 9.51 mm
TABLE E-9. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
XSulfur
»t. XAih Total Pyrltlc
14.7 4.06 .98 .19
26.0 9.17 1.23 .37
12.7 16.01 2.23 .74
9.6 45.73 1.94 1.60
37.0 85.36 1.92 1.68
CUMULATIVE RECOVERY FLOAT
XSulfur
XHt. XAsh Total PyHtlc
14.7 4.06 .98 '.19
40.7 7.32 .14 .30
53.4 9.39 .40 .41
63.0 14.93 .48 .59
100.0 40.99 .64 .99
40.95 .57 0.99
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total PyHtlc
100.0 40.99 1.64 .99
85.3 47.35 1.76 1.13
59.3 64.09 1.99 1.4?
46.6 77.20 1.92 1.66
37.0 85.36 1.92 1.68
a) 1.41 mm x 0 (14 mesh x 0) - 100.0? of Raw run of Mine Coal Crushed to 1.41 mm
158
-------
Mathies Coal Company
Mathies Mine - Pittsburgh Seam
Washington County, Pennsylvania
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-10. 38.1 mm X 149y
X 100 mesh)
SPECIFIC SUAVITY
Sink Float
1 .30
I.JO 1.40
1.40 1.60
1.60 1.90
1 .90
Head Sample3
Fineb
FRACTION ANALYSIS
SSulfur
IWt. SAsh ToUl Pyrltlc
29.3 4.32 1.38 .54
23. -J 25.21 2.96 2.35
7.6 32.06 3.06 2.44
3.3 49. b4 2.H3 2.57
36.3 U2.50 . 7b .60
CUMULATIVE RECOVERY FLOAT
SSulfur
Wt. SAsh Total Pyrltlc
29.3 4.32 I.3H .54
52. « 13.62 2. OH 1.35
60.4 15.94 2.21 1 .4d
63.7 1 7.69 2.24 1 .54
1 00.0 41.22 1.70 1.20
41.01 1.59 1.09
36.18 2.18 1.54
CUMULATIVE REJECT SINK
tSulfur
tut. SAsh Total Pyrltlc
100.0 41.22 1.70 1.2
70.7 56.51 1.83 1.47
47.2 72.09 1.27 1.03
39.6 79. 7b .92 .76
36.3 82.50 .75 .60
a) 38.1 rim x 149u (1-1/2" x 100 mesh) = 98.1% of Raw Run of Mine Coal Crushed to 38.1 m.
b) 149p x 0.000 mesh x 0) = 1.9* of Raw Run of Mine Coal Crushed to 38.1 m.
TABLE E-ll. 9.51 mm X 149y (3/8M X TOO mesh)
SPECIFIC WAVm
Sink Float
1 .30
1 . 30 1 . 40
1.40 1.60
1.00 1.90
1 .90
Head Sample8
Fineb
FRACTION ANALYSIS
SSulfur
at. SAsh ToUl Pyrltlc
23.5 3.38 1.17 .38
20.5 9.66 2.52 1.71
9.6 17.33 4.19 3.52
3.9 26.91 3.20 2.63
42.5 85.78 .85 .73
CUMULATIVE RECOVERY FLOAT
(Sulfur
JWt. »$h Total Pyrltlc
23.5 3.38 1.17 .38
44.0 6.31 1.80 .00
53.6 8.28 2.23 .45
57.5 9.54 2.29 .53
100.0 41.94 1.68 .19
40.82 1.61 .04
41.89 1.79 1.41
CUMULATIVE REJECT SINK
SSulfur
tHt. SAsh Total Pyrltlc
100.0 41.94 1.68 1.19
76.5 53.79 1.84 1.44
56.0 69.95 1.59 1.34
46.4 80.83 1.05 .89
42.5 85.78 .85 .73
a) 9.51 mm x 149^ (3/8" x 100 mesh) = 94.0* of Raw Run of Mine Coal Crushed to 9.51 nm.
b) 149u x 0 (100 mesh x 0) = 6.0% of Raw Run of Mine Coal Crushed to 9.51 mm.
TABLE E-12. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC SRAVin
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Samplea
FRACTION ANALYSIS
tSulfur
Wt. SAsh Total Pyrltlc
23.0 5.45 1.08 .37
22.3 11.86 1.73 .98
11.4 25.20 2.48 1.95
6.9 39.16 2.12 1.75
36.4 85.11 1.20 1.12
CUMULATIVE RECOVERY FLOAT
SSulfur
sut. SAsh Total Pyrltlc
>
23. O 5.45 .08 .37
45.3 8.61 .40 .67
56.7 11.94 .62 .93
63.6 14.89 .67 1.02
100.0 40.45 .50 1.05
40.20 1.56 1.09
CUMULATIVE REJECT SINK
SSulfur
IWt. SAtlt Total Pyrltlc
100.0 40.45 .50 .05
77.0 50.91 .63 .26
54.7 66.83 .58 . >7
43.3 77.79 .35 .22
36.4 85.11 .20 .12
a) 1.41 mm x 0 (14 mesh x 0) = 100.0% of Raw Run of Mine Coal Crushed to 1.41 ran.
159
-------
Consolidation Coal Co., Mountaineer Coal Co. Dlv.
Williams Mine, Pittsburgh Seam
Marion County, West Virginia
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-13. 38.1 mm X 149y (lV2" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
(Sulfur
(Ht. (Ash Total Pyrltlc
55.0 6.18 1.84 .49
31.3 8.52 2.86 1.59
6.5 21.88 6.40 3.78
1.6 34.38 9.04 8.21
5.6 75.84 15.95 15.79
CUMULATIVE RECOVERY FLOAT
iSulfur
(Wt. tAsh Total Pyrltlc
55.0 6.18 1.84 .49
86.3 7.03 2.21 .89
92.8 8.07 2.50 1.09
94.4 8.51 2.61 1.21
100.0 12.29 3.36 2.03
14.01 3.42 2.08
21.69 3.81 2.51
CUMULATIVE REJECT SINK
ISulfur
(Wt. (Ash Total Pyrltlc
100.0 12.29 3.36 2.03
45.0 19.75 5.22 3.91
13.7 45.40 10.61 9.21
7.2 66.63 14.41 14.11
5.6 75.84 15.95 15.79
a) 38.1 ran x 149u (l-l/2"x ICO mesh)= 97.65; of Raw Run of nine Coal Crushed to 38.1 mm.
b) 149u x 0 (100 mesh x 0) = 2.456 of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-14. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC GRAVITY
Sink neat
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
(Sulfur
(Ht. (Ash Tot«l Pyrltlc
47.4 3.63 1.72 .20
38.2 12.97 3.33 1.89
7.1 24.51 7.41 6.50
1.9 31.46 9.55 8.64
5.4 74.43 14.24 14.13
CUMULATIVE RECOVERY FLOAT
(Sul fur
(Ht. (Ash Total Pyrltlc
47.4 3.63 1.72 .20
85.6 7.80 2.44 .95
92.7 9.08 2.82 1.38
94.6 9.53 2.95 1.52
100.0 13.03 3.56 2.21
12.85 3.41 1.97
17. 30 3.56 2.15
CUMULATIVE REJECT SINK
iSulfur
(Wt. (Ash Total Pyrltlc
100.0 13.03 3.56 2.21
52.6 21.51 5.23 4.01
14.4 44.15 10.25 9.64
7.3 63.25 13.02 12.70
5.4 74.43 14.24 14.13
a) 9.51 mm x 149ii (3/8" x 100 mesh) = 92.0" of Raw Run of Mine Coal Crushed to 9.51 mm.
b) 149 x 0 (100 mesh x 0) = 8.0* of Raw Run of Mine Coal Crushed to 9.51 irm.
TABLE E-15. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample8
FRACTION ANALYSIS
(Sulfur
IWt. (Ash Total Pyrltlc
50.3 4.28 1.69 .24
34.1 8.72 2.33 .82
5.7 22.20 5.16 3.94
2.3 38.11 8.99 8.20
7.6 72.74 16.99 15.63
CUMULATIVE RECOVERY FLOAT
(Sulfur
(Ht. (Ash Total Pyrltlc
50.3 4.28 1.69 .24
84.4 fi.07 1.95 .47
90.1 7.09 2.15 .69
92.4 7.87 2.32 .88
100.0 12.80 3.44 2.00
12.59 3.56 2.11
CUMULATIVE REJECT SINK
(Sulfur
IWt. (Ash Total Pyrltlc
100.0 12.80 3.44 2.00
49.7 21.42 5.20 3.78
15.6 49.17 11.49 10.26
9.9 64.69 15.13 13.90
7.6 72.74 16.99 15.63
a) 1.41 mm x 0 (14 mesh x 0) = 100% of Raw Run of Mine Coal Crushed to 1.41
160
-------
Consolidation Coal Company
Robinson Run Mine, Pittsburgh Seam
Harrison County, West Virginia
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-16. 38.1 mm X 149y
X 100 mesh)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head.Sample8
Fine
FRACTIOH ANALYSIS
ISulfur
JWt. XA*h Tot*l PyHtlc
43.7 4.13 2.24 .37
39.8 8.52 3.38 1.62
6.9 18.64 6.69 5.48
1.8 33.24 9.06 8.33
7.8 74.33 15.65 15.52
CUMULATIVE RECOVERY FLOAT
ISulfur
Wt. XAsh Total Pyrltlc
43.7 4.13 2.24 .37
83.5 6.22 2.78 .97
90.4 7.17 3.08 1.31
92.2 7.68 3.20 1.45
100.0 12.88 4.17 2.55
13.36 3.95 2.61
17.21 4.16 2.39
CUMULATIVE REJECT SINK
ISulfur
IWt. lAsh Total PyrUlc
100.0 12.88 4.17 2.55
56.3 19.67 5.67 4.23
16.5 46.56 11.18 10.54
9.6 66.63 14.41 14.17
7.8 74.33 15.65 15.52
a) 38.1 mm x 149U (1-1/2" x 100 mesh) = 97.OS of Raw Run of Mine Coal Crushed to 38.1 nm.
b) 149y x 0 (100 mesh x 0) = 3.05J of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-17. 9.51 mm X 149y (3/e" x 10°
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
HeadbSamplea
Fine
FRACTION AKALYSIS
ISulfur
»t. XAsh Total Pyrltlc
53.7 4.14 2.19 .46
28.8 9.08 3.38 1.40
6.4 16.02 6.40 5.20
2 1 31.74 9.74 8.86
9 0 74.37 16.47 16.40
CUMULATIVE I&COVERY FLOAT
JSulfur
Bit. JAsh Total PyrUlc
53.7 4.14 2.19 .46
82.5 5.86 2.61 .79
88.9 &.60 2.88 1.11
91.0 7.18 3.04 1.28
100.0 13.22 4.25 2.65
13.17 4.37 2.77
17.62 4.11 2.51
CUMULATIVE REJECT SINK
tSulfur
XWt. lAsh Total Pyr1t1c
100.0 13.22 4.25 2.65
46.3 23.76 6.63 5.18
17.5 47.91 11.98 11.40
11.1 66.30 15.20 14.97
9.0 74.37 16.47 16.40
a) 9.51 mm x 149u (3/8" x 100 mesh) = 95.6; of Raw Run of Mine Coal Crushed to 9.51 mm.
b) 149p x 0 (100 mesh x 0 ) = 4.4t of Raw Run of Mine Coal Crushed to 9.51 trni.
TABLE E-18. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FMCTIOM ANALYSIS
tSulfur
Wt. lAsh Total Pyrltle
54.1 4.62 2.25 .41
27 5 9.43 3.05 1.31
6.9 18.70 6.28 4.71
2.4 35.20 10.30 9.23
9.1 63.85 18.26 17.60
CUMULATIVE RECOVERY FLOAT
JSulfur
%Wt. %Ash Total Pyrltle
54.1 4.62 2.25 .41
81.6 6.24 2.52 .71
88.5 7.21 2.81 1.02
90.9 7.95 3.01 1.24
100.0 13.04 4.40 2.73
13.00 4.18 2.63
CUMULATIVE REJECT SINK
ISul fur
XWt. tAsh Total PyrUlc
100.0 13.04 4.40 2.73
45.9 22.96 6.93 5.46
18.4 43.18 12.73 11.67
11.5 57.87 16.60 15.85
9.1 63.85 18,26 17.60
a) 1.41 mm x 0 (14 mesh x 0) = lOOi of Raw Run of Mine Coal Crushed to 1.41 mm.
161
-------
Consolidation Coal Company
Shoemaker Mine, Pittsburgh Seam
Marshall Co., West Virginia
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-19. 38.1 mm X 149p
x 10°
SPECIFIC SUAVITY
Sink Float
1.30
1 . 30 1 . 1(0
1.40 1.60
1.60 1.90
1.90
Head Sample9
Fine6
FRACTION ANALYSIS
XSul fur
at. XAsh Total Pyrltlc
32. « "t.28 2.46 .53
24.8 14.09 3.57 1.83
10.2 18.49 5.86 4.25
3.2 30. 7k 6.85 5.64
29. 4 83.98 5.71 5.61
CUMULATIVE RECOVERY FLOAT
ISulfur
Hit. XAsh Total Pyrltlc
32.4 4.28 2.46 .53
57.2 8.53 2.94 1.09
67.4 10.04 3.38 1.57
70.6 10.98 3-54 1.76
100.0 32.44 4.18 2.89
32.55 4.03 2.73
32.62 3.38 2.53
CUMULATIVE REJECT SINK
XSul fur
XWt. XAsh Total Pyrltlc
100.0 32.44 4.18 2.89
67.6 45.94 5.00 4.02
42.8 64.39 5.83 5.29
32.6 78.75 5.82 5.61
29.4 83.98 5.71 5.61
a) 38.1 mm x 149u(l-l/2" x 100 mesh) - 97.8% of Raw Run of Mine Coal Crushed to 38.1 mm
b) I49v x 0 (100 mesh x 0) - 2.2% of Raw Run of Mine Coal Crushed to 38.1 mm
TABLE E-20. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC SUAVITY
Sink Float
1-30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
XSul fur
XWt. XAsh Total Pyrltlc
26.3 3-73 2.40 .54
28.6 9.08 3.14 1.65
12.2 20.52 5.59 4.04
3.0 29.31 7.29 6.26
29.9 84.73 5.29 5.26
CUMULATIVE RECOVERY FLOAT
SSulfur
m. XAsh Total Pyrltlc
26.3 3.73 2.40 .54
54.9 6.52 2.79 1.12
67.1 9-06 3.30 1.65
70.1 9.93 3-<<7 1.85
100.0 32.29 4.01 2.87
32.96 3-74 2.53
36.35 3.75 2.51
CUMULATIVE REJECT SINK
XSul fur
XWt. XAsh Total Pyrltlc
100.0 32.29 4.01 2.87
73.7 42.49 4.59 3.70
45.1 63.67 5.50 5.00
32.9 79.68 5.47 5.35
29-9 84.73 5.29 5.26
a) 9-51 mm x I49u (3/8" x 100 mesh) = 96.5% of Raw Run of Mine Coal Crushed to 9.51 mm
b) 149u x 0 (100 mesh x 0) - 3.51 of Ran Run of Mine Coal Crushed to 9.51 mm
TABLE E-21. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC SUAVITY
Sink FlMt
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample*
FRACTION ANALYSIS
XSul fur
XUt. XAsh Total PyHtlc
23-3 3.49 2.34 .45
28.7 7.50 2.93 1.47
12.8 20.45 5.47 4.00
7.5 43.45 7.08 6.15
27.7 85.44 5.15 5.03
CUMULATIVE RECOVERY FLOAT
XSul fur
XWt. XAsh Total Pyrltlc
23.3 3.49 2.34 !45
52.0 5.70 2.67 1.01
64.8 8.62 3.22 1.60
72.3 12.23 3.62 2.07
100.0 32.51 4.04 2.89
32.46 3.71 2.60
CUMULATIVE REJECT SINK
XSul fur
XWt. XAsh Total Pyrltlc
100.0 32.51 4.04 2.89
76.7 41.32 4.56 3.64
48.0 61.55 5-54 4.93
35.2 76.49 5.56 5.27
27.7 85.44 5.15 5.03
a) 1.41 DOT x 0 (14 mesh x 0) =• IOOS of Raw Run of Mine Coal Crushed to 1.41 urn
162
-------
Eastern Associated Coal Corp.
Delmont Mine, Upper Freeport Seam
Westmoreland County, Pennsylvania
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE 1-22. 38.1 mm X 149y
X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
ISul fur
Wt. IAjh Total Pyrltlc
37.6 4.85 1.33 .79
18.9 11.82 3.34 2.95
13.1 19.08 6.15 5.60
5.3 27.99 7.66 7.39
25.1 76.69 8.59 8.46
CUMULATIVE RECOVERY FLOAT
ISul fur
»t. lAsh Total Pyrltlc
37.6 4.85 1.33 .79
56.5 7.18 2.00 1.51
69.6 9.42 2.78 2.28
74.9 10.74 3.13 2.64
100.0 27.29 4.50 4.10
26.80 4.37 4.01
16.85 3.63 2.14
CUMULATIVE REJECT SINK
ISul fur
IWt. lAsh Total Pyrltlc
100.0 27.29 4.50 4.10
62.4 40.81 6.41 6.10
43.5 53.41 7.74 7.47
30.4 68.20 8.43 8.27
25.1 76.69 8.59 8.46
a) 38.1 mm x 149u (1-1/2" x 100 mesh) = 97.9% of Raw Run of Mine Coal Crushed to 38.1 m
b) 149p x 0 (iou mesh x 0) = 2.1% of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-23. 9.51 mm X 149y (3/e" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
ISul fur
Wt. lAjh Total Pyrltlc
39.1 4.23 1.09 .62
19.5 14.83 3.44 3.06
11.6 22.62 5.68 5.15
5.0 31.51 7.34 7.06
24.8 72.27 10.29 10.16
CUMULATIVE RECOVERY FLOAT
ISul fur
IHt. lAsh Total Pyrltlc
39.1 4.23 1.09 .62
58.6 7.76 1.87 1.43
70.2 10.21 2.50 2.05
75.2 11.63 2.82 2.38
100.0 26.67 4.67 4.31
26.78 4.59 4.20
21.53 3.31 1.95
CUMULATIVE REJECT SINK
ISul fur
IHt. lAsh Total Pyrltlc
100.0 26.67 4.67 4.31
60.9 41.07 6.98 6.68
41.4 53.44 8.64 8.38
29.8 65.43 9.80 9.64
24.8 72.27 10.29 10.16
a) 9.51 mm x 149u (3/8" x 100 mesh) -- 93.5% of Raw Run of Mine Coal Crushed to 9.51 mm.
b) 149u x 0 (100 mesh x 0 ) = 6.5% of Raw Run of Mine Coal Crushed to 9.51 mm.
TABLE E-24. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
ISul fur
Wt. lAsh Total Pyrltlc
40.4 4.48 1.14 .41
20.1 11.22 2.16 1.41
8.1 23.69 4.54 3.66
3.9 37.89 7.15 6.62
27.5 71.59 10.94 10.88
CUMULATIVE RECOVERY FLOAT
ISul fur
Wt. lAsh Total Pyrltlc
40.4 4.48 1.14 .41
60.5 6.72 1.48 .74
68.6 8.72 1.84 1.09
72.5 10.29 2.13 1.38
100.0 27.15 4.55 4.00
27.55 4.38 4.18
CUMULATIVE REJECT SINK
ISul fur
Wt. lAsh Total Pyrltlc
100.0 27.15 4.55 4.00
59.6 42.52 6.86 6.43
39.5 58.44 9.25 8.98
31.4 67.40 10.47 10.35
27.5 71.59 10.94 10.88
a) 1.41 mm x 0 (14 mesh x 0) = 100% of Raw Run of Mine Coal Crushed to 1.41 mm.
163
-------
Tunnel ton Mining Co.
Marion Mine - Upper Freeport Seam
Indiana County, Pennsylvania
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-25. 38.1 mm X 149y (l1/2" X 100 mesh)
SPECIFIC GRAVITY
Sink "oat
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample
Fineb
FRACTION ANALYSIS
Bui fur
XHt. XAsh ToUT Pyrltlc
34.5 3.81 .93 .24
26.1 12.46 1.24 .81
9.1 17.77 1.48 1.28
7.0 38.62 1.86 1.50
23.3 76.08 2.56 2.50
CUMULATIVE RECOVERY FLOAT
XSulfur
XHt. XAsh Total Pyrltlc
34.5 3.81 .93 .24
60.6 7.54 .06 .49
69.7 8.87 .12 .59
76.7 11.59 .19 .67
100.0 26.61 .51 1.10
25. 7F .37 0.80
20.53 1.51 0.83
CUMULATIVE REJECT SINK
XSulfur
XUt. XAsh Total Pyrltlc
100.0 26.61 1.51 1.10
65.5 38.62 1.81 1.55
39.4 55.°6 2.19 2.04
30.3 67.43 2.40 2.27
23.3 76.08 2.56 2.50
a) 38.1 mm x 149M (1-1/2" x 100 mesh) = 96.3:: of Raw Run of Mine Coal Crushp<< tn 28.1 mm.
b) 149c x 0 (100 mesh x 0) = 3.7% of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-26. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC SRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90 ,
Head Sample
Fine"
FRACTION ANALYSIS
Bui fur
XHt. lAsh Total Pyrltlc
37.8 3.15 .82 .21
23.4 12.84 1.12 .52
7.8 19.53 1.79 1.34
6.6 34.73 2.02 1.63
24.4 74.28 2.68 2.45
CUMULATIVE RECOVERY FLOAT
XSulfur
ait. *Ash Total PyHtlc
37.8 3.15 .82 .21
61.2 6.85 .93 .33
69.0 8.29 1.03 .44
75.6 10.60 1.12 .55
100.0 26.14 1.50 1.01
26.01 1.50 0.97'
25.13 1.57 0.84
CUHULATIVE REJECT SINK
XSulfur
XWt. tAsh Total Pyrltlc
100.0 26.14 1.50 1.01
62.2 40.10 1.91 1.50
38.8 56.55 2.39 2.09
31.0 65.86 2.54 2.28
24.4 74.28 2.68 2.45
a) 9.51 nm x 149ii (3/8" x 100 mesh) = 94.6': of Raw Run of Mine Coal Crushed to 9.51
b) 149« x 0 (100 mesh x 0) = 5.4S of Raw Run of Mine Coal Crushed to 9.51 mrc.
TABLE 1-27. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC SRAVITY
Sink Float
1.30
1 . 30 1 . 40
1.40 1.60
1.60 1.90
1.90
Head Sample
FRACTION ANALYSIS
Bui fur
»t. XAsh Total Pyrltlc
35.8 3.72 .88 .19
22.3 9.24 1.14 .57
12.6 17.86 1.66 1.25
5.6 36.08 1.98 1.67
23.7 77.11 2.76 2.52
CUMULATIVE RECOVERY FLOAT
XSulfur
Mit. XAsh Total Pyrltlc
35.8 3.72 .88 .19
58.1 5.84 .98 .34
70.7 7.98 l.in .50
76.3 10.04 1.17 .58
100.0 25.94 1.54 1.04
25.42 1.50 0.75
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total Pyrltlc
100.0 25.94 1.54 1.04
64.2 38.33 1.91 1.52
41.9 53.81 2.32 2.02
29.3 69.27 2.61 2.36
23.7 77.11 2.76 2.52
a) 1.41 nm x 0 (14 mesh x 0) = inn.O1:. of Mine Coal Crushed to 1.41 mm.
164
-------
Buckeye Coal Mining Company
Lucas Mine - Middle Kittanning Seam
Columblana County, Ohio
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-28. 38.1 mm X 149y (ll/2" * 100 mesh)
SPECIFIC SUAVITY
Sink FlNt
1 .30
1 . 30 1 . 40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
XSulfur
XWt. XAsh ToUl Pyrltlc
68.5 5.19 .90 .54
23.3 10.22 1.81 1.43
4.2 21.06 3.71 3.62
1.5 38.33 6.24 6.20
2.5 65.69 Id. 66 18.11
CUMULATIVE RECOVERY FLOAT
SSulfur
XMt. JAsh Total Pyrltlc
68.5 5.19 .90 .54
91.8 6.47 1.13 .77
96.0 7.11 1.24 .89
97.5 7.59 1.32 .97
100.0 9.04 1.75 1.40
8.79 1.76 1.33
17.33 2.51 1.74
CUMULATIVE REJECT SINK
XSulfur
XHt. XAsh Total Pyrltlc
100.0 9.04 1.75 1.40
31.5 17.41 3.61 3.27
8.2 37.83 8.73 8.51
4.0 55.43 14.00 13.64
2.5 65.69 18.66 18.11
a) 38.1 run x 149y (1-1/2" x 100 meshl = 98.5% of Raw Run of Mine Coal Crushed to 38.1
b) 149p x 0 (100 mesh x 0) = 1.5* of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-29. 9.51 mm X 149y (Ve" X 100 mesh)
SPECIFIC SUAVITY
Sink Float
1.30
1 . 30 1 . 40
I.4O 1.60
I.6O 1.90
I.9O
Head Sample3
FRACTION ANALYSIS
f Sulfur
XWt. XAsh ToUl Pyrltlc
70.0 3.32 .69 .13
20.2 11.76 1.76 1.31
3.9 26.92 3.61 3.05
1.4 33. Od 5.59 5.27
4.5 63.00 17.64 17. OO
CUMULATIVE RECOVERY FLOAT
XSulfur
XWt. XAsh Totil Pyrltlc
70.0 3.32 .69 .13
90.2 5.21 .93 .39
94.1 6.11 1.04 .50
95.5 6.51 l.ll .57
100.0 9.05 1.85 1.31
8.88 1.92 1.41
CUMULATIVE REJECT SINK
XSulfur
XUt. XAsh ToUl Pyrltlc
100.0 9.05 1.85 1.31
30.0 22.41 4.56 4.07
9.8 44.37 10.34 9.77
5.9 55.90 14.78 14.22
4.5 63.00 17.64 17.00
Fine
10.34
1.50
0.95
a) 9.51 mm x 149u (3/8" x 100 mesh) = 95.2% of Raw Run of Mine Coal Crushed to 9.51 mm.
b) 149u x 0 (100 mesh x 0) = 4.8% of Raw Run of Mine Coal Crushed to 9.El mm.
TABLE E-30. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC SRAVITY
Sink FlMt
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
SSulfur
XHt. XAsh Tot«1 Pyrltlc
62.7 3.12 .53 .17
23.3 7.71 .69 .35
6.2 14.37 1.26 .93
2.2 37.65 2.81 2.64
5.6 65.89 19.91 19.57
CUMULATIVE RECOVERY FLOAT
, XSulfur
XHt. XAsh ToUl Pyrltlc
62.7 3.12 .53 .17
86.0 4.36 .57 .22
92.2 5.04 .62 .21
94.4 5.80 .67 .32
100.0 9.16 1.75 1.40
Q.12 1.81 1.43
CUMULATIVE REJECT SINK
XSulfur
XUt. XAsh Total Pyrltlc
100.0 9.16 1.75 1.40
37.3 19.32 3. BO 3.47
14.0 38.64 «.96 8.65
7.8 57.92 15.09 14.79
5.6 65.89 IV. 91 19.57
a) 1.41 mm x 0 (14 mesh x 0) = 100.0% of Raw Run of Mine Coal Crushed to 1.41
165
-------
Island Creek Coal Company
Bird No. 3 Mine, Lower Kittanning Seam
Somerset County, Pennsylvania
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-31. 38.1 mm X 149y (l1/2" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
ISulfur
twt. lAsh Total Pyrltlc
24.5 3.51 .84 .38
34.1 7.75 1.82 1.41
9.7 17.55 2.57 2.12
5.4 38.67 4.43 4.04
26.3 77.83 6.13 5.92
CUMULATIVE RECOVERY FLOAT
ISulfur
I«t. lAsh Total Pyrltlc
24.5 3.51 .84 .38
58.6 5.98 1.41 .98
68.3 7.62 1.57 1.14
73.7 9.90 1.78 1.35
100.0 27.76 2.93 2.55
27.09 2.97 2.55
16.69 2.46 1.78
CUMULATIVE REJECT SINK
SSulfur
tWt. lAsh Total Pyrltlc
100.0 27.76 2.93 2.55
75.5 35.63 3.60 3.26
41.4 58.60 5.07 4.78
31.7 71.16 5.84 5.60
26.3 77.83 6.13 5.92
a) 38.1 mm x 149U (1-1/2" x 100 mesh) = 97.4% of Raw Run of Mine Coal Crushed to 38.1 ram.
b) 149t x 0 (100 mesh x 0) = 2.6% of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-32. 9.51 mm X 149y (3/e" X 100 mesh)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample9
F1neb
FRACTION ANALYSIS
SSulfur
XWt. XAsh Total Pyrltlc
20.8 2.74 .74 .26
38.8 5.78 1.13 .63
9.6 15.24 2.26 1.30
3.5 30.32 3.52 2.63
27.3 79.14 7.17 7.11
CUMULATIVE RECOVERY FLOAT
ISulfur
IHt. «Ash Total Pyrltlc
20.8 2.74 .74 .26
59.6 4.72 .99 .50
69.2 6.18 1.17 .61
72.7 7.34 1.28 .71
100.0 26.94 2.89 2.46
26.04 3.01 2.57
20.24 2.49 1.89
CUMULATIVE REJECT SINK
ISulfur
JWt. lAsh Total Pyrltlc
100.0 26.94 2.89 2.46
79.2 33.30 3.45 3.03
40.4 59.73 5.69 5.34
30.8 73.59 6.76 6.60
27.3 79.14 7.17 7.11
a) 9.51 fm x 149w (3/8" x 100 mesh) = 96.IS of Raw Run of Mine Coal Crushed to 9.51 ram.
b) 149u X 0 (100 mesh x 0) = 3.9J of Raw Run of Mine Coal Crushed to 9.51 mm.
TABLE E-33. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
SSulfur
»t. IA»h Tot»l Pyrltlc
24.2 3.17 1.06 .26
35.7 7.22 1.33 .77
8.6 18.87 2.61 2.06
3.4 39.97 4.06 3.74
28.1 74.07 6.38 6.29
CUMULATIVE RECOVERY aOAT
ISulfur
I«t. lAsh Total Pyrltlc
24.2 3.17 1.06 .26
59.9 5.58 1.22 .56
68.5 7.25 1.40 .75
71.9 8.80 1.52 .89
100.0 27.14 2.89 2.41
26.98 3.03 2.49
CUMULATIVE REJECT SINK
ISulfur
IHt. lAsh Total Pyrltlc
100.0 27.14 2.89 2.41
75.8 34.79 3.47 3.10
40.1 59.34 5.37 5.17
31.5 70.39 6.13 6.01
28.1 74.07 6.38 6.29
a) 1.41 mm x 0 (14 mesh x 0) = 100% of Raw Run of Mine Coal Crushed to 1.41 mm.
166
-------
American Electric Power Company
Martinka Mine, Lower Kittanning Seam
Loqan County, West Virginia
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-34. 38.1 mm X 149y
X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample8
Fineb
FRACTION ANALYSIS
XSulfur
XWt. XAsh Total Pyrltlc
12.0 4.01 .77 .13
23.0 14.11 1.14 .61
16.1 28.84 1.86 1.57
11. S 41.56 1.96 1.73
37.4 81.91 2.51 2.46
CUMULATIVE RECOVERY FLOAT
XSulfur
XWt. XAsh Total Pyrltlc
12.0 4.01 .77 .13
35.0 10.65 1.01 .45
51.1 16.38 1.28 .80
<>2.6 21.01 1.40 .97
100.0 43.78 1.8: 1.53
44.86 1.78 1.64
49.26 2.20 2.02
CUMULATIVE REJECT SINK
ISulfur
XWt. XAsh Total Pyrltlc
100.0 43.78 1.82 1.53
88.0 49.21 1.96 1.72
65.0 61.63 2.25 2.11
48.9 72.42 2.38 2.29
37.4 81.91 2.51 2.46
a) 38.1 mm x 149p (IV1 x 100 mesh) = 96.5% of Raw Run of Mine Coal Crushed to 38.1 mm
b) 149u x 0 (100 mesh x 0) = 3.5°. of Raw Run of Mine Coal Crushed to 38.1 mm
TABLE E-35. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
JSulfur
XWt. XAsh Total Pyrltlc
8.2 5.26 .78 .19
21.8 15.04 1 .12 .66
18.5 25.92 1.55 1.23
13.0 42.71 1.60 1.36
38.5 82.13 2.87 2.80
CUMULATIVE RECOVERY FLOAT
XSulfur
XWt. tAsh Total Pyrltlc
8.2 5.26 .78 .19
30.0 12.37 1.03 .53
48.5 17.54 1.23 .80
61.5 22.86 1.31 .92
100.0 45.68 1.91 1.64
46.06 1.88 1.63
48.38 2.11 1.80
CUMULATIVE REJECT SINK
JSulfur
IWt. XAsh Total Pyrltlc
100.0 45.68 1.91 1.64
91.8 49.29 2.01 1.77
70.0 59.95 2.29 2.12
51.5 72.18 2.55 2.44
38.5 82.13 2.87 2.80
a) 9.51'mm x 149u (3/8" x 100 mesh) = 98% of Raw Run of Mine Coal Crushed to 9.51 urn
b) 149u x 0 (100 mesh x 0) = 21e of Raw Run of Mine Coal Crushed to 9.51 mm
TABLE E-36. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
tSuUur
XWt. XAsh Total Pyrltlc
15.8 6.25 .68 .10
18.4 15.32 .72 .32
10.4 26.40 .90 .58
11.9 47.16 1.20 1.06
43.5 79.11 3.46 3.38
CUMULATIVE RECOVERY FLOAT
, JSulfur
m. XAsh Total Pyrltlc
15.8 6.25 .68 .10
34.2 11.13 .70 .22
44.6 14.69 .75 .30
56.5 21.53 .84 .46
100.0 46.58 1.98 1.73
46.18 1.82 1.74
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total Pyrltlc
100.0 46.58 1.98 1.73
84.2 54.14 2.23 2.04
65.8 65.00 2.65 2.52
55.4 72.25 2.97 2.88
43.5 79.11 3.46 3.38
a) 1.41 ram x 0 (14 mesh x 0) " 100% of Raw Run of Mine Coal Crushed to 1.41 mn
167
-------
American Electric Power Company
Meigs Mine - Clarion 4A Seam
Meigs County, Ohio
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-37. 38.1 mm X 149y C\l/2" X 100 mesh)
SPECIFIC GRAVITY
S1i* Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample8
Fineb
FRACTION ANALYSIS
«Sulfur
Wt. JAsh Total Pyrltlc
37.1 3.50 1.87 .41
29.4 14.76 3.17 1.56
8.7 25.55 4.33 3.18
4.4 39.55 3.89 2.95
20.4 77.75 6.59 5.51
CUMULATIVE RECOVERY FLOAT
tSulfur
IHt. iAsh Total Pyr1t1c
37.1 3.50 1.87 .41
66.5 8.48 2.44 .92
75.2 10.45 2.66 1.18
79.6 12.06 2.73 1.28
100.0 25.46 3.52 2.14
24.62 3.70 1.91
24.60 3.27 1.86
CUMULATIVE REJECT SINK
tSulfur
IWt. IAsh Total PyHtlc
100.0 25.46 3.52 2.14
62.9 38.42 4.49 3.16
33.5 59.18 5.65 4.57
24.8 70.79 6.11 5.06
2(1.4 77.75 6.59 5.51
a) 38.1 mm x 149u (l-l/2"x!00 mesh) = 96.0? of Raw Run of Mine Coal Crushed to 38.1 mm.
b) 149M x 0 (100 mesh x 0) = 1.0% of Raw Run of the Mine Coal Crushed to 38.1 mm.
TABLE E-38. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample8
Fineb
FRACTION ANALYSIS
SSulfur
Wt. SA$h Totil Pyrltlc
34.0 3.71 2.10 .39
32.8 13.13 2.97 1.45
10.0 38.33 4.56 3.36
4.0 40.65 4.56 3.77
19.2 77.19 5.80 5.66
CUMULATIVE RECOVERY FLOAT
SSulfur
Bit. SAsh Total Pyrltlc
34." 3.71 2.10 .39
66.8 8.34 2.53 .91
76.8 10.94 2.79 1.23
80.8 12.41 2. 88 1.36
100.0 24.85 3.44 2.18
25.23 3.63 2.02
30.32 3.29 2.0V
CUMULATIVE REJECT SINK
SSulfur
Bit. IAsh Total Pyrltlc
100.0 24.85 3.44 2.18
66.0 35.74 4.13 3.10
33.2 58.07 5.28 4.74
23.2 70.89 5.59 5.33
19.2 77.19 5.80 5.66
a) 9.9( irri x 149W (3/8" x 100 mesh) - 93.11 of Raw Run of Mine Coal Crushed to 9.51
B) 149u x 0 (100 mesh x 0) = 6.95 of Raw Run of Mine Coal Crushed to 9.51 ran.
TABLE E-39. 1.41 mm X 0 (14 mesh X 0)
IKCIF1C OMVITT
Sll* FlMt
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Mod Swple*
FMCT10N MMLYSIS
SSulflir
tMt. Stall Toul Pyrltlc
22.2 3.95 2.05 .23
38.6 11.98 2.66 .79
14.9 18.99 3.63 1.90
7.4 45.79 4.41 3.39
16.9 73.11 S.87 5.25
CUMJIAT1VE ttCOKIH FIOAT
ISulfur
«(t. lAsh Teul Pyrltlc
22.2 3.95 2.05 .23
60.8 9.05 2.44 .59
75.7 11.00 2.67 .84
83.1 14.10 2.83 1.07
100.0 24.07 3.34 1.78
24.52 3.38 1.75
CUMUtATlVt RtJECT SINK
ISulfur
Wt. tAih ToUl Pyrltlc
100.0 24.07 3.34 1.78
77.8 29.82 3.71 2.22
39.2 47.38 4.74 J.63
24.3 .64.79 5.43 4.68
16.9 73.11 5.87 5.25
i) 1.41 •> x 0 (14 flesh « 0) = 100.Ot of Rav Run of Mine Coal Crushed to 1.41 m.
168
-------
Royal Dean Coal Co., Inc.
Dean Mine, Dean Seam
Scott County* Tennessee
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (55 w/w DRY BASIS)
TABLE E-40. 38.1 m X 149y (H/211 X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head. Sample
Fine"
FRACTION ANALYSIS
XSulfur
XWt. XAsh Total Pyrltle
32.7 4.03 2.44 .48
31.6 8.13 2.88 1.15
13.0 18.53 3.74 2.23
6.8 36.56 5.85 4.93
15.9 71.11 11.02 10.92
CUMULATIVE RECOVERY FLOAT
SSulfur
XWt. XAsh Total Pyrltlc
32.7 4.03 2.44 .48
64.3 6.04 2.66 .81
77.3 8.14 2.84 1.05
84.1 10.44 3.08 1.36
100.0 20.09 4.34 2.88
19.12 4.37 2.75
28.97 3.96 2.51
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total Pyritlc
100.0 20.09 4.34 2.88
67.3 27.89 5.27 4.05
35.7 45.38 7.38 6.61
22.7 60.76 9.47 9.13
15.9 71.11 11.02 10.92
a) 38.1 mm x 149y (1-1/2" x 100 mesh) = 99.0% of Raw Run of Mine Coal Crushed to 38.1 mm.
b) 149p x 0 (100 mesh x 0) = 1.0* of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-41. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head. Sample
Fine"
FRACTION ANALYSIS
ISulfur
XWt. XAsh Total Pyrltlc
35.8 4.21 2.30 .46
32.3 13.45 3.20 1.60
15.0 22.62 4.21 3.01
5.7 40.88 6.21 5.40
11.2 69.48 11.44 11.32
CUMULATIVE RECOVERY aOAT
XSulfur
XHt. XAsh Total Pyrltlc
35.8 4.21 2.30 .46
68.1 8.59 2.73 1.00
83.1 11.12 2.99 1.36
88.8 13.03 3.20 1.62
00.0 19.36 4.12 2.71
19.03 4.23 2.68
18.10 2.86 1.99
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total Pyrltle
100.0 19.36 4.12 2.71
64.2 27.80 5.14 3.96
31.9 42.34 7.11 6.35
16.9 59.83 9.68 9.32
11.2 69.48 11.44 11.32
a) 9.51 mto x 14% (3/8" x 100 mesh) = 95.35! of Raw Run of Mine Coal Crushed to 9.51 mm.
b) 149u x 0 (100 mesh x 0) = 4.7% of Raw Run of Mine Coal Crushed to 9.51 mm.
TABLE E-42. .1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample
FRACTION ANALYSIS
XSul fur
XWt. XAsh Total Pyrltlc
»2.9 8.91 2.67 .92
>5.3 9.99 3.09 1.25
14.9 22.58 3.71 1.93
5.0 28.68 4.13 2.20
11.9 65.60 12.70 12.24
CUMULATIVE RECOVERY aOAT
XSulfur
XWt. XAsh Total Pyrltlc
42.9 8.91 2.67 .92
PS. 2 9.31 2.83 1.04
83.1 11.69 2.98 1.20
88.1 12.65 3.05 1.26-
100.0 18.95 4.20 2.57
19.00 4.09 2.60
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total Pyrltlc
100.0 18.95 4.20 2.57
57.1 26.50 5.35 3.80
31.8 39.64 7.14 5.83
16.9 54.68 10.16 9.27
11.9 65.60 12.70 12.24
a) 1.41 mm x 0 (14 mesh x 0) = 100.0% of Raw Run of Mine Coal Crushed to 1.41 mm.
169
-------
Eastern Associated Coal Corp.
Kopperston No. 2, Campbell Creek Seam
Wyoming County, West Virginia
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-43. 38.1 mm X 149y (l1/2" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 i.4o
l.liO 1.60
1.60 1.90
1.90
Head Sample3
Fine6
FRACTION ANALYSIS
tSulfur
Wt. IAsh Total PyHtlc
40.2 3.94 .79 .24
20.5 7.11 .88 .31
7.3 15.00 1.23 .63
3.5 34.17 1.74 1.06
28.5 81.06 .98 .95
CUMULATIVE RECOVERY FLOAT
ISulfur
IWt. IAsh Total Pyrltlc
40.2 3.94 .79 .24
60.7 5.01 .82 .26
68.0 6.08 .86 .30
71.5 7.46 .91 .34
100.0 28.43 .93 .51
28.15 .95 .49
28.61 .94 .36
CUMULATIVE REJECT SINK
%Sulfur
IHt. tAsh Total Pyrltlc
100.0 28.43 .93 -51
59.8 44.90 1.02 .70
39-3 64.61 1.09 .90
32.0 75.93 1-06 .96
28.5 81.06 .98 .95
a) 38.1 mm x I49u (1-1/2" x 100 mesh) = 99.5% of Raw Run of Mine Coal Crushed to 38.1 nrn
b) I49t x 0 (100 mesh x 0) - .5£ of Raw Run of Mine Coal Crushed to 38.1 mm
TABLE E-44. 9.51 mm X 149y (3/e" X 100 mesh)
SPECIFIC GRAVITY
Sink Heat
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
(Sulfur
Oft. tAjh Total Pyrltlc
47.7 3.06 .95 .27
19.5 18.22 1.04 .54
6.0 29.01 1.53 1-14
2.1 37.70 2.29 1.77
24.7 83.01 -92 .76
CUMULATIVE RECOVERY ROAT
ISulfur
Int. IAsh Total Pyrltlc
47.7 3.06 .95 .27
67.2 7.46 .98 .35
73.2 9.23 1.02 .41
75.3 10.02 1.06 .45
100.0 28.05 1.02 .53
27.98 .97 .51
28.89 .91 .39
CUMULATIVE REJECT SINK
tSulfur
int. IAsh Total Pyrltlc
100.0 28.05 1.02 .53
52.3 50.84 1.09 .76
32.8 70.23 1.12 .89
26.8 79.46 1.03 .84
24.7 83.01 .92 .76
a) 9.51 mm x l<49u (3/8" x 100 mesh) - 97. U of Raw Run of Mine Coal Crushed to 9.51 mm
b) 149u x 0 (100 mesh x 0) - 2.9* of Raw Run of Mine Coal Crushed to 9.51 mm
TABLE E-45. 1.41mm X 0 (14 mesh X 0)
SPECIFIC 6RAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
tSulfur
»t. lAsh Total PyHtlc
22.9 3.08 .63 -23
32.7 8.14 .75 -21
15.7 19.98 1.09 .52
5.0 42.46 1.48 1.17
23.7 78.48 1.08 1.02
CUMULATIVE RECOVERY FLOAT
JSulfur
m. IAsh Total Pyrltlc
22.9 3.08 .63 .23
55.6 6.06 .70 .22
71.3 9.12 .79 -28
76.3 11.31 .83 -34
100.0 27.23 -89 -50
27.85 -90 .48
CUMULATIVE REJECT SINK
tSulfur
IWt. IAsh Total Pyrltlc
100.0 27.23 .89 -50
77.1 34.40 .97 -58
44.4 53-74 1.13 -86
28.7 72.20 1.15 1.05
23.7 78.48 1.08 1.02
a) 1.41 mt x 0 (14 lesh x 0) • 1001 of Raw Run of Mine Coal Crushed to 1.41 m
170
-------
Eastern Associated Coal Corp.
Harris Mines #1 & #2, Eagle & #2 Gas Seam
Boone County* West Virginia
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/W DRY BASIS)
TABLE E-46. 38.1 mm X 149y (l1/2" * 100 mesh)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample
Fineb
FRACTION ANALYSIS
XSulfur
XUt. XAsh Total Pyrltlc
44.9 2 91 -93 .15
18.6 14.35 1.17 .64
12.4 23.18 1.45 .84
9.1 47.45 1.13 .72
15.0 66.59 .77 .75
CUMULATIVE RECOVERY FLOAT
XSulfur
XWt. XAsh Total Pyrltlc
44.9 2.91 .93 .15
63.5 6.26 1.00 .29
75.9 9.03 1.07 .38
85.0 13.14 1.08 .42
00.0 21.16 1.03 .47
20.95 1.10 .55
14.36 1.07 .40
CUMULATIVE REJECT SINK
tSulfur
XWt. XAsh Total Pyrltlc
100.0 21.16 1.03 .47
55.1 36.03 1.12 .73
36.5 47.07 1.09 .77
24.1 59.36 .91 .74
15.0 66.59 .77 .75
a) 38.1 urn x 149y (1-1/2" x 100 mesh) = 98.8% of Raw Run of Mine Coal Crushed to 38.1 urn.
b) 149u x 0 (100 mesh x 0) = 1.2% of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-47. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample
Fineb
FRACTION ANALYSIS
(Sulfur
XHt. XAsh Total Pyrltlc
44.1 3.75 .84 .23
25.5 15.85 1.28 .69
8.9 27.93 1.38 .72
8.4 35.91 1.49 1.14
13.1 68.23 .83 .71
CUMULATIVE RECOVERY FLOAT
SSulfur
XHt. XAsh Total Pyrltlc
44.1 3.75 .84 .23
69.6 8.18 1.00 .40
78.5 10.42 1.04 .43
86.9 12.89 1.09 .50
00.1 20.14 1.05 .53
19.85 1.01 .50
26.95 1.06 .56
CUMULATIVE REJECT SINK
ISulfur
XWt. XAsh Total Pyrltlc
100.0 20.14 1.05 .53
55.9 33.06 1.22 .77
30.4 47.50 1.17 .83
21.5 55.60 1.09 .88
13.1 68.23 .83 .71
a) 9.51 mfn x 149u (3/8" x 100 mesh) = 98.4% of Raw Run of Mine Coal Crushed to 9.51
b) 149p x 0 (100 mesh x 0) = 1.6? of Raw Run of Mine Coal Crushed to 9.51 mm.
TABLE E-48. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample
FRACTION ANALYSIS
SSulfur
XWt. XAsh Total Pyrltlc
34.7 3.93 .72 .19
28.7 8.27 .93 .30
12.6 21.65 1.16 .62
12.8 40.62 1.20 .71
11.2 67.17 2.07 169
CUMULATIVE RECOVERY FLOAT
' XSulfur
IVt. XAsh Total Pyrltlc
34.7 3.93 .72 .19
63.4 5.89 .82 .24
76.0 8.51 .87 .30
88.8 13.14 .92 .36
00.0 19.19 1.05 .5^
19.47 1.03 .46
CUMULATIVE REJECT SINK
XSulfur
tut. XAsh Total Pyrltlc
100.0 19.19 1.05 .51
65.3 27.30 1.22 .68
36.6 42.21 1.45 .98
24.0 53.01 1.61 1.17
11.2 67.17 2.07 1.69
*
a) 1.41 mm x 0 (14 mesh x 0) = 100.0% of Raw Run of Mine Coal Crushed to 1.41 mm.
171
-------
Republic Steel Corporation
North River Mine, Corona Seam
Jefferson County, Alabama
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-49. 38.1 mm X 149y
X 100 mesh)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1 . 60 1 . 90
1.90
riead Sample3
Fine1'
FRACTION ANALYSIS
(Sulfur
XHt. XAsh Total Pyrltlc
10.8 5.16 1.59 .S8
21.5 20. 4S 2.22 1.40
10.3 31.10 2.97 2.66
4.6 42.56 5.08 2.77
52.8 90.14 1.08 .44
CUMULATIVE RECOVERY FLOAT
SSulfur
Wt. XAsh Total Pyrltlc
10.8 5.16 1.59 .88
32.3 15.36 2.01 1.23
42.6 19.16 2.24 1.57
47.2 21.42 2.32 1.69
100.0 57.71 1.67 1.03
55.05 1.62 1.01
52.97 1.78 .88
CUMULATIVE REJECT SINK
XSulfur
XWt. XAsh Total Pyrltlc
100.0 57.71 1.67 1.03
89.2 64.07 1.68 1.05
67.7 77.91 l.SO .94
57.4 86.31 1.24 .63
52.8 90.14 1.08 .44
a) 38.1 mm x 149t (IV * 100 mesh) = 98.0'. of Raw Run of Mine Coal Crushed to 38.1 mm
b) 149u x 0 (100 :nesh x 0} = 2.0*. of Raw Run of Mine Coal Crushed to 38.1 mm
TABLE E-50. 9.51 mm X 149y (3/e" X 100 mesh)
SPECIFIC SRAYITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
Fineb
FRACTION ANALYSIS
XSulfur
XHt. XAsh Total Pyrltlc
14.2 4-40 !-37 -39
19.6 21.51 2.24 1.32
JO 4 28.48 2.73 1.84
5 9 44.27 2.9., 2.18
^g'g 89.03 1.23 .98
CUMULATIVE RECOVERY FLOAT
XSulfur
ttt. XAsh Total Pyrltlc
14.2 4.40 . 1.37 .39
33.8 14.32 1.87 .93
44.: 17.65 2.08 1.14
50.1 30.79 2.18 1.27
100.0 54.84 1.70 • 1.12
53.65 1.70 1.08
57.87 1.56 .93
CUMULATIVE REJECT SINK
XSulfur
XWt. tAsh Total Pyrltlc
100.0 54.84 1.70 1.12
85.8 63.19 1.76 1.24
66.2 75.53 1.62 1.22
55.8 84.30 1.41 1.11
49.9 89.03 1.23 .98
a) 9.51 mm x 149u (3/8" x 100 mesh) = 92.1'. of Raw Run of Mine Coal Crushed to 9.51 mm
b) 149p x 0 (100 mesh x 0) = ~.9°, of Raw Rim of Mine Coal Crushed to 9.51 mm
TABLE E-51. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC 6RAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1 . 60 1 . 90
1.90
Head Sample3
' FMCTION ANALYSIS
tSulfur
XWt. XAsh Total PyHtlc
21.3 5.11 1.59 .44
16.2 9.68 2.31 1.08
12.1 22.70 2.60 1.58
11.0 60.32 2.69 1.76
39.4 87.07 1.23 1.12
CUMULATIVE RECOVERY ROAT
XSulfur
XW. XAsh Total Pyrltlc
21.3 5.11 1.59 .44
37.5 7.08 1.90 .72
49.6 10.89 2.07 .93
60.6 19.87 2.18 1.08
100.0 46.34 1.81 I.v09
47.22 1.86 1.16
CUMULATIVE REJECT SINK
XSulfur
XHt. XAsh Total Pyrltlc
100.0 46.34 1.81 1.09
78.7 57.50 1.87 1.27
62.5 69.90 1.75 1.32
50.4 81.23 1.55 1.26
39.4 87.07 1.23 1.12
a) 1.41
x 0 (14 mesh x 0} = 100', of Raw Run of Mine Coal Crushed to 1.41 mm
172
-------
Peabody Coal Company
Homestead Mine, No. 11 Seam
Ohio County, Kentucky
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-52. 38.1 mm X 149y (1V2" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1 . 30 1 . 40
1.40 1.60
1.60 1.90
1.90
Head Sample8
Finalb
FRACTION ANALYSIS
(Sulfur
(Wt. (Ash Total Pyrltlc
51.7 4.44 2.36 1.07
31.0 11.75 3.30 1.93
8.1 18.69 5.62 4.39
1.6 34.00 8.29 7.94
7-6 73.49 11.65 11.20
CUMULATIVE RECOVERY FLOAT
(Sulfur
JWt. JAsh Total Pyrltlc
51.7 4.44 2.36 1.07
88.7 6.69 2.53 i 30
90.8 8.21 2.97 i 66
92.4 8.65 3.06 1.77
100.0 13.58 3.72 2.49
13.72 3.99 2.71
26.64 2.93 2.17
CUMULATIVE REJECT SINK
(Sulfur
JWt. JAsh Total Pyrltlc
100.0 13.58 3.72 2.49
'•S. 3 23.37 5.17 4.00
17.3 44.18 8.52 7.71
9.2 66.62 11.07 10.63
7-6 73-49 11.65 11.20
a) 38.1 irrn x 149u (1-1/2" x 100 mesh) = 97.3% of Raw Run of Mine Coal Crushed to 38.1
b) I49u x 0 (100 mesh x 0) = 2.7* of Raw Run of Mine Coal Crushed to 38.1 im.
TABLE E-53. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC 6RAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1 . 60 1 . 90
1.90
HeacT Sample3
Flnalb
FRACTION ANALYSIS
SSulfur
Wt. JAsh Total Pyrltlc
48.2 4.25 2.29 1.05
30.8 10.57 3-44 2.17
12.8 24.69 4.80 3.67
1.5 32.27 9.05 8.20
6.7 67.51 12.16 11.90
CUMULATIVE RECOVERY FLOAT
(Sulfur
JWt. JAsh Total Pyrltlc
48.2 4.25 2.29 1.05
79.0 6.71 2.74 1.49
91.8 9.22 3.03 1.79
93.3 9.59 3.12 1.89
100.0 13.47 3.73 2.56
13.78 3.89 2.76
1?.OB 4.22 3 11
CUMULATIVE REJECT SINK
(Sulfur
(Wt. (Ash Total Pyrltlc
100.0 13.47 3.73 2.56
51.8 22.05 5.07 3.97
21.0 38.89 7.45 6.62
8.2 61.06 11.59 11.22
6.7 67.51 12.16 11.90
a) 9.51 mm x lt9w (3/8" x 100 mesh) - 98.0?, of Raw Run of Mine Coal Crushed to 9.51 mm
b) 149u x 0 (100 mesh x 0) - 2.0* of Raw Run of Mine Coal Crushed to 9.51 mm.
TABLE E-54. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC SUAVITY
Sink Float
1.30
1.30 1.40
1 . 40 1 . 60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
SSulfur
Wt. (Ajh Total PyHtlc
48.3 4.70 2.47 .71
25.1 11.61 3.55 2.01
14.8 20.58 4.19 3.19
3.8 40.19 7.60 6.68
8.0 62.85 13-92 13.57
CUMULATIVE RECOVERY FLOAT
(Sulfur
Wt. JAsh Total Pyrltlc
48.3 4.70 2.47 .71
73.4 7.06 2.84 1.15
88.2 9.33 3.07 1.50
92.0 10.61 3.25 1.71
100.0 14.79 4.11 2.66
14.83 4.19 2.73
CUMULATIVE REJECT SINK
(Sulfur
(Wt. (Ash Total Pyrltlc
100.0 14.79 4.11 2.66
51.7 24.21 5.64 4.48
26.6 36.09 7.60 6.81
11.8 55.55 11.88 11.35
8.0 62.85 13.92 13.57
a) 1.41 mm x 0 (14 mesh x 0) * 100.0* of Raw Run of Mine Coal Crushed to 1.41
173
-------
Peabody Coal Company
Ken Mine, #9 Seam
Ohio County, Kentucky
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (% w/w DRY BASIS)
TABLE E-55. 38.1 mm X 149y
" X 100 mesh)
SPECIFIC SRAVITY
sit* n»«t
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head.Sample
Fine"
FRACTION ANALYSIS
SSulfur
SWt. SAih ToUl Pyrltlc
37.5 4.51 2.41 .56
41.3 10.28 3.72 1.87
12.8 18.84 5.68 4.10
2.1 29.81 9.53 8.27
6.3 75.51 8.79 8.67
CUMULATIVE RECOVERY FLOAT
SSulfur
SWt. SAsh Total Pyrltlc
37.5 4.51 3.41 .56
78.8 7.53 3.10 1.25
91.6 9.11 3.46 1.65
93.7 9.58 3.59 1.79
100.0 13.73 3.92 2.23
13.78 4.34 2.54
30.32 4.22 2.51
CUMULATIVE REJECT SINK
SSulfur
SWt. SAsh Total Pyrltlc
100.0 13.73 3.92 2.23
62.5 19.26 4.83 3.23
21.2 36.77 6.99 5.87
8.4 64.09 8.97 8.57
6.3 75.51 8.79 8.67
a) 38.1 nm x 149p (1-1/2" x 100 mesh) = 98.4S of Raw Run of Mine Coal Crushed to 38.1 ran.
b) 149p x 0 (100 mesh x 0) = 1.6* of Raw Run of Mine Coal Crushed to 38.1 mm.
TABLE E-56. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC QMVITV
Sink Heat
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
HeaciSample8
Fin?
FRACTION ANALYSIS
SSulfur
ttt. SAsh Tottl Pyrltlc
32.6 4.29 2.46 .54
45.2 10.34 3.22 1.46
13.7 19.90 4.83 3.24
2.6 29.94 8.45 7.31
5.9 69.69 14.93 14.72
CUMULATIVE RECOVERY FLOAT
SSulfur
S¥t. SAsh ToUl Pyrltlc
32.6 4.29 2.46 .54
77.8 7.80 2.90 1.07
91.5 9.62 3.19 1.40
94.1 10.18 3.34 1.56
100.0 13.69 4.02 2.34
13.66 3.96 2.56
35.05 4.58 2.32
CUMULATIVE REJECT SINK
SSulfur
SWt. SAsh Total Pyrltlc
100.0 13.69 4.02 2.34
67.4 18.23 4.77 3.21
22.2 34.31 7.94 6.77
8.5 57.53 12.95 12.45
5.9 69.69 14.93 14.72
a) 9.51 ran x ]49u (3/8" x 100 mesh) = 96.9% of Raw Run of Mine Coal Crushed to 9.51 nm.
b) 149u x 0 (100 mesh x 0) - 3.1% of Raw Run of Mine Coal Crushed to 9.51 ran.
TABLE E-57. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1 . 30 1 . 40
HO 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
SSulfur
SWt. SAsh Total Pyrltlc
35.0 4.08 2.59 .64
37.1 8.85 3.27 1.24
17.8 21.32 5.10 3. 43
2.3 32.00 7-46 6.02
7.8 63. 24 15.55 15. 0^
CUMULATIVE RECOVERY FLOAT
SSulfur
SWt. SAsh Total Pyrltlc
35.0 4.03 2.59 .64
77.1 6.53 2.04 .95
89.9 9.46 3.37 1.44
92.2 10.0? 3.47 I.b5
100.0 14.18 4.41 2VM
14.12 4.05 2.51
CUMULATIVE REJECT SINK
SSulfur
SWt. SAsh Total Pyrltlc
WO.O 14.18 'i.4l 2.61
(•5.0 19.61 5.39 3.67
27.9 33.92 8.22 6.90
10. 1 56.13 13.71 13-02
7.8 63.24 15.55 15.09
a) 1.41 mm x 0 (14 mesh x 0) = I00> of Raw Run of Mine Coal Crushed to 1.41 mm
174
-------
Peabody Coal Company
Star Mine, #9 Seam
Hopkins County, Kentucky
Raw Run of Mine Coal
FLOAT & SINK ANALYSIS (35 w/w DRY BASIS)
TABLE E-58. 38.1 mm X 149y
X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1 . 90 1 . 00
Head Sample3
Fineb
FRACTION ANALYSIS
SSuUur
JWt. JAjh Total Pyrltlc
40.2 4.24 2.13 .82
40.6 9.55 3.30 1.65
9.5 20.43 4.76 4.34
2.0 32.52 6.83 6.50
7.7 67.35 11.01 10.98
CUMULATIVE RECOVERY FLOAT
XSulfur
m. lAsh Total Pyrltlc
40.2 4.24 2.13 .82
80.8 6.91 2.72 1.24
90.3 8.33 2.93 1.56
92.3 8.85 3.02 1.67
100.0 13.36 3.63 2.39
13.95 3.77 2.33
28.32 4.06 2.00
CUMULATIVE REJECT SINK
XSuIfur
*Wt. lAsh Total Pyrltlc
100.0 13.36 3.63 2.39
59.8 19.49 4.64 3.44
19.2 40.51 7.48 7.23
9.7 60.17 10.15 10.06
7.7 67.35 11.01 10.98
a) 38.1 mm x I49y (1-V * 100 mesh) = 98.K of Raw Run of Mine Coal Crushed to 38.1 mm
b) 149u x 0 (100 mesh x 0) = 1.8% of Raw Run of Mine Coal Crushed to 38.1 mm
TABLE E-59. 9.51 mm X 149y (3/8" X 100 mesh)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90 1.00
Head Sample3
f ineb
FRACTION ANALYSIS
SSutfur
SWt. SAsh Total Pyrltlc
40.7 5.92 2-20 .89
41.5 10.83 3.12 1.69
9.6 16.88 4.12 3.44
2.7 30.04 7.18 6.58
5.5 70.97 14.02 13-91
CUMULATIVE RECOVERY FLOAT
tSulfur
tut. JAsh Total Pyrltlc
40.7 5.92 2.20 .89
82.2 8.40 2.66 1.29
91.8 9.29 2.82 1.52
94.5 9.88 2.94 1.66
100.0 13.24 3.55 2.34
13.69 3.65 2.37
25.67 4.30 2.30
CUMULATIVE REJECT SINK
ISulfur
IWt. lAsh Total Pyrltlc
100.0 13.24 3.55 2.34
59.3 IP. 26 4.48 3-33
17.8 35.59 7.64 7.15
8.2 57.49 11.77 11.50
5.5 70.97 14.02 13.91
a) 9.51 mm x I49u (3/8" x 100 mesh) = 97.2% of Raw Run of Iline Coal Crushed to 9.51 mm
b) I49u x 0 (100 mesh x 0) = 2.8$ of Raw Run of Mine Coal Crushed to 9.51 mm
TABLE E-60. 1.41 mm X 0 (14 mesh X 0)
SPECIFIC GRAVITY
Sink Float
1.30
1.30 1.40
1.40 1.60
1.60 1.90
1.90
Head Sample3
FRACTION ANALYSIS
SSuIfur
SWt. JAsh Total Pyrjtlc
41.6 8.31 2.45 1.31
42.4 9.88 3.09 1.45
8.6 19.03 4.32 3.40
2.0 31.02 7.44 6.52
5.4 64.97 16.20 15.70
CUMULATIVE RECOVERY FLOAT
tSulfur
IKt. lAsh Total Pyrltlc
41.6 8.31 2.45 1.31
84.0 9.10 2.77 1.38
92.6 10.02 2.92 1.57
94.6 10.47 3.01 1.67
100.0 13.41 3.72 2.43
CUMULATIVE REJECT SINK
SSuIfur
SWt. SAsh Total Pyrltlc
100.0 13.41 3-72 2.43
58.4 17.05 4.63 3.23
16.0 36.03 8.72 7.94
7.4 55.79 13.83 13.22
5.4 64.97 16.20 15.70
a) 1.41 mm x 0 (14 mesh x 0) * 100% of Raw Run of Mine Coal Crushed to 1.41 mm
175
-------
Appendix F
Methods and Trace Element Analysis Data
176
-------
COAL TRACE ELEMENT ANALYSIS
F.I GENERAL INTRODUCTION
The initial handling of coal samples is just as important to the
final result as the analytical procedures and techniques utilized for the
individual determinations. To ensure the validity of the values reported,
the following guidelines must be adhered to:
c The composition of all sample handling and grinding equipment must
be considered to prevent possible contamination of the sample.
For example, stainless grinding equipment must not be used when Ni
or Cr are to be determined; similarly, a brass screen should not
be used for sieving when Cu is one of the elements of interest.
• All reagent additions must be kept at a minimum; blanks must
always be run concurrently; and where possible, high purity
reagents should be used.
• Prior to any dissolution, fusion, or ashing that is to be done on
the coal, all glassware should be meticulously cleaned. A recom-
mended cleaning procedure is to first wash all glassware with soap
(such as Alconox, Dutch Cleanser, etc.) and hot water in order to
remove traces of grease and oils. Then, rinse the glassware with
deionized or distilled water and place it in a 50% (v/v) nitric
acid bath and allow to soak for two hours minimum. This will
remove traces of any inorganics that may be left behind by the
soap and water washing. Remove from the bath, flush thoroughly
with distilled water, follow with acetone rinse, and dry in a clean
drying oven at 80°C until dry. Remove from the oven and store in
a protected area free of contamination.
• All elements of interest should be completely dissolved by the
procedure employed. If not, they must be identified and appro-
priate steps must be taken in order to ensure complete dissolution.
t Sample solutions should be maintained at pH 2 or less to prevent
precipitation. Once the pH is adjusted tto tyiis level, the sample
solutions must be transferred immediately to polyethylene
177
-------
containers to minimize adsorption1 on the walls of glass (Reference
29) and they should be refrigerated (5-10°C) if it becomes necessary
to store them for any period of time.
• Heating of the solutions to effect dissolution should be kept at a
minimum and closely controlled. This is to eliminate the possible
loss of volatile elements (notably chlorides of Sb, Se, As).
Because of this possibility of loss, only HN03 should be used and
the solutions kept below the boiling point.
F.2 SAMPLE PREPARATION
To ensure both the homogeneity of the sample and to expedite the
decomposition of the coal, the coal should be ground to pass a 100 mesh
screen in a clean one-quart ball mill. Once the samples have been ground
to the required 100 mesh size, they are spread evenly in large petri
dishes and dried overnight at 50°C (± 10°). Sample decomposition is
accomplished using a low temperature oxygen plasma asher (such as Inter-
national Plasma Corporation Plasma Asher, Model 1001B). This method was
chosen over high temperature muffle furnace ashing because at high
temperatures, some trace elements may be lost by volatilization (Reference
9).
A needle valve assembly is installed on the purge outlet of the plasma
asher in order to control the purge rate and prevent physical loss of the
sample by blowing. In the standard operating procedure, both gas flow
valves can be initiated simultaneously. However, by doing so, a temperature
differential is formed between the two sample chambers. To eliminate this
problem, only one gas flow valve is initiated and adjusted to peak operating
conditions at a time. When correct adjustment is reached, the other gas
valve is initiated and adjusted to start specifications. To prevent sample
blowing when the vacuum system is started, a tight seal must be maintained
at the chamber door.
Weigh duplicate 2.0 g samples in acid-cleaned petri dish covers.
Place the covers and contents into the plasma asher and begin the ashing
procedure. Approximately every four hours, open the console and stir the
coal sample to expose fresh surface. Ashing is continued 2-3 days or
until no black particles remain.
178
-------
Transfer the sample ash to a Parr Instrument Co. Model 4745 combustion
bomb's 24 ml Teflon acid digestion cup by tapping the edges of the petri
dish and allowing the ash to flow through a wide-tip funnel into the cup.
By first tapping the dish, a minimum of ash will escape into the room
atmosphere. Once the bulk of the ash has been removed from the dish,
transfer the remaining fine particles of ash by repeated distilled water
washings. To minimize the final volume, keep these washings as small as
feasible. Six ml of ultra pure concentrated HNC>3 (70% w/w) and 2.5 ml of
ultra pure concentrated HF (52% w/w) are then added to the digestion cup.
Although Teflon is chemically inert, the surface may contain scratches
after repetitive usage which could retain small amounts of material. It
is advisable to periodically check the blank by running the HN03-HF directly
in the Teflon bomb. If excessive background is encountered, the inside
surface should be remachined.
Caution: HF attacks glass so polyethylene or polypropylene pipets or
graduated cylinders must be used.
The solution is then placed on an asbestos-covered hot plate at
140°C (±10°) and evaporated without boiling until the final volume is 50%
of the original. The sample cup is then placed in the bomb and the bomb
assembled. The bomb is placed in an oven at 130°C (±5°) for a minimum of
four hours.
Remove the sample from the bomb and cool. After cooling, filter the
solutions through Whatman #41 filter paper into Nalgene polypropylene
volumetric flasks. Polypropylene funnels must also be used. Rinse with
a small amount of distilled water. With a small clean rubber policeman,
scrape the Teflon inner liner to remove any adhering ash and rinse into
filter paper. When filtering is completed, cap the volumetric flasks
and transfer the filter paper to platinum crucibles. Ignite the filter
paper in a muffle furnace at 800°C ± 50°C until no filter paper ash
remains. Remove from oven, allow to cool, then add 2 small scoops of
ultra pure Nagt^. Ratio of Na2C03 to residue should be 'vlO/l. Fuse the
ash and Na2C03 over a burner flame until the crucible is cherry red and
the fusion components are in a molten state. Allow to remain at this
condition for 1-2 minutes or until complete fusion has taken place.
179
-------
Remove from flame and allow to cool, then dissolve the fusion cake
using a 1:1 HCl/water solution. Filter into the original volumetric flask
and repeat washing with the 50% HC1 until cake has been completely dissolved.
Wash filter paper with the same acid solution and dilute to final 100 ml
volume with distilled water.
Ultra pure reagents are used throughout because of their high purity
and low ash residues. However, in many cases reagent grade chemicals
could be used provided a blank or neat sample is run simultaneously with
the unknowns. This would need to be tested in the lab, for it depends on
the amount of reagent used, the reagent contamination level and the
concentration of the element of interest in the sample.
F.3 ATOMIC ABSORPTION
The analysis of the dissolved coal ash samples for the elements Mn,
Cu, Cr, Ni, Sn, Ag, Sb, V, Pb, Cd, Zn, Li, Se, Hg and Be is done by flame
or flameless techniques. Atomic Absorption Spectroscopy (AAS) as a general
analytical tool is normally considered free of interelement interferences
and because of the large dilutions employed, is usually unresponsive to
matrix changes. However, trace elemental analysis of coal ash does not
follow these general rules because the elements of interest are present in
a very dilute form in a relatively concentrated matrix consisting of the
major inorganic components of the coal ash, and because of the relatively
high concentrations of fluxes and acids needed for the dissolution. These
relatively high concentrations encountered as well as the complicated
matrix make it mandatory for the analyst to be aware of and to investigate
the presence of interferences. The types of interferences encountered
are classified into the following three categories (References 18,22)1
• Interelement or chemical interferences - for the most part, these
interferences, when present, can be eliminated by using a high
temperature N20-acetylene flame or by addition of suppressants.
• Matrix effects - these interferences are physical in nature and
are due to the large concentrations of acids and solids in
solution. These effects are compensated -for by specially preparing
the standards to match the expected acid and salt content of the
sample.
180
-------
• Molecular absorption - this type of spectral interference can be
particularly troublesome when determining trace elements in
solutions of high salt content. Molecular absorptions predomin-
ately occur from species such as CaOH or SrO and result in a
positive error in the absorption measurement. The Jarrell-Ash
810 AA or equivalent is especially suited for the evaluation and
elimination of this type of interference. This is accomplished
by first ascertaining the presence of the interference
by monitoring a nonabsorbing wavelength near the wavelength of
interest on a second channel. This molecular absorption when
present is visually recorded on a strip chart recorder concurrently
with the absorption of the desired element. The interference is
then subtracted from the combined signal.
The solutions prepared as per section F.2 can be analyzed directly by
AAS for Mn, Cu, Cr, Ni, Sn, Ag, Sb, V, Pb, Cd, Zn, Li, Se and Be using the
operating conditions specified in Table F-l. Background correction must
be used for Cd and in some instances for Mn, Be, Zn, and Sb. In all cases,
the standards employed for calibration of the instrument must contain the
same quantities of HN03-HF, Na2C03 and HC1 used in the preparation of the
samples.
F.3.1 Arsenic Analysis (References 15,16,17,27,28,33)
F.3.1.1 Summary
A sample of coal is mixed with MgO and combusted at 550°C in a muffle
furnace. The residue is transferred to a 125 ml Erlenmeyer flask and
treated with HC1 and KI. The arsenic is then volatilized as arsine,
using SnCl2 and Zn, and absorbed in a silver diethyldithiocarbamate
pyridine solution. The quantitative determination is then performed
by comparing the absorbance of the developed color at 540 nm to standards.
F.3.1.2 Reagents
• 15% KI - 15 g KI dissolved in 100 ml D.I. water
• 20% SnCl2 - 20 g SnCl2 dissolved in 100 ml HC1, heat slowly to
effect dissolution
181
-------
Table F-l.
ATOMIC ABSORPTION ANALYTICAL PARAMETERS
Element
Mn
Cu
Cr
Ni
Sn
Ag
Sb
V
Pb
Cd
In
Li
Be
Se
Fe
Ca
Hg
Analytical
X
2795
3247
3579
2320
2246
3281
2176
4408
2833
2288
2139
<70fl
2349
1960
2482
4227
2852
Slit A
4
10
4
2
4
10
4
2
10
4
10
in
10
10
2
10
10
Background
X
2882
3171
3563
2316
2186
3257
2241
2850
2297
2197
6698
2312
1879
2511
Slit A
4
10
4
2
4
10
4
10
4
10
10
10
10
Flame
Conditions
Air-acetylene
Air-acetylene
N.O-acetylene
NpO-acetylene
Hydrogen-air
Air-acetylene-
lean
Air-acetylene-
lean
N-0-acetylene
Air-acetylene-
lean
Air-acetylene-
lean
Air-acetylene-
lean
f.r tv1pw_
lean
N20-acetylene
Hydrogen-argon
Air-acetylene
N,0-acetylene
Air-acetylene
Detection Limit
(ppm)
Based on 2 g
0.15
0.25
0.25
0.5
2.5
0.25
5.0
5.0
1.5
0.15
0.15
0.1
0.025
5.0
2.5
3.5
0.2
Reported
Interferences
SI, and molecular
absorbance by K,
Na, Cr
Ca molecular
adsorption
Ni, Fe, pH
Fe, Cr, Ca mole-
cular adsorption
H2S04, H3P04,
5000 ppm Na
Th, H2S04> HjP04
Cu at 1 000 ppm
H3P04
200 ppm N1, Cr,
Mo, Si gave
slight inter-
ference, P0.=
SO,., formate,
phlhalate
Molecular adsorp-
tion by Ca, Mg,
Na, K and Fe
Ca, Na, K, Mg,
and Fe molecular
absorptions
Sr at 50 pom
None reported
None reported
Molecular
absorbance
Sulfate.
phosphate
aluminum and
silica
Same as for •
calcium
Method of
Interference Removal
Ca at 2000 pnm or use
background correction
Use background correction
N?0 acetylene flame or
addition of 2» NH4C1
Use background correction
or N20 acetylene flame
Keep acid concentration
constant
Keep sample well diluted
Use EOTA
Use background correction
Use backqround correction
Use background correction
Add 11 La or use N-0-
acetylene flame
Add U La
References
15,16,17,18,
22,24,26,35,
36
15,16,18,22,
23,26,35,36
15,17,18,22,
32,35.36
17,18,22,26
36
18,22
18,22
18,22
18,21,22
15,17,18,22,
26,35,36
15,17,18,20,
22,23,26,35
15,16,17,18,
22,23,26,35,
36
18,22
15,18,22,37
18,22
18,22
16,17,18,22
18.22
• Acidified water - 5 ml cone. H2$04 in 500 ml water
• MgO - Reagent
t Zn - 40 mesh granular
• Lead acetate solution - saturated in water
t Silver diethyldithiocarbamate, pyridine solution - 5 g in one
liter of pyridine. Allow solution to stand in a covered container
for 48 hours. Filter through a Whatman #40 filter and store over
molecular sieves in a brown bottle.
182
-------
F.3.1.3 Procedure
To a porcelain crucible, add 1.0 g sample and 0.1 g MgO, and mix.
To another procelain crucible, add 1.0 g and no sample. This will be used
later for the blank. Place all crucibles into a muffle furnace and heat
slowly to 550°C and maintain at this temperature for 1-1/2 hours. Remove
from oven and allow to cool. Transfer to a wide mouthed Erlenmeyer flask
using three 5 ml rinsings of acidified water. Before transferring, wet the
sample by slowly rinsing down the sides of the crucible with the acidified
water. Repeat until the sample is completely wetted. Wash crucible with
the acid water solution until an approximate volume of 50 ml is attained.
Repeat, following the same procedure for the blank.
To all the flasks, add 5.0 ml cone. HC1, 2.0 ml of the 15% KI solution,
and 1.0 ml of the 20% SnCl2 solution. Allow the solutions to stand for 15
minutes. At the end of this time, the reaction flasks are connected to a
receiving flask by a tube containing glass wool to which a few drops of a
saturated lead acetate scrubbing solution has been added. Ten ml of the
silver diethyldithiocarbamate solution is added to the receiving flask and
3 grams granular zinc is added to the reaction flasks. Connect the reaction
and receiving flask together in as short a time as possible to prevent any
arsine gas loss. After allowing 30 minutes for complete gas evolution,
remove vessel and mix the solution by bubbling nitrogen through the solution
to remove any residue that is adhering to the side wall. Transfer the
absorbing solution to 1 cm quartz cells and measure its absorbance at
540 nm against the blank reagent using a spectrophotometer.
"F.3.1.4 Standard Curve
Before running As determinations, prepare a 100 ppm As stock solution
(10 ml of 1000 ppm As and dilute to 100 ml with distilled water). Once
the stock solution is prepared, take 1, 2, 5 and 10 mis of the 100 ppm
standard, transfer to four 100 ml volumetric flasks and dilute to marks
with distilled water. These 1, 2, 5 and 10 ppm As solutions are the
working standards.
Place one gram of MgO in each of five ceramic crucibles and heat in
a 550°C muffle for 1-1/2 hours. Remove and cool, then transfer to a
183
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125 ml Erlenmeyer with acidified water. Pi pet one ml of each of the four
standards into the respective Erlenmeyers and one ml of distilled water
into a fifth Erlenmeyer for a blank, and proceed according to the procedure
in F.3.2.3. Note the following:
1) The pyridine - silver diethyldithiocarbamate solution will
deteriorate slightly, and if not filtered, will lead to erratic
values.
2) The type of mesh zinc used appears to have some bearing on the
arsine evolution. Therefore, only one bottle should be designated
for use and a new calibration curve should be run when another
bottle is employed.
3) Heating the reaction solution facilitates the evolution of arsine
and has proved helpful in improving the accuracy of the analysis.
F.3.2 Boron (References 15,16,29,30,33)
F.3.2.1 Summary
Gently ash the coal at 550°C, then fuse the ash with Na2C03. After
dissolving the fusion mixture in HC1, the boric acid is extracted with
2-ethyl-l,3-hexanediol and determined as the rosocyanine complex in 95%
ethanol. This procedure is applicable to coals containing between 1-400
ppm B.
F.3.2.2 Reagents
• 10 ppm standard boron solution - prepare by appropriate dilution
of 1000 ppm stock boron solution
• 2-ethyl-l,3-hexanediol - 10% solution in chloroform
0 Curcumin reagent - 0.375% (w/v) dissolved in glacial acetic acid,
filtered, and stored in a darkened polyethylene bottle
• Ethanol - 95% reagent grade
• Sulfuric acid - high purity (Van Waters and Rogers Ultrex grade)
t Na2C03 - high purity (Van Waters and Rogers Ultrex grade)
• IN HC1 - use high purity acid and distilled water
184
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F.3.2.3 Procedure
Weigh 1 g coal ± 0.1 mg into a platinum crucible; ash at 550°C for
one hour. Fuse residue with 1 g of Na2C03, then dissolve the melt with
IN HC1 and dilute to 100 ml. Pipet 2 ml of this solution into a 10 ml
Nalgene centrifuge tube and extract, by shaking with 2 ml of 2-ethyl-l,3-
hexanediol in CHC13. Syringe off the liquid phase, and pi pet 0.5 ml of
the organic phase into a 50 ml Nalgene volumetric flask. Add 1 ml of
curcumin reagent followed by 0.3 ml of cone. H2S04 and allow to react for
15 minutes. Adjust volume to 50 ml with reagent grade 95% ethanol and
read absorbance at 500 nm against 95% ethanol. Run a reagent blank
concurrently and subtract this absorbance from the sample absorbance. The
boron concentration of the sample is calculated from a standard curve
using the adjusted sample absorbance reading.
F.3.2.4 Standardization
Prepare standard solutions containing 0.1, 0.2, 0.5, 1.0, 2.0 and 3.0
ppm boron by appropriate dilution of the 10 ppm standard. Pipet 2 ml of
prepared standard into a Nalgene centrifuge tube and proceed as per general
procedure. Note that all apparatus is to be washed with 1:1 aqueous HN03.
F.3.3 Fluoride Analysis (References 9,15,31,34)
F.3.3.1 Summary
Coal is mixed with benzoic acid, pressed into a pellet and combusted
in a Parr bomb and the combustion gases scrubbed with a dilute caustic
solution. The pH of the solution is now adjusted to 5.2-5.3, and C02 is
expelled by gentle heating. The fluoride concentration is then determined
after pH readjustment and addition of a citrate - KN03 buffer solution
using a specific ion electrode procedure.
F.3.3.2 Results
• IN NaOH - prepared from high purity reagents
• 0.5N H2S04 - prepared from high purity reagents
185
-------
• 1M sodium citrate, 0.2M KNOs buffer solution - dissolve 294 g of
citric acid trisodium salt dihydrate and 20 g of KN03 in one liter
of high purity water (pH 6.3)
0 Fluoride standard - prepare a series of fluoride standards in the
following molar concentrations, .0005, .001, .005, .01, .05 and
.10, by dissolving high purity KF in the citrate-KN03 buffer.
F.3.3.3 Procedure
Mix a 1 gram coal sample, ground to pass a 100 mesh screen, with
approximately 0.25 g benzoic acid (primary standard) and place in a fused
quartz sample holder within a Parr combustion bomb that contains 10 ml of
IN NaOH. The bomb is pressurized to about 28 atmospheres and then fired.
At leased 15 minutes are allowed to elapse before the bomb is depressurized.
Three approximate 5 ml aliquots of distilled water are used to rinse the
bomb contents into a 50 ml plastic beaker (plastic-ware is used from this
point on).
The beaker contents are magnetically stirred with a Teflon bar while
the pH is adjusted to 5.2-5.5 with 0.5N H2S04. (The initial pH before
adjustment will be about 7.0). The beaker is then placed in a hot water
bath for about 10 minutes, removed, and again stirred to drive off most
of the dissolved C02- Five ml of the sodium citrate - KN03 buffer solution
is added to the beaker contents. The total volume is adjusted to 50 ml
with distilled water and cooled to room temperature. At this time, the
potential is read using a fluoride specific ion electrode vs a saturated
calomel reference electrode. In some cases, about 10 minutes are required
for equilibrium to be reached. Then 1 ml of 0.01M F is added and the
potential of the solution is again read.
The pH is quite critical for the initial potential reading. At
5.0-5.5, final results tend to be low because of F~ complexing with H.
Above 6.5, final results tend to be high because of interference by OH~
or HCOo' at 1000 to 1 concentration over the F".
186
-------
The concentration of fluoride in the coal sample is calculated
using the following formulas:
F (soln) = AF
exp (AE/S) - 1
F (coal) = 50 x F
Where AF = change in F cone, due to addition of spike = 3.8 ppm
AE = change in potential readings = E2~E^
S = slope of mv vs In (F~) concentration for the electrode
= -22.95
WB = weight benzoic acid
FB = F~ content of benzoic acid = 7.15 ppm
F.3.4 Mercury Analysis (References 18,19,22,25,38)
F.3.4.1 Summary of Method
A coal sample is decomposed by burning in a combustion bomb containing
a dilute nitric acid solution under 24 atmospheres of oxygen pressure.
After combustion, the bomb washings are diluted to a known volume, and
mercury is determined by atomic absorption spectrophotometry using a flame-
less cold vapor technique.
F.3.4.2 Apparatus
• Oxygen bomb - Standard 360 ml stainless steel combustion bomb
as used for coal calorimetry (ASTM D 2015).
• Combustion crucible - Vycor or quartz crucible of proper size
to fit the bomb sample holder (A.M. Thomas No. 3879-C or
equivalent).
• Firing wire - No. 34 B & S gauge nickel-chromium alloy wire,
10 cm length.
187
-------
Firing circuit - as described in ASTM D 2015.
Atomic Absorption Spectrophotometer - Use mercury hollow cathode
lamp and a wavelength of 253.7 nm.
Absorption cell - a cylindrical tube of approximate dimensions
25 mm I.D. X 125 mm long, with quartz windows, and incorporating
inlet and outlet sidearms to permit introduction and discharge
of carrier gas. This type of cell is available commercially from
several manufacturers of atomic absorption equipment, or it may
be constructed from readily available materials (Note 1). In the
latter case, the cell should be tested carefully for possible
leakage after assembly. The cell is mounted in the optical path
of the AA spectrophotometer.
Mercury reduction vessel - a cylindrical, flat-bottom cold test
jar (Fisher No. 13-415 or equivalent), containing a glass or
polypropylene covered magnetic stirring bar, and incorporating a
two-hole rubber stopper through which are passed a gas bubbler
tube (Note 1) and a short gas outlet tube. The bubbler tube is
connected to the carrier gas source, and the outlet tube is
connected to the absorption cell; all connections should be made
with polypropylene tubing (Note 2). Calibrate the reduction vessel
at the 50 ml mark.
Magnetic stirrer - for use in conjunction with the mercury
reduction vessel.
Flowmeter - capable of measuring gas flows in the range of one
liter per minute.
Note 1 - A constricted, open gas bubbler tube is preferred over the fritted
glass dispersion type. With the latter, there is the possibility
of mercury retention in the frit, at least if the solution is not
stirred sufficiently.
Note 2 - There is some evidence that certain materials such as Tygon and
Teflon can adsorb mercury to a significant extent. For this
reason, the use of standard Teflon-covered stirring bars is also
discouraged.
188
-------
F.3.4.3 Reagents
• Stock mercury solution, approximately 1 gram/liter (1,000 ppm).
Weigh 1 gram of pure, elemental mercury to the nearest 0.1 mg
and dissolve in a solution consisting of 150 ml of distilled water
and 50 ml of concentrated HN03 (sp. gr. 1.42). Dilute this
solution to 1000 ml with distilled water. The final solution
contains approximately 1,000 ppm of mercury (record exact
concentration) in a matrix of 5% (v/v) nitric acid.
• Standard mercury solutions - Prepare working standard solutions of
mercury down to 1 ppm by serial dilutions of the 1,000 ppm Hg
stock solution with 5% HN03. Such solutions may be assumed to be
stable for up to one week. Below 1 ppm Hg, standard solutions
should be prepared daily and diluted with 5% HN03 and/or distilled
water as appropriate, so that the final solution matrix is
approximately 1% HN03.
• Nitric acid solution, 10% (v/v) - Dilute 100 ml of concentrated
HN03 (sp. gr. 1.42) to 1000 ml.
• Stannous chloride solution, 10% (w/v) - Dissolve 10 g of
SnCl2-2H20 in 10 ml of concentrated HC1 (warm the solution if
necessary to accelerate the dissolution process) and dilute to
100 ml. Add a few pieces of metallic tin.
• Helium carrier gas - Use Matheson High Purity grade or equivalent.
The gas may contain a trace amount of mercury, and the use of a
small amalgamator trap (gold or silver wire coils packed in about
1 inch of tubing) between the gas cylinder and the flowmeter is
advisable.
F.3.4.4 Standardization
Transfer an aliquot of a standard mercury solution containing 0.10
micrograms of mercury to the mercury reduction vessel. Dilute to 50 ml
with 10% HN03, and add 5 ml of 10% stannous chloride solution. Insert
the stopper containing the carrier gas inlet and outlet tubes, and start
the magnetic stirrer. Stir the solution for one minute, then initiate
189
-------
helium flow at a rate of one liter per minute (Note 3). Record the
absorption peak and measure peak height. Repeat this procedure using
varying amounts of mercury throughout the range of 0.01 to 1.00 micro-
grams.
Run a blank using all reagents except the standard mercury solution.
Plot absorption (peak height) against micrograms of mercury present, after
correcting for the reagent blank, to establish a working curve.
F.3.4.5 Procedure
Mix 1 g of coal and ^0.25 g of benzoic acid. Press into a pellet and
place in a fused quartz crucible. Transfer 10 ml of 10% nitric acid to
the bomb, place the crucible in the electrode support of the bomb, and
attach the fuse wire. Assemble the bomb and add oxygen to a pressure of
24 atmospheres (gauge). Place the bomb in the calorimeter (a cold water
bath in a large stainless steel beaker is also satisfactory) and ignite
the sample using appropriate safety precautions ordinarily employed in
bomb calorimetry work.
After combustion, the bomb should be left undisturbed for 10 minutes
to allow temperature equilibration and the absorption of soluble vapors.
Release the pressure slowly and transfer the contents of the bomb (and
crucible) to the mercury reduction vessel by washing with 10% nitric acid
(Note 4).
Rinse the bomb, electrodes, and crucible thoroughly with several
small washings of 10% nitric acid, then dilute the contents of the reduc-
tion vessel with 10% nitric acid to a total volume of 50 ml. Proceed with
the determination as described under Standardization. Determine the amount
Note 3 - The optimum flow rate will depend on the size of the absorption
cell. Several flow rates should be tried until maximum sensi-
tivity is obtained.
Note 4 - If there is any question as to whether the sample has undergone
complete oxidation during combustion, add 5% potassium perman-
ganate solution dropwise until a pink color persists.
190
-------
of mercury in micrograms and divide by the sample weight in grams to
obtain the mercury value in parts per million.
As the bomb ages, there may be a tendency for mercury to become
trapped in the bomb wall fissures during combustion. In addition, if the
same bomb is used for normal calorimetry work, there may be a tendency for
mercury to accumulate in the bomb with time. Consequently, before a
series of mercury determinations is undertaken, several blank determina-
tions should be made by firing benzoic acid pellets (approximately 1 gram)
in place of the coal. Benzoic acid firings should be repeated until a
stable, consistently low blarvk value is obtained. This final blank value
is then used to correct the mercury values obtained for subsequent coal
samples (Note 5).
F.4 ANALYSIS RESULTS
The results of trace element analyses for 18 elements in ten coals
before and after treatment by the Meyers and float-sink procedures are
presented in Tables F-2 to F-ll. All analyses were run in duplicate on
both untreated and treated coals in order to get a good estimate of
precision of the results and a reliable estimate of the trace element
removal. These analyses were run on two samples of untreated coal in
order that all sources of error such as sampling, ashing, dissolution,
handling, and final analysis would be included in the final precision
estimate. In a similar manner, two samples each of the extracted and
float-sink separated coal samples were each analyzed once for two sets of
two values on the treated coal.
A standard deviation was then calculated for each set of results and
was then used to determine which results should be discarded. A value
falling outside 2a of the mean was not used. Discarded values are in
parentheses in the data tables. The differences between the initial
Note 5 - The condition of the interior of the bomb should be inspected
at frequent intervals. If evidence of significant pitting or
corrosion is observed (usually indicated by erratic mercury
values for samples or benzoic acid blanks) the bomb should be
returned to the manufacturer for reconditioning.
191
-------
average and the final average value are also presented in the tables.
The deviations of the differences were calculated using Equation 1:
Also reported are the calculated % removals. The standard deviation for
the amount removed was calculated using Equation 2:
/b2 2.1
7 ' °a 7 ' °b
In cases where 0(a_b)/a is larger or the same as the value of the % diff-
erence, N.D. is entered in the % Loss column to indicate that any apparent
difference in the initial and final values is not statistically valid.
In all cases where the elrnent was not detected in the starting coal, "Ind"
appears in the PPM Change and % Loss columns.
192
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Table F-2
TRACE ELEMENT ANALYSIS (PPM)
MUSKINGUM MINE, MEIGS CREEK NO. 9 SEAM, MORGAN COUNTY, OHIO
Element
Ag
As
B
Be
Cd
Cr
Cu
F
Hg
Li
Mn
Ni
Pb
Sb
Se
Sn
V
Zn
Individual Values
Raw Coal
1.7 3.5 1.7
2.0 - 1.9
48 - 60
1.7 2.2 2.1
1.5 1.7 (o.i;
121 95 114
14 16 15
116 - 118
0.10 - 0.08
55 53 58
26 24 26
25 33 30
13 11 12
<5 - <5
64 - 54
20 16 10
37 33 28
34 27 30
Treated Coal
Meyers Process
0.7 0.2
-
80 60
2.0 1.7
0.6 0.4
56 47
12 19
165 180
-
58 37
7.7 4.8
21 13
289 144
<5 <5
<1 <1
16 30
38 16
12 13
Float-Sink
<1 <1
2.0 2.0
30 30
2 3
2 2
64 58
20 19
90 78
-
16 15
30 25
47 41
32 32
49 36
-
31 41
37 49
22 20
Average Values
Raw Coal
2.3+1.04
2.0±0.07
54±8.5
2.0±0.26
1.6+0.14
110±13.5
15±1.0
117±1.4
0.09+0.014
55+2,5
25+1.2
29+4.0
12±1.0
<5
59+7.1
15±5.0
33±4.5
30±3.5
Treated Coal
Meyers Process
0.4±0.35
-
70±14.1
1.8+0.21
0.5±0.14
52+6.4
16+4.9
172+10.6
-
48+14.8
6.3+2.1
17±5.7
216+103
<5
<1
23±9.9
27±15.6
12+0.7
Float-Sink
<1
2.0+0
30+0
2.5+.071
2+0
61+4.2
19.5±0.7
84±8.5
- -
16+0.7
28+3.5
44+4.2
32±0
42+9.2
- -
36±7.1
43±8.5
18±3.6
PPM Change
Meyers
Process
1.9+1.1
. -
+16+16.5
0.2±0.33
1.U0.20
58±14.9
+1+5.0
+56+10.7
- -
7±15.0
18.7±2.9
12±7.0
+204+103
Ind
- -
+8+11.1
6+16.2
18+3.6
Float-Sink
>1.3+1
0±0.1
24+8.5
+0.5+0.27
+0.4+0.14
49±14.1
+4.5+1.2
33±8.5
- -
39.5+2.6
+3.0+3.7
+15+5.8
+20+1
>+37
- -
+21+8.7
+10+9.6
12+5.0
% Loss
Meyers
Process
83+17
- -
N.D.
N.D.
67+14
53+8
N.D.
Gain
-
N.D.
75±9
41+21
Gain
Ind
- -
N.D,
N.D.
60±5
Float-Sink
>57±20
N.D.
44+7
Gain
Gain
45±8
Gain
28±7.2
- -
72+1 .8
N.D.
Gain
Gain
Gain
- -
Gain
N.D.
40±14
vo
GO
-------
Table F-3
TRACE ELEMENT ANALYSIS (PPM)
MATHIES MINE, PITTSBURGH SEAM, WASHINGTON COUNTY, PENNSYLVANIA
Element
Ag
As
B
Be
Cd
Cr
Cu
F
^3
Li
Mn
Ni
Pb
Sb
Se
Sn
V
Zn
Individual Values
Raw Coal
2.2 2.0 1.2
7.1 - 5.1
48 - 60
2.6 2.7 2.7
0.7 1.1 0.5
114 - 106
31 30 27
222 - 197
0.08 - 0.10
70 60 62
64 73 62
35 35 33
25 17 15
<5 <5 <5
78 69
14 - 10
46 68 65
41 41 40
Treated Coal
Meyers Process
0.2 0.2
1.0 1.0
58 60
1.6 1.9
<0.5 <0.5
53 58
23 20
200 219
-
38 42
5.0 8.4
16 15
<5 10
<5 <5
<1 4
<5 <5
15 33
12 13
Float-Sink
1 1
<.l .3
50 45
3 2
4 4
47 49
20 18
82 94
-
24 28
24 23
46 38
36 30
54 46
-
79 77
14 29
21 26
Average Values
Raw Coal
1.8+0.53
6.1+0.41
54+8.5
2.7+0.06
0.8+0.31
110+5.7
29+2.1
210+17.7
0.09+0.014
64+5.3
66+5.9
34+1.2
19+5.3
<5
.74+6.4
12+2.8
60+11.9
41+0.6
Treated Coal
Meyers Process
0.2+0.0
1.0+0.0
59+1 .4
1.8+0.21
<0.5
56+3.5
22+1 .7
210+13.4
-
40+2.8
6.7+2.4
16+0.7
6+5.3
<5
2+2.8
<5
24+12.7
12+0.7
Float-Sink
1+0
0.18+0.18
48+3.5
2.5+0.71
4+0
48+1.4
19+_1.4
88+_8.5
- -
26+2.8
23.5+0.71
42+5.7
33+4.2
50+_5.7
- -
78+1.4
22+10.6
24+3.5
PPM Change
Meyers
Process
1.6+0.53
5.1+0.41
5.0+8.6
0.9+0.22
>.3+0.3
54+6.7
7+2.7
0+22.2
- -
24+6.0
59+6.4
18+1.4
13+7.5
Ind
_. _
>7+2.8
36+17.4
29+0.9
Float-Sink
0.8+0.53
5.9+0.45
6 +9. 2
0.2+0.71
+3.2+0.31
.62+5.9
10+2.5
122+19.6
- -
38+6.0
43+5.9
+8+5.8
+14+6.6
>45+5.7
- -
+66+3.1
38+15.9
21 + .9
% Loss
Meyers
Process
89+3
84+1
N.D.
33+8
>38+24
49+4
24+8
N.D.
- -
38+7
90+4
53+3
68+30
Ind
_ _
>58+10
60+23
71+2
Float-Sink
44+16
97+3
N.D.
N.D.
Gain
56+3
34+7
58+5
- -
59+6
64+3
N.D.
Gain
Gain
— ._
Gain
63+T9
41+9
IO
-------
Table F-4
TRACE ELEMENT ANALYSIS (PPM)
ROBINSON RUN MINE, PITTSBURGH SEAM, HARRISON COUNTY, WEST VIRGINIA
Element
Ag
As
B
Be
Cd
Cr
Cu
F
US
Li
Mn
Ni
Pb
Sb
Se
Sn
V
Zn
Individual Values
Raw Coal
1.5 1.7
P. 2 5.6
60 60
1.0 n.3
l.fi 2.1
102 98
10 10
114 88
0.13 0.14
15 9
41 42
26 27
13 12
20 18
40 58
15 <5
28 28
32 28
Treated Coal
Meyers Process
1.5 1.0
<0.3 <0.3
75 95
0.7 1.3
1.6 0.9
37 37
17 21
68 94
-
8 8
8.1 6.2
20 16
20 17
4 2
22 13
<5 <5
2 7
11 10
Float-Sink
1 1
1 1
60 60
<0.5 <0.5
3 3
29 32
16 13
113 82
-
5 5
24 23
39 29
23 21
44 32
-
68 91
<5 7
21 14
Average Values
Raw Coal
1.6+0.14
5.9+0.42
60+0
0.6+0.49
1.8+0.35
100+2.8
10+0
100+18.4
0.14+0.007
12+4.2
42+0.7
26+0.7
12+0.7
mi. 4
.49+12.7
8
28+0
30+2.8
Treated Coal
Meyers Process
1.2+2.35 '
<0.3
85+14.1
1.6+0.42
1.2+0.49
37+0
19+2.8
81+18.4
- -
8+0
7.1+1.3
18+2.8
18+2.1
3+1.4
18+6.4
<5
4+3.5
16+0.7
Float-Sink
1+0
1+0
60+0
<0.5
3+0
30+2.1
14+2.1
98+22
- -
5+0
24+0.7
34+7.1
22+J.4
38+8.5
- -
80+16.2
5+3.2
18+5.0
PPM Change
Meyers
Process
0.4+0.38
>5.6+0.4
+15+14.1
+0.4+0.65
0.6+0.60
63+2.8
+9+2.8
19+26.0
- -
4+4.2
35+1.5
8+2.9
+6+2.2
16+1.9
31+J4.2
Ind
24±3-5
14+2.9
Float-Sink
0.6+0.14
4.9+0.42
0+0
>0. 1+0.49
+1.2+0.35
70+3.5
+4+2.1
2+29
- -
7+4.2
18+1.0
+8+7.1
+10+1.6
+18+8.6
- -
>38
23+3.2
12+.5.7
I Loss
Meyers
Process
N.D.
>95+_l
N.D.
N.D.
N.D.
63+1
Gain
N.D.
-
33+23
83+3
31+1
Gain
84+7
-
Ind
86+12
47+5
Float-Sink
38+5
83+1
N.D.
N.D.
Gain
70+2
Gain
N.D.
-
58+J5
43+2
N.D.
Gain
Gain
-
Gain
82+>l
40+18
vo
tn
-------
Table F-5
TRACE ELEMENT ANALYSIS (PPM)
POWHATTAN NO. 4 MINE, PITTSBURGH NO. 8 SEAM, MONROE COUNTY, OHIO
Element
Ag
As
b
Se
Cd
Cr
Cu
f
Hg
Li
«n
Ni
Pb
Sb
Se
Sn
V
Zn
Individual Values
Raw Coal
0.7 1.0
A. 6 4.0
65 fin
3.6 3.0
1.1 1.4
130 143
24 26
281 282
0.07 0.07
53 51
56 58
3* 38
23 18
<1 7
53 54
<5 <5
56 65
40 39
Treated Coat
Meyers Process
2.0 2.0
-
87 87
2.3 2.3
1.0 0.5
82 86
31 19
219 216
-
48 46
16 16
32 22
225 215
2 <5
6 27
23 47
63 59
26 16
Float-Sink
1.0 0.5
2 2
50 50
1 3
4 2
•61 62
23 18
115 118
-
16 18
30 28
48 26
40 26
45 25
_
49 38
42 40
24 22
Raw Coal
0.8+0.21
4.3+0.42
62+3.5
3. 3+0; 42
1.2+0.21
141+2.8
25+0.4
282+0.7
0.07+0.00
52+1 .4
57+1.4
37+J.4
20+3.5
<6
54+0.7
<5
60+6.4
40+0.7
Average Values
Treated Coal
Meyers Process
2.0+0.00
-
87+0.1
2.3+0.0
0.8+0.35
84+2.8
25+8.5
218+2.1
-
47j+1.4
16+9
27+7.1
220+7.0
<1.5
16+14,9
35+17.0
61+2.8
21 +.7.1
Float-Sink
0.8+0.35
-
50+_1
2+1.4
3^1 A
62+0.7
20+3.5
116+2.1
- -
17+1.4
29+1.4
37+J5.6
33+9.9
35+14.1
- -
44+7.8
41+J.4
23+1.4
PPM Change
Meyers
Process
+1.2+0.21
-
+25+3.5
1+0.42
+1.8+1.4.
57+4.0
0+8.6
64+2.2
-
5+2.0
41+1 .4
10+7.2
+200+7.8
Ind
- -
>+30
+1+7.0
19+7.1
Float-Sink
0+0.41
—
12+3.6
1.3+1.5
0.4+0.41
79+2.9
5+3.8
166+2.2
- -
35+2.0
20+2.0
0+15.6
+13+10.5
>+30
- -
>+39
19+6.6
17+1.6
% Loss
Meyers
Process
Gain
-
Gain
30+9
N.D.
40+2
N.D.
23+1
-
10+4
72+1
27+19
Gain
Ind
-
Gain
N.D.
48+18
Float-Sink
N.D.
-
19+5
N.O.
Gain
56+1
20+15
59+.1
-
67+3
49+.S
N.D.
N.D.
Gain
-
Gain
32+8
42+4
vo
o>
-------
Table F-6
TRACE ELEMENT ANALYSIS (PPM)
DELMONT MINE, UPPER FREEPORT SEAM, WESTMORELAND COUNTY, PENNSYLVANIA
Element
Ag
As
B
Be
Cd
Cr
Cu
F
Hg
Li
Mn
Hi
Pb
St>
Se
Sn
V
Zn
Individual Values
Raw Coal
3.0 2.2
At) 41
15 20
4.0 4.3
1.7 2.0
lAfi 141
20 21
125 137
<0.2 <0.2
24 24
94 94
6fi 70
31 31
11 21
2fi 24
16 23
41 40
7fi 76
Treated Coal
Meyers Process
2.8 5.9
1 1
15 27
3.6 3.4
1.3 1.0'
75 87
20 22
126 131
-
23 24
10 12
35 45
27 47
4 5
<1 <1
9 21
46 48
35 30
Float-Sink
1 1
12 10
5 5
2 2
3 3
50 54
11 11
55 54
-
9 10
35 35
21 22
18 17
14 15
-
34 38
14 11
63 65
Average Values
Raw Coal •
2.6+0.57
40+0.7
18+3.5
4.2+0.21
1.8+0.21
144+3.5
20+0.7
131+8.5
<0.2
24+0
94+0
68+2.8
31+0
16+7.1
.25+1.4
20+5.0
40+0.7
76+0
Treated Coal
Meyers Process
4.4+2.19
1+0
21+8.5
3.5+0.14
1.2+0.21
81+8.5
21+1.4
128+3.5
-
24+0.7
11+1.4
40+7.1
37+14.1
4+0.7
<1
15+8.5
47+1.4
32+3.5
Float-Sink
1+0
11+0.7
5+0
2+0
3+0
52+1.4
11+0
54+0.7
- -
10+0.7
3.5+0
22+0.7
18+1.4
1.4+0.7
-
36+2.8
12+2.1
64+J.4
PPM Change
Meyers
Process
+ 1.8+2.3
39+0.7
+3+9.2
0.7+0.25
0.6+0.30
63+9.2
+1+1.6
3+9.2
- -
0+0.7
83+1.4
28+7.6
+6+14.1
12+7.1
- -
5+9.9
+7+1.6
44+3.5
Float-Sink
1.6+0.57
29+1.0
13+3.5
2+0.21
+1.2+0.21
92+3.8
9+0.7
77+8.5
- -
14+0.7
90+0
46+2.9
13+1.4
15+7.1
- -
+16+5.7
+16+5.7
12+1.4
% Loss
Meyers
Process
N.D.
98+1
N.D.
17+5
33+.14
44+6
N.D.
N.D.
-
N.D.
88il
41+1
N.D. •
75±12
- -
N.D.
Gain
58+5
Float-Sink
62+8
73+2
72+5
52+2
Gain
64+1
45+2
59+3
-
58+3
96+1
68+2
42+5
91+6
-
Gain
Gain
16+2
VO
-------
Table F-7
TRACE ELEMENT ANALYSIS (PPM)
MARION MINE, UPPER FREEPORT SEAM, INDIANA COUNTY, PENNSYLVANIA
Element
Ag
As
a
Be
Cd
Cr
Cu
F
Mg
Li
Mn
Ni
Pb
Sb
Se
Sn
V
Zn
Individual Values
Raw Coal
1.5 1.5
9.5 10.0
5.0 14.9
2.1 2.3
1.5 1.5
78 75
39 38
160 150
0.05 0.06
76 75
24 26
24 22
15 15
7 <5
50 30
5 <5
62 46
36 33
Treated Coal
Meyers Process
<1 <1
<.3 <.3
5.0 14.9
2.0 2.6
<0.5 <0.5
40 35
19 19
136 159
-
63 62
71 80
34 29
14 14
<5 <5
<5 <5
23 7
68 70
n 12
Float-Sink
<1 <:!
8 7
10 10
1 1
2 2
49 46
21 24
78 82
-
27 27
21 19
47 43
32 36
47 55
-
39 47
54 50
21 24
1.5+0.0
9.8+0.35
10+7.0
2.2+OJ4
1.5+0.0
76+2.1
38+0.7
155+7.1
0.06+0.014
76+0.7
25+1.4
23+J.4
15+0
<6
• _ ~
<5
54+11.3
34+2.1
Average Values
Treated Coal
Meyers Process
<1
<0.3
10+7.0
2.3+0.42
<0.5
38+3.4
19+0
148+16.3
-
62+0.7
7.6+0.64
32+3.5
14+0
<5
_ -
15+11.3
69+1.4
12+1.4
Float-Sink
<1
8+0.7
10+0.7
1+0
2+0
48+2.1
22+2.1
80+2.8
- -
27+0
20+1 . 4
45+2.8
34+2.8
51+5.7
_ _
43+5.7
52+2.8
22+2.1
PPM Change
Meyers
Process
>0.5
>9.5
0+10
+0.1+0.44
>1.0
38+4.0
19+0.7
7+17.8
- -
14+J.O
17.4+1.5
+9+3.8.
1+0
Ind
— —
>+io+n
+15+11.4
22+2.5
Float-Sink
>0.5
1.8+_.78
0+7
1.2+0.14
+.5+0
28+3.0
16+2.2
75+7.6
. .
49+0.7
5+2.0
+22+3.1
19+2.8
>45
_
>+38+_6
2+J1.6
12+3.0
* Loss
Meyers
Process
>33
97+4
N.D.
N.D.
>67
50+,5
50+1
N.D.
-
18+1
70+3
Gain
N.D.
Ind
_
Gain
Gain
65+5
Float-Sink
>33
18+8
N.D.
54+3
N.D.
37+3
42+6
48+3
-
64+1
20+^7
Gain
Gain
Gain
_
Gain
N.D.
35+.7
VO
CX5
-------
Table F-8
TRACE ELEMENT ANALYSIS (PPM)
LUCAS MINE, MIDDLE KITTANNING SEAM, COLUMBIANA COUNTY, OHIO
Element
Ag
As
b
Ee
Cd
Cr
Cii
F
Hg
Li
,'ln
N i
Pb
Sb
Sc
Sn
V
Zn
Individual Values
Raw Coal
2.0 2.0
72 75
20 20
3.6 3.9
1.5 1.4
53 52
13 13
63 67
-0.1 .-0.1
« R
17 13
35 35
IB 17
••5 <5
<5 16
5 16
11 9
ifi 55
Treated Coal
".eyers Process
2.1 2.1
8.5 12.9
20 25
3.6 3.7
1.9 1.0
26 28
16 17
56 59
-
5 6
7.7 5.4
33 21
18 14
6 6
2 3
•:5 8
19 15
14 16
Float-Sink
1 <1
14 15
20 20
3 3
3 3
'28 26
fi 7
43 41
-
4 5
10 9
30 20
27 19
7 5
-
23 14
5 12
25 33
Average Values
Raw Coal
2.0+0.0
73.5+2.1
20+0
3.8+0:21
1.4+0.07
52+0 . 7
13+0
65+2.8
-..1
8+0
15+2.8
35+0
18+0.7
-5
8+8.0
10+7.8
12+3.5
50+6.4
Traated Coal
Beyers Process
2.1+0.0
10.7+3.1
22+3.5
3.6+0.07
1,4+0.64
27+1.4
16+0.7
58+2.1
- -
6+0.7
6.6+1.63
27+8.5
16+2.8
6j_0
2+1.4
5+3.9
17+2.8
15+1.4
Float-Sink
<1
14+0.7
20+0
3+0
2+0 .7
27+J.4
8+0.7
42+1.4
- -
4+0.7
10+0.7
25+7.1
23+5.6
6+1.4
- -
18+6.4
10+5.0
29+5.6
PPM Change
heyers
Process
+0.1+0
60+2 . 2
+2+3.5
0.2+0.22
0.0+0.64
25+;. 6
+3+0.7
7+3.5
- -
2+0.7
8.4+3.2
8+8.5
2+2.9
>5
6+_8.1
5+8.8
+5+4.5
35+6.6
Float-Sink
>1
60+2.2
0+0
0.8+0.21
+0.6+0.7
25+1.6
5+0.7
23+3.1
- -
4+0.7
5+2.9
10+7.1
+5+_5.6
>5
- -
+8+10.1
2+_6.1
21+8.5
% Loss
Meyers
Process
N.D.
81+J
N.D.
N.D.
N.D.
48+3
Gain
11+5
-
25+9
56+14
N.D.
N.D.
N.O.
75+_30
N.D.
N.D.
70+5
f loot-Sink
>50
81+_1
N.D.
21+_4
N.D.
48+3
38+5
36+6
-
50+9
33+_13
29+20
N.D.
N.D.
-
N.D.
N.D.'
42+_13
10
10
-------
Table F-9
TRACE ELEMENT ANALYSIS (PPM)
BIRD NO. 3 MINE, LOWER KITTANNING SEAM, SOMERSET COUNTY, PENNSYLVANIA
Element
Ag
As
6
Be
Cd
Cr
Cu
F
Hg
Li
Mn
Hi
Pb
Sb
Se
Sn
V
Zn
Individual Values
Raw Coal
1.5 4.3
17.5 14.8
29.8 29.9
3.5 3.6
1.5 1.4
152 146
23 29
115 95
o.in n.in
63 45
46 44
35 36
26 20
16+1.9
14.8+0.10
1.0+.07
0.5+0.29
88+5.9
15+4.4
+10+15.2
-
9+13.4
36+1.8
2+14.8
+21+15.4
Ind
_
+5+15.0
+5+21.0
71+14.2
Float-Sink
1.9+1.98
12+1.9
27+. 21
+0.4+_.07
+0.1+_.70
93+4.2
10+4.3
57+14.1
-
38+12,7
25+2.5
+8+J4.9
1+6.5
>+39+8
_ _
+26+24
26+19.8
56+14.1
% Loss
Meyers
Process
N.D.
98+1
50+0.3
28+1
36+20
59+3
58+9
N.D.
-
N.D.
80+3
N.D.
Gain
Ind
_
N.D.
N.D.
89+3
Float-Sink
66+24
75+3
92+1
Gain
N.D.
62+J
38+10
54+6
-
70+7
56+5
N.D.
N.D.
Gain
_
N.D.
43+T9
70+5
ro
o
o
-------
Table F-10
TRACE ELEMENT ANALYSIS (PPM)
MEIGS MINE, CLARION 4A SEAM, MEIGS COUNTY, OHIO
Element
Ag
As
b
Be
Cd
Cr
Cu
F
Hg
Li
Mn
Ni
Pb
Sb
Se
Sn
V
Zn
Individual Values
Raw Coal
0.5 0.7
2.7 2.5
120 110
1.6 1J
0.8 0.7
99 100
24 22
220 224
0.04 0.06
22 23
40 49
20 23
12 13
16 <5
58 68
5 25
55 46
40 36
Treated Coal
Meyers Process
<1 <1
-
100 100
2.0 1.5
<0.5 <0.5
49 47
13 14
197 223
-
21 22
14 18
22 24
2 11
<5 <5
. <5 <5
32 23
41 42
10 8
Float-Sink
<1 <1
-
100 90
1 1
2 1
50 51
12 10
71 65
-
-
23 19
26 21
22 23
32 35
-
17 20
45 45
28 29
Raw Coal
0.6+0.14
2.6+0.14
115+7.1
1.4+0.35
0.8+.07
100+0.7
23+1.4
222+2.8
0.05+0.014
22.5+0.71
44+6.4
22+2.1
12+0.7
9+9.6
63+7.1
15+14.1
50+6.4
38+2.8
Average Values
Treated Coal
teyers Process
<1
-
100+0
1.8+0.35
<0.5
48+1.4
14+0.7
210+18.4
-
21.5+0.71
16+2.8
23+1.4
6.5+6.4
<5
<5
28+6.4
42+0.7
9+1.4
Float-Sink
<1
-
98+3.5
1+0
1.5+0.7
50+0.7
11+0.7
68+4.2
- -
11+0
21+2.8
24+3.5
22+0.7
34+2.8
- -
18+2.1
45+0
28+0.7
PPM Change
Meyers
Process
Ind
-
15+7.1
+ 0.4+.43
>0.3
52+1.6
9+1.6
12+18.6
- -
1+1.0
28+7.0
+1+2.5
5.5+6.44
N.D.
- -
+13+15.8
8+6.4
29+3.1
Float-Sink
<1
_
17+7.9
0.4+.35
+0.7+.70
50+_1.0
12+1.6
154+5.0
- -
12+_.7
23+7.0
+2+4.0
+10+1.0
+25+10
- -
+3+14.2
5+6.4
10+2.9
% Loss
Meyers
Ind
_
13+5
N.D.
>38
52+1
39+5
N.D.
-
N.D.
64+8
N.D.
N.D.
N.D.
-
N.D.
16+10
76+4
Float-Sink
Ind
_
15+6
29+J8
N.D.
50+1
52+4
69+2
-
51.+2
52+9
N.D.
Gain
Gain
-
N.D.
N.D.
26+6
ro
o
-------
Table F-ll
TRACE ELEMENT ANALYSIS (PPM)
KEN MINE, NO. 9 SEAM, OHIO COUNTY, (WEST) KENTUCKY
Element
Ag
As
B
Be
Cd
Cr
Cu
F
Hg
Li
Mn
Ni
Pb
Sb
Se
Sn
V
Zn .
Individual Values
Raw Coal
1.7 1.2
6.5 6.5
60 60
2.0 2.0
2.3 1.1
75 78
17 16
126 123
<0.2 <0.2
9 9
64 56
35 26
19 13
30 17
<5 <5
<5 21
32 38
40 39
Treated Coal
Meyers Process
1 2
0.5 0.5
60 60
3 3
1 <.5
37 35
12 12
87
-
10 10
5 5
16 17
4 4
29 40
_
4 4
22 19
19 15
Float-Sink
<1 <1
1 1
55 50
1 1
2 3
40 40
9 8
59 49
-
5 6
33 34
27 25
23 19
12 8
-
43 25
31 26
35 36
Raw Coal
1.4+0.35
6.5+0
60+0
2.0+0
1.7+0.8
76+2.1
16+0.71
124+2.1
<0.2
9+0
60+5.7
30+6.4
16+4.2
24+9.2
1+1.4
12+13.1
35+4.2
40+0.7
Average Values
Treated Coal
teyers Process
1.5+0.71
0.5+0
52+3.5
3+0
2.5+0.71
36+1.4
8+0.7
54+7.1
- -
10+0
5+0
16+0.71
4+0
34+7.8
- -
4+0
20+2.1
17+2.8
Float-Sink
<1
1+0
52+3.5
1+0
2+0.7
40+0
8+0.7
87
- -
6+0.7
34+0.7
26+1.4
21+2.8
10+3.5
- -
34+12.7
28+3.5
36+0.7
PPM Change
Meyers
Process
+0.1+0.79
6+0
8+3.5
+1+0
+0.8+1.1
40+2.5
8+1.4
70+7.4
- -
+1+0
55+5.7
14+6.4
12+4.2
+10+12
- -
8+13.1
15+4.7
23+2.9
Float-Mnk
>0.4+_.35
5.5+0
8+3.5
1+0
+0.3+J.1
36+2.1
8+1.4
37+7.4
- -
3+0.7
26+5.7
4+6.6
+5+5.0
14+9.8
- -
+22+18
7+5.5
4+1.0
* Loss
Meyers
Process
N.D.
92+0
13+6
Gain
N..O.
53+2
50+5
56+6
-
N.D.
92+1
47+J2
>5+7
N.D.
-
67+36
43+9
58+7
Float-Sink
28+17
85+0
13+6
50+0
N.D.
47+2
50+5
30+6
-
33+8
43+6
N.D.
N.D.
58+22
-
Gain
20+14
10+3
r>o
o
ro
-------
REFERENCES FOR APPENDIX F
15. American Public Health Association (APHA), American Water Works
Association, and Water Pollution Control Federation, "Standard
Methods for the Examination of Water and Waste Water," 13th ed.
16. Horowitz, W. ed., "Official Methods for Analysis of the Association
of Official Analytical Chemists," llth ed. "(1970).
17. ASTM Committees D-19 and D-23, "Water: Atmospheric Analysis,"
Part 23, D2972-71-T, "Tentative Method of Test for Arsenic in
Water," (1971), 859-61.
18. Angino, E. E. and G. K. Billings, "Atomic Absorption Spectrometry,"
in Geology Methods in Geochemistry and Geophysics. Elsevier
Publishing Co., New York (1967).
19. Rains, T. C. and 0. Menis, "Accurate Determination of Submicrogram
Amounts of Mercury in Standard Reference Materials by Flameless
Atomic Absorption Spectrometry," Analytical Chemistry Division,
National Bureau of Standards, Washington, D.C.
20. Wilson L., "The Determination of Cadmium in Stainless Steel by
Atomic Absorption Spectroscopy," Anal. Chim. Acta., 35, (1966),
123-126'.
21. Delgado, L. C. and D. C. Manning, "Determination of Vanadium in
Steels and Gas Oils," Atomic Absorption Newsletter, 5 (1), (1966).
22. Slavin, W., "Atomic Absorption Spectrometry," Interscience Publishers,
(1968).
23. Ramakushna, T. V., et al, "Determination of Copper, Cadmium and Zinc
by Atomic Absorption Spectroscopy," Anal. Chim. Acta., 37, (1967),
20-26.
24. Delgado, L. C. and D. C. Manning, "The Determination by Atomic
Absorption Spectroscopy of Several Elements Including Silicon,
Aluminum and Titanium in Cement," Analyst, 92 (Sept. 1967),
553-557,
25. Hatch, R. R. and W. L. Ott, "Determination of Sub-Microgram
Quantities of Mercury by Atomic Absorption Spectrophotometry,"
Anal. Chem. 40 (14), (Dec. 1968), 2085-2087.
26. Perhac, R. M. and C. J. Whelan, "A Comparison of Water-Suspended
Solid and Bottom Sediment Analysis for Geochemical Prospecting
in a Northeast Tennessee Zinc District," Journal of Geochemical
Exploration. 1. 47-53, (1973).
27 US Bureau of Mines, Report No. 7184, " Colon'metric Method for
Arsenic in Coal," No. 7184, (1968).
203
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REFERENCES FOR APPENDIX F (continued)
28. Fisher Technical Paper TD 142, "Reagent of Choice for Arsenic,"
TD 142, (1960).
29. Peterson, H. P. and D. W. Faranski,-Anal. Chem. 44(7), 1291, (1972).
30. Mair, J. W., Jr. and H. G. Day, "Curcumin Method for Spectrophotometric
Determination of Boron Extracted from Radio-Frequency Ash Animal
Tissues Using 2-Ethyl-l,3-Hexanediol," Anal. Chem. 44 (12) 2015-2017,
(Oct. 1972).
31. McFarren, E. F. , et al, Water Fluoride No. 3, Study No. 33, "Report
of a Study Conducted by Analytical Reference Service for the U.S.
Department of Health, Education, and Welfare," PB 215-504, (1969).
32. Kneip, J. J., et al, "Tentative Method of Analysis for Chromium
Content of Atmosp. Part. Matter by Atomic Absorption Spectres copy,"
Health Lab. Sci. . 10 (4), 357-361, (Oct. 1973).
33. Lishka, R. J. and E. F. McFarren, Water Trace Elements No. 2, Study
No. 26. "Report of a Study Conducted by the Analytical Reference
Service for the U.S. Department of Health, Education and Welfare,"
PB 218-501 (1966).
34. Peters, E. T., J. E. Oberholtzer and J. R. Valentine, "Development
of Methods for Sampling and Analysis of Particulate and Gaseous
Fluorides from Stationary Sources," Prepared for EPA by Arthur D.
Little under Contract 68-02-0099, PB 213-313, (November 1972).
35. "Instrumental Analysis of Chemical Pollutants," Training Manual
Published by Environmental Protection Agency Water Quality Office,
April 1971, PB 214-504.
36. "Determination of Hazardous Elements in Smelter-Produced Sulfuric
Acid," Prepared for EPA by Monsanto Research Corp. under Contract
68-02-0226, EPA 650.2-74-131, (Dec. 1974).
37. Tucker, G. H. and H. E. Malone, ^Atmospheric Diffusion of Beryllium,"
Final Report A/F Sys. Command AFRLP-TR-70-65, Vol. No. 1, 113,
(July 1971).
38. Baldeck, C. and G. W. Kalb, "The Determination of Mercury in Stack
Gases of High S02 Content by the Gold Amalgamation Technique,"
Prepared for EPA by TraDet, Inc., under Contract 68-02-0697,
PB 220-323.
204
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TECHNICAL REPORT DATA
(Hcne n* ImUiBCliau am IlK irvent ttfon t
. REPORT NO.
EPA-650/2-74-025-a
I. RECIPIENTS ACCISSIOKNO.
4. TITLE AND SUBTITLE
Applicability of the Meyers Process for Chemical
Desulfurization of Coal: Survey of 35 Coals
I. REPORT DATE
September 1975
I. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
J.W. Hamersma and M. L. Kraft
1 PERFORMING ORGANIZATION REPORT NO.
22234-6023-RU-00
I. PERFORMING ORGANIZATION NAME AND ADOREM~
Systems Group of TRW, me.
One Space Park
Redondo Beach, CA 90278
10. PROGRAM ELEMENT NO.
13: ROAP 21ADD-096
|11. CONTRAcT/flRANT NO.
J8-02-0647
12. SPONSORING AGENCY NAME AND AOORESS
EPA, Office of Research and Development
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
IIX TYPE OF REPORT AND PERIOD COVERED
final
14. SPONSORING AGENCY CODE
18. SUPPLEMENTARY NOTES
is. ABSTRACT The report details experimentation on the application of chemical cleaning
(desulfurizatton) technology to a variety of U.S. coals. Run-of-mine coal samples
were collected from 35 U.S. coal mines in 13 states. Each sample was treated
separately by the Meyers process for selective chemical removal of coal-pyrite and
by float-sink procedures for physical coal cleaning. Raw and chemically treated coals
were examined for sulfur distribution as well as for selective trace element distri-
bution and other process characterizing features, such as heat content and ash
changes and leaching agent residuals. Comparisons of physical and chemical impacts
on sulfur reductions are discussed.
7.
KEY WORM AND DOCUMENT ANALYSIS
DESCRIPTORS
k. IDENTIFIERS/OPEN ENDED TEM
f. COSATI
Air Pollution
Coal
Coal Preparation
Desulfurization
Sulfur
Pyrite
Trace Elements
Air Pollution Control
Stationary Sources
Meyers Process
Chemical Cleaning
Ferric Sulfate Extraction
Float-Sink Fractionation
13B
8G, 21D
81
7A
7B
'*. DISTRIBUTION STATEMENT
Unlimited
t»-7»
tiTHc
JnclMSified
ao. sieuRifV CLAM <++**•>
Unclassified
».PMICC
205
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