TFRT.-RTP-I115 TECHNICAL REPORT DATA
(Please read Instructions on the reverse be fore completing)
1. REPORT NO, 2.
EPA—600/7—81 —m ft
3. RECIPIENT'S ACCESSION-NO.
EBC1-1525'30
4, TITLE AND SUBTITLE
Planning Study To Model and Monitor Coal Pile
Runoff
5. REPORT DATE
FEBRUARY 1981 ISSUING DATE.
6. PERFORMING ORGANIZATION CODE
7. AUTHOR(S)
G. T. Brookman, J. A. Ripp, P.B.Katz, B.C.Middle-
sworth, and D. K. Martin
S. PERFORMING ORGANIZATION REPORT NO.
S. PERFORMING ORGANIZATION NAME AND ADDRESS
TRC-Environmental Consultants, Lie.
125 Silas Deane Highway
Wethers fie Id, Connecticut 06109
10. PROGRAM ELEMENT NO.
C2GN1E
11. CONTRACT/GRANT NO.
'68-02-3115, Task 104
12. SPONSORING AGENCY NAME AND ADDRESS
EPA,' Office of Research and Development* ""
Industrial Environmental Research Laboratory
Research Triangle Park, NC 27711
13. TYPE OF REPORT AND PERIOD COVERED
Task Final; 6/79-7/80
14. SPONSORING AGENCY CODE
EPA/600/13
is. supplementary notes jerl-RTP project officer is D.Bruce Harris, MD-62, 919/541-
2557. Cosponsor is Edison Electric Institute, 1111 Nineteenth St. , NW. Washington.
DC 20036
is. abstract rep0rj. describes a planning study for predicting and monitoring the
hydrologie and chemical characteristics of effluent streams resulting from precip-
itation impacting on open storage of coal. It includes; a survey of utilities on storage
habits and treatment systems for coal pile runoff, the development of a runoff model,
a work plan to field test the model, and procedures for the field program. The sur-
vey includes information from 81 plants on size, shape, and handling practices for
coal stocks and criteria used to design coal pile runoff treatment. The model devel-
oped in this program is in two sections; a hydraulic model TRCH20 and a quality
model TRCCOAL. The model is capable of describing the surface and interior reac-
tion in the coal pile as well as in the groundwater. A sensitivity analysis of several
model parameters is also provided.
17. KEY WORDS AND DOCUMENT ANALYSIS
a. DESCRIPTORS
b,IDENTIFIERS/OPEN ENDED TERMS
c. cos ati Field/Group
Pollution Leaching
Coal Storage Field Tests
Utilities Pyrite
Runoff
Water Treatment
Mathematical Models
Pollution Control
Stationary Sources
Reactive Modeling
Non-point Sources
13B 07D,07A
081 14B
08G
08H
12 A
IS. DISTRIBUTION STATEMENT
Release to PubEe
l
18. SECURITY CLASS (ThisReport)'
¦Unclassified
21. MQ. OF PAGES
20. SECURITY CLASS (Thisp&
Unclassified
22. PBICE
EPA Form 2220-1 (S-73)
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DISCLAIMER
This report has been reviewed by the Industrial Environ-
mental Research Laboratory (RTF), U.S. Environmental
Protection Agency, and approved for publication. Approval
does not signify that the contents necessarily reflect the views
and policies of the Agency, nor does mention of trade names
or commercial products constitute endorsement or recommen-
dation for use.
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CONTENTS
Figures . . .
Tables
Acknowledgements .
1. Introduction .......... .
2. Executive Summary ............
3. Utility Questionnaire Survey of Coal Piles and
Runoff Treatment Systems .............
Introduction ..............
Summary . .......
Questionnaire Tabulations
General Plant Information . .
General Coal Pxle Data*
Reserve/Non-Segregated Coal Piles ........
Physical Characteristics
Coal Characteristics. . . ......
Active or "Live" Coal Piles .
Physical Characteristics. ... . .
Coal Characteristics
Coal Pile Runoff Treatment System Design. . . . .
Conclusions ...............
4. Coal Pile Runoff Model
Introduction
Physical/Chemical Phenomena to be Addressed
in the Coal Pile Drainage Model .........
Quantitative Phenomena
Qualitative Phenomena .... .....
Coal Pile Drainage Model Development. ..... .
Modifications to the OSU Models
OSU Version of Stanford watershed Model
Refuse Pile Model
Technical Aspects of the TRCH20 Hydrological
Model for Coal Pile Drainage
Coal Pile Responses to Precipitation
Surface Phenomena ... .....
Direct infiltration
Delay Infiltration
Interior Phenomena. ..............
In-Pile Moisture. ..............
Interflow ..... .......
Ground Water Phenomena. ............
Input Data Requirements of TRCH20 ........
Site Specific Data
Meteorological Data ........
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CONTENTS (Continued)
Plotter Data 40
Basic and Optional Output of TRCH20 . . 48
Basxc Outputs 48
Optional Outputs 48
Technical Aspects of the TRCCOAL Model. ....... 49
Dry Weather Reactions ... ...... 49
Wet Weather Reactions ............... 53
Option EXPO 54
Input Data for TRCCOAL. 54
Output of TRCCOAL ......... ... 59
Sensitivity Analysis. ................ 59
TRCH20 - Quantitative Model . . 59
CB — Infiltration Index 59
LZSN - Pile Moisture Storage Capacity ...... 61
KK24 Baseflow Recession Constant. ....... 61
IRC - Daily Interflow Recession Constant. .... 61
GWS - Current Value of Ground Water
Slope Index 61
TINC - Selected Time Routing interval 66
TRCCOAL — Qualitative Model 66
DEPTH - Depth of Reactive Surface
of Coal Pile. ................. 66
RATEPY - Rate of Pyrite Oxidation ........ 69
FACDIR — Factor for the Amount of
Pollutants Going into Direct Runoff ...... 69
PERPS" - Percentage of Praraboidal Pyrite
In Coal 73
AK - Exponential Washoff Factor for Acid 73
Shortcomings and Limitations of CPD Model ....... 73
TRCH2Q. ' . . 76
Coal Pile Hydrology 76
Snowmelt 76
Infiltration 76
Evaporation ..... 76
Precipitation ...... . 77
TRCCOAL 77
Uses of the CPD Model in Treatment Design 78
Computing Requirements 78
5. Field Work Plan 80
Introduction. ..... .... 80
Selection of Representative Plant Sites ....... 83
Initial Site "Visit . 84
¦ Selection of Sampling Sites 85
Selection of Locations for Installation of
Meteorological Station and Field Laboratory
Trailer ....... 85
Acquisition of Background Data 86
Preliminary Site Work 89
Acquisition of Representative Coal Samples. .... 89
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CONTENTS (Continued)
Phase I - Sampling for Determination of
Coal Variability. ....... ... 89
Phase II - Sampling of Coal for Precision .... 90
Field Testing of Coal Pile Characteristics. .... 90
Physical Measurements and Visual Observations ... 90
Coal Pile Hydrology Testing ............ 90
Ground Water Field Tests. ... 91
Laboratory Testing of Coal Samples 92
Physical Testing 92
Phase I Variability Testing 92
Phase II Variability Testing 92
Framboidal Pyrite Analysis. « 92
Sulfur Analysis ..... 92
Trace Metal Chemistry 93
Acquisition of Background Data Not Attainable
at Site 93
Design of Field Program ............... 94
Parameters to be Analyzed ....... 94
Numbers of Samples and Sampling Frequency 96
Sampling, Flow Monitoring, and Meteorological
Equipment 97
Plan for Shipping Samples for Laboratory
Analysis 99
Laboratory Analysis ..... .. 99
Data Reduction and Presentation 101
Program Costs and Time Schedule ........... 108
Manpower Requirements . 108
Other Direct Costs .108
Time Schedule Ill
6. Field Procedures Manual ................ 113
introduction. .................... 113
General Rules of Conduct. .............. 113
Training of Field Technicians 114
Acquisition of Representative Coal Samples. ..... 118
Phase I - Sampling for Determination of
Coal Variability. ......... 118
Phase II - Collection of Coal Samples for
Precision 118
Coal Pile Hydrology and Ground Water Tests. 118
Coal Pile Hydrology Tests ............. 119
Ground Water Tests. 119
Site Setup (Equipment Installation) . 119
Utility Assistance ................ 120
Flow Monitoring Station ..... 122
Runoff Monitoring Station . 125
Meteorological Station ........ 126
Mobile Field Laboratory ......... 127
Daily Equipment Status Checks 129
Calibrations. 129
Status Checks and Equipment Maintenance 130
Dry Weather Sampling 130
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CONTENTS (Continued)
Wet Weather Sampling. 133
Anticipation of a Storm Event 133
Event Sampling 134
Sample Identification and Custody Procedures 135
Number of Sampling Stations and Sample
Identification. . . . 135
Sampling Custody Procedures ..... 136
Sample Shipping Procedures 136
Sample Preservation Procedures and Field
Laboratory Analyses . . ...... 142
Sample Preservation . . . 142
Compositing Samples ...... ..... 142
Filtration Method for Dissolved Metals and
Dissolved Mercury ...... 144
' Preserving Samples. ........ 144
Field Laboratory Analyses ............. 146
References
Appendices
A. Coal Fired Power Plant Questionnaire For Assessment of
Coal Stocks and Treatment Design of Coal Pile Runoff
B.. Standard Methods for Collection of A Gross Sample of Coal
C. Standard Test Method for Total Moisture in Coal
D. Standard Test Method for Infiltration Rate of Soils in
Field Using Double-Ring Infiltrometers
E. Standard Method of Sieve Analysis of Coal
F. Standard Test Method for Ash in the Analysis Sample of
Coal and Coke
G. Standard Test Methods for Total Sulfur in the Analysis
Sample of Coal and Coke
H. Analyses Performed in the Mobile Field Laboratory
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FIGURES
Number
1 Plants that Responded to Coal Pile Questionnaire . .
2 Plant Capacity (MW) Vs Tons Coal Stored (I) .....
3 Schematic of Hydrologic Cycle, OSU" Version of
Stanford Watershed Model . . .
4 Schematic of Hydrologic Cycle Coal Storage Pile . . .
5 Block Diagram for TRCH20 ..............
6 Block Diagram for TRCCOAL ...
. 7 Example Sensitivity Analysis,
CE-Inf iltration Index ................
8 Example Sensitivity Analysis,
LZSN-Pile Moisture Storage
9 Example Sensitivity Analysis,
KK24—Baseflow Recession . .
10 Sensitivity Analysis, IRC-Daily
Interflow Recession. Constant . .
11 Sensitivity Analysis, GWS-Ground Water Slope . . . .
12 Sensitivity Analysis-Simulation Time Intervals . . .
13 Example Sensitivity Analysis DEPTH ...
14 Example Sensitivity Analysis RATEPY .
15 Example Sensitivity Analysis FACDIR ..........
16 Example Sensitivity Analysis PBRPY .........
17 Example Sensitivity Analysis AK ....
18 Coal Pile Runoff Data Requirements at Individual
Sites
19 Example of Historical Meteorological Data Plots . . .
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figures (Continued)
Number Page
20 Example of Runoff Hydrograph. and
Hyetograph Plots ........ 106
21 Example of Runoff Hydrograph and Continuous
Measurement Data Plots ....... .... 107
,.22 Estimated Time Schedule for Runoff Program
(Per Utility Site) 112
23 ¦ Schematic of Coal Pile Runoff Monitoring Station . . . . 121
24 General Schematic of a Par shall Flume . . 123
25 Schematic of Flume and "V" Notch Weir Flow Station .¦. . 124
26 Schematic for a 20' x 8* Mobile Field Laboratory
for Analysis of Coal Pile Runoff Water V 128
27 Daily Equipment Status Check List .. 131
28 Sample Log Sheet 137
29 Initial Sign In Sheet .......... 138
30 Request for Water Analysis 139
31 Sign Out Sheet 140
32 Report of Water Analysis ..... .. 141
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TABLES
Page
Distribution of Generating Capacities of
Plants Responding to the Questionnaire 6
Distribution of Percentages of Coal Usage for
Electricity Generation ... 8
Distribution of Coal Pile Construction Bases .... 8
Distribution of Reserve/Non-Segregated
Coal Pile Sizes 11
Distribution of Reserve/Won-Segregated
Coal Pile Densities ................. 11
Distribution of Rcserve/Non-Segregated
Coal Pile Heights 11
Distribution of Reserve/Non-Segregated
Coal Pile Slopes . . 12
Distribution of Reserve/Non-Segregated
Coal Storage Durations ......... 12
Distribution of Plants with Reserve/Non-Segregated
Coal Piles Composed of Coal From One or More States . 13
Sulfur Content of Reserve/Non-Segregated
Coal Piles 13
Pyritie Sulfur Content of Reserve/Non-Segregated
Coal Piles ........ ....... 13
Distribution of % Ash in Coals Comprising
Reserve/Non-Segregated Piles ............ 14
Distribution of % Moisture in Coals Comprising
Reserve/Non-Segregated Piles ............ 14
Distribution of btu Values of Reserve/Non-Segregated
Coals 14
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tables (Continued)
Page
Distribution of Active Coal Pile Sizes 15
Distribution of Active Coal Pile Densities ..... 15
Distribution of Active Coal Pile Heights ...... 15
Distribution of Active Coal Pile Slopes 16
Distribution of Active Coal Pile Storage Durations . . 16
Distribution of Plants With Active Coal Piles
Composed of Coal From One or More States ...... 16
Sulfur' Content of Active Pile -Coals 17
Pyritic Sulfur Content of Active Pile Coals ..... 17
Distribution of % Ash in Coals Comprising
Active P x le s 17
Distribution of % Moisture in Coals Comprising
Active Piles .. ....... 18
Distribution of BTO Values of Active Pile Coals ... 18
Distribution of Plants by
Treatment Methods Employed . 19
-Distribution by Year of Treatment System
Start Dp 19
Distribution of Design Storm Criteria 19
Design Storm References ...... 20
Distribution of Runoff Coefficients (From Rational
Formula) Used in Treatment System Design . .20
Number of Plants Treating Specified Chemical
Parameters 20
Number of Plants and the Parameters Monitored . . . . 21
Libraries, Universities, and Others Contacted
by TRC for Coal Pile Drainage Study ......... 24
Input Data - Site and Calendar - TRCH2G 41
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TABLES (Continued)
Number • - . .Page
35 Meteorological Data 44
36 . Input Data - Plotter - TRCH20 45
37 TRCCOAL - Input Data Calendar Parameters ...... 55
38 TRCCOAL - Input Data Adjustment Parameters ....... 56
39 TRCCOAL - Input Data Site Specific Parameters . . . . 58
40 Summary of Results of the Sensitivity
Study - TRCH20 ................... 60
41 Site Selection Matrix for the Monitoring of
Coal Pile Runoff . 84
42 Coal Extraction and Analytical Procedures 93
43 Pollutant Parameters to be Analyzed During
Field Program and Minimum Volume Required 95
44 Types of Field Data for Digitization and Frequency
of Gerber Readings .... ...... 102
45 Estimated Manpower Requirements for Runoff Program . 109
46 Estimated Equipment Rental and Purchase
Costs and Other Direct Costs for Runoff Program . . . 110
47 Summary of Utility Assistance Items In Order to
Monitor Coal Pile Runoff ....... 122
48 Checklist for Mobile Field Laboratory ........ 129
49 Frequency of Calibrations and Field
Calibration Checks .......... 130
50 Storm Types to be Samples With Corresponding
Sample Frequency ...... ...... 134
51 Sample Volumes, Parameters to be Analyzed,
Preservation Methods, and Maximum Holding Times . . . 143
52 Sample Storage Bottles and Corresponding Parameters . 145
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ACKNOWLEDGEMENTS
For helping in the acquisition of background materials for the model;
Dr. Vincent T. Ricca
Ohio State University
Columbus» Ohio 43210
Eugene Harris
Extraction Technology Branch
U.S. EPA - Industrial Environmental Research Laboratory
Cincinnati, Ohio 45268
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SECTION 1
INTRODUCTION
In August 1979, TRC began Phase I of a multiphased effort to predict
the quantity and quality of coal pile runoff from utility sites. The
Phase I effort commenced with an intensive literature search to scope the
desired model capabilities, review the most recent developments -in treat-
ment and characterization of coal pile runoff, and assess the theoretical
research in quantifying and qualifying coal pile runoff. Based on the
information gathered in the literature search, TRC outlined a model
structure able to predict both volume and quality of drainage from any
coal storage area. Along with the model format an outline was developed
for the field monitoring program which will provide input as well as
verification data to the model.
This report concludes the Phase I effort by presenting the following:
1. The results of the questionnaire sent to members ¦ of the Edison
Electric Institute in which recent coal pile characteristics and
coal pile runoff treatment systems information was gathered.
Refer to Section 3.
2. A report on the Model Development task. Refer to Section 4.
3. A detailed Field Work Plan, which itemizes those tasks necessary
to describe the physical, chemical and hydrologic character-
istics of a coal pile, the meteorological conditions contingent
to that pile, and the framework for conducting an intensive
runoff sampling program. Refer to Section 5.
4. A Field Procedures Manual which details all the steps necessary
'to monitor coal pile runoff'from the training of field personnel
to the analysis of runoff samples. Refer to Section 6.
This report will be used as the foundation for Phase II of the
program, the Modeling and Monitoring of Coal Pile Runoff.
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SECTION 2
EXECUTIVE SUMMARY
This report on the Phase I - Planning Study to Model and Monitor Coal
Pile Runoff is the culmination of approximately ten months of effort to
pave the way in predicting and monitoring the hydrologic and chemical
characteristics of the effluent streams resulting from precipitation
impacting on open storage of coal. Through the continuing interest and
technical guidance of the Utility Water Action Group (UW&G) Committee and
later the Environmental Protection Agency/Edison Electric Institute
Technical Advisory Committee set up to monitor this program, ' a plan of
action has been formulated to study coal pile runoff mathematically using
a recently developed predictive model and analytically through actual
field testing. The recommendations, observations and criticisms of many
of the researchers in previous coal pile runoff field programs have been
incorporated into this plan. A major concern of previous investigators
has been that individual runoff studies had failed to acquire important
data on site meteorology, coal characteristics and pile characteristics
so' that comparisons of data between different runoff streams could be
made. The plan detailed in this report synthesizes these concerns and
allows for a program which, when applied nationally, will produce viable
data to be used for engineering design of treatment works for coal pile
runoff.
. The report on Phase I is divided into four, major sections, each of
which may be considered a separate document in itself.
Section 3 is a Report on the questionnaire circulated to members of
the Edison Electric Institute requesting information on their coal stock-
piles and treatment systems for runoff. The questionnaire was strictly a
voluntary document and the response was noteworthy. A total of 30
utilities representing 81 plants responded. Useful information on the
size, shape, slope and handling practices for coal stocks was gathered.
Ranges of values for many parameters describing each pile were collected
including proximate analysis of the coals, mining origin, cleaning
practices and coal storage practices. This data which comprised the
first part of the questionnaire was and will be used to determine how the
coal pile at a prospective utility site fits into the overall pattern of
coal piles. The second part of the questionnaire dealt with the design
criteria used for treatment design of coal pile runoff. ' The information
gathered showed that the common practice of designing for the 10 year -
24 hour storm is widely used. Treatment for runoff appears to be aimed
at the most economical method for neutralizing the acidity and lowering
the suspended solids content. For the TVA system and many others this
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means directing all runoff into the ash ponds. Few utilities treat for
metals, oil and grease or organics removal. Containment for storm flows
are for the majority designed according to the 'Rational Formula*. Also,
less than half of the utilities monitor their coal pile runoff and those
which do monitor only pH and suspended solids.
Section 4 is the report on the Model Development Task. It describes
the physical/chemical phenomena and data requirements needed to describe
the quantity and quality of the runoff.' Examples of these include pre-
cipitation, snownielt, percolation, pyrite oxidation and gully erosion.
A summary of the model development is included with a' description of
the Ohio State University Model which served as the basis for the runoff
model. TRC modified the OSU model extensively to describe the surface
and interior reaction in the coal pile as well as in the groundwater.
The final version of this model resulted in a pair of co-models, one
describing the hydraulic characteristics of the runoff, labeled TRCK20
and the other describing the quality of the runoff, labeled TRCCOAL. The
hydraulic model can be used separately for predicting runoff volumes but
the runoff quality model relies on the routines of the hydraulic model
for predicting pollutant loadings. The most signficant algorithms of
each are discussed in detail. Input requirements for the model as well
as example outputs are presented.
This section discusses the sensitivity analysis of selected para-
meters in both co-models which was conducted to determine the data having
the most impact on the results. A discussion is also presented on the
model's limitations and shortcomings and its use in treatment design.
Finally, the hardware and software requirements to run the model are
outlined.
Section 5 presents the Field Work Plan to be used as a guidance
document for carrying out the field monitoring program. It details the
data requirements necessary for inputs to the model and those data
requirements for comparison of runoff from coal piles' of various locales
and climatic regions. The plan includes the basic scope of work to be
followed to collect the data, to format the data and present the data. A
general schedule is outlined for conducting the field work along with
manpower requirements and anticipated other direct costs. Actual costs
were not calculated since these will be contingent on the location of the
utility sites.
Section 6 is a Draft Field Procedures Manual that will be revised
once the field program has been enacted. As closely as practicable, it
itemizes those procedures necessary to carry out a field monitoring
program in coal pile runoff. It is intended to be a working document
which may be utilized by anyone with a certain amount of technical
training in water pollution field monitoring to conduct a field program
which will supply comparable data on a particular coal pile. Procedures
listed include everything from training of site technicians to field
analysis of solids and acidity. Illustrations are presented to assist in
the visualization of a monitoring station and field laboratory.
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SECTION 3
UTILITY QUESTIONNAIRE SURVEY OF COAL PILES
AND RUNOFF TREATMENT SYSTEMS
INTRODUCTION
The Environmental Protection Agency (EPA) in conjunction with the
Edison Electric Institute (EEI) has contracted TRC-Environmental
Consultants, Inc. to conduct a program to model and monitor the quantity
and quality of coal pile runoff from utility sites. As part of Phase I
of this project, the planning phase, the necessary data relating to coal
types, stockpile sizes, regional meteorology, and control strategies were
identified as parameters important to planning a field testing program.
To compile recent (1979-1980) information necessary to both plan a
field study and to be used for predictive modeling, TRC conducted an
independent poll of coal-burning utilities owning plants with a
generating capacity greater than 25 megawatts (MW). TRC compiled the
questionnaire to include data pertinent to the design of a field sampling'
program. Review of the data received will be used in the selection of
representative sites for the field sampling program.
In early November 1979, the Edison Electric Institute sent the TEC
questionnaire to member utilities and requested a quick response. A copy
of the questionnaire is found in Appendix A.
A total of thirty utilities responded to the questionnaire, ' five of
which do not operate coal fired plants and do not store coal on-site.
One utility has two plants which do not currently operate coal-fired
units, however, they do store coal on-site in the event that they will be
required to convert the existing units.
TRC received completed or partially completed questionnaires from
eighty-one plants with 109 bituminous coal piles. The quality of com-
pleteness of the information was variable, and in data compilation, the
number of questionnaires with no response to a specific question was
noted.
TRC also received completed questionnaires from three plants burning
lignite and one plant burning subbituminous coal. The information
supplied by these plants was not used in the tabulations for this report.
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TRC will report the information collected from the questionnaires
back to the responding companies so that the exchange of technology on
coal pile runoff treatment may be continued.
SUMMARY
ft total of 81 responses to the coal pile/runoff treatment question-
naire was used in tabulating the data. From the data received, mean
plant operating characteristics, coal pile characteristics, and treatment
methods were determined.
Of the 81'plants, 19 plants segregate the active and reserve piles.
One point of interest was the possible relationship between coal segre-
gation and rotation of the coals. The responses indicate that segre-
gation of the piles does not influence the practice of rotating stored
coal.
Coal is compacted at 79 plants. One plant reports compaction of the
reserve coal only, while the remaining 78 compact both active and reserve
coals. Two plants do not compact the coal. Partial or complete coal
cleaning is conducted at 42 plants? 27 plants do not clean the coal; 12
plants did not respond.
. The mean reserve coal pile size is 332,400 tons (range 404-2x10®
tons) compared with 249,400 tons (range 2703-2x10® tons) for the mean
active pile. The coal piles at 50 plants are heterogenous mixtures of
coals from several states. Coals from' 12 states have been reported as
sources, with Kentucky coals the most common.
Mean sulfur content of the reserve/non—segregated piles is 1.75%
(range 0.45-4.1%); mean sulfur content of the active pile's is 1.98%
(range 0.48-4.1%). Pyritic sulfur contents of the reserve/non—segregated
piles and the active piles are 0.75% (range 0.06-2.05%) and 0.96% (range
0.38-2.05%), respectively.
A variety of treatment systems is employed at the plants, including
diversion to ash ponds, chemical or polymer- addition, oil skimmers, and
flow equalization ponds. The systems at three plants are not yet
on-line. Seven plants do not treat coal pile runoff.
. . Total suspended solids are treated at 59 plants, pH at 53 plants,
metals at 19 plants, and oil and grease at 17 plants. Flow equalization
is employed at 37 plants. Twenty—eight plants monitor TSS concentrations
while 42 plants monitor pH. Other parameters monitored include flow, oil
and grease, iron and sulfur. Forty-five plants do not conduct any
monitoring of coal pile runoff.
One utility reports that three of its plants store lignite on-site.
The plants operate both active and reserve piles; the active piles are
not compacted, while the reserve piles are compacted. The coal in the
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piles is riot cleaned and the plants do not rotate the coal. The reserve
piles range in volume from 112,000 tons to 422,380 tons. The live piles
range from 7,750 tons to 162,250 tons. The plants have not designed
systems specifically for treating the runoff from the lignite piles,
however, the coal piles are diked. The runoff from the plant areas is
treated for total suspended solids by polymer addition. The three plants
do conduct monitoring of runoff and groundwater pH, conductivity,
precipitation, iron, total suspended solids, 'sulfates, chlorides, total -
dissolved solids and ground water level.
One utility has a plant that burns sub-bituminous coal and maintains
both active and reserve piles. The coals in the active piles are not
compacted while the coals in the reserve pile are compacted. The coals
are cleaned in both the active and the reserve piles. The active storage
piles contain 90,800 tons; the reserve pile contains 1.8xl06 tons of
sub-bituminous coal. A treatment system has been designed for coal pile
runoff at this plant. It is also used to treat the runoff from ash
handling areas. The piles are diked with the runoff directed through
Parshall flumes. The runoff is treated for total suspended solids by
liquid alum addition. The plant monitors precipitation, runoff pE,
temperature, conductivity, and bacterial concentrations.
QUESTIONNAIRE TABULATIONS
General Plant Information
Thirty utilities (comprising 85 plants) responded to the question-
naire. Their regional distribution is shown in Figure 1. Of the thirty
utilities, five do not operate coal-fired plants and do not store coal
on-site. One utility operates two plants which do not currently burn
coal, however, they have coal stockpiles on-site'in anticipation of coal
conversion requirements. The data from these two plants were used in the
tabulations. Not used in the tabulations was the information supplied by
the plants burning sub-bituminous 'and lignite coals.
The tables below contain the information dealing with general plant
characteristics, such as generating capacity, coal usage, and coal pile
base construction.
TABLE 1. DISTRIBUTION OF GENERATING CAPACITIES' OF
PLANTS RESPONDING TO TEE QUESTIONNAIRE
Capacity (MW) : Number of Plants
<100
100 - 500
501 - 1000
1001 - 1500
1501 - 2000
& 2000
No Response
Mean = 782 MW
Range = 35-3160 Mff
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20
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1119-015
FIGURE 1:
plants that responded to
COM PILE QUESTIONNAIRE
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TABLE 2. DISTRIBUTION OF PERCENTAGES OF COAL USAGE
FOR ELECTRICITY GENERATION
Coal Usage (%) Number of Plants
100 51
80-99 9
60-79 5
40-59 2
20-39 2
0 2
Variable 1
No Response 9
TABLE 3. DISTRIBUTION OF COAL PILE CONSTRUCTION BASES
Base Type Number of Plants
Clay 29
Compacted Coal 16
Compacted Ash, Slate, Bony, etc. 10
Compacted Ash 8
Clay &. Compacted Coal 5
Compacted Slag - * 3
Compacted Earth 1
Sand 1
Cinders 1
Clay, Slate, Shale 1
Sand & Gob Coal 1
Gravel 1
Solid Limestone 1
No Response 3
Figure 2 shows the distribution of plant capacity vs tons of coal
stored. As can be seen from the figure, the majority of the plants store
less than 500,000 tons of coal and their generating capacities are less
than 1000 MW.
General Coal Pile Data
Twenty-five utilities operate a total of 110 coal piles at 81
plants. Information was provided for 109 coal piles and organized 'into
non-segregated/reserve or active pile categories. A non-segregated pile
8
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1119-014
3000
vo
<_>
«c
2000
[n
1000
100 200 500 1000 1500 2000
TONS STORED(THOUSANDS)
FIGURE 2: PLANT CAPACITY (MW) VS TONS COAL STORED (T)
-------
is one in which both active usage and reserve storage occur within the
same pile, rather than maintaining a separate pile for active use and a
separate pile for reserve storage.
Eighty-nine piles at 62 plants are non-segregated or reserve piles.
Twenty-one piles are live or active at 19 plants. The plants that do not
separate active and reserve piles report . lack of adequate storage space
as a reason for non-segregation. For ten plants, their proximity to the
source mine accounts for non-segregation.
Eighty-seven of the 89 reserve piles are compacted; 12 of 20 active
piles are compacted. Compaction information was lacking for 21 active
coal piles.
The response to coal cleaning is as follows:
Of the plants that segregate their live and reserve piles, 4 plants
rotate the coal. Six plants that do not segregate the live and reserve
coal practice rotation. This indicates that segregation does not
influence the practice of coal rotation.
Reserve/Non-Segregated Coal Piles
Physical Characteristics—
Information relative to coal pile size, volume, and storage duration
is necessary for the selection of representative plant sites for the
field sampling phase of this study. In addition, coal pile slopes and
degrees of compaction (density), will influence the rates and volumes of
runoff generated. Tables 4 through 8 summarize the information collected
on pile size, volume, density, and other physical characteristics.
Coal Characteristics-
Information on the sources of coal used and stored on-site was
requested from the utilities. The degree of specificity varies widely -
from no response to the exact seam, county, and state. Only the coal
source states were tabulated because of the wide variability in responses.
No cleaning
No response
Coal cleaned
Partial cleaning
16 plants
26 plants
27 plants
12 plants
10
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TABLE 4. DISTRIBUTION OF RESERVE/NON-SEGREGATED
COAL PILE SIZES
Size
(1000 tons)
Number of Piles
<50
50 - 100
101 - 500
501 - 1000
>1000
Mean = 332,400 tons
Range = 404 - 2x10® tons
17
13
35
20
4
TABLE 5. DISTRIBUTION OF RESERVE/NON-SEGREGATED
COAL PILE DENSITIES
Density Range (tons/yd ) Number of Piles
0.1 1
0.1 - 0.49 24
0.5 - 0.89 17
0.9-1.19 16
£1.2 11
Mean = 0.80 tons/yd^
Range = 0.08 - 4.19 tons/yd3
TABLE 6. DISTRIBUTION OF RESERVE/NON-SEGREGATED
COAL PILE HEIGHTS
Height (ft) Number of Piles
5-15 10
16-30 29
31-50 21
>51 ft 5
Variable Height 11
Conical 1
No Response 13
Mean = 31 ft
Range = 8.8 - 85 ft
11
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TABLE 7. DISTRIBUTION OF RESERVE/NON-SEGREGATED
COAL PILE SLOPES
Slope Number of Piles
0.025 - 0.05 11
0.06 - 0.10 5
0.11 - 0.25 5
0.26 - 0.50 8
0.51 - 0.75 6
0.76 - 1.0 16
>1.0 4
Variable 10
Ho response 23
Mean = 0.63
Range = 0.025 — 5
TABLE 8. DISTRIBUTION OF KESERVE/NON-SEGREGATED
COAL STORAGE DURATIONS
Storage Time (Month)
Number of Piles
1 month
,1-1.9
2.0 - 2.9
3.0 - 3.9
4.0 - 4.9
5-12
12
Variable
No response
Mean = 3.9 months
Range = 1 day to 30 months
1
25
23
6
2
1
12
8
11
The plants report using coal from 12 states, with Kentucky coal the
most common component of the coal piles. West Virginia and Ohio are the
next most commonly reported source states. All coal piles are composed
of the coal from one or more states. The distribution is as follows:
12
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TABLE 9. DISTRIBUTION OF PLANTS WITH RESERVE/NQN-SEGREGATED
COAL PILES COMPOSED OF COAL FROM ONE OR MORE STATES
Number of Source States Number of Plants
1
2
3
4
Multiple
No Response
31
15
9
6
6
14
The following tables list the distributions? ranges ^ and ave r300
values of the various reserve/non-segregated coal characteristics. This
information was requested so that data from the future field sampling
study can be used to determine whether any correlations exist between the
concentrations of pollutants in the runoff and the characteristics of the
coal stored.
TABLE 10. SULFUR CONTENT OF RESERVE/NON-SEGREGATED
COAL PILES
% Sulfur Number of Coals
0.45 - 1.0 39
1.1 - 2.0 37
2.1 - 3.0 31
Z.3.1 14
No Response 10
Mean = 1.75%
Range 0.45 - 4.11
TABLE 11. FYRITIC SULFUR CONTENT OF RESERVE/NON-SEGREGATED
COAL PILES
% Pyritic Sulfur
Number of Coals
0.1
2
0.1 - 0.3
5
0.31 - 0.5
3
0.51 - 1.0
3
>1.0
7
No Response
109
Mean = 0.75%
Range 0.06 - 2.05%
13
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TABLE 12. DISTRIBUTION OF % ASH IN COALS COMPRISING
RESERVE/NON—SEGREGATED PILES
% Ash Number of Coals
4.0 - 9.9 40
10.0 - 14.9 67
>15.0 14
' No Response 10
Mean =11.0%
Range 4.3 ~~ 19%
TABLE 13. DISTRIBUTION OF % MOISTURE IN COALS COMPRISING
RESERVE/NON—SEGREGATED PILES
% Moisture Number of Coals
4.0 - 9.9
10.0 - 14.9
15.0 - 20.9
>_21.0
No Response
Mean = 10.1%
Range 4.5 - 25%
55
12
6
8
50
TABLE 14. DISTRIBUTION OF BTU VALUES OF RESERVE/NON-SEGREGATED
COALS
Heat Value (BTU/lb) Number of Coals
9,000 - 9,999 8
10,000 - 10,999 15
11,000 - 11,999 41
12,000 - 12,999 46
13,000 - 13,999 10
>14,000 1
No Response 10
Mean = 11,700 BTU/lb
Range 9,000 - 14,000 BTU/lb
Active or "Live" Coal Piles
Physical Characteristics—
The following tables contain information on the physical character-
istics of the active or "live™ coal piles, including height, size,
density, and slope.
14
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TABLE 15, DISTRIBUTION OF ACTIVE COAL PILE SIZES
Size
(1000 tons)
Number of Piles
<50
8
50 - 100
2
101 - 500
5
501 - 1000
4
1000
1
No Response
1
Mean = 249,400 tons
Range 2703 - 2xlG6 tons
TABLE 16. DISTRIBUTION OF ACTIVE COAL PILE DENSITIES
Density (tons/yd3) Number of Piles
$0.1 1
0.1 - 0.49 5
0.5 - 0.89 ' 7
0.9 - 1.19 2
>1.2
No Response 6
Mean = 0.63 tons/yd3
Range 0.05 - 1.16 tons/yd3
TABLE 17. DISTRIBUTION OF ACTIVE COAL PILE HEIGHTS
Height (ft) Number of Piles
5-15 1
16-30 6
31-50 7
51 2
Variable -
Conical -
No Response 5
Mean = 35.8 ft
Range 13.5 - 80 ft
15
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TABLE 18. DISTRIBUTION OF ACTIVE COAL PILE SLOPES
Slope ; Number of Piles
0.025 - 0.05 1
0.06 - 0.10
0.11 - 0.25 ¦ 3
0.26 - 0.50 3
0.51 - 0.75 6
0.76 - 1.0 5
>1.0 1
Variable 1
No Response 1
Mean =0.64
Range =0.04-1.5
TABLE 19. DISTRIBUTION OF ACTIVE COAL PILE STORAGE DURATIONS
Storage Time (Month) Number of Piles
1 . 6
1-2 3
3-4 3
5-9 2
10-12 1
No Response 6
Mean = 2.8 months
Range = 1 day - 12 months
Coal Characteristics—
The same types of information that were requested on the reserve/
non-segregated pile coal were requested for the active or "live" pile
coal. The tables that follow summarize the data on coal comprising the
active coal piles.
TABLE 20. DISTRIBUTION OF PLANTS WITH ACTIVE COAL PILES
COMPOSED OP COAL PROM ONE OR MORE STATES
Number of Source States Number of Plants
1 7
2 5
3 3
4 -
Multiple -
No Response 6
16
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TABLE 21. SULFUR CONTENT OF ACTIVE PILE COALS
% Sulfur Number of Coals
0.45 -1.0 10
1.1 - 2.0 5
2.1 - 3.0 12
3.1 7
•¦No Response 2
Mean = 1.98%
Range = 0.48 - 4.1%
TABLE 22. PYRITIC SULFUR CONTENT OF ACTIVE PILE COALS
¦ % Pyrite Sulfur Number of Coals
< 0.1 -
0.1 - 0.3 2
0.31-0.5
0.51 - 1.0 1
>1.0 4
No Response 28
Mean = 0.96%
Range = 0.38 - 2.05%
TABLE 23. DISTRIBUTION OF % ASH IN COALS COMPRISING
¦ ACTIVE PILES
% Ash ; Number of Coals
4.0 - 9.9 7
10.0 - 14.9 25
>15.0 2
No Response 3
Mean = 14.3%
Range = 4.6 - 17.7%
17
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TABLE 24. DISTRIBUTION OF % MOISTURE IN COALS COMPRISING
ACTIVE PILES
% Moisture : Number of Coals
4.0 - 9.9 14
10.0 - 14.9 4
15.0 - 20.9 1
£121.0 2
No Response 6
Mean = 10.4%
Range = 4.6 - 23.961
TABLE 25. DISTRIBUTION OF BTU VALUES OF ACTIVE PILE COALS
Heat Value (BTU/lb) Number of Coals
9,000 - 9,999 2
10,000 - 10,999 6
11,000 - 11,999 11
12,000 - 12,999 12
13,000 - 13,999 1
114,000 1
No Response 4
Mean = 11,640 BTU/lb
Range = 9,000 — 14,000 BTU/lb
Coal Pile Runoff Treatment System Design
Of the 85 plants that responded to the questionnaire, . 72 plants
report having some type of coal pile runoff treatment system. The tables
that follow summarize the reported information on treatment system types,
basis for design, date of system startup, parameters treated, etc.
As can be seen from the tables presented above, a number of systems
are employed for runoff treatment. ¦ One-half of the plants that responded
(41 plants) have separate treatment systems for coal pile 'runoff.
Twenty-five plants combine coal pile runoff with other plant discharges
prior to treatment. Fifteen plants did not respond to this question.
At 27 plants, one type of treatment is employed, diversion of the
runoff to an ash pond. At 47 plants a combination of treatment methods
are used. These combinations include chemical addition and diversion to
a sedimentation pond, oil skimmer, chemical addition, and diversion to a
sedimentation pond.
18
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TABLE 26. DISTRIBUTION OF PLANTS BY TREATMENT METHODS EMPLOYED
Treatment Type
Number of Plants
Sedimentation Pond
Dikes or Ditches
Ash Pond Only
Chemical Addition
Ash Pond and Other
Equalization Pond
Polymer Addition
Clarifier
Oil Skimmer
Filtration
Percolation Pond
Centr if ligation
Sump
Grit Chamber
No Treatment
Treatment
31
38
26
28
10
9
4
5
15
4
1
1
10
4
7
TABLE 27. DISTRIBUTION BY YEAR OF TREATMENT SYSTEM
START UP
Year Nuraber of Plants
1967 - 1976 6
1977 37
1978 3
1979 13
No Response , 12'
No Treatment 7
Not yet in Service 3
TABLE 28. DISTRIBUTION OF DESIGN STORM CRITERIA
Storm Type : Number of Plants
10 yr - 24 hr 50
100 yr 1
1 yr - 24 hr. and 10 yr - 24 hr 1
No Treatment 7
No Response 22
19
-------
TABLE 29. DESIGN STORM REFERENCES
Reference Number of Plants
National Weather Service Technical
Paper #40 ' 24
Local Data 13
Other 5
No Response 39
TABLE 30. DISTRIBUTION OP RONQFF COEFFICIENTS (FROM RATIONAL
FORMULA.} USED IN TREATMENT SYSTEM DESIGN
Runoff Coefficient Number of Plants
0.2 1
0.25 , 1
0.55 1
0.7 1
0.73 2
0.75 12
1.0 3
0.1 -1.0 1
0.5 -1.0 3
TABLE 31. NUMBER OF PLANTS TREATING SPECIFIED CHEMCIAL
PARAMETERS
Parameter • Number of Plants
Total Suspended Solids
60*
pH
53**
Oil and Grease
17
Metals
19
Flow Equalization
37
Organics
0
*7 Plants treat only total suspended solids
**4 Plants treat only pH
20
-------
TABLE 32. NUMBER OP PLANTS AND THE PARAMETERS MONITORED
Parameter Number of Plants
Total Suspended Solids
25
pH
38
Flow
21
Oil and Grease
17
Other*
11
No Monitoring
45
*Qther includes - bacterial populations.
iron, sulfur, ground
water level, ground water quality
CONCLUSIONS
It is apparent that, to meet the effluent - limitations for pH and
suspended solids, most utilities have incorporated some form of.treatment
to their runoff from coal piles. From the responses to the question-
naire, it is shown that 85% of the plants responding have some form of
treatment. Recently obtained information for the 12 Tennessee ¦ Valley
Authority coal fired plants is not included in the summaries.
The design criteria for collecting the coal pile runoff for the
majority of plants is the 10 year - 24 hour storm taken from either local
data or the National Weather Services' Technical Paper #40. By using the
'Rational Formula' the runoff coefficients for these plants has been
estimated. The Rational Formula relates rainfall and peak runoff. The
formula is Q = CIA, where Q is the peak discharge (cfs) , C is a runoff
coefficient depending on drainage basin characteristics, 'I is rainfall
intensity (inches/hour), and A is drainage area (acres).
The above facts clearly indicate that most utilities are relying on
unsophisticated and untested techniques to design a coal pile runoff
treatment system. Once the proposed program to actually field monitor and
model the quantity and quality of runoff begins, the historical criteria
for runoff treatment design will be challenged. With accurate field
monitoring of precipitation, runoff flow, runoff coefficients and runoff
quality, the field data will be compared directly with the historic
design criteria. It is anticipated that the field testing will take
place at one or more sites which have been included in this survey and
have treatment systems already installed. This program should begin in
the fall of 1980.
21
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SECTION 4
COAL PILE RUNOFF MODEL
INTRODUCTION
In August 1979, TRC began Phase I of an intensive two .to three year
effort to predict the quantity and quality of coal pile runoff from
utility * sites. The thrust of the program is to develop and validate
mathematical modeling techniques that could be used to characterize coal
pile runoff in a dynamic model; i.e., predict the quantity and quality of
coal pile runoff within a storm event. This simulation can then be used
to design a treatment system (Best Management Practice) based on the
changing conditions of the runoff during the storm. Recent studies1
completed by TRC indicate that during a 10-yearr 24-hour design storm the
initial coal runoff is "dirty" but after a few hours the runoff becomes
"clean". Therefore, why not store and treat the "dirty" water 'and bypass
the "clean" water. The model can also be modified to characterize the
runoff from other material storage piles.
The program is divided into two phases. ¦ Phase I is to scope the
desired model capabilities, to initiate model development, and to design
a field measurements program that will acquire representative data for
model modification and validation. Phase II is to conduct the field
program and to modify and develop the model to reflect the field measure-
ment program results. Phase I was initiated in August 1979.
This section of the Phase I report outlines the development of the
Coal Pile Drainage (CPD) Model by TRC. Discussed in the report are:
1) Physical/chemical phenomena included in the CPD Model
2) The base model used and modifications made
3) The sensitivity analysis of model parameters
4} Shortcomings/limitations of the CPD Model
5) Field data required by the CPD Model
'6) Suggestions for using the output in treatment system design
PHYSICAL/CHEMICAL PHENOMENA TO BE ADDRESSED IN THE COAL PILE DRAINAGE
MODEL
In 1977 TRC completed a study of sampling and modeling of non-point
sources at a coal-fired utility. In this application, TRC utilized the
22
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Short Stormwater Management/RECEIV-Il Model (SSWMK-RECEIV-II) to address
sheet washoff from coal storage piles. At the completion of this
modeling program TRC identified a number of shortcomings in the
SSWMM-RBCEIV—II Model. For example, the model could not address:
1) storm erosion of material from the coal storage pile
2) stormwater percolation through the coal pile
3) pyrite oxidation/acid production in the coal pile
As part of Phase I TRC undertook an extensive literature search of
coal pile drainage. The universities, institutes, and libraries con-
tacted are listed in Table 33? particularly valuable was the Bituminous
Coal Research Library in Monroeville, Pennyslvania. In this search TRC
determined what physical/chemical phenomena associated with coal piles
have been researched and would be • valuable in characterizing coal pile
drainage in a modeling effort. The phenomena can be divided into quan-
titative and qualitative aspects.
Quantitative Phenomena
The quantitative pheonomena addressed by the model are:
1) Precipitation (rain/snowfall). The model should require several
years of meteorological data or selection of a design storm(s)
for use in runoff simulation.
2) Surface Runoff/Infiltration. The model should have mechanisms
to address infiltration into the coal pile as well as runoff-
from the surface. While some urban runoff models consider the
phenomena of exponentially decreasing infiltration, this is not
thought appropriate to coal storage piles.
3) Pile Percolation/Interflow/Moisture. While many previous model-
ing efforts have been concerned with only the surface of a
watershed, the percolation of rainfall and snowmelt through a
material storage pile is also significant. This internal flow
is responsible for eruptions from the sides of the coal pile as
well as drainage from the base of the pile. These flows usually
continue after the precipitation has ceased and usually carry a
more concentrated stream of pollutants than does surface
runoff. Some moisture is retained in the coal storage pile on a
continual basis. TRC evaluated models to address these
phenomena.
4) Snowmelt. While snowmelt is more significant In . the runoff
pattern of large watersheds, it should also be considered for
coal storage piles in the northern climates. TRC researched
23
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TABLE 33. LIBRARIES, UNIVERSITIES, AND OTHERS CONTACTED BY TRC FOR COAL
PILE DRAINAGE STUDY
1) Appalachian Resources Project 9)
University of Tennessee
Environmental Center
Knoxville, TN
10)
2) Atlantic Research Corp.
Alexandria, VA
3} Canadian Institute of Mining 11)
Montreal? Quebec, Canada
4) Coal Research Bureau 12)
University of West Virginia
Morgantown, W. VA
13)
5) Army Corps, of Engineers
Hydrologic Engineering Center
Davis, CA 14)
6} National Coal Association
Washington, DC 15)
7) National Coal Board 16)
London, England
8) NYSEG
(New York State Electric & Gas)
Larfs i nc, NY
17)
)ak Ridge National Laboratory
Environmental Sciences Division
Oak Ridge, TN
Ohio State University
Water Resources Center
Columbus, OH
SCS (Soil Conservation Service)
Mansfield, CT
Tennessee Valley Authority
Chattanooga, TN
Tennessee Valley Authority
Kingston, TN
University of Kentucky
¦Lexington, KY
U.S. Bureau of Mines
U.S. EPA
Industrial Environmental Research
Laboratory
Extraction Technology Branch
Cincinnati, OH
Bituminous Coal Research Library
Monroeville, PA
24
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several snowmelt routines to be incorporated in a runoff model
which would not require extensive input data,
5) Ground water Infiltration. Some rainfall and snowmelt percolate
through the coal pile into the ground water. The amount of
rainfall entering the ground water depends on several factors
including the permeability of the material underlining the coal
pile. In addition, when the water table i rises to the surface,
it impacts the flow at the base of the pile. The model should,
therefore, consider ground water.
Qualitative Phenomena
A number of chemical and physical reactions occur in the coal pile
which affect the characteristics of the runoff. The simulation of these
phenomena, as discussed below, is important:
1) ' Pyrite Oxidation/&cid Production
During non-rainfall periods pyrite in coal, especially fram-
boidal pyrite, oxidizes, producing acid, iron, and sulfates.
The acid further ¦ reacts, dissolving trace materials in the
coal. During rainfall events or snowmelt, dissolved materials
which have accumulated are distributed to the direct runoff,
interflow through the pile, baseflow, and ground water.
2) Freeze—Thaw Factor
During alternating cycles of freezing and thawing coal lumps
expand, contract, and subsequently break up, exposing more
reactive surface area. The freeze-thaw cycles subsequently
increase the production of dissolved materials which character-
ize the runoff.
3) Gully Erosion
Coal piles are subject to gully erosion and . the subsequent
transport of solids into the runoff stream. The volume of coal
solids detached and deposited at the pile base is related to the
slope of the coal pile, the slope length, and rainfall intensity
and duration, as well as a coal erosion coefficient.
4) Coal Pile Washoff
A portion of the accumulated dissolved materials washes off
immediately during rainfall by the direct runoff. Some of the
base load of pollutants also remains. The model user should be
able to select a linear or exponential decay function to express
the washoff phenomena.
25
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COAL PILE DRAINAGE MODEL DEVELOPMENT
TRC researched the existing runoff models to ascertain which one
could best be utilized as the basis for TRC coal pile drainage simulation
effort. Pew models have been developed to describe industrial stormwater
runoff situations and none specifically for material storage piles. A
description of the more pertinent models researched is shown below:
1) Stormwater Management Model (SWMM)2
SWMM simulates single or multiple storm events on the basis of
rainfall hyetographs and a spatial 'description of the catchment
and sewer routing system. The model was 'developed under' EPA to
represent the quantity and quality of urban runoff. The current
version of SWMM, "Release 2", includes an additional component
for erosion prediction using the Universal Soil Loss equation.
TRC also modified a version of SWMM to address the washoff from
coal piles. Although SWMM does address the sheet washoff
phenomena adequately, it cannot address percolation through a
pile or the chemical reactions that take place in the pile.
2) Storage, Treatment, Overflow, and Runoff Model (STORM) 3
This runoff model was developed by Water Resources Engineers,
Inc., for the U.S. Army'Corps of Engineers. Its primary purpose
was to aid in the selection of storage and treatment facilities
to control the quantity and quality of runoff. ' STORM is a
continuous simulation model and has subroutines•for snowmelt and
land erosion, but has the same shortcomings as SWMM in relation
to handling storage piles.
3) Agricultural Runoff Management Model (ARM)4
The model was developed by Hydrocomp, Inc. to simulate runoff,
snow accumulation and melt, sediment loss, pesticide-soil
interactions, and soil ¦ nutrient transformations from agricul-
tural lands. ARM simulates sediment transport through rill and
sheet erosion but not gully erosion as may be found on coal
piles.
4) Pyritic Systems5
The EPA pyritic systems model simulates acid mine drainage in
underground mines. While the model addresses acid production
and removal, it is limited in scope and'has little applicability
to coal pile drainage.
' 5) Ohio "State Model^
The OSU version of the' Stanford Watershed Model was published
initially in 1972 and updated several times. • The OSU watershed
model simulates the hydrologic cycle of a rural area pictured in
Figure 3. Features are included in the model for interception
26
-------
1119-017
ho
^4
UPPER ZONE STORAGE=£
INTERCEPTION
^Ci^^Sjtranspiration
EVAPORATION
LI
ion—==F====-~'
INFILTRATION
PERCO
ATION
•SOIL MOISTURE
WATER TABLED
PRECIPITATION f ^
INTERCEPTION PLUS
DEPRESSION STORAGE
DEPRESSION
OVERLAND FLOV^ STORAGE
SURFACE DETENTION
INTERFLOW ^ EVAPORATION
LOWER ZONE STORAGE
GROUND WATER FLOW— TO STREAM
TO
DEEP
STORAGE
FIGURE 3: SCHEMATIC OF HYDR0L0GIC CYCLE,OSU VERSION OF STANFORD WATERSHED MODEL
-------
of rainfall by vegetation, transpiration, infiltration into the
soil, percolation, evaporation, overland flow, soil moisture,
depression storage, and ground water flow to deep storage. All
runoff is directed to a stream channel.
While the OSD version of the Stanford Watershed Model considers
hydrology, it does not simulate the chemical constituents
associated with runnoff. For coal applications, OSD developed
qualitative strip mine and refuse pile models to be used in
conjunction with the OSU version of the Stanford Watershed
Model. The surface of the pile is considered the upper zone.
Rainfall percolates into a lower zone, the interior of the
pile. From the lower zone the flow is routed toward deep ground
water storage or to the stream channel. The only chemical
parameter simulated in the OSU model is acidity.
The OSU models use a magnetic tape or data cards of several
years of hourly site meteorological data as input. This input
must be developed by the user.
TRC selected the Ohio State University (OSU) version of the Stanford
Watershed Model and the Ohio State University co-model for coal refuse
piles as a basis for TRC s coal storage pile developmental work.
TRC utilized the 1977 version, made available through the Extraction
Technology Branch of the U.S. EPA.
MODIFICATIONS TO THE OSU MODELS
OSU Version of Stanford Watershed Model
While TRC utilized the OSU model as a base for its model development,
a number of modifications were made. These are summarized below:
'1) Deletion from the watershed model of all calculations related to
the interception of rainfall by vegetation
2) Deletion of evapo-transpiration by vegetation
35 Substitution of a. less complex snowmelt routine requiring less
input data and using hourly temperature data
4} Deletion of lake evaporation
5) Deletion of streamflow diversion
6) Inclusion of a routine to count the number of freeze-thaw cycles
28
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7) Deletion of routines related to impervious surfaces
8) Calculation of average daily rainfall and average daily air
temperature
9) Deletion of several output options
10} Addition of the simulation of gully erosion on the coal pile
Refuse Pile Model
For the refuse pile model, the following modifications were made;
1) Addition of the simulation of pyrite oxidation and acid pro-
duction with the subsequent release of dissolved iron, sulfate,
and trace materials during rainfall events
2) ¦ Addition of an exponential decay function as an optional method
of simulating the pollutant washoff from the surface of the coal
pile
3} Use of the number of freeze-thaw cycles during the preceding dry
periods to escalate the production of dissolved pollutants
4} Consideration of the acxdxty of rainfall and alkalinity of coals
5} ' Use of a variable time interval for wet weather modeling
6) Plotter output of qualitative data
As a major modification, TEC altered the model so that a standard
National Climatic Center (NCC) magnetic tape #CD144 could be utilized for
the input of hourly meterological data. These tapes are available for
most U.S. Weather Service Stations from the NCC for under $100 (Spring
1980)-
TBC's versions of the QSU coal storage pile models are termed:
1) TECH20 - hydrologic model
2) TRCCOAL - qualitative model
They are described in detail in the following sections.
29
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TECHNICAL ASPECTS OF THE TECH20 HYDROLOGICAL MODEL FOR COAL PILE DRAINAGE
The coal storage pile is viewed in the model as a small' unvegetated
watershed with many features similar to larger watersheds. A schematic
diagram of the hydrologic cycle of a coal pile is shown in Figure 4.
Coal Pile Responses to Precipatation
Surface Phenomena—
The TRCH2Q model reads hourly precipitation data in the form of rain
or snow from the input meteorological tape. The' phenomena of direct
infiltration, gully erosion, delay infiltration, .direct runoff, snow
accumulation, and snowmelt are hydrologic surface reactions to precipi-
tation.
The amount of rainwater which immediately enters the pile is known as
direct infiltration. It is dependent upon input factors of pile moisture
and pile surface moisture storage capacity as well as time and adjustment
factors. Some rainwater is retained by depressions in the coal pile
surface and this infiltration is delayed. The depression storage- is
considered to be the upper zone of the coal pile, and the amount of
depression storage on the pile surface is estimated by 'the -model user.
The entire coal pile is considered pervious.
The equations in the model for infiltration are developed below;
1) Direct Infiltration
D4F = Current peak infiltration rate
D4F = FRAC * CB/2.0**LNRATM ; (4-1)
FRAC = Selected routing interval (TINC) converted to
fraction of an hour
CB « infiltration index
lnratm = pile ¦ moisture index used in- estimating current
infiltration rate. It is calculated from ratio
of pile moisture to pile moisture storage index,
LNR&T
2) Delay Infiltration .
PRE = Fraction of incoming moisture that is not retained in
upper zone storage
ERE = (1.0/1.0 + DZI) ** UZI (4-2)
UZI = - Intermediate pile surface moisture - storage parameter
UZ-I = 2.0 * ABS (UZS/UZSN - 1.0) + 1.0 (4-3)
30
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1119-016
PRECIPITATION
UPPER ZONE STORAGE = DEPRESSION STORAGE
DEPRESSION
STORAGE
EVAPORATION
DIRECT RUNOFF
NFILTRATION
LOWER ZONE
STORAGE
PILE MOISTURE
INTERFLOW
PERCOLATION
DIKE
DIKE
BASE FLOW
RUNOFF
STREAM
RUNOFF.
STREAM
WATER TABLE
GROUND WATER
TO DEEP STORAGE
FIGURE 4: SCHEMATIC OF HYDROLOGIC CYCLE COAL STORAGE PILE
-------
UZSN =
Pile surface moisture index
UZSN = CX * EXP (-2.7 * LNRAT) (4-
CX = Index for estimating pile surface moisture storage
(4-4)
LNRAT= Current ratio of pile moisture to pile moisture
storage index
LNRAT= LZS/LSZN
(4-5)
LZS = Current pile moisture storage
LZSN = Pile moisture storage index
P4 = rainfall that is depleted from pile surface
P4 = PR * PRE
(4-6)
PR = Current rainfall
PES = See equation 4-2
UZS = current pile surface moisture storage
UZS - UZS + PR - P4
(4-7)
The rainwater which does not infiltrate into the coal pile becomes
direct runoff- The Chezy-Manning equation for turbulent flow was
utilized in the model to derive this relationship. Input variables are
slope of the coal pile, length of the slopes, and a roughness coefficient.
Based on the Manning equation, the overland flow discharge off the
coal pile is:
Where q is flow in ft3/sec/ft, S = slope in ft/ft, and where y is
the flow depth in feet at the base of the coal pile.
In addition to rainwater, the model considers the effect"of snow .on
the coal pile. The model reads the meterological tape and determines the
amount of snow which falls on the coal pile. The snow pack ' accumulates
over time, and snow is converted to its liquid component by snowmelt. In
this model snowmelt is estimated by the air temperature above freezing
and a degree—day melt factor. Once snow is melted, it is handled in the
model as rainwater for infiltration and runoff purposes.
The snowmelt equation developed from work by J. A. Anderson? and
used in the model is:
q = 1'466 y5/3 S3-/2
(4-8)
n
32
-------
SMELT = RMELf * (TEMPH-32) (4-9)
SMELT = snowmelt, inches
RMELT = degree day melt factor
TBMPH = hourly air temperature, °F
The impact of rain on the coal pile, causes solids to erode and
creates gullies on the side of the coal pile. Using measured data on
pile slope, length, and rain intensity, as- well as erosion coefficients,
the Foster-Meyer equation^ calculates the pounds of coal solids moved
to the base of the pile per day during a day with rainfall.
The formulations based on the Poster-Meyer erosion' equation are
described below:
GFXW = lb/day of eroded coal solids at base per foot of gully width
GFXW = TBANSK*C1*(1.-(1.-L*SOILK/TRANSK*(P1SUM(I)/12**2.G)/C1)L*DETACH/
THANSK) *EXDEC (4-10)
TRANSK
SOILK
P1SUM
DETACH
CI
transport capacity coefficient
coal surface constant •
total daily rainfall, inches
detachment coefficient
YDEPTH * SS ** 1.5
(4-11)
YDEPTH = depth of runoff flow, feet
SS = slope of coal pile, feet per foot
EXDEC = 1. - EXP (-L*DETACH/TKANSK)
(4-12)
Interior Phenomena —
The moisture which percolates from the upper zone of the pile is
stored in the lower zone. Some of the moisture erupts from the side of
the coal pile and is termed interflow. In addition, some moisture per-
colates through the pile to the ground water. The amount of rainwater
which emerges as interflow is proportional to the -amount of rainwater
which infiltrates from the surface, the current in-pile moisture storage,
and adjustment coefficients. These equations for interflow and in-pile
moisture are given below:
.15 in-Pile Moisture
RECE = current rate of pile surface moisture infiltration
RECE = 0.003*CB*UZSN*DEEPL**3.0 (4-13)
33
-------
CB = infiltration index
UZSN = pile surface moisture index
DEEPL — (UZS/UZSN) — (LZS/LZSN)
(4-14)
QZS = current pile surface moisture storage
UZSN = pile surface moisture index
LZS = current pile moisture storage
LZSN = pile moisture storage index
The fraction of moisture that infiltrates from the upper zone and is
retained in the lower zone is computed by:
PRE = fraction of incoming moisture retained in pile storage
PRE = (1.0/1.0 + LZI))**LZI (4-15)
LZI = intermediate pile moisture parameter for estimating
infiltration
LZI = ' 1.5*AB5 (LNRAT - 1.0) + 1.0 (4-16)
LNRAT = current ratio of pile moisture storage to pile
moisture storage index
2) Interflow
C3 = variable controlling entry of moisture into interflow
C3 = CY*2.0**LNRAT (4-17)
CY = interflow index
LNEAT!= . current ratio of pile moisture storage to pile
moisture storage index
Outflow from interflow storage is computed by: .
INTP = current rate at which interflow is entering runoff
channel
INTF = LIRC4 * SKGX (4-18)
LIEC4 = natural logarithm of interflow recession constant
SRGX - current volume of water in interflow storage
34
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Ground Water Phenomena —
While some water is retained in the coal pile# some infiltrates to the
interface that consists of the layer immediately beneath the coal pile.
For the purposes of the model, moisture in this layer is termed ground
water, and moisture below the interface is deep storage. The moisture
into ground water can be routed to deep storage or emerge from the base
of the pile as a flow stream. The amount of seepage or baseflow from the
pile is dependent upon the ground water storage, the ground water slope,
and flow recession constants. Infiltration into the ground water
increases the slope and the resulting base flow emerging from the coal
pile.
Percolation to deep, inactive ground water storage or ground water
flow out of the basin is modeled by allowing a fixed portion of inflow to
ground water storage to bypass the active storage that contributes to
seepage. The equations for ground water flow are given below:
GWF = Baseflow
GWF = SGW * LKK4 * (1.0 + LKV4 * GWS) (4-19)
SGW = Ground water moisture storage
SGW = SGW + Fl (4-20)
F1 = infiltration reaching ground water from lower zone storage
Fl = (1.0 - PRE) * (P4 - SHKD) * (1.0 - K24L) (4-21)
PRE = see equation 4-2
P4 = see equation 4-6
SHRD = sum of current moisture entering surface runoff plus interflow
K24L.= parameter indicating ground water entering deep storage
PI = infiltration reaching ground water from the upper zone
Fl - (1.0 - PRE) * RECE * (1.0 - K24L) (4-22)
RECE = see equation 4-13
LKK4 = natural logarithm of hourly base flow recession constant
LKV4 = natural logarithm of hourly base flow recession adjustment
factor
GWS = current value of ground water slope index
ft block diagram of the TRCH20 model is shown in Figure 5.
Input Data Requirements of TRCE20
The data required to run the hydrologic model TRCH2G consists of three
parts:
35
-------
Read and Write Oetai
Starm Data
Calculate Ground Water
Flow
Read Detail
Storm Hydrograph
Axis Data
Initialization of
Snow Variables
Calculate Surface
Calculate Recession
Constants
Plotting the Detail
Storm Hydrograph Axis
Labeling Ordinate of
Runoff Hydrograph
Initial ization
REAL
INTEGER
DIMENSION
LOGICAL
COMMON
Read Input
Including:'
Options, Pile Moisture
Parameters, Erosion and
Interflow Parameters,
and Groundwater Parameters
Hydrograph Axis Data
FIGURE 5: BLOCK DIAGRAM FOR TRCH20
36
-------
1119-004
Calculate Pile Surface
Moisture Storage Index
i ~~
Plotting or Rainfall
Distribution as Used
in the Model
I
Call Subroutine OYIOOP
(see Page 4)
Reading in Frozen and
Liquid Precipitation,
Air Temperature
T
Call Subroutine ARITHP
if OKN (17](= 1
(see Page 7)
Call Subroutine ARIiH
if DKN (17) = 1
(see Pace 7)
ill
Call Subroutine DAYOUT
(see Page 7)
t z
Write Results
t
Subroutine DYLOOP
Performs most of the
hydro! ogic computations
Count Freeze-Thaw
Cycles
REAL
INTEGER
DIMENSION
LOGICAL
COMMON
Initialization
FIGURE 5: BLOCK DIAGRAM FOR TRCH20 (CONT.)
37
-------
Call Subroutine SNOWMELT
Compute Variable
Groundwater Recession
Constants
Begin Variable i itne
Accounting and Routing
i
Rainfall Upper Zone
Interaction
Plotting of Storm
Output
Hourly Overland Flow
and Rainfall Sorting
Storm Output
Draining of Upper
Zone Storage
Adding of Ground Water
Flow
Routing Calculations
Lower Zone and
Ground Water
Infiltration
Calculations
Calculating Gully
Erosion
T
FIGURE 5: BLOCK DIAGRAM FOR TRCH20 (CONT.)
-------
1119-006
Subroutine SNOWMELT
Snow Details are
Stored
Subroutine fiOOPUN
punches data in
card format
Subroutine ARITHP
Plots Recorded flow an
and arithmetic scale of
the user's choice in cfs
Subroutine DASHC
Used in ARITH to Plot
Cashed Hycirograph
Call Subroutine DASHC
Call Subroutine DASHC
Store Errors arid
Flow Durations
4 P.M. Adjustmen
of Values
Monthly Summary
Storage
Set-up data for
output for one
particular day
Subroutine OAVOliT
Subroutine ARITH
Plots Synthesized Flow
in cfs With a Dashed
Arithmetic Curve of the
Same Scale as ARITHP
FIGURE 5: BLOCK DIAGRAM FOR TRCH20 (CONT.)
39
-------
¦Site specific data - Card Deck
Meteorological data - NOAA magnetic tape for U.S. Weather Service
Station
Plotter instructions - Card Deck
Site Specific Data —
The user of the TRCH20 model must provide coal pile data not related
to meteorology. This data includes infiltration factors, flow adjustment
factors and ground water information. Many of these adjustment para-
meters will be further defined by TRC in the user's manual developed in
Phase 2 of this program. Table 34 outlines the TRCH20 site input data
and the source of this data#
Meteorological Data —
TRC has designed the TRCH20 model to use a standard National Climatic
Center (NCC) meteorological data tape, CD 144 format, available for U.S.
Weather Services stations. In this manner, the user will not have to
generate his own data tape of historical weather information. Pre-1965
data is utilized as it contains 24 observations per day.
The TRCH20 model reads values from the tape for rainfall, snowfall,
and temperature 'for a selected number of years. The rainfall and
snowfall values on the tape are given in ranges of light, medium, and
heavy. The model assigns average intensity values to each. These
variables are described in Table 35. •
If the model user has performed a coal pile field program, and has
developed data on site for precipitation and temperature, this data may
be used as input in lieu of the NCC tape. In addition, the user may read
in actual runoff flow data and the model will plot a comparison of sim-
ulated and actual runoff flow.
Plotter Data
The user includes data to label the axes of the hydrograph plots
developed by the model for both a selected storm and an entire year of
simulation. If the plotter options are not used, those cards are not
included.
The plotter variables are listed in Table 36.
40
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TABLE 34. INPUT DATA - SITE AND CALENDAR - TRCH20
1. SITE
Input
Variable
Name
Definition
Units
Source
TINC The selecting routing min
interval in minutes
From TCONC
LZS Current soil moisture
storage
in
Initial value is
estimate; checked
against final
simulated value
LZSN Soil moisture storage
index
in
Developed in
field program
CY
Interflow index
Developed in
field program
UZS * Current soil surface in
moisture storage
TRANSK Erosion transport
capacity coefficient
Normally zero un-
less start of
model preceded
by recent preci-
pitation
Developed in
field program
DETACH Erosion detachment ¦
capacity coefficient
CX
Index for estimating
soil surface moisture
storage
AREAP Area of coal pile
drainage
IRC Daily interflow
recession constant
acres
Developed in
field program
Developed in
field program
Site map
Graphical tech-
'niques for
hydrograph
analysis
K24L Parameter indicating
ground water flow
leaving basin
Graphical tech-
niques for
hydrograph
analysis
41
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TABLE 34. INPUT DATA - SITE AND CALENDAR - TRCH2G
Input
Variable
1. SITE Name
Definition
KK24 Daily base flow
recession constant
KV24 Daily base flow
recession adjustment
factor
RMELT Degree-day snowmelt
coefficient
C Time-area histogram
(May be modified in
program according to
streamflow)
GULLY Total width of
gullies
SGILK Coal surface con-
stant
GWS Current value of
ground water slope
index
Dnits
in/QF
ft
in
Source
Graphical tech-
niques for
hydrograph
analysis
Graphical techni-
ques for hydro-
graph analysis
Developed in
field program
Site map and
TCONC
Measured in
field
Developed in
field program
Developed in
field program
NN
Mean overland flow
path length
Manning"s n for over-
land flow on pile
surface
ft
Site map
Developed in
field program
CB
SGW
Infiltration index
Ground water moisture
storage
xn
Developed in
field program
Developed in
field program
(Continued)
42
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TABLE 34. INPUT DATA - SITE AND CALENDAR - TRCH2Q
SITE
Input
r xabxe
Name
Definition
Units
Source
TCONC The time for water
originating in the
most remote region
to reach the
measuring station
2 Number of elements
in current time-area
histogram
mm
Estimated from
data on length
and. slope of
pile
Site map and
TCONC
ss
Average pile slope
ft/ft "Coal pile con-
struction
2. CALENDAR
YRDET No. of years of data
for the selected storm
data
IOUT Day of the year of current
day of storm detail out-
' put being provided
inum Number of days of
storm detail output
DKN I.D. number of user selected
options
Title of computer run
3. OTHER
DDYR2 Last two digits of
2nd year in water
year
DDYRl Last two digits of
first year in water
year
(Continued)
43
-------
TABLE 35. METEOROLOGICAL DATA
1) Tape input
Variable from # ECC Tape Definition
IR rain - 0.1 in/hr, 0.1-0.2 in/hr, or 0.3 in/hr
IRDZL drizzle 0.01 in/hr, 0.01-0.02 in/hr or 0.2 in/hr
IS*. snow 0.1 in/hr, 0.01-0.02 in/hr or 0.3 in/hr
ISW* snow showers 0.1 in/hr, 0.1-0.2 in/hr or 0.3 in/hr
IP* hail 0.1 in/hr, 0.1-0.2 in/hr or 0.3 in/hr
TEMPH hourly temperature, °F
2) Card Input
PI rainfall, in/hr
TSNQWH* snow, sleet, hail, in/hr
TEMPH hourly temperature, °F
*in water equivalents
44
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TABLE 36. INPUT DATA - PLOTTER - TRCH20
Variable Name
Definition
Units
AXISX
AXISY
DDELDR
DDX
DDYY
Length of abscissa for
plotting hydrographs
Length of ordinate for
plotting hydrographs
The number of cubic feet
per second per inch of
ordinate used in plotting
the arithmetic hydrograph
Label of abscissa for
individual storm plot
Label of ordinate for
individual storm plot
m
m
cfs/in
DELDR
DELDR2
DELDR1
DL
DRORG
DRRORG
The number of cubic feet
per second per inch of
ordinate used in plotting
the logarithmic hydrograph
The spacing between tic
marks for the ordinate of
the arithmetic hydrograph
The spacing between tic-
marks for the ordinate of
the logarithmic hydrograph
The dash length used in
plotting the synthesized
hydrographs
The numeric label for the
minimum value of the ordinate
at the axis origin for the
logarithmic hydrograph
The numeric label for the
minimum value of the ordi-
nate at the axis origin for
the arithmetic hydrograph
cfs/in
in
xn
in
45
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TABLE 36. INPUT DATA - PLOTTER - TRCH20
Variable Name
Definition
Units
QQQ
QQY
SL
SYM
XAX
XORG
XTIC
XONIT
Y AX
YORG
YTIC
YUNIT
Description of gage location
Title of ordinate for runoff
hydrograph
The space length used in
plotting the synthesized
hydrographs
m
Title of absissc
hydrograph
for runoff
The length of abscissa for
the individual storm plot
Numeric label for the mini-
mum value of the abscissa at
the axis origin for the indi-
vidual storm plot
The spacing between tic marks
for the abscissa of the
detail storm plot
The number of hours per inch
of abscissa used in plotting
the individual storm
The length of ordinate for
the detail storm plot
The numeric label for the
minimum value of the ordinate
at the axis origin for detail
plot
The spacing between tic marks
for the ordinate of the storm
plot
The number of cubic feet per
second per inch of ordinate
used in the selected storm
plot
in
in
hr/ii
m
in
cfs/in
(Continued)
46
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TABLE 36. INPUT DATA - PLOTTER
^ariafole Name Definition Units
ZTIC The spacing between tic marks . in
for the ordinate of the rain-
fall hyetograph plot
zunit The number of ordinate used in in/in.
the rainfall hyetograph
(Continued)
47
-------
Basic and Optional Output of TRCH20
TRCH20 provides a basic printed output of daily, monthly, arid annual
runoff flows, plus optional output of selected precipitation events with
hourly or sub-hourly data. In addition, the' program creates a tape file
of hydrologic data for use in the qualitative co-model, TRCCOAL. The
outputs of TRCH20 are listed below:
Basic Outputs —
1) A table of average daily rainfall in inches.
2) Summation of synthesized daily runoff rates, in cubic feet per
second, for each month, followed by the annual total.
. 3) Synthesized monthly and annual totals for each of overland
runoff, interflow, baseflow, and total flow, in inches.
4) Monthly and annual totals of liquid precipitation, in inches,
developed from the meteorological input.
5) Monthly and annual totals of frozen precipitation, in water
equivalent inches, developed from the meteorological input.
6) End of month values, in inches, of pile, surface, and ground
water moisture.
7) End of month values for indexes of around water slope and pile
depression storage.
8) End of month values for snowpack in water equivalent inches.
9) Annual balance, in inches, of unaccounted for moisture.
Optional Outputs —¦ .
1) Echoes all input data.
2) For one selected storm per year, prints values, in inches, of
rainfall deposition, moisture storage, runoff origin, and runoff
outflow for each time interval.
3) Prints daily values of UZSN, UZS, GWS, SGW, SINT, SRGX, and
SSGWF to give a better indication of the program interactions in
the upper, lower, and deep zones of the pile.
4} Echoes recorded runoff flows, in cubic feet per second, for
comparison with simulated flows.
48
-------
5} Records the twenty highest clockhour rainfall events in the
water year.
6) Prints daily pile moisture storage, in inches.
7) Prints daily values of the snowpack, snowmelt, and snowfall, in
water equivalent inches.
8) Prints out average daily temperature, in degrees °f.
9) Prints out number of freeze-thaw cycles in preceding dry days.
10) Prints out simulated gully erosion of solids to the base of pile
in pounds per day.
11) Plots•an arithmetic hydrograph for water year comparing recorded
and simulated flows.
12) Plots an arithmetic hydrograph and rainfall hyetograph for
select detailed storm.
13) Prepares tape output file for use as input to TRCCOAL.
TECHNICAL ASPECTS OF THE TRCCOAL MODEL
During dry weather the surface of the coal pile undergoes the
physical/chemical processes of pyrite oxidation; acid, iron, and sulfate
production as well as the dissolving of trace materials. "During wet
weather these materials are washed off the surface and out of the
interior of the coal pile. Seepage is generated during both wet and dry
weather. These phenomena are simulated in TRCCOAL using the hydrologic
balance developed in TRCH20. The block diagram for TRCCOAL is shown in
Figure 6.
Dry Weather Reactions
.During non-rainfall periods the coal pile is subjected to atmospheric
conditions which break up the coal lumps and the moisture and oxygen in
the surface of the pile cause oxidation of the pyrite in the coal. The
products of pyrite oxidation are acid, sulfates, and iron. The acid
further acts to dissolve trace materials.
In TRCCOAL the user inputs data on coal characteristics and reaction
rates. The model simulates the total amount of pollutants in the coal
and the total amount of pollutants in a dissolved state during a dry
weather period. The number of freeze/thaw cycles calculated in TRCH20 is
used to accelerate the break up of coal and the subsequent pyrite oxida-
49
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READ IN HYDRQLOGIC
DATA FROM TRCH20
READ IN INPUT PARAMETERS
ADJUST REACTION RATES
FOR TEMPERATURE
DO DRY/WET WEATHER TEST
ADJUST CALENDAR
FOR LEAP YEARS
INITIALIZE AMOUNT OF ACIDS, IRON, TRACE
MATERIALS, SULFATE IN 4 ZONES OF COAL PILE
INITIALIZE DAILY, MONTHLY, ANO YEARLY VALUES OF
FLOW AND POLLUTANTS
FIGURE 6; BLOCK DIAGRAM FOR TRCCOAL
50
-------
EVALUATE POLLUTANT PRODUCTION INCREASE
DUE TO FREEZE/THAW PHENOMENA
DIRECT DISSOLVED MATERIALS DURING PRECIPITATION
EVENTS FROM SURFACE TO ZONES OF PILE
REMOVE SULFATE FROM PILE
CALCULATE MONTHLY VALUES
REMOVE TRACE
MATERIALS FROM PILE
CALCULATE YEARLY VALUES
REMOVE ACID FROM PILE
REMOVE IRON FROM PILE
WRITE OUT POLLUTANT PRODUCTION AND FLOW
CALCULATE THE AMOUNT OF POLLUTANTS
PRODUCED PER DRY DAY
CALCULATE DAILY VALUES OF FLOW, ACID, IRON
SULFATE, AND TRACE MATERIALS
FIGURE 6: BLOCK DIAGRAM FOR TRCCOAL (CONT.)
51
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tion. The dissolved material is then available for washoff during the
next storm event. Also during dry weather moisture is emitted from the
lower zone as seepage.
The formulations in the model for these reactions are shown below;
AMTPY = lbs of framboidal pyrite in surface of coal pile
AMTPY = PERPY * DENCOL * DEPTH * AREA * 43560. (4-23)
PERPY = % framboidal pyrite
DENCOL = Coal density, lb/ft3
DEPTH = depth of coal surface layer, ft
AREA = area of coal pile, acres
AMTACI = lbs of acidity produced/dry day interval
AMTACI = AMTPY * RATEPY * TIME 1/24. * ALKFAC (4-24)
BATEPY = pvrite oxidation rate, day""
T1ME1 = dry day time interval
ALKFAC = factor for alkalinity of coal
AMTTM(K) = lbs of trace material, K, in coal pile surface
AMTTM(K) - PBRTM(K) * DENCOL * DEPTH * AREA * 43560. (4-25)
PERTM(K) - % of trace material, K, in coal
TMDIS(K) = lbs of trace material, K, dissolved per dry day interval
TMDIS(K) = AMTTM(K) * AKTACD * FACTM (K) (4-26)
FACTM(K) = trace material, K, dissolving factor per lb. acid
SULDIS = lbs of sulfate dissolved per dry day interval
SULDIS = 19.2 * AMTACD (4-27)
TFEDIS = lbs. of T. iron dissolved per dry day interval
TFEDIS = 42. * AMTACD (4-28)
TAMTAC = lbs. of acid produced for' sequential dry day
TAM'i'AC = TAMTAC * FRTHAW * FT (4-29)
FRTHAW = no. of freeze-thaw cycles in preceding dry days.
FT = freeze-thaw factor
52
-------
The model conducts a wet/dry test to determine if the wet weather mode
of washoff or the dry weather mode of acid production, and seepage will
be utilized for a given day* If the total rainfall is less than Q.l
inches, then the model considers it a dry day and only acid production
and seepage generation takes place. The cutoff value of 0.1 inches is
arbitrarily chosen.
Wet Weather Reactions
During wet weather, rainfall entering the pile distributes a portion
of the dissolved metals, sulfates, and the acid on the surface to the
interior of the pile and to direct runoff. In addition, the acidity of
the rain is added to the available acid in the pile.. The amount of
pollutants that is distributed to the upper zone {depression storage),
lower zone {pile interior), direct runoff, and interflow is proportional
to the solubility of the pollutants and an adjustment 'factor. The
material stored in the lower zone is further distributed to deep storage
and the baseflow. Following are example equations for acid in direct
runoff. The equations for other pollutants in the other zones are
similar.
ACRMN = lbs of acid in acid rain/wet weather interval
ACRAIN = RAINCO * PR * AREA * 5.2 E-6 (4-30)
RAINCO = acidity of rain, mg/1
PR = rain (in.)/wet weather time interval
ACDDIR — lbs of acid going to direct runoff
ACDBIR = FACDIR * SOLACD * OWL ST * CP (4-31)
FACDIR = factor for the amount of acid going into direct runoff
SOLACD = solubility of acid, lb/ft3
GVFLST = inches of current rainfall entering direct runoff
CF = conversion to cubic feet of runoff
EXADIR = Excess acid in direct runoff storage
EXADIR = ACDDIR + EXADIR {4-32)
The amount of acid, metals, and sulfate in storage zones that is
washed out of the pile can be linearly or exponentially related to the
available material. The user determines the best fit to the field data
and chooses either' option. The option, EXPO—1, simulates an exponential
decay rate. This relationship is best demonstrated by the "first flush"
effect and considers the removal of both dissolved and suspended
material. Therefore, either the exponential washoff function in TRCCOAL
53
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is used to simulate suspended material or simulate the erosion routine of
TRCH20, but not both. The equations for acid are shown below as an
example:
WAS HA. = exponential factor for acid
WASHA - 1. - EXP (—AK*TIME2)
(4-33)
AK ' = exponential coefficient for acid
TIME2 = wet weather time interval
AREDIR = lbs of acid being removed by direct runoff
AREDIR = DIRRNF * SOLACD * FACRED * CP
(4-34)
DIRRNF - Current rate, in inches, of direct runoff entering
runoff channel
FACRED - factor for amount of pollutant going into runoff channel
Option EXPO —
AREDIR = (EXADIR + EXAUZ) * WASHA * CF
(4-35)
TRCCOAL then calculates daily, monthly, and annual totals of the acid,
metals, and sulfates contained in all components of the runoff stream.
Input Data for TRCCOAL
The TRCCOAL model has two sources of input data:
1) The magnetic tape file of hydrologic data
2) . Card input describing qualitative aspects of the coal pile.
The tape file created by TRCH20 contains data on rainfall, amount of
rainfall directed to the pile zones, the flowrate of direct runoff,
interflow, and baseflow, the total daily rainfall, the average daily air
temperature, and the number of freeze-thaw cycles for each simulated time
period.
The card input consists of three types: calendar data, adjustment
coefficients, and site specific input.
54
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1} The calendar input data is shown in Table 37. The user selects
the time period of the simulation as well as .the select storm
for output. These must match-the calendar data in TRCH20.
2) Table 38 lists the adjustment coefficients for the coal pile
model. These parameters allow the simulated qualitative output
for the distribution of pollutants within the coal pile as well
as the runoff flow, to be "fine-tuned" to match actual values as
found in field data. Recommended values for these parameters
will be developed by TfiC in the second phase of this program.
¦3} Values for the coal pile under consideration which can be
measured are listed in Table 39. These include the solubility
of acid, iron, sulfate, and trace metals, the density and area
of the coal pile, and the acidity of the rain, for example.
TABLE 37. TRCCOAL - INPUT DATA CALENDAR PARAMETERS
Variable Definition
YEARLP Last 2 digits of next leap year divided by four
YEARST Last 2 digits of starting year of model
YEAR1 ¦ ¦ Year of detailed output request
M0NTH1 Month of detailed output request
DAY1 First day of detailed output request
nday Number of consecutive days of output requested
55
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TABLE 38. TRCCOAL - INPUT DATA
ADJUSTMENT PARAMETERS*
Variable
Definition
FACDEP
FACDIR
FACINT
FACLZ
FACUZ
FACRED
FACREI
FACREB
FACHDS
FACFD
FACFI
FACFB
TK
AK
FK
SE '
Factor 'for depth of outer mantle
Factor for amount of pollutants going into direct
runoff
Factor for the amount of pollutants going into inter-
flow storage
Factor for the amount of pollutants going into lower
zone
Factor for the amount of pollutants going into upper
zone
Factor for pollutants entering runoff stream by direct
runoff
Factor for the amount of pollutants going into the
runoff stream by interflow
Factor for the amount of pollutants -going into the
runoff stream by baseflow
Factor for the amount of pollutants going into deep
storage
Factor for the amount of runoff coming from direct
runoff
Factor for the amount of runoff coming from interflow
Factor for amount of water coming from baseflow
Coefficient for exponential washoff of trace metals
Coefficient for exponential washoff of acid
Coefficient for exponential washoff of iron
Coefficient for exponential washoff of sulfate
* No units
56
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TABLE 38. TRCCOAL - INPUT DATA ADJUSTMENT PARAMETERS*
Variable
Definition
FT
FACTM
RATEPY
ALKFAC
Freeze-thaw factor for increased production of dis-
solved materials
Trace material dissolving factor per lb. of acid
Pyrite oxidation rate per day
Factor for alkalinity of coal
* No units
(Continued)
57
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TABLE 39. TRCCOAL -
INPUT DATA SITE SPECIFIC PARAMETERS
Variable Name
SOLACD
DEPTH
AHEAP
TIME 2
PERPY
DENCOL
N
TM
PERTH
PERSUL
PERTFE
RAINCO
SOLTFE
SOLTM
SOLSVL
EXPO
Definition
Solubility of acid
Depth of outer ¦ mantis
Area of coal pile
Time interval from TRCH20
Percentage of framboidal pyrite
in coal
Density of coal in pile
No. of trace materials in coal
simulated in model (max=8)
Name of trace materials in coal
(max=8)
Percentage each trace material
in coal
Percentage sulfur in coal
Percentage 1'. iron in coal
Acidity of rain
Solubility of total iron
Solubility of each trace material
Solubility of sulfate
Option for linear or exponential
washoff
Units
mg/l
ft
clC2T0S
hour
Ib/ft^
mg/l
mg/l
mg/l
mg/l
58
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Output of TRCCOAL
TRCCOAL provides output concerning the pollutant loadings from the
coal pile. The output products are listed below:
1) A calendar showing which days of the year in the simulation were
considered wet or dry.
2) A calendar of simulated daily .runoff flow volume, in cubic feet
per second.
3) Daily loadings of total acid as well as in direct runoff, inter-
flow, and seepage, in pounds.
4) Daily loadings of sulfate, iron, and trace materials in direct
runoff, interflow, and seepage, in pounds.
5) A calendar of total daily rainfall, in inches.
6) A calendar of direct runoff, interflow, and seepage volume, in
cubic feet per second.
7) Optional plots showing the relationship between rainfall, runoff
flows, and pollutant loadings on a detailed storm basis.
SENSITIVITY ANALYSIS
TRCH2Q - Quantitative Model
The input data • to the coal pile drainage model will require varying
degrees of accuracy. The model will be very sensitive to some parameters
and their value will greatly impact the runoff stream yield and shape of
flow recession curve. Other parameters are used for fine-tuning purposes
only.
A sensitivity analysis was conducted on several selected parameters.
Those chosen deal principally with the moisture balance of the water and
are difficult to measure in the field. The values chosen were'CB, LZSN,
KK24, IRC, and GWS. The results of varying the parameters are summarized
in Table 40.
CB — Infiltration Index —
CB is the infiltration index that controls the rate of infiltration.
It functions in the model's formula for peak infiltration rate:
D4F = FRAC*CB • {see equation 4—1)
2.0**LNRATM
59
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TABLE 40
SUMMARY OF RESULTS OF THE SENSITIVITY STUDY - TRCH20
Key: A Increased * Slightly
Decreased ** Moderately
Not Affected *** Significantly
I
Selected Input
Simulation Feature
Parameter
Parameter Change Yield Peaks
CB
LZSN
KK24
IRC
GWS
TINC
TCQNC
t
t
t
ic-k-k
Interflow
Recession
t*
\
Interflow
Recession
Pile
Moisture
60
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Increasing CB significantly increased infiltration and subsequently
lowered runoff flow yields and peaks. As expected, pile moisture
increased with increasing infiltration and the recession flows more
gradually approached zero.
¦ The impact of three values of CB on runoff flows is shown in Figure 7.
LZSN - Pile Moisture Storage Capacity —
LZSN is the pile moisture storage capacity index. It represents the
volume of water which may be held in the interior of the pile.
Increases in LZSN increase the recharge capacity in the coal pile.
Subsequently runoff volume and peaks decrease.
With the increase in LZSN, interflow and baseflow recession flows
decrease slightly. Figure 8 shows the runoff hydrograph for three values
of LZSN.
KK24 - Baseflow Recession Constant —
KK24 is the baseflow recession constant. Its effect on runoff flow
yields, peaks and pile moisture is insignificant, as shown in Figure 9.
Little impact can be detected in interflow and baseflow recession flows
also •
IRC - Daily Interflow Recession Constant —
IRC is the daily interflow constant. Varying IRC had no impact on
peaks and runoff flow yields. In addition there was only a slight
variation in interflow recession flows. Like KK24, there was no
significant variation in pile moisture.
Because of the nature of the exponential equation that utilizes IRC,
its values must be less than and equal to 1.
Figure 10 shows two values of IRC.
GWS - Current Value of Ground Water Slope Index —
GWS is the value of the ground water slope index and represents the
antecedent moisture conditions at the interface' of the pile and the
underlying material.
61
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1119-018
LEGEND
-CB = 0.8
280.00 290.00
JUL
300.00 310.00 320.00
AUG
330.00 340.00 350.00
SEP
360.00
FIGURE 7: EXAMPLE SENSITIVITY ANALYSIS, CB-INFILTRATION INDEX
-------
1119-019
LEGEND
—— LZSN = 24 IN
LZSN = 150 IN
LZSN = 480 IN
__A
310.00
330.00
290.00
340.00
350.00
360.00
280.00
300.00
JUL AUG SEP
FIGURE 8: EXAMPLE SENSITIVITY ANALYSIS, LZSN-PILE MOISTURE STORAGE
-------
1119-020
.EGEND
- KK24 ~ 0.096
- KK24 =0.96
• KK24 =9.6
, 11
280.00 290.00
JUL
300.00 310.00 320.00
AUG
330.00 340.00 350.00 360.00
SEP
FIGURE 9: EXAMPLE SENSITIVITY ANALYSIS, KK24 - BASEFLOW RECESSION
-------
1119-021
LEGEND
- TRC - 0.001
- TRC = 0.8
AJ
%
ft
'A
280,00 290.00 300.00 310.00 320.00 330.00 340.00 350.00 360.00
JUL AUG SEP
FIGURE 10: SENSITIVITY ANALYSIS, TRC - DAILY INTERFLOW RECESSION CONSTANT
-------
GWS is used in the equation:
GWF = S6W*LKK4*(1.0+LKV4*GWS) (see equation 4-19)
As expected, it had little impact on runoff flow volume and peaks.
However, it also had no impact on ground water flow. It should be noted
that GWS did not reach steady state • in these sensitivity tests and for
this example of an 11 acre coal pile, an initial value of greater than 21
was warranted.
Figure 11 shows the impact of variations in GWS.
TINC'- Selected Time Routing Interval —
In the OSU model decreasing the time interval of simulation shifted
the peak flow earlier in time and increased synthesized peak flows.
However, because of the small watersheds involved in coal piles and the
short time of travel, these changes were not seen in decreasing the
routing interval time, from 30 minutes to 5 minutes.
As seen in Figure 12, the routing interval had no impact on runoff
flow and peaks.
TRCCOfiL - Qualitative Model
Five parameters associated with the production and washout of acid
from the coal pile were chosen for the sensitivity analysis of TKCCOAL.
These are DEPTH, FACDIR, RATEPY, PERPY,¦and AK. All sensitivity analyses
were plotted for a two month period and the graph lines are offset
slightly to show the three parameters evaluated. The ' model output
utilized was the acid loading in the coal pile drainage stream.
DEPTH - Depth of Reactive Surface of Coal Pile —
DEPTH is the parameter which reflects the depth of the reactive
surface of the coal pile, in feet, in which pyrite oxidation take place.
It is used in the equation to calculate the pounds of framboidal pyrite
in coal.
AMTPY = PERPY * DENCOL * DEPTH * AREA * 43560 (see equation 4-23)
It is also used in similar calculations to calculate the amount of
sulfur, iron, and trace metals in the surface.
66
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1119-022
as
*¦**1
280.00 290.00 300.00 310.00 320.00 330.00 340.00 350.00 360.00
JUL AUO SEP
FIGURE 11: SENSITTVTTY ANALYSIS PiWS - GROUND WATER SLOPE
-------
1119-023
LEGEND
- TINC = 30 MIN
- TINC = 5 MIN
- TINC = 15 MIN
320.00
280.00
290.00
340.00
350.00
360.00
330.00
310.00
300.00
JUL AUG SEP
FIGURE 12: SENSITIVITY ANALYSTS SIMULATION TIME INTERVALS
-------
The depth to which oxygen, which controls the reaction, penetrates
the pile is difficult to estimate. Values of 0.01", 0.1', and 0.25' were
evaluated. The loading of acid in the coal pile drainage stream was
determined to be very insensitive to the depth values in this range.
The sensitivity analysis for DEPTH is shown in Figure 13.
RATBPY - Rate of Pyrite Oxidation —
While the model showed no sensitivity to the depth of the reactive
surface, there was slight sensitivity to the rate of pyrite oxidation,
RATEPY. RATEPY is used in the equation:
AMTACI = AMTPY * RATEPY * TIME 1/24. * AIKFAC (see equation 4-24}
Three values of the pyrite oxidation rate were evaluated in the
sensitivity analysis, 0.01, 1., 100, as shown in Figure 14. ¦' While
increasing the pyrite oxidation rate from 0.01 to 1. is reflected in an
increase in the peak acid loading in the outflow stream, an increase from
1. to 100. does not produce a similar increase. While increased pyrite
oxidation increases acid loadings in the runoff stream at low levels,
after a certain point the washoff parameters are the limiting factors,
despite an increase of acid in the coal pile.
FACDIR - Factor for the Amount of Pollutants Going into Direct Runoff —
FACDIR is the adjustment factor for the amount of pollutants going
from the surface to the direct runoff zone of the pile. It is used in
the equation for acid, for example:
ACDDIR = acid in direct runoff zone
ACCDIR = FACDIR * SOLACD * OVFLST * CF {see equation 4-31)
There are similar adjustment values for the amount of pollutants
directed to the lower zone, upper zone, and interflow zone of the coal
pile as well as adjustment factors for the washout of pollutants from
these zones to the outflow channel.
Three values were selected for FACDIR - 0.00001, 0.0001, 0.0002. As
shown in Figure 15, increasing FACDIR caused a moderate increase in the
acid loading in the runoff stream. It is one of the more sensitive
parameters in the qualitative model.
69
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1119-024
cn
es
«cE
<£
us ¦
£K
O
O
<
LEGEND
DEPTH-0.01
DEfTH-G.l
DEPTH-0.25
OCT
NOV
FIGURE 13: EXAMPLE SENSITIVITY ANALYSIS DEPTH
70
-------
LEGEND
RATEPY= 0.01
RATEPV-1.0
RATEPY-!0fl.
OCT
NOV
FIGURE 14: EXAMPLE SENSITIVITY ANALYSIS RATEPY
71
-------
1119-027
CSi
LEGEM
FACDIB-Q.QQ001
FAS01R-0.0001
FACDIR-O.Q002
Cft
C3
as
o
-------
PERFY - Percentage of Framboidal Pyrite in Coal —
The amount of acid production is related to the degree of framboidal
pyrite in coal, PERPY. However, a coal pile will represent several coal
seams and sources, therefore the sensitivity of the model to an estimate
of the percentage of framboidal pyrite is important.
PERPY is used in the equation:
AMTPY = PERPY * DEMCOL * DEPTH * AREA * 43560 (see equation 4-23)
Three values were chosen for PERPY - 1%, 3%, and 5%. Like the
parameter DEPTH, the amount of pollutants washed out of the coal pile is
not sensitive to PERPY. This is shown in Figure 16.
AX - Exponential Washoff Factor for Acid —
The model has the option of considering the linear washoff of the
pollutants from the coal pile or a "first flush" or exponential washoff.
The variable AK is the exponential coefficient for acid in the latter
algorithm.
WASHA = 1. - EXP (-AK * TIME 2) (see equations 4-33
AREDIR = (EXADIR + EXAUZ) * WASHA * CP & 4-34)
Three values were chosen for AK - 0.06, 0.6, and 6. As shown in
Figure 17, the acid loading removed from the pile is somewhat sensitive
to AK, especially with the lower range of values 0.06 - 0.6.
SHORTCOMINGS AND LIMITATIONS OF CPD MODEL
Mathematical models are, by definition, simplifications ' of complex
physical and chemical reactions. Within each model are assumptions which
make the model a workable tool. By understanding the shortcomings and
limitations of the coal pile drainage model, the user can better use the
results of the model in engineering applications and can better design
the input data for the model.
73
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1119-028
CS:
e=
*4
<¦
o
o
cs
32
a
<
o
o
o
a
<
JBnMr
ill!!:
!«»•
OCT NOV
FIGURE 16: EXAMPLE SENSITIVITY ANALYSIS PERPY
74
-------
LEGEND
— AK = 0.06
— AK = 0,6
— AK - 6.0
X
10
20
OCT
70
FIGURE 17: EXAMPLE SENSITIVITY ANALYSIS AK
-------
TRCH20
Coal Pile Hydrology —
The hydrologic model, TRCH2Q, concerns the flow from one runoff
drainage point from the coal pile under consideration. It assumes that
the runoff stream is channeled and can be measured. It also assumes one
runoff stream per coal pile.
Therefore the model should be used with contained coal piles only.
When there is more than one runoff outlet per coal pile, the coal pile
should be considered as several piles. The input variable for the area
of the coal pile will then reflect only the fraction of the pile in the
runoff drainage area for that model run.
Snowmelt —
Snowmelt is addressed by TRCH20, but in a more simplified form than
the previous Ohio State Model. In reality snowmelt is the result of
solar radiation, ground temperature, and snow density. TRCH20 considers
only air temperature to generate snowmelt.
¦ The snowmelt is expressed in water equivalent inches of snow. Water
equivalent inches are 5%-15% of the total snowfall. The snowmeltsnowpack
values generated by sample runs produced values which correlated reason-
ably well with recorded data.
Infiltration —
.In coal piles there are working faces as well as inactive sections of
the pile where no coal has been recently removed, in reality these areas
probably have different surface characteristics, with the working face
much more pervious than the inactive portions of the coal pile. However,
in the model, there is only one average surface infiltration rate for the
coal pile and • one interior percolation rate, with no differentiation
between active and inactive faces. However, if the coal pile drains to
several different runoff points, then the program run which includes the
working face of the coal pile, can have modified infiltration parameters.
Evaporation —
Most models which consider evaporation in the hydrologic balance are,
in reality, evaluating evapotranspiration by vegetation on the watershed
or 'lake evaporation off water surfaces. Little work has been done
concerning pan evaporation from unvegetated surfaces, including coal
piles. Since the coal pile is pervious and unvegetated, evapatrans-
76
-------
piration should have little Impact on the moisture balance. One
exception is the depression storage on top of the coal pile. ' In these
areas, puddles could occur which would be subject to evaporation effects.
TRC has not found a totally satisfactory simulation of daily evapor-
ation which can be used for coal piles and therefore has not included
evaporation in the CPD model at this time. However, a system of
algorithms relating evapotranspiration from short vegetation to average
daily air temperature has been developed. During the field program pan
evaporation will be measured and if it appears that evaporation from the
depression storage is very significant, the algorithms on evapotrans-
piration will be included in the model to attempt to simulate this
phenomena.
Precipitation —
The NCC magnetic tape which is used as meteorological input to the
program expresses the precipitation each hour as light# medium, and heavy
and an average value is assigned to each. These model ' values under-
estimate actual precipitation when there is heavy rainfall greater than
0.4"/hr and overestimate trace rainfall.
In the average year these approximations cancel out. For example, in
the test water year 1963-1964 the total simulated rain and snow was 43.9
water equivalent inches and the actual was 42.0 inches.
However, for detailed storms more exact data may be needed.
Therefore the model has the option to replace the magnetic tape input
with card input of exact hourly precipitation data.
TRCCOAL v
The qualitative model, TRCCOAL, also makes certain simplifying
assumptions to simulate coal pile drainage.
For example, the model views each day as a wet day or a dry day. On
wet days, previously dissolved materials are washed out of . the coal
pile. On dry days, pyrite oxidation and dissolved materials production
takes place. In reality, only a part of each day will the coal pile be
wet enough to preclude pyrite oxidation. Therefore the model has this
simplification inherent to its structure. The model could be modified to
do the wet/dry test on an hourly basis, but this would make the cost of
computing prohibitive.
The TRCCOAL model also makes assumptions that certain values are
average values for the year and do not fluctuate by day or hour. These
are listed below;
77
-------
1} the percentage of framboidal pyrite in the coal pile
2) the alkalinity factor of the coal
3) the pyrite oxidation rate (modified by air temperature)
4) the percentage of trace metals, iron, and sulfur in coal pile
5) the production rate of dissolved iron and sulfate
6) the acidity of rainfall
USES OF THE CPD MODEL IN TREATMENT DESIGN
The ultimate purpose of simulating coal pile drainage is for use in
the design of systems to treat the acid drainage before discharge.
To design treatment facilities, data is needed on both the quantity
of runoff that can be expected and its average and worst case qualitative
characteristics.
On the initial level, the model uses meteorological data tapes to
simulate "average" conditions. From a run of several years worth of
data, the user can simulate a range of values for the volume of runoff
expected and the pollutant loadings.
However, an examination of worst case conditions must also be
included in design engineering for collection basins and treatment
works. . Often treatment facilities are designed to contain the 10 year -
24 hour storm without any actual knowledge if this storm frequency is
appropriate. Only the first hours of a heavy storm may contain a
pollutant loading requiring treatment and the runoff flow from the
remainder of the storm can be safely bypassed without treatment. In
addition, the actual worst case may be several sequential storms during a
short period .with a continuous stream of pollutants washing out of the
coal pile.
The model is structured to allow the user to input simulated meteoro-
logical data instead of actual historical values. The user then creates
different combinations of storm events and evaluates the simulated runoff
output.
The plotter output of the model for both detailed storms and an
entire year presents the most salient data in an easy to use form. Plots
of hydro logic and pollutant data for the same time period can be super-
imposed for comparison purposes. From these plots, the volume and
duration of pollutant loadings can be determined.
COMPUTING REQUIREMENTS
TRC developed the combined coal pile drainage models (TRCH20,
TRCCOAL) utilizing time-sharing capabilities. TRC performed time-sharing
78
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on the Apex 'system of CDC computers through United Computing Service
centered in Kansas City and serving 150 metropolitan areas.
The costs below for running the model are for one year of output. Of
course, initial runs will be performed on small time spans and costs will
be significantly 'less.
Estimated Cost (spring 1980) for running the model for one year are
given:
Most utilities will be able to access the models utilizing a small
portable keyboard terminal 'and telephone hook-up through a local
telephone exchange or by submitting input data to TRC. Meteorological
information can be obtained from the National Climatic Center's tape
library of data from U.S. Weather Service Stations. The tapes will then
be forwarded to the UCS data center in Kansas City where they are mounted
for model use.
The card input deck is very small and can be typed in at the terminal
or' read in by card reader by the user at a local UCS office.
1) TRCH20 with no options
2) TRCH20 with all options
3) TRCCQAL with no plotter output
4) TRCCOAL with platter output
$200
$300
$ 80
$ 90
Printout ana plotter output are mailed directly to the user
79
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SECTION 5
FIELD WORK PLAN
INTRODUCTION
The primary objectives of a phased field program for coal pile runoff
from utility sites are as follows:
1) To obtain representative data to fine tune and modify the coal
pile runoff model.
2) To test the runoff model for a variety of climatic regions, coal
pile configurations, and coal characteristics.
3) To generate a substantial data base on the quantity and quality
of coal pile runoff from various utility sites throughout the
country.
The end results of these objectives will be:
' ' 1) A field proven mathematical model for predicting the quantity
and quality of coal pile runoff. This model will be a useful
tool for the design of runoff treatment systems. The primary
emphasis of the model will be in predicting the volume of storm-
water runoff from a coal pile so that accurate estimates of
runoff coefficients can be compared against the coefficients
used in the Rational Formula. This information can then be used
as design data.
2) Simpler tools, such as nomograms, charts, and/or tables to
assist those without computer resources in designing• treatment
for coal pile runoff.
In addition, the phased field measurement program has' the following
secondary objectives, all of which will be useful in the design of runoff
treatment systems. These include:
1) Determination as to whether the quality of coal pile runoff
exhibits either a "first flush" effect or a "flow dependent"
effect. The "first flush" effect is a .condition whereby the
80
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maximum pollutant loading occurs at the start of .a storm event;
i.e., the pollutants are flushed from the pile at the start of a
storm event. The "flow dependent" effect is a condition in
which the quantity and quality of coal pile runoff varies
directly with storm duration and intensity, i.e., peak pollutant
concentrations and runoff flow occur during peak rainfall
intensity. This will be valuable information in the design of
runoff treatment systems.
2) Establishment of a water balance for coal piles. The hydrologic
balance would consider runoff flow, base flow, and interflow
from the coal piles, as well as water retained by the piles and
: water which infiltrates into ground water beneath the piles.
3) Performance of correlation analyses for various pollutants in
runoff from coal piles. Correlation analyses will be used to
preclude the need for extensive analyses of various pollutants
and also to establish important trends in runoff character-
istics. . Past research has shown that the degree of framboidal
pyrite oxidation can be correlated with the acidity of the
runoff. In addition, temperature and oxygen availability may be
correlated with the degree of pyrite oxidation. Other research
has shown that conductivity may be correlated with total
dissolved solids (TDS) and sulfate. In turn, TDS may be
. . correlated with sulfate. TDS and total suspended solids (TSS)
may also be correlated with the dissolved and . 'suspended
fractions of metals.
4) Initial screening of coal samples for metals potentially avail-
able for washoff. This will determine which metals should be
analyzed during the field program. These metals will then be
analyzed for both dissolved and suspended fractions to determine
speciation according to the acidity/alkalinity of the runoff.
The overall field program will be designed to attain these primary
and secondary objectives. The field program will be conducted at 12
different utility sites throughout the country over a three year period.
The field program will begin with two "test" sites to gather infor-
mation to be used to fine tune and modify the coal pile runoff model. In
addition, the field testing procedures will be refined and modified as
necessary at these two sites. The "test" sites will also be used to
satisfy the secondary objectives of the program. . As such, these sites
will serve to refine the field program for the remaining ten sites. The
sampling program at each test site will be approximately of 10 weeks
duration.
The remaining ten sites will be used to test the runoff model for a
.variety of climatic regimes, coal pile configurations, and coal
characteristics, as well as to generate a substantial data base on coal
pile runoff. These sampling programs will vary in duration from one
month to nine months.
"81
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All data collected in the field will be put in a form which is
compatible for use in the runoff model. In addition, this data will be
digitized and made easily accessible through magnetic tape. • Thus, the
user, who may wish to design a treatment system for coal pile runoff for
a coal pile similar in characteristics to one of the studied sites, has
only to acquire the magnetic tape and review the data.
This data will incorporate the following;
1) Site description data, including:
a) General plant information
b) Coal pile characteristics
e} Coal characteristics
2) Meteorological conditions (historical and concurrent with field
program);
3) Daily runoff flows and pollutant loadings;
4) Single storm hyetographs, hydrographs, and pollutographs; and
5) Statistical summaries of storm events indicating worst case
conditions encountered during the field program.
The field work plan to be discussed will serve as a guide to planning
the overall field program. The work plan addresses the. following com-
ponents necessary in the design of a field program of this magnitude:
1} Selection of -12 utility sites.
2) initial site visit including background data acquisition.¦
3) Preliminary work, including acquisition of coal samples, and
coal pile and ground water testing.
4) Laboratory testing of the coal samples.
5) Choice of pollutant parameters for analysis.
6) Determination of sampling frequency.
7} Selection of sampling, flow monitoring and meteorological
equipment.
8) Development of a plan for shipping samples for analysis.
9} Laboratory analysis of the 'runoff samples.
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In addition, data reduction, analysis, and presentation procedures,
manpower requirements, and the overall program schedule and budget are
considered.
SELECTION OF REPRESENTATIVE PLANT SITES
The identification of plant sites to be used in the study of coal
pile runoff is the first step in preparing a detailed work plan for a
monitoring program. The study of selection criteria describing repre-
sentative coal pile characteristics and site conditions resulted in a
listing of parameters that can be divided between macro-parameters and
micro-parameters. Macro-parameters include generating capacity of the
plant, percent sulfur content of the coals, general region where the coal
is mined and annual total precipitation for the power plant locations.
Micro-parameters include actual coal pile sizes that are representative
of a certain group of plants, seasonal precipitation patterns, amount of
snow accumulation, and plant operating conditions which may influence the
characteristics of the runoff such as lined piles, coal cleaning, etc.
For the purposes of the field work plan, only the macro-parameters are
used in the selection. Once the individual monitoring sites are
identified, they will be distinguished according to the micro-parameters
during the preliminary site setup task.
The field work plan is based on monitoring the coal pile runoff from
12 different coal fired utility plants. Two of the 12 sites are
identified as "test" sites where the runoff will be monitored from a low
sulfur medium size pile and a high sulfur medium size pile for a 10 week
period. Medium size plants will be selected for scale purposes so that
it will be easy to adjust follow-on monitoring at small plants and large
plants. High and low sulfur containing coals were selected for test
sites because there is agreement in the ' literature that sulfur,
expecially pyritic sulfur content of the' coals, is the major determinant
in the quality of the runoff water.
Table 41 presents the site selection matrix to be used to identify
the category in which a prospective site may fall. Referring to the last
row of plant categories, only one category is marked for plants burning
coal mined in the southwestern region because there are very few plants
in this 'category. An additional medium size plant burning Appalachian
coal is included because this represents a very large category of older
plants and will include many plants reconverting from other fuels back to
coal. An additional large size plant burning Western and Great Northern
Plains coal is included because this represents those future plants using
coal from states with the largest reserves of coal, i.e., Wyoming and
Montana. Once the prospective monitoring sites have been identified,
only those plants with different micro-parameters will be selected for
the medium size Appalachian and large size Western coal burning plants.
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table 41. SITE SELECTION MATRIX FOR THE MONITORING
OP COAL PILE RUNOFF
Small Plant
Medium plant
Large Plant
W/GNP Coal
W/GNP Coal*
W/GNP Coal
Small Plant
Medium Plant
Large Plant
IE/IW Coal
IE/IW Coal
IE/IW Coal
Small Plant
Medium Plant
Large Plant
AP Coal
AP Coal*
AP Coal
Medium Plant
Medium Plant
Large Plant
AP Coai.
SW Coal
W/GNP Coal
Plant Size: Small 25-100 MW
Medium 100-800 MW
¦ Large 800 MW
Coal Source Region: Mean % Sulfur by Weight
W/GNP coal - Western & Great Northern Plains
IE/IW coal - Interior Eastern & Inter. Western
AP coal - Appalachian
SW coal - Southwestern
0.83
2.86
1.83
0.57
* = Test Sites to be identified with medium size plants, one using low
sulfur coal and one using high sulfur coal.
INITIAL SITE VISIT
The field survey at each of the 12 utility sites will be specific to
each site. This will necessitate a visit to each site as the first step
in the design of the field program. The site visit should accomplish the
following tasks ?
1) Selection of suitable locations for runoff and base flow
sampling.
2) Selection of suitable locations for installation of the meteoro-
logical station and the field laboratory trailer.
3} Acquisition of necessary background information as input to the
runoff model.
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Each of these tasks must be addressed in the development of test
plans for each site. The on-site visit and discussions with plant
personnel should be sufficient to accomplish these tasks.
Selection of Sampling Sites
A visual survey will be used to select suitable locations for storm-
water runoff and base flow sampling. Coal piles typically have several
runoff and base flow streams which, due to the local topography, do not
flow in the same direction. This will necessitate treating each stream
as an individual sampling site. For instance, a particular coal pile may
have as many as 2-5 streams which must be considered individually.
Attempts will be made to schedule the initial on-site visit so that at
least one storm event with post—storm baseflow conditions is observed to
determine the number of streams to be sampled and the best location for
sampling each stream.
Some of the sites may already have flow measurement devices, such as
weirs and flumes, for monitoring coal pile runoff. These devices will be
incorporated into the test plan for the site.
Selection of Locations for Installation of Meteorological Station and
Field Laboratory Trailer
Continuous meteorological data will be collected throughout the field
program. This data will serve as necessary inputs to the coal pile
runoff model and also as a data base on meteorological conditions at each
site. The meteorological information to be collected includes:
a) Precipitation
b) Air temperature/relative humidity
cj Solar radiation
d) Evaporation
The data will be obtained with automated monitoring equipment. fell
measurements will be recorded on continuous strip charts. The equipment
will be housed on site in a louvered shelter. A suitable location will
be selected for the installation of the meteorological station during the
initial on-site visit. This location should be in an open, flat area
free from obstructions but in close proximity to a power source.
In addition, a suitable location for setting up the field laboratory
trailer will be selected. This trailer will be used for performing
on-site laboratory analyses, for containing the continuous monitoring
equipment and preserving samples for other analyses. The trailer will
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also contain a drying oven for solids and moisture content analyses. A
central location will be chosen close to the coal piles with easy access
but away from the flow of plant traffic.
Acquisition of Background Data
Another objective of the on-site visit will be the acquisition of
necessary background data which is recorded at the site. These data will
satisfy several 'of the data requirements at the individual sites. Figure
18 shows the major categories of data requirements. These data will
serve as inputs to the runoff model and also to generate a data base for
each site. The data to be'collected during the on-site visit includes:
1) site description data
a) General plant information
b) Coal data
c) Coal pile data
d) Ground water data
2) Historical site meteorological data (if available)
The remaining data requirements for each site, including meteoro-
logical and runoff data, ' will be satisfied during the actual field
testing program.
The majority of the site description data will be gathered from plant
operating records, plant correspondence, coal delivery¦ records, and from
discussions with plant personnel. These data are listed below by major
category.
. The general plant information' to be gathered will include the
following elements:
a) . Plant name or station
b) Utility name
c) Location (city, county, state)
d) Type of plant (base load or peaking)
e) Number of coal-fired units
f) Generating capacity
The following information will be collected for each type of coal
burned at the site:
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SOLAR
RADIATION
EVAPORATION
TEMPERATURE
EVAPORATION
PRECIPITATION
PRECIPITATION
COAL PILE(S)
DATA (PHYSICAL)
GENERAL PLANT
INFORMATION
GROUND WATER
DATA
COAL(S)
DATA (CHEMICAL)
AIR
TEMPERATURE
SOLAR
RADIATION
ROUTINE WATER
ANALYSES.
ROUTINE WATER
ANALYSES
CONTINUOUS IN-SITU
MEASUREMENTS OF
RUNOFF
CONTINUOUS IN-SITU
MEASUREMENTS OF
BASE FLOW
RUNOFF DATA
. HISTORICAL DATA
(3 MONTHS PRIOR
TO FIELD PROGRAM)
SITE DESCRIPTION DATA
FIELD DATA
(DURING FIELD
PROGRAM)
METEOROLOGICAL DATA
STORM EVENTS
(>O.IO INCHES OF
PRECIPITATION)
DRY DAYS (INCLUDE STORM
EVENTS WITH <0.10 INCHES
OF PRECIPITATION)
FIGURE 18: COAL PILE RUNOFF DATA REQUIREMENTS AT INDIVIDUAL SITES
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a) Coal rank
b) Coal source:
1) County, state
2) Seam
c) Method of coal cleaning
d) Coal characteristics (if available):
• 1) Bulk density
2} tump size {by sieve analysis)
3) Average BTU content
4) Average percent sulfur
5) Average percent pyritic sulfur
6) Average percent framboidal pyrite
7) Average percent ash
The following data will be gathered for each individual coal pile at
each site:
a) Type of pile (active or reserve)
b) Drainage basin area
c) Description of pile construction
d) Description of pile compaction
e) Pile storage time
The following recorded data on ground water in the vicinity of the
coal piles will be collected (if available):
Local geology description:
a) Types of soil beneath the coal piles
b) Average percent soil moisture
c) Soil infiltration rates
d) Ground water elevations
It is possible that soils survey maps of the sites may be available
which will provide some of this information.
If available, the following historical meteorological data will be
gathered at the site for the three-month period prior to the start of the
field survey: -
a) Total daily precipitation
b) Average daily air temperature
c) Average daily solar radiation
d) Average daily evaporation
e) Average daily relative humidity
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Local airport and/or National Weather Service (NWS) records for the
general plant vicinity will be sought for this information. If the
utility maintains its own meteorological records, then the NWS informa-
tion will be collected to supplement the plant data.
PRELIMINARY SITE WORK
The preliminary site work (prior to the field survey) will include
the following tasks;
(1) Acquisition of representative coal samples for laboratory
testing.
(2) Field testing of coal pile characteristics and ground water "in
the vicinity of the coal pile.
A second site visit will be necessary to accomplish both of these
tasks.
Acquisition of Representative Coal Samples
Coal sampling is difficult because of the high variability of the
coal itself. In sampling from a storage pile the difficulties * are com-
pounded by having a mixed source of coals and size segregation during
handling. Therefore, acquisition of representative coal samples will be
conducted in two phases: the first to determine overall variability
based on ash content; the second to collect a sufficient number of
samples to give a representative characterization of the parameters of
concern.
Phase I - Sampling for Determination of Coal Variability—
The traverse method will be utilized to determine coal variability in
each coal pile. This method involves obtaining samples systematically
along a traverse of the entire pile. The methodology for Phase I is
described in Appendix A of ASTM procedure D-2234 (refer to Appendix B of
this report). Variability determinations will be based on gross 'ash
content of the samples.
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Phase II - Sampling of Coal for Precision—
The methodology as described in Section 7 of ASTM procedure D-2234
will be used to obtain samples of coal for precise results. The number
of coal samples per coal pile will be determined by the results of
Phase I.
Field Testing of Coal Pile Characteristics
The field tests to be performed on the coal piles at each site can be
grouped into two major categories:
a) Physical measurements and visual observations of the coal piles
b) Coal pile hydrology testing
1) Average percent moisture content of pile
2) Water infiltration rates
Physical Measurements and Visual Observations
The physical measurements and visual observations listed below will
be recorded for' each coal pile. These data will serve primarily as
inputs to the runoff model.
a) Average pile volume
1) "Average length
2} Average width
3) Average depth
b) Average pile side slope
c) Average depth of outer mantle
d) Average bulk density and porosity
e) Average depth of depression storage on top of pile
f) Average depth of ice and snow on top of pile
g) Gully erosion observations
1} Approximate number of gullies
2} Average width
3) Approximate volume of displaced material
h) Number of visible springs from side of pile.
i) Typical particle size distribution of surficial coal
Coal Pile Hydrology Testing
Coal pile hydrology tests to be performed during the on-site visit
include;
• : 9 0 '
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¦ a) Average percent moisture content of each pile
b) Water infiltration rates
These data will be important both as inputs to the runoff model and
also in water balance calculations for the coal piles.
Two types of moisture content measurements are • necessary in the
evaluation of coal pile hydrology. These include the measurements of the
moisture content of the unsaturated zones and the dimensions of the
saturated zones within the pile.
Standard drilling techniques will be used to determine the moisture
content of these zones on a preliminary basis. Five to ten hollow stem
auger borings, depending on the size of the coal piles, and split spoon
samples taken every five feet will be used to obtain discrete samples for
the determination of the variation of moisture content with depth in the
unsaturated zone. Piezometers consisting of slotted PVC pipe with Ottawa
sand packed in the lower part of the annulus and a bentonite seal above
the zone of interest will be used both as a monitoring well for depth to
the saturated zone and a sampling point for water quality.
Surface resistivity techniques will also be used to extend the data
base. Changes in moisture content with depth should be correlative with
the electrical resistivity of the pile as measured at the surface of the
pile. In particular, the depth of the saturated layer will be deter-
mined. Using these data, as well as the data from the drilling program,
a contour map of the top of the saturated zone in each pile will be
prepared.
The moisture content of the unsaturated zone will be determined from
the discrete samples obtained during the drilling program. ASTM pro-
cedure D3302, refer to Appendix C, will be employed to determine the
total moisture content of these coal samples. The moisture content will
be correlated with the resistivity information to extend this data base.
Water infiltration rates will be determined for each coal • pile.
These rates are to be used in developing the overall water balance for
the piles and in determining erosion potential.
ASTM procedure D3335 (see Appendix D) will be used in the determi-
nation of infiltration rates. A double ring permeameter or infiltrometer
will be used to measure these rates. Infiltration rates are time
variable and reflect the change of permeability with saturation.
Ground Water Field Tests
In the same manner as the coal pile tests, average percent soil
moisture and soil infiltration rates will be determined in the vicinity
of the coal piles. Also, the depth to ground water, or ground water
elevations, will be determined. However, the resistivity survey will not
be performed as part of these tests.
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¦Laboratory Testing of Coal Samples
Laboratory testing.of the coal samples will include;
Physical testing - particle size distribution
Phase I - variability testing
- ash content
Phase II testing -
. Percent framboidal pyrite
Percent sulfur
Trace metal content
Physical Testing—
Particle size distribution will be determined for the field collected
samples by sieve analysis using ASTM method D410 (see Appendix E).
Phase I Variability Testing—
Ash content of coal serves as a gross indicator as to overall
chemical variability. Ash content will be determined using ASTM method
D3174, refer to Appendix F.
Phase II Variability Testing—
Three types of analyses will be required for overall chemical
characterization of the coal piles framboidal pyrite analysis, percent
total sulfur, and trace metal chemistry. The pyrite and sulfur data will
be used for evaluation of the acid forming potential and the trace metal
data will be used for the water quality modeling program.
Framboidal Pyrite Analysis — The framboidal pyrite analysis will be
performed by the method described by F.T. Caruccio in his paper "Estirnat-
ing the Acid Potential of Coal Mine Refuse" in The Ecology of Resource
Degradation and Renewal, Chadwick and Goodman, (Editors) 1973. Samples
will be crushed and formed into pellets. A point count will then be
performed to determine the percent framboidal pyrite.
Sulfur Analysis — Total sulfur determination will be made using the
procedures outlined in ASTM D3177, Method A or Method B (refer to
Appendix 6).
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Trace Metal Chemistry — Trace metals content of the coal samples
will be- determined using the extraction procedures developed by the TVA
in the study of coal and ash samples at the Colbert' Steam Plant (in
press). Extraction procedures and analytical procedures for specific
metals are shown in Table 42.
TABLE 42. COAL EXTRACTION AND ANALYTICAL PROCEDURES
Metal
Be, Ca, Cr
Cu, Pe, Mg, Mn, Mo
Ni, Pb, V, Zn
Al, Cd, Co
As
Se, Sb
Hg
Extraction
Ashed, Digested with HF
HCIO4
Digested with Lithium
Metaborate
Digested with HNO3
and H2SO4
Digested with Escfaka
¦Mixture
Digested with NaOH
Digested with Aqua
Regia
Analytical Procedure
Atomic Adsorption
'Atomic Adsorption
Atomic Adsorption
Atomic Adsorption
Specific Ion
Electrode
Atomic Adsorption
Acquisition of Background Data Mot Attainable at Site
In addition to the recorded background data obtained during the
initial on-site visit, additional background data will be obtained from
outside sources. These data are listed below along with their source.
a) Soils' survey maps - Soils Conservation Service (SCS)
b) Surficial geology maps - United States Geological Survey (U3GS)
c) Bedrock geology maps - United States Geological Survey (USGS)
d) Historical meteorological data - National Oceanic and Atmos-
pheric Administration (NOAA) - National Weather Service
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The soils survey and geology maps will provide information on the
types of material beneath the coal piles. In addition, approximate
ground water elevations will be determined. .
The' historical meteorological 'data will be obtained for .the three
month period prior to the start of the field survey at each of the 12
sites. These data will be used for several purposes:
a) as input to the runoff model;
b) to show trends in meteorological conditions at the site; and
c) to determine when the last storm event occurred at the site so
that pre-runoff event water content can be estimated.
DESIGN OF FIELD PROGRAM
The field measurements program will be designed to attain the
objectives of the overall program with minimal cost. The individual
tasks to be addressed in the development of the field program are
discussed in detail in the following sections.
Parameters to be Analyzed
Table 43 is the list of pollutant parameters to be monitored in the
runoff and base flow streams during the field program.
Continuous monitoring of pB, temperature, and conductivity will be
conducted throughout the field program. pH is important in the determi-
nation of the degree of acidity or alkalinity of the stormwater runoff
and base flow streams. It will also be an important parameter for
correlation analysis and phase -distribution analysis of the various
pollutant parameters. Water temperature may serve as an indication of
the degree of pyrite oxidation occurring within the pile. Conductivity
can be correlated with total dissolved solids (TDS) and through initial
testing may preclude the need for extensive TDS analysis.
From previous studies^' 10, 11, 12 related to coal pile runoff, it
has been shown that IDS, total suspended solids (TSS), sulfate, iron,
manganese, and aluminum are characteristic pollutants. TSS will be
analyzed for correlation . purposes and for pile washoff coefficient
determinations.
Antimony, arsenic, beryllium, cadmium, calcium, total . chromium,
copper, lead, magnesium, mercury, nickel, selenium, and zinc were
identified in past literature reviews^3' " as being present in coal
pile runoff. In addition, cobalt, fluoride, molybdenum, and vanadium
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TABLE 43. POLLUTANT PARAMETERS TO BE ANALYZED DURING
FIELD PROGRAM AND MINIMUM VOLUMH REQUIRED
Sample Volume Requirements
Minimum Volume
Required, raid)
pK
Temperature - ,
Conductivity
Acidity/Alkalinity
Total Suspended Solids (TSS)
Total Dissolved Solids {TDS)
Total Organic Carbon (TOC)
Sulfate {SO4}
Total ardnoss
Metals (Total and Dissolved Forms):
100
100
100
25
50
100
300(2)
Aluminum (Al)
Antimony (Sb)
Arsenic (As)
Beryllium (Be)
Cadmium (Cg)
¦ Calcium (Ca)
Chromium, Total (CrT)
Cobalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Magnesium (Mg)
Manganese (Mn)
Molybdenum (Mo)
Nickel (Ni)
Selenium (Se)
Vanadium (V)
Zinc (Zn)
Fluoride (F) 300
Mercury (Hg) 200(3)
(1) Minimum volumes obtained from Methods for Chemical Analysis of Water
and Wastes, EPA-600/4-79-020..
(2) 100 ml for total form
200 ml for dissolved form
(3) 100 ml for total form; 100 ml for dissolved form.
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were found to be present in coal pile leachate studies^5. Included in
this list of metals are the metals identified in the list of 129 Priority
Pollutants, with 'the exception of silver and thallium.
Due to the large variety of metals which may be present in the runoff
and base flow streams, coal samples at the two "test" sites will be
screened using laboratory procedures as discussed previously in
"Laboratory Testing of Coal Samples". This may allow elimination of
certain metals from extensive analysis during the field program. The
metals earmarked for analysis will be analyzed in both their total and
dissolved forms to determine speciation or phase distribution' according
to the acidity or alkalinity of the stormwater runoff and base flow.
Total organic carbon (TOC) will be analyzed as an indication of the
presence of organic pollutants.
The sample volume requirements will be dictated by the pollutant
parameters to be analyzed in the field. The minimum sample volume
required for each of the parameters identified in Section 4 is'shown in
Table 43. These requirements indicate that the volume of each runoff or
base flow sample should be at least 1275 milliliters (ml) to ensure
sufficient sample for analysis of all of the pollutant parameters.
Number of Samples and Sampling Frequency
The number of samples and the frequency of sampling during a storm or
dry day sampling event will be based on:
a} The specific needs of the runoff model, In terms of dry day or
base flow input; and
b} • The data requirements for ' establishing a base of -coal pile
runoff data.
Data on base flow or dry day conditions will be necessary as input to
the runoff model. This data will be necessary to calibrate the runoff
model, both qualitatively and quantitatively, for the particular coal
pile being modeled. As such, the number of samples and sampling
frequency should be compatible with the input needs of the model. This
will necessitate daily sampling of base flow during dry day conditions.
Assuming an average of two base flow streams per coal pile, daily grab
samples from each stream will be composited to produce one sample for
chemical analysis. It is estimated that, due to climatic patterns in
different parts of the country, 36 total base flow samples will be
analyzed per site for all pollutant parameters.
The number of samples and sampling frequency for storm events should
be selected to:
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a) be compatible with the runoff model outputs for ease in com-
parison; and
b) be sufficient to establish a data base on coal pile runoff for
different climatic regions, coal types, and coal pile con-
figurations.
In order to satisfy the above requirements, one of each of the
following four types of storm events should be sampled at each site;
a) 24-hour.storm
.b) 12-hour storm
c) 4-hour storm
d) 2-hour storm
Samples will be obtained half-hourly during' the first four hours of
the 24 and 12-hour storm events. Hourly samples will' then be taken for
the remainder of these events. Half-hourly samples will be collected
throughout the two and four-hour storm events. This schedule will result
in a total of approximately 112 total runoff samples per utility test
site. This number assumes an average of two runoff streams per coal
pile, each of which will be monitored separately, and one coal pile per
utility site. This can be broken down further as 56 total samples for
each runoff stream.
Sampling, Flow Monitoring, and Meteorological Equipment
The various types of equipment to be employed for runoff sampling,
runoff and base flow monitoring, water quality measurements, and meteoro-
logical data collection are discussed below.
Runoff samples will be collected automatically during storm events
using pumping type sequential samplers. These samplers will collect
samples automatically at a pre-set volume ' and frequency. Sampling is
triggered by a flow actuator switch which senses a change in water
level. The initial work plan calls for sample collection on a time pro-
portional basis.' However, depending on the characteristics of the runoff
quantity, it may be desirable to switch to, flow proportional sampling.
For example, if the runoff exhibits a "first flush" effect, it will be
desirable to sample more frequently then half-hourly during the first
flush period to adequately characterize the runoff quality. The
automatic sampling equipment minimizes manpower requirements and allows
workers to perform other tasks during sample collection.
Coal pile runoff and base flow will be monitored continuously during
the field program. As previously mentioned, it is assumed that there
will be two streams emanating from a coal pile. Each of these streams
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will be monitored separately. A primary measuring device, such as a weir
or flume, will be installed across each of these streams.. These devices
indicate the level of the liquid passing through or over the device.
Flumes are specially shaped open channel flow sections which provide a
restriction in area. These devices are compatible with coal pile runoff
flow measurement because they are self-cleaning. The high velocity
through the flume prevents deposition of solids and sediment. • Also, the
accuracy of the flume is less affected by varying approach velocities
than the weir. However, the flume is more expensive than a weir in terms
of initial cost and is generally less accurate.
. Weirs are basically obstructions built across the stream over which
the liquid flows, often through a specially shaped opening. The weir is
less expensive than the flume in terms of initial costs. However, main-
tenance costs are higher due to the deposition of material behind the
weir. In addition, time delays behind the weir can cause problems with
the correlation of highly variable flow conditions to water quality.
Assuming that the weir is well maintained, greater accuracy in flow
measurement is obtained than with the flume.
The situation at the site will determine which of these primary
devices to use. In areas of relatively flat or average slope, flumes
will be employed to prevent deposition of material. Weirs will be
installed in areas of steeper slope.
Existing weirs or flumes at the sites will be utilized as ' much as
possible.
The weirs and/or flumes will be used in conjunction with a secondary
measuring device, or flow meter, to measure the flow rate of the stream.
The flow meter measures the water level in' the primary device with a
submerged plastic tube which continuously emits bubbles upstream of the
weir or flume. As the water level changes, back-pressure changes in the
tubing are measured with a sensitive electronic transducer. The trans-
ducer then converts this pressure into a digital electronic signal pro-
portional to water level. The water level is then converted to flow rate
by an electronic module specially designed for each type of primary
measuring device. Flow rate is recorded on a built-in strip chart
recorder and total flow is displayed on a sis-digit totalizer.
The pH, conductivity and temperature of the runoff and base flow will
be monitored continuously during the field program using automatic equip-
ment. Each piece of equipment will be connected to one multichannel
chart recorder which will facilitate comparison of these parameters and
indicate significant trends. Special probes will be used for each
parameter which are resistant to highly acidic water. In addition, these
probes will be subject to a regular maintenance program.
As previously discussed in the section "Selection of Locations for
Installation of Meteorological Station and Field Laboratory Trailer", the
following meteorological data will be continuously recorded at each site:
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a) Precipitation
b) Air temperature/relative humidity
c) Solar radiation
d) Evaporation
'Precipitation will be measured with a heated tipping bucket gage.
This standard National Weather Service gage is operable in temperatures
down to -20°f, at a maximum snowfall rate of 3 inches per hour. The
gage will be used in conjunction with an event-type recorder and
counter. The recorder indicates every 0.01 inch of precipitation while
the digital counter shows cumulative rainfall.
Air temperature and relative humidity will be measured with a hygro-
thermograph. This instrument, made to National Weather Service specifi-
cations records both temperature and relative humidity on the same time
coordinate of a curvilinear chart. The temperature sensitive element is
a highly polished chrome plated bourdon tube. The humidity element
consists of multiple strands of specially treated human hair. Through a
system of linkages these elements operate individual recording pens.
Solar radiation will be measured with a bimetallic recording
pyranoaeter (actinometer). The measuring element consists of two
bimetallic strips mounted to show pen motion corresponding to a differ-
ential temperature with ambient temperature compensation.. A blackened
strip is exposed to both the ' sun's radiant energy and the ambient
temperature, while a chrome plated strip is exposed only to ambient
temperature.
Evaporation will be measured with an evaporation pan equipped with a
chart recorder. The instrument is designed to record the amount of water
evaporated from a surface area of 250 square centimeters.
Plan for Shipping Samples for Laboratory Analysis
In order to.maintain the integrity of the samples prior to laboratory
analysis, the samples will be shipped to the laboratory as quickly as
possible after a sampling event. This will necessitate establishing a
plan for shipping the samples. A courier service will be chosen for each
utility site. The courier service should provide direct pickup and
delivery to the laboratory within a 24 hour period. The courier will be
notified as soon as the field personnel have an idea when the samples
will be ready for shipping in order to expedite sample delivery.
Laboratory Analyses
Analytical procedures described in EPA's Methods for Chemical
Analysis of Water and Wastes (EPA-600/4-79-020, March 1979) will be used
99
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for the analysis of the pollutant parameters listed in Table 43. In
addition, a rigorous quality control program will be maintained for all
samples analysed in the laboratory. This program is based on the general
guidelines given in EPA'a Handbook for Analytical Quality Control in
Water and Wastewater Laboratories (EP&-600/4-79-019, March 1979). This
program suggests guidelines for;
a)
Laboratory services
b)
Instrument selection
c)
Glassware
d)
Reagents
e)
Analytical performance
f)
Data handling and reporting
g)
Laboratory safety
In addition, the program will include the followings
a) Triplicate analyses are performed for each parameter on 10% of
the samples.
b) Monthly analysis of secondary quality control samples are
prepared by the laboratory manager or his designate.
c) 10% of the samples are spiked by the laboratory manager with
known amounts of the parameters of interest and re-analyzed to
determine the percent recovery. A Shewhart control chart is
used for the percent recovery control. (EPA, Handbook of
Analytical Quality Control in Water and Wastewater Laboratories,
1979.)
d) Standard curves are determined for each analysis using the
appropriate standard. Least squares linear regressions calcula-
tions are used in determining the "best fit" to the data.
Correlation coefficients are also calculated and are required to
be 1.000 over the linear range of the method.
e) Quarterly EPA Quality Control samples are obtained from the
Environmental Monitoring and Support Laboratory in Cincinnati.
The analytical results are required to be within a 951 con-
fidence level of the true value.
f) One sample per month will be sent to an outside laboratory as
part of an intra-laboratory quality control program.
The quality control program thus provides for the analysis of blanks,
blind spiked samples, and EPA quality control samples on a routine
basis. In addition, control limits are established for the operation and
maintenance of all laboratory equipment to provide strict limits on the
acceptability of'the data.
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DATA REDUCTION AND PRESENTATION
During the field measurements program, a large amount of raw field
data as well as historical data in various forms will be collected at
each site. The various data forms include:
a) Field data sheets
b) Plant operating records
c) Plant coal analysis records
d) Soils survey and geology maps
e) NO&A historical meteorological data magnetic tapes
f) NOAA local climatological data sheets
g) Plant meteorological records
h) Strip charts for continuous monitoring data
i) Laboratory analysis results sheets
These data will be both alphanumeric and numeric. The numeric data,
including the continuous monitoring data in the field as well as the
results of the laboratory analyses, will be digitized and made easily
accessible through magnetic tape. In addition, both this data and the
alphanumeric data from each site will be manipulated using computer
programs for final presentation.
The first task in the manipulation of the field data will be the
reduction or digitization of the strip chart data. This will be
accomplished using a Gerber Scientific Instrument Company Digitizer. The
following procedure will be followed for processing field data;
a) Scan strip charts for validity
b} Digitize data
c) Input data into a data file
d) Produce preliminary listings of data
e) Edit the data
1) Manually input correct data
2) Delete questionable data
3) Correct data for field calibrations
f) Produce finalized data listings
The types of field data which will be digitized and the frequency of
the Gerber readings are shown in Table 44.
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TABLE 44. TYPES OF FIELD DMA FOR DIGITIZATION
AMD FREQUENCY OF GBRBER READINGS*
Type of Field Data
Flow
Runoff pH
Runoff Conductivity
Runoff Temperature
Precipitation
Air Temperature/Relative Humidity
Solar Radiation
Evaporation
Frequency of Readings, Minutes**
15
30
30
30
15
60
60
30
* Readings refer to data points taken from the strip charts using the
Gerber Scientific Instrument Digitizer.
**A11 readings are actual values from the strip charts.
The field and historical data from each site will appear in tabular
form and/or as plots showing parameter variations with time. In
addition? a statistical analysis of the field data will be included.
Computer programs will be used to generate the tabular summaries, plots,
and statistical analysis. The final format of the data from each site
will be broken down by major categories of data as discussed below.
Tabular summaries will be generated for the following categories of
data:
a} General plant information
b) Coal data
c) Coal pile data
d) Ground water data
In addition, a summary table will be generated for each site contain-
ing the following information;
a) Number of storm events
b) Description of each storm event
1} Form of precipitation (rain, snow, sleet, hail)
2) Total precipitation
3) Duration
4) Intensity
c) Description of conditions between events
Number of antecedent dry days
102
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The meteorological data from each test site will appear both in
tabular form and as plots. Both forms of this data will be generated by
computer programs. The meteorological data will be broken down into
historical and actual field data.
Historical meteorological data for the three-month period prior to
the beginning of the field survey at each site will be presented in the
following forms:
a) A summary table of all data pertaining to:
1) Total daily precipitation
2) Average daily air temperature/relative humidity
3) Average daily solar radiation
4) Average daily evaporation
b} Plot of this daily data. Figure 19 is an example of such plots
for total daily precipitation and average daily air temperature.
As with the. historical meteorological data# the continuous field
meteorological data will be presented in tabular form as well as plots
showing variations with time.
In the same manner as the meteorological data, the runoff and base
flow data will appear both in tabular form and as plots. Each form will
be generated by computer programs. 'The runoff data will be broken down
into continuous measurement data and routine laboratory analysis data.
Included with the laboratory analysis data will be periodic rainfall pH
and acidity data.
As previously discussed, the following parameters will be .measured
continuously at each site during both storm events and dry days:
a) Flow
b) pH
c) Conductivity
d) Water temperature
This data will be presented in the following forms:
a) Summary Tables
A separate summary table will be generated for each parameter
showing all of the data collected in the field. If there is'
more than one runoff stream from a coal pile, these tables will
be presented for each stream.
103
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r\
60
O
LiJ
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b) Plots (Storm Events Only)
Two types of plots will be generated for each stormwater runoff
stream:
1) Plot of the runoff hydrograph and the rainfall hyetograph
for each' storm event. Figure 20 is an example of such
plots.
2) Plots of the runoff hydrograph and the continuous measure-
ment data (pH, conductivity, and water temperature).
Figure 21 is an illustration of these plots.
The routine laboratory analysis data will include the results of the
chemical analyses performed on stormwater runoff and dry day base flow
samples. Periodic rainfall pH and 'acidity measurements will also be
included in this category. Storm event and dry day (base flow) data will
be presented separately.
Storm event data will be presented in both of the following forms:
a) A summary table for each runoff 'stream for each storm event
showing all of the laboratory analysis results and rainfall
quality measurements.
b) Plots of the runoff hydrograph and a maximum of three
"pollutographs" {pollutant concentration versus time) on the
same figure. One or more of the continuous measurement
parameters may replace the pollutographs to show interesting
trends. For example, a figure showing runoff pH, total arsenic,
and dissolved arsenic, along with runoff flow, versus time would
be particularly useful in showing the change in arsenic
speciation with pH as a function of time.
A summary table will be generated for dry day sampling events showing
the average values of the continuous measurement data for the sampling
event and the laboratory analysis results.
The results of the statistical analysis of each storm event will be
presented in tabular form. The statistical analysis and tabular summary
will be performed by computer programs. The summary tables will include;
a) Means, coefficients of variation, and standard deviations for
all runoff data collected during a storm event.
b) Statistical summaries indicating worst case conditions monitored
during a storm event.
c) Correlation analysis of chemical parameters for each storm event.
105
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1119-011
LULU-LI
<
t-u
tu
o
a:
20
DAY l
DAY I HOURS
FIGURE 20: EXAMPLE OF RUNOFF HYDROGRAPH AND HYETOGRAPH PLOTS
-------
1119-012
O
e
>-
o
/\
CM
-J
O
o
m .1
FIGURE 21: EXAMPLE OF RUNOFF HYDROGRAPH AND CONTINUOUS MEASUREMENT DATA PLOTS
-------
The final requirement for data manipulation is the generation of a
magnetic tape containing data for direct input into the coal pile runoff
model. This will necessitate that the data be in a form which is com-
patible with the model. A detailed discussion of this data is included
¦in Section 4.
PROGRAM COSTS AND TIME SCHEDULE
The entire runoff program at each utility test site will cover a 22
week period from the initial site visit to' the final report preparation.
This period includes the 10 week runoff sampling program. The manpower
and equipment requirements for the program are discussed in the following
sections.
Manpower Requirements
.'Table 45 shows an estimate of the manpower requirements for the
runoff program broken down by major tasks and personnel categories. The
Senior Engineer/Scientist will act as project manager and review the
results of the program. The Principal Engineer/Scientist will supervise
the laboratory analysis of the water and 'coal samples. The' Engineer/
Scientist category will include the field supervisor and the computer
analyst. The field supervisor will develop the field procedures manual,
direct the field effort, analyze the results, and prepare the final
report. The computer analyst will be responsible for all computer
programs for data reduction and final presentation. The Laboratory
Technician will be responsible for performing all -laboratory analyses,
except those performed in the field. The Technician will handle the
field preparation and conduct the field work, as well as perform the
field laboratory analyses.
Other Direct Costs
Table 46 shows estimated rental and purchase costs for various equip-
ment as well as other direct costs excluding 'travel and subsistence for
the runoff program. These estimates include the cost for a drilling crew
and an outside laboratory to perform special analyses, such as determi-
nation of the percent framboidal pyrite in the coal samples. Also
included is the estimated cost for computer usage, i.e., the computer
time required for data reduction and presentation. These costs are
broken down by major task.
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TABLE 45. ESTIMATED MANPOWER REQUIREMENTS FOE
RUNOFF PROGRAM (PER TEST SITE)
Task
1. Project Management
2. Initial Site
Visit
3. Preliminary Site
Work
4. Laboratory Coal
Testing
5. Acquisition of
Additional
Background Data
6. Field Procedures
Manual
7. Field Survey
8. Laboratory Analysis
9. Data Reduction
and Presentation
TOTAL HOURS
GRAND TOTAL
Senior Principal Labora-
Engineer/ Engineer/ Engineer/ tory
Scientist Scientist Scientist Technician Technician
(Hours)
100
(Hours)
100
20
56
76
(Hours)
(Hours)
(Hours)
32
40
156
112
12
8
16
240
16
728
900
254
590
1065
100
968
2800
109
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I
TABLE 46. ESTIMATED EQUIPMENT RENTAL AND PURCHASE COSTS
AND OTHER DIRECT COSTS FOR RUNOFF PROGRAM
(Spring, 1980 Dollars)
Task 3 - Preliminary Site Work
Drilling Crew $2,200
PVC Screen and Sand 1,000
Resistivity Survey 1,500
Miscellaneous .200
Task.4- Laboratory Coal Testing
Laboratory" Expendables (Chemicals; Glassware) $ 500
Analysis for Framboidal Pyrite 2,200
Miscellaneous 50
Task 5 - Acquisition of Additional Background Data
NOAA Tapes? Geological Maps $ 200
Task 7 - Field Survey
Equipment Rental and Purchase Costs
Sequential Samplers (3) 10 wks @$5Q/wk (Rental) $1,500
Flow Meters (3) 10.wks @$75/wk (Rental) 2,250
pH Meters (3) 10 wks @$50/wk (Rental) 1,500
Conductivity/Temperature Meters (2) (Purchase) 800
Three channel recorders (2) (Purchase) 4,400
Recording Rain Gage (1) (Purchase) 950
Hygrothermograph (1) (Purchase) 400
Pyranometer (1) (Purchase) 500
Evaporation Recorder (1) (Purchase) 500
Flume or weir (2) (Purchase) 1,000
Mobile Lab (1) 10 wks @ $15G/week (Rental)
1,500
Shelter (1) (Purchase) 300
Shipping 1,000
Vehicle Rental ¦ $1,000
Expendables $1,000
- Chart paper? pH probes; buffer/solution, conductivity
cells? ice
Task 8 - Laboratory Analysis
Laboratory Expendables . $ 300
(Chemicals? Glassware)'
Task 9 ~ Data Reduction and Presentation
Computer Usage $ 900
110
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Time Schedule
Figure 22 indicates the estimated time schedule for conducting the
entire program at each utility site. The entire effort, including 10
weeks of field monitoring, will be approximately 22 weeks.
Ill
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1119-024
ET.APSED DAYS
8 .14 16 20 24 32 35 40 42 48 56
64 66 72 75 00 88 96 ]04 110 112 120 128 136 144 152
Site Visit
Preliminary
Site Work.
Laboratory
Coal Testing
Acquisition
of Additional
Background
Data
Field
Procedures
Manual
Field
Survey
Laboratory
Analysis
Data
Reduction
and
Presentation
FIGURE 22: ESTIMATED TIME SCHEDULE FOR RUNOFF PROGRAM (PER UTILITY SITE)
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SECTION 6
FIELD PROCEDURES MANUAL
INTRODUCTION
An important step in the design of the field program for monitoring
coal pile runoff is the development of a field procedures manual. This
manual will serve as a guideline or working document for conducting the
field monitoring program. Among the areas discussed in detail in the
manual are procedures for the training of field technicians, operation
and installation of meteorological, flow monitoring, and water quality
monitoring equipment, dry day sampling, and storm event sampling. In
addition, the manual covers procedures for coal sampling, coal pile and
ground water testing, sample identification and custody, sample pre-
servation, on-site chemical analyses, and sample shipping.
The field procedures manual is presented in a general manner which
is applicable to any utility site. However, once a specific utility
site is chosen, it will be necessary to modify the manual to reflect the
specific site conditions. In addition, the manual presented herein is
written in draft form. The procedures described herein will be field
tested at the two "test" sites, after which time the procedures will be
finalized. Procedures will also be added or deleted as necessary.
GENERAL RULES OF CONDUCT
During the field monitoring program there are a number of general
rules of conduct which must be followed to ensure the safety of the
field crew. All field- personnel will be briefed on site' safety
regulations at the beginning of the program. Each person will also
receive a copy of these regulations, it is expected that the field crew
will adhere to these without exception. Should any questions arise,
these should be promptly resolved with the utility contacts. Rules for
all field personnel are summarized as follows:
a) Sign in and out at the guardhouse. This must be done without
exception.
113
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b) Check each day with the utility contacts. This should be done
immediately after gaining access to the site if they are
available. Any questions regarding the site should be directed
to them.
c) Use extreme caution when walking or driving around the site.
Be aware that all trucks and trains have the right of way and
will take it. Vehicles should be driven in low gear. Observe
speed limits, flashing lights, and stop signs.
d) Make sure that all equipment is as inconspicuous as passible at
all times to prevent vandalism. The equipment shed and mobile
laboratory trailer should be kept locked when unattended.
Other responsibilities required to expedite to the program include
the following:
a) Call the nearest National Weather Bureau daily regardless of
the weather.
b) Establish a laboratory vendor for purchasing expendables such
as chemical preservatives, glassware, and filters. In terms of
preservatives, nitric acid (HNO3) and sulfuric ¦ acid
(H2SO4) will be required.
c) Make sure that everything is ready for the next sampling
event. This entails:
1) Filling the sequential sampler canisters with clean
bottles.
2) Cleaning up the mobile field laboratory.
3) Making sure that there is enough distilled water, dry ice,
chemical preservatives, and clean sample shipping bottles.
4) Contacting the courier to forewarn him that samples will
be shipped in the near future.
TRAINING OF FIELD TECHNICIANS
Due to the nature of stormwater runoff sampling, the designated
field technicians will be trained both in the laboratory and in simu-
lated field conditions before any sampling takes place. The two job
functions for conducting this type of field work are separated between:
114
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1. Technical Specialist - permanent on—site technician
2. Technical Assistant - assistant during runoff event-sampling.
The Technical Specialist will be responsible for carrying out all
aspects of the monitoring program from initial equipment installation to
the sample analyses to be performed in the mobile laboratory. He will
be the prime on-site representative of the monitoring .effort and will
remain on-site for the duration of the field program. Responsibilities
assigned to the Technical Specialist include the following;
1. Equipment operation, maintenance and calibration
2. Dry period sampling
3. Wet period sampling
4. On-site safety procedures
5. Field analyses of collected samples
6. Field preparation of samples to be shipped to the laboratory
7. Documentation of field activities
The Technical Assistant has the responsibility to be ready, on a
moment's notice, to travel to the site when a runoff event occurs and
assist in the collection, analyses and preparation of samples. This
person should not only be familar with the seven duties of'the Technical
Specialist shown above but also be most familiar with the procedures of
sample collection, preparation, analyses and documentation. His prime
duty is to lend a hand to the on-site technician at the time of a runoff
event. Once the sampling, sample preparation, analyses and documenta-
tion has been completed, the Technical Assistant will return to his
former duties.
Depending on the number of runoff streams to be monitored, -there may
be more than one Technical Assistant designated for field duty. In
either case, all field personnel will be trained together in all aspects
of the field program.
Training begins with a classroom type series of discussions on each
component of the field effort. The topics with a listing of components
is shown below:
Topic
Components
1. Field Objectives
program objectives, monitoring object-
ives, site objectives, types of .runoff
events, discrimination of data
2. Site Descriptions
climatic conditions, features of the' coal
pile, general layout of monitoring
stations
115
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3. Equipment Installation
meteorological equipment, runoff flow
measurement system, automatic sampling
devices, and continuous water quality
recorders, . field laboratory, plant
facilities
4. Equipment Operation
and Calibration
review of the operator's manual and cali-
bration procedures for each piece of
equipment including:
1. heated tipping bucket rain gage
2. hygrothermograph
3. solar pyran.ora.eter
4. evaporation recorder
5. pH meter
6. conductivity and temperature meter
7. multichannel recorder
8. sequential sampler
9. recording flow meter
10. Parshall flume
11. sample actuator
12. pH, temperature and conductivity
probes
5. Equipment Maintenance -
daily maintenance, checks for - field
calibrations, probe cleaning and
replacing, chart paper replacement,
backup devices, procedures to follow when
equipment breaks down.
The training program should be divided between classroom discussion and
hands on experience.
The second set of topics can be instructed within the chemistry
lab. It is assumed that most technical staff have had some chemical
experience in their background but for consistency in procedures, the
field analysis of samples and preparation of samples for other analyses
should be given consideration in the training of .technicians. The
following items should be reviewed:
6. Total Suspended Solids
and Total Dissolved
Solids Analysis
equipment, amount of sample, calculations,
expendables, recording data, procedures
7. Alkalinity/Ac id ity
Analysis
equipment, amount of sample, calculations,
expendables, recording data, procedures
8. Filtering Metals for
Dissolved Analysis
equipment, procedures,
recording data
calculations,
116
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9. Preservation and
Refrigeration of EPA procedures, logging samples in,
Samples for Shipment - labeling instructions
10. pH of Rain - equipment, procedures, recording data
Once the first 10 topics have been discussed, the training should be
centered on the actual site specific applications' for all the pro-
cedures. With the field equipment on hand, the instructor should give a
series of instructions to each technician, in the form of a site set-up
sequence, and allow him to physically set-up and start the equipment
into operation. Different set-ups can be chosen for practice and the
following minimal situations should be simulated;
11. Dry Weather Base Flow
Monitoring
composite sampling; calibration checks on
the flow meter, pH, conductivity and
temperature probes; sample frequency;
contingency procedures
12. Pre-storm Event
Procedures
13. Wet Weather Sampling
pre-storm, monitoring of precipitation, ad-
justing all equipment for runoff monitor-
ing, alerting Technical Assistant, pre-
paring all sample containers and mobile
field laboratory
estimating the length of the storm;
selecting sample frequencies; final
equipment status check; collection, pre-
paration and analyses of samples
14. Reporting and
Documentation
daily site log, sample preparation
log, analytical log, equipment
maintenance log, sample labeling, sample
custody procedures
15. Post storm Event
Procedures
reprogram sequential sampler and flow me-
ter, calibration checks on continuous
monitors, verification of meteorological
data, shipment of samples to analytical
laboratory
The training session should conclude by allowing the technicians to
ask questions. Emphasis should be placed on the historical problems in
dealing with stormwater runoff programs. The idiosyncrasies of each
piece of equipment should be spelled out and the detection of a faulty
piece of data or faulty equipment operation should be of prime concern.
Keeping the training rigorous from the start with as much hands-on
practice as possible can only help simplify the procedures when the
first storm event occurs. Finally, the training in this type of study
117
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should be considered an ongoing process. Having the trained technicians
install the equipment and even practice a trial run using simulated
runoff, e.g., a fire hose discharging through the flume, can only help
prevent mistakes during the crucial storm' event¦monitoring.
ACQUISITION OF REPRESENTATIVE COAL SAMPLES
As part of the preliminary site work (prior to the 'actual runoff
sampling program), representative coal samples will be obtained from the
coal pile for laboratory testing. This will be conducted in two
phases. Phase I will involve determining the overall coal variability.
Phase II will-entail collecting a sufficient number of samples to pro-
vide representative coal quality data.
'Phase I - Sampling for Determination, of Coal Variability
The traverse method will be employed to determine coal variability.
This is a systematic method for obtaining coal samples along a traverse
of the entire coal p i le. This method is described in Appendix A of ASTM
procedure D-2234. Appendix B of this report includes this method.
Phase II - Collection of Coal Samples for precision
The methodology as described in Section 7 of ASTM procedure D-2234
will be used to obtain representative coal samples for laboratory
analysis. Phase I will determine the number of coal samples required.
This method is 'described in detail in Appendix B.
Each coal sample should be placed in a zip lock bag for preser-
vation. The samples should be shipped to the chemical laboratory as
soon as possible after collection.
COAL PILE HYDROLOGY AND GROUND WATER TESTS
Coal pile hydrology tests to be conducted as part of the preliminary
site work include determination of the average percent moisture content
of the coal pile and water infiltration through the pile. The ground
water tests to be performed include determination of average percent
moisture content and infiltration rates, as well as the depth to ground
water, or ground-water elevations.
118
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Coal Pile Hydrology Testa
Standard drilling techniques will be used to determine the moisture
content in the pile on a preliminary basis. Five to ten hollow stem
auger borings, depending on the size of the coal piles, and split spoon
samples obtained every five feet will be used ' to collect discrete
samples for determination of the variation of moisture content with
depth in the unsaturated zone. Piezometers consisting of slotted PVC
pipe with Ottawa sand packed in the ' lower part of the annulus and a
bentonite seal above the zone of interest will be used both as a
monitoring well for determining the depth to the saturated zone and as a
sampling point for water quality.
Surface resistivity techniques will also be used to determine the
depth of the saturated zone. The results of the resistivity survey and
the drilling program will be used to construct a contour map of the top
of the saturated zone in the pile.
The drilling program and the resistivity survey will be conducted by
an outside drilling crew. The field crew will be on hand at all times
to supervise the drilling and obtain the coal samples. The' moisture
content of the discrete sample will be determined in the field according
to ASTM procedure D3302. This procedure is included in Appendix C.
The field crew will also be responsible for obtaining water samples
'from the coal pile for laboratory analysis. A total of five samples
will be obtained at various locations throughout the pile. These should
be treated in the same manner as the runoff and base flow samples (see
Section 6, "Sample Preservation Procedures and Field Laboratory
Analyses").
Infiltration rates into the coal pile will be determined using ASTM
procedure D3385. This procedure is described in Appendix D. A double
ring permeameter or inf iitrometer will be used to measure these rates.
Ground Water Tests
In the same manner as the coal pile hydrology tests, the average
percent soil moisture content and soil infiltration rates will be
determined in the vicinity of the coal pile. In addition, ground water
elevations will be determined periodically. A total of five ground
water samples will also be obtained for laboratory analysis. (See
Section 6, "Sample Preservation Procedures and Field Laboratory
Analyses".
SITE SETUP (EQUIPMENT INSTALLATION)
The installation of equipment
only through the assistance of the
and facilities will be accomplished
specific utility at which the program
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is located. There are four categories of equipment which have to' be
installed in order to monitor the coal pile for runoff. . Each of these
is detailed below. But prior to ' any equipment setups,- the project
manager will meet with the utility plant manager and the foreman in
charge of the coal pile to arrange for certain facilities. A descrip-
tion of these follows.
Utility-Assistance
Once a coal pile has been selected for runoff monitoring, the
following information should be collected and studied prior to meeting
with the utility personnel.
1. Aerial photographs of the coal pile
2. Topographic map of the coal pile area
3. Location of the natural drainage patterns of the runoff water
4. Determination of whether the pile is lined, diked or ditched on
the perimeter
At the 'meeting, the focus of discussion should center on con-
structing permanent facilities for monitoring flow. ¦ It would be to the
advantage of the utility to install a flume or weir, depending on the
topographic configuration of the area around the pile, not only for this
program but to be used as a permanent primary device for monitoring
runoff flow. A flume would be recommended for coal piles built in flat
terrains. it should be permanently mounted' in a concrete slab with the
coal pile dike or ditch butting on the converging' section of the flume.
For coal piles built on hills or slopes the use of a weir with quiescent
chamber is recommended. In either case each device should be mounted in
a permanent, concrete structure.
. Other items to be considered by the utility are the pouring of three
concrete slabs adjacent to the flow device as depicted in Figure 23.
These will be used for monitoring an instrument shelter and ¦ meteoro-
logical station. Assistance will also be required for bringing in AC
power to both the runoff monitoring station and a mobile field labora-
tory. Fresh water will have to be connected to the field laboratory but
this can easily be done by garden hose hookups.
A summary of utility assistance items necessary prior to instal-
lation of a runoff monitoring station are listed in Table 47.
Once an agreement has been made between the project team and the
utility for the following items, the installation of equipment can begin.
120
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1119-009
PORTABLE
ALUMINUM-
SHELTER
_ 24-HOUR
WALL CLOCK
RECORDING
FLOW —
METER
EVAPORATION
RECORDER ,
HYGROTHERMOGRAPH
pH METER
HEATED
TIPPING
BUCKET
RAIN
GAUGE
_ SOLAR
PYRANOMETER
CONDUCTIVITY
<— AND
TEMPERATURE
METER
MULTICHANNEL RECORDER
pH, CONDUCTIVITY AND'
, TEMPERATURE RECORDERS
WITH FLOW SENSOR AND
SAMPLE INTAKE
ICE
COOLER
SEQUENTIAL
SAMPLER
DIKE
COAL PILE
DIKE
FIGURE 23: SCHEMATIC OF COAL PILE RUNOFF MONITORING STATION
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TABLE 47. SUMMARY OP UTILITY ASSISTANCE ITEMS IN ORDER
TO MONITOR COAL PILE RUNOFF
1. Dike or ditch the coal pile area.
2. Locate and 'construct a permanent flow monitoring station '(flume or
weir),
3. Pour concrete slabs for locating an instrument shelter and meteoro-
¦ - logical station.
4. Provide power to the instrument station and mobile field laboratory.
5. Provide water to the field laboratory.
Flow Monitoring Station
The coal pile runoff project team will assist the utility in the
design of a primary flow device. Important design criteria for the flow
device would include:
1. Design flow - calculated from the Rational Formula using 1.5 times
the flow from the 10 year 24 hour storm
2. Materials - the highly acidic character of the runoff stream
warrants the use of non-corrosive materials such as
fiberglass, acid resistant concrete, and high grade
stainless steel such as Carpenter 20.
For the runoff monitoring program accurate measurements of .flow are
mandatory. Because both wet weather flows and dry weather base flows
are to be measured, a combination of measuring devices is recommended.
A large flume or weir built for a design storm would be installed per-
manently to measure the wet weather conditions. For dry weather base
flows a small "V" notch 90° weir built downstream of the flume would
be installed because of its inherent accuracy at low flows. This weir
would be a temporary device to be used only for the monitoring program.
A detachable weir plate would be made so that this weir would not
restrict flows in times of wet weather. Also the flow meter to be used
on the flume, through a quick change of sensors and internal programming
cards, can be used for both flow devices. An illustration of the flume
with various dimensions and capacities is shown in Figure 24. An
illustration of the combined flume and "V" notch weir is shown in Figure
25.
122
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1119-025
i-1
N3
OJ
16i
FIGURE 24; GENERAL SCHEMATIC OF A PARSHALL FLUME'
(Reprinted, with permission, from "Planning and Making Industrial Waste Surveys,"
page 15. Copyright, Ohio River Valley Water Sanitation Commission, 414 Walnut
Street, Suite 900, Cincinnati, OH 45202 -- 1952.)
Q
SLCTlON N-N
Creot-
t? ;!.t.»t»UXu.,.
ifnV* ArqW
SECTION L-L
(kIkVv Angit
LEGEND
W Size ot fliime, In lnchoa or feet.
A Usniitli of side wall of converulnB suction,
2/3 A Distance bitelt from end of crust to itugu point.
I) Axial lunBtl) of convertfinK section.
C Width of downstruiim end of flume.
D Width of upatruitm end of flume.
(S Depth of flumii,
l» Ujiiuth of throut,
(I Length of diverging section.
K Difference in olevntlon between ltwier ami of flume
und crest.
U Length of approach floor,
N Depth of depression In throut below crest.
P Width between ends of curved wlna iviilla,
It lliidlna of curved wing wiill. ''
X Horizontal distance to lib gage point from low point
In throut.
V Vertical distance to lib gage point from low point In
thiotvl.
Dimensions and capacities of the Parslutil measuring flume, for various throat widths, IV
CMjMicUy
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-------
1119-008
CONCRETE PAD
FLOW MONITORING
STILLING WELL
BED LOAD
SAMPLE
COLLECTOR
V" NOTCH WEIR
DIKE'
PARSHALL FLUME
CONCRETE PAD
FIGURE 25: SCHEMATIC OF FLUME AND "VM NOTCH WEIR FLOW STATION
-------
Installation of the flow recording device would be performed after
the primary devices have been installed. A bubbler type flow meter
would be used because of simplicity of installation and maintenance.
The meter itself is housed in the instrument shelter and powered by AC.
Two bubble tubes would be used: one on the flume and one mounted 4 times
the "V" notch height behind the weir plate. Confirmatory flow readings
will be taken from staff gages mounted on the wall of the converging
section of the flume and on the approach to the weir plate. These staff
gages can also be used to calibrate the flow meter by referring to stage
versus discharge tables for each device. All bubbler tubing will be
routed by electric conduct between the instrument shelter .and primary
devices. The bubble flow meter can be wall mounted and should have a
spare parts box located nearby. The spares box will contain desiccant
replacement/ spare flow programming cards, spare recorder paper and
spare ink cartridges. The installation of the flow meter system can be
checked by having a water line, i.e. fire hose, discharge through the
flume and by calibrating the meter accordingly.
Runoff Monitoring Station
Besides the flow system, the runoff monitoring station will include
continuous recorders for pH, conductivity and temperature together with
the automatic sequential wastewater sampler. The wastewater'sampler is
also housed within the instrument shelter. A pump inlet velocity of at
least 1400 milliliters per minute is specified in order that most of the
susupended solids are captured. The automatic sampler is programmable
and ail dial settings will be set depending on the type of samples to be
collected. The most critical parameter in the installation of the
sampler is the position of the intake tubing. The inlet tubing should
be mounted upstream of the neck of the flume and in a position not to be
susceptible to runoff bedload effects. This may conflict with the
ability to sample the initial flows of a runoff stream during a storm
event. An adjustable arm for holding the inlet tubing should therefore
be installed so that the sampler may collect samples from any vertical
position upstream of the flume. Spare parts to be kept with the sampler
include spare pump tubing, desiccant, small hose clamps and extra sample
collection bottles.
Conductivity, pH and temperature sensors will be mounted on the
flume or within a stilling well on the flume for the continuous record-
ing of all parameters. Conductivity and temperature will be recorded
from the same probe and meter but the separate analog signals will be
recorded individually. pH will have its own meter and channel on the
recorder. -Sensor cables from each of these probes will be routed though
electrical conduit between the instrument shelter and the flow channel.
Analog meters will be used to have a visual indication of the data
coming from each probe. The pH, conductivity and temperature meters can
be either wall mounted* or installed in a rack also holding the multi-
channel recorder. The wall mounted setup is shown in Figure 23. Care
must be taken when submerging the probes in the runoff stream due to the
125
-------
high acidity of the water. Experience has shown that iron oxide can
quickly foul the pH and conductivity probes. Therefore daily obser-
vations of probe fouling and deterioration must be made by the Technical
Specialist. Also all probes should be either plastic or teflon coated
to avoid corrosion. Spare items to be kept with the continuous metering
devices will include:
1. Spare probes for all sensors
2. Desiccant
3. Calibration buffers for pH and solutions for conductivity
4- ASTM thermometer
5. Spare chart paper, ink and pens for the multi channel recorder
Meteorological Station •
The meteorological station will consist of four instruments, three
of which are battery powered and one which is AC powered. The station
consists of:
1. Solar pyranometer
2. Evaporation recorder
3. Hygrotheraograph
4. Heated typing bucket rain gage (AC powered)
All four instruments are to be mounted on level surfaces and their in-
dividual locations should be sited according to the following criteria.
1. Solar pyranometer - in an open space away from any
obstructions that may block the sun's
rays. Also it should ' be kept away
from heavy traffic areas due- to the
sensitivity of the recorder pen to
ground vibrations.
2. Evaporation recorder - in a non-shaded area away from heavy
traffic areas.
3. Hygrothermograph
on a level surface inside a louvered
shelter which will allow free passage
of air. Ground vibrations can also
affect its recorder sensitivity.
4. Heated Tipping Bucket-
Rain Gage
absolutely away from all ground^
vibrations, on a level platform and
close to a power source. This
instrument will record snowfall when
the heater has been turned on and for
all other cases will record precipi—
126
-------
Heating Tipping Bucket (Cont) - tation. This gage should be at least
four' times the height of the closest
obstruction away from that obstruc-
tion so that wind effects are minimal.
Figure 23 depicts the meteorological station, adjacent to the runoff
monitoring site but as is the case around most utility coal piles, this
is in an area of intense heavy traffic movement. Therefore the meteoro-
logical station should be positioned out-of-the way in a field or vacant
lot within the confines of the power plant. Roof installations should
be avoided so that the field technician will not have to walk too far in
order to check on the equipment's operation. Spares for the meteoro-
logical equipment can be kept in the instrument shelter and consist of
charts, pens, batteries, ink, desiccant, etc.
Mobile Field Laboratory
Prior to sampling any runoff, a field laboratory must be sited and
set-up in order to handle the samples once they have been collected at
the monitoring station. & 20 x 8 foot mobile laboratory is of suffi-
cient size to handle the storage, sample preparation and analysis of 4
to 5 parameters. Assistance from the utility will be necessary in the
form of -a power source and freshwater inlet. If at all possible, the
sink drain should be directed into a holding tank.
The general layout for the laboratory is shown in Figure 26. It
includes specified bench areas for the following tasks:
1. Storage and logging of incoming samples
2. Sample labeling and preservation with acids
3. Filtering for metals and solids
4. Titration for acidity and alkalinity
5. Cleaning and washing area
6. Ice making and refrigerated sample storage
A checklist of items to be included in the field laboratory is found
in Table 48. Many of the items are expendable so provisions should be
made to have plenty on hand. Once the laboratory has been moved to its
field location, it should be set-up on blacks and leveled. The scale
will have its own leveling screws but the trailer should be as level as
possible before use. A heater/air conditioner along with plenty of
storage cabinets is recommended for comfort and ease of equipment mani-
pulation.
127
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1119-007
SAMPLE
PRESERVATION
AREA
INCOMING
SAMPLES
pH METER
3-™
EUME HOOD
! HOT PLATE !
9
VACUUM
EILTER
JILTER
HOLDER
ICE
CHEST
ICE
CHEST
TANlT^
DRY ICE-
MAKER
SCALE
o-o—o
BURETTE
STAND
pll METER
I 1 PIPETTE
I | CLEANER
MAGNETIC
STIRRER
lililililil.l
DRYING RACK
HEATER/AC
POWER IN-
FIGURE 26: SCHEMATIC FOR A 20' x 8' MOBILE FIELD LABORATORY FOR
ANALYSIS OF COAL PILE RUNOFF WATER
-------
TABLE 48. CHECKLIST FOR MOBILE FIELD LABORATORY
1. Heater/AC 3.
2. Fume hood/hotplate
3 Vacuum Filter
4. Millipore filter holder
5. Filters
6. Burette stand and burettes
7. Two pH meters (portable)
8. Magnetic Stirrer
9. Drying oven
10. Scale
11. Pipette cleaner
12. Drying rack for glassware
13. Water still or demineralizer
(Type II Reagent Grade Water)
14. C0£ Tank/Dry Ice Maker
15. Graduated cylinder
16. 200 and 500 ml beakers
17. Assorted flasks
18. Squeeze bottles
19. Pipettes, squeeze bulb,
tweezers
20. Concentrated nitric and
sulfuric acids
21. Paper towel, kemwipes
22. pH paper, eyedroppers,
rubber gloves
23. Lab markers, labels
24. Insulated shipping containers
25. 250 nil polyethylene sample
bottles
26. Log book, analytical
reference manuals
DAILY EQUIPMENT STATUS CHECKS
Calibrations
Calibration of the equipment used at the runoff monitoring station
is essential to a field program where reliable data is to be generated.
By either adjusting an instrument to a calibration curve or adjusting
the raw data from the instrument to a calibration curve, the reduced
field data will be more accurate.' Procedures for calibrating a par-
ticular instrument are normally found in the instruction manual accom-
panying the instrument. The frequency of calibrations is usually not
stated in the instrument manual and is established according to the fre-
quency of use of the equipment. Table 49 presents a frequency of cali-
bration and field calibration checks for each piece of equipment
illustrated in Figure 23.
Field calibration checks are a system of procedures to quickly check
the zero, span and overall operation of each piece of equipment while it
is being used in the field. These checks will let the Technical
Specialist know when a certain instrument has drifted out of calibration
or if maintenance is required. For the solar pyranometer, evaporation
recorder and tipping bucket rain gage quick checks can be made for zero
and span. The hygrothermograph can be calibrated in the field against
an ASTM thermometer and wet/dry bulb sling psychrometer. Daily checks
should be made by the Technical Specialist on the recording .flow meter
and pH meter because these instrument sensing units may be grossly
affected by the low pll and iron deposits in the 'runoff stream.
129
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Conductivity and temperature meters can be checked on a weekly basis.
AH calibration and field check data is to be kept in a separate log
book which is maintained by the Technical Specialist onsite.
TABLE 49. FREQUENCY OF CALIBRATIONS AND FIELD CALIBRATION CHECKS
Equipment
Full Calibration
Field Check
1. Solar Pyranometer
2. Evaporation Recorder
3. Hygrothermograph
4. Heated Typing Bucket
5. Sequential Sampler
6. Recording Flow Meter
7. pH Recorder
8. Conductivity/Tempera-
ture Recorder
once every three months once every two weeks
pre and post field monitoring
pre and post field monitoring
once per month
once per month
daily
daily
weekly
Status Checks and Equipment Maintenance
The purpose of equipment status checks is to insure that all mon-
itoring equipment, especially the automated devices, is in a' state of
readiness so that once a storm event happens, the samples are collected
and continuous data is recorded without interruption. Figure 27
provides a sample check list to be used by the onsite Technical
Specialist on his daily rounds to each runoff station. All checklists
will be kept on site in a separate log book. From' this log the history
of each piece of equipment while in the field can be traced.
The only time that a daily site check is omitted is during a runoff
sampling event. In this case other monitoring site documentation will
be used. Once a storm event has ceased and all the equipment is put
back into the dry weather mode, the Technical Specialist will continue
with his status checks.
DRY WEATHER SAMPLING
' Coal pile runoff samples will be collected once per day at each
runoff point and composited to form one sample. The use of automatic
sampling equipment is not necessary during dry weather sampling. Grab
sampling techniques will be used on dry days.
130
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Figure 27: Daily Equipment Status Check List
Project. No. Runoff Station
its Date
Instruments
TS
o
(0
¦—i
04
o
&
-P
u
x:
o
'O
.
u
-------
Flows of dry weather runoff resulting from seepage from the base of
the pile will be continuously measured by using the "V" notch weir plate
and the recording flow meter. Samples are to be collected from the same
point and at the' same time of day for each dry weather day. The dis-
charge from the weir plate is the recommended grab sampling point.
Sampling should occur once the•equipment status checks have been com-
pleted .
The routine procedures to be followed on a dry weather day are
itemized as follows;
1. Install "V" notch weir plate, reposition flow bubble line at
weir and readjust the flow meter for size and capacity of
weir. (This should be completed immediately after each storm
when the flow approaches base flow.)
2. Perform daily equipment status checks (refer to the' previous
Section).
3. Using clean one liter glass bottles, collect a sample from the
discharge from each runoff station weir remembering to keep the
time of sampling consistent.
4. Place an event mark on the flow record and the pH, conductivity
and temperature records indicating that a dry weather sample
was taken.
5. Return the samples to the field laboratory and pour each 1
liter sample into a large beaker capable of containing all run-
off samples.
6. Stir the collected sample and split the composite into indi-
vidual sample containers.
7. Perform the field analyses and preservation on the composite
samples.
8. Log in the dry weather sample and record the results of the
field analysis.
9. Clean the 1 liter collection bottles, compositing beaker and
associated glassware used in the analyses and preservations.
10. Check on the weather forecast and make the necessary pre-
parations if a precipitation event is likely.
132
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WIT WEATHER SAMPLING
Anticipation of a Storm'Event
The Technical Specialist will have the responsibility to monitor
weather forecasts in • the area of the site so that basic preparations
necessary before sampling can be accomplished. There are various ways
to keep an eye on the weather, e.g. TV reports, radio, etc., but one of
the best Methods is to arrange a contact with the nearest National
Weather Service that maintains a weather radar. The closest National
Weather Service station is most likely at the closest national airport.
Weather radar may or may not be used but it is the best method to have
confirmatory information on the approach of precipitation. Once a storm
event has been predicted, the Technical Specialist must perform the
following at each runoff station:
1. Make a final check on the meteorological instruments to insure
there is enough chart paper to last at least through the pre-
cipitation period. Changing charts in the middle of a storm
can lead to wet charts and blurred data.
2. Remove the "V" notch weir plate and clean out the bed load
sediment trap between the flume and weir.
3. Check on the pH, conductivity and temperature probes to see
that they are responding and operational.
4. Check the sequential sampler's intake strainer for debris.
5. Check that the sample activator switch is in its correct
position. This device will only be used when a storm event
occurs at night or at times when the site technician is not
available to turn on the sampler.
6. Check that the flow meter bubble line is in its proper position
in the flume.
7. Check the multichannel recorder to see that there is enough
chart paper.
8. Turn all runoff monitoring instruments to "ON".
9. Call the Technical Assistant and alert him of the approaching
storm. The -assistant should make plans to travel to the site
once the runoff event has been confirmed.
10. Make ready a second set of sample collection bottles in case
the event lasts long enough to fill the first set of bottles.
The Technical Specialist should' be ' ready for the storm -event no
matter what time of the day it starts. If the storm is to break during
133
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the night, the technician should put the equipment on automatic so that
sampling for the initial storm runoff can be accomplished. If the storm
breaks during the day, the technicians should manually start the sampler
once the flow has risen above base flow.
Event Sampling
The Technical Specialist must be able to differentiate a runoff
event from a non-runoff storm event. There will be many cases when the
precipitation will be of such light intensity that either no runoff will
be observed or there will be ;a lag in the timing of the runoff. For the
purposes of this program only those storms causing the runoff to
increase above base flow will be considered storms. Table' 50 lists the
types of storms desired during the program and the frequency of sampling
for each runoff stream. There may be cases when sampling may have
commenced and after the samples have been collected it is determined
that the runoff event duplicated the conditions of a previous event. If
this situation arises the Technical Specialist should confer with the
project manager to determine whether the samples should be prepared for
analyses or thrown out. The final decision can be made only by the
project manager.
TABLE 50. STORM TYPES TO BE SAMPLED WITH CORRESPONDING SAMPLE FREQUENCY
Storm
Frequency
24 hour*
12 hour
4 hour
2 hour
1/2 hour for the first four hours,
1/2 hour for the first four hours,
1/2 hour for runoff duration
1/2 hour for runoff duration
1 hour after 4 hours
1 hour after 4 hours
*24 hour refers to the length of time the runoff hydrograph is above
base flow.
Procedures to be followed by the Technical Specialist during a
runoff event are listed below:
1. Monitor the runoff stream and record visual observations of the
character of the runoff, e.g. color, intensity, flow peak, etc.
2. Monitor all the automatic recorders and equipment to'see that
they are recording properly.
3. When the initial samples (first four hours) have been
collected, switch the automatic sampler to a 1 per hour rate.
134
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4. Call the Technical Assistant if the amount of laboratory work
anticipated requires his presence. For most storms where
sampling occurs through the night, the assistant will be
required.
5. Place event marks on all records and charts indicating the
start of sampling, storm number, data and time,
6. Once the runoff has dropped back to base flow make an estimate
of the volume of bed load sediment trapped between the flume
and weir and collect a representative sample' for moisture con-
tent determinations.
7. After the runoff has ceased, make the necessary adjustments for
dry weather monitoring.
8. Once a set of samples has been collected, carry them to the
field laboratory and perform the preservations and analysis.
9. Collect a sample from the rain gage for pB and acidity
analysis. ' Clean out the rain collector once the sample has
been collected.
10. Clean off all probes immersed in the runoff stream, all sample
intakes and bubblers from the flow meter. Desiccant charges,
on instruments having them, should be checked also.
SAMPLE IDENTIFICATION AND CUSTODY PROCEDURES
In order to avoid confusion in the handling of water samples, a
system for numbering the sampling stations and identifying samples is
crucial. In addition, custody procedures are necessary to track the
samples from the time of collection through laboratory analysis. Sample
shipping procedures are also an important part of the field program.
Each of these areas will be discussed in this section.
Number of Sampling Stations and Sample Identification
All sampling'stations will be identified with three-digit -numerical
codes. For example, if there are two sampling stations for a particular
program, these would be identified as site #001 and #002 respectively.
Each sample shipping bottle will be pre-labeled with sticky back
waterproof labels. The following example shows the format of the labels
and the information to be pre-printed. on each:
135
-------
Project No.
Date
1234-A12
Sample Ho,
Analysis
HOC
Cool, 4°C 5 H2S04 to pH 2
Preservation
Sample Type
In the field, the only information that has to be entered on the labels
is the date, sample number, and sample type (i.e., surface water, ground
water, precipitation, or coal pile water).
Sampling Custody Procedures
Sample custody procedures will be established to ensure that the
samples are not lost prior to chemical analysis. These procedures will
consist of a number of data sheets which will be used to track the
samples. - in the field, each sample will be entered into a sample log
sheet prior to being packed for shipping to the chemical laboratory.
Figure 28 is an example of the log sheet showing the information to be
entered. A copy of this sheet will be included with the samples being
shipped.
When the samples arrive at the- chemical laboratory, ' a laboratory
check-in sheet will be completed prior to storing the samples in the
cold ¦ storage room. This .sheet will be kept outside of the storage
room. Figure 29 is an example of this sheet. At the same time, a
Request for Water Analysis sheet, as shown in Figure 30, will be. com-
pleted and submitted to the laboratory director.
When samples are to be taken' from the cold storage room for
analysis, a laboratory checkout sheet will be completed. As with the
check-in -sheet, this sheet will be kept outside of the cold storage
room. Figure 31 is ail example of this sheet.
After the chemical analyses have been performed, a report of water
analysis sheet, as shown in Figure 32, will be filled out and sent to
the project manager. In addition, all chemical analyses performed in
the field will be entered on one of these sheets with a copy mailed to
the project manager.
The project manager and laboratory director will each retain a copy
of all data sheets and will be responsible for setting up individual
data files.
Sample Shipping Procedures
A courier will be chosen to deliver the sample shipping boxes to the
chemical laboratory. The location of the utility site will determine
136
-------
OJ
•^1
cn id t-1
o
o
p n
13 0
fl> "-!¦ P)
H (II ft
< O (->¦
By
Time Preserved
Preservation
Method
Reserved for
Analysis of
w
o
%
H
n>
t-i
o
iQ
W
cr
(D
n>
rf
Volume of Sample
Date Shipped to
Chem. Lab
Shipping Box No.
-------
FIGURE 29: INITIAL SIGN IN SHEET
All samples must be logged in when they are Initially
stared in the cold room.
PROJECT NO.
SAMPLE ID
DATE
SAMPLE
COLLECTED
DATE/TIME
ENTERED
COLD ROOM
INITIALS
138
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FIGURE 30: REQUEST FOR.WATER ANALYSIS;
CLIENT: ; LABORATORY NO:
CONTRACT NO,: NUMBER OF SAMPLES:.
SENT BY: : DATE RECEIVED:
REPORT TO: BY DATE COMPLETED:
ESTIMATED TIME FOR ANALYSIS: !
SURFACE WELLWATER CITY WATER WASTE WATER_ SEA WATER_
1
2
3
4
5 ¦
S
7
8 | 9
Demand Analysis;
BOD5
|
TOC
COD
Residue Analysis;
Total Solids
Volatile Solids
Fixed Solids
Total Suspended Solids
Total Dissolved Solids
Nitrogen Constituents:
Total Kjetdshl Nitrogen
Ammonia
Organic Nitrogen
Nitrate
Nitrite
Phosphatase
Total
ortho
Condensed
Physical Analysis:
Color
Odor
Turbidity
PH
Oil and Grease
Sulfate
Cyanide
Phenol
Fluoride
Chloride
Alkalinity
Acidity
Hardness
Detergent (MBAS)
Specific Conductance
Metals (Specify)
Others (Specify)
Notes: Split Sample Yes No.
Form CL-003
139
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FIGURE 31: SIGN OUT SHEET
All samples taken from the cold room must be
signed out and also signed in when they are
returned.
REASON
FOR DATE DATE
PROJECT NO. SAMPLE ID REMOVAL REMOVED INITIALS RETURNED INITIALS
140
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FIGURE 32: -REPORT OF WATER ANALYSIS
Client: , Laboratory No:_
.Contract Nq: ; ' 'Date R«ceived:_
Reviewed by: ; Date Reported;_
Reported tc: ; : Type(s) of Sampie(s):_
mg/L as
1
2
3
4
5 '
6
7
S
Notes:
ANALYZED:
CHECKED:
Form CL.-004
141
-------
I
whether air or land transportation is necessary. The main objective is
to transport the samples to the chemical laboratory in as short a time
as possible. This will ensure that the integrity of the samples is
maintained prior to analyses.
The courier should be contacted as soon as the field crew has an
idea when the samples will be preserved and packed for shipping. A
location at the 'Utility site will be designated as the pickup paint. At
the time of pickup, the field crew will give the courier a packing list
indicating the number of shipping boxes and the contents of each. The
courier will then specify the waybill number (i.e., shipping number) and
all other pertinent shipping information, including the name of the air-
lines or trucking company, the flight number, and the delivery date and
time. The field crew will convey this information to the person at the
laboratory receiving the shipment.
The shipping boxes should be made of metal to avoid serious damage
during shipping. In addition, the boxes should be insulated with some
type of foam or other packing material as added protection and also to
keep the samples cool. ' Dry ice will be added to the boxes to preserve
the integrity of the samples. The shipping address should be clearly
visible on the boxes.
SAMPLE PRESERVATION PROCEDURES AND FIELD LABORATORY ANALYSES
This section discusses the procedures to follow when compositing,
filtering and preserving samples. In addition, the laboratory analyses
to be performed in the field are also discussed.
Sample Preservation
Table 51 indicates the parameters to be analyzed in the stormwater
runoff and base flow samples, the volume required for each analysis, the
proper preservation method, and the maximum holding time for each. A
minimum of 1275 ml of sample will be required for each sample. This
will necessitate that three sequential sampler bottles be filled during
the storm event {each bottle holds approximately 460 ml of sample) which
will be composited to produce one sample for analysis. During dry day
events the individual grab samples from each base flow stream will be
composited to again produce one sample.
Compositing Samples
Equipment Required: 1500 ml beakers
Magnetic stirrer
Stirring bars
142
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TABLE 51. SAMPLE VOLUMES, PARAMETERS TO BE ANALYZED,
PRESERVATION METHODS, AND MAXIMUM HOLDING TIMES
(IS
Parameter
Sample Volume, ml
Preservation Method
Maximum
Holding Time (2)
Acidity/Alkalinity
Total Suspended Solids (TSS)
Total Dissolved Solids (TDS)
Total Organic Carbon (TOG)
Sulfate (SO )
Total Hardness
100
100
100
25
50
100
Cool, 4 C
Cool, 4°C
Cool, 4°C
Cool, 4°C, M^SQ^ to pH
Coal, 4°C
Cool, 4°C, HK03 to pH 2
24 hrs.
7 days
7 days
24 hrs.
¦ 7 days
6 mas.
Metals:
Aluminum (Al!
Antimony (Sb)
Arsenic (As)
Beryllium (Be)
Cadmium (Cd)
Calcium (Ca)
Chromium, Total (CrT)
Cohalt (Co)
Copper (Cu)
Iron (Fe)
Lead (Pb)
Magnesium (Ma)
Manganese (Mn)
Molyldenum (Mo)
Nickel (Si)
Selenum (Se)
Vanadium (V)
Sine (Zn)
Fluoride (F)
300
(3)
Mercury (Eg)
Total: HNO^ to pH
Dissolved: Filter on site;
HNO to pH 2
300
200!4)
Total = 1275 nil
None Req'd
¦Total: HH03 to pH 2
Dissolved: Filter on sitet
EN03 to pH 2
6 IBOS.
6 mos.
7 days
13 days
13 days
1 Sample volumes, preservation methods, and holding times taken from Methods for Cheatictl ftnlysis
of Water and Wastes, EFA-600/4-79—020, March 1979.
^ 'EPA has proposed extending these holding times {Federal Register, Tuesday, December 18, 1979,
Vol.'44, No. 244, pp. 75050-52).
200 ml for dissolved metals? 100 nil for total metals.
100 ml for dissolved mercury? 100 nil for total mercury-
143
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Procedure: Pour the contents of the three automatic
bottles (storm events) or the grab sample bottles
(dry weather events) corresponding to one sample
into the beaker. Place the beaker on the magnetic
stirrer. Stir rapidly about one minute to obtain a
homogeneous mixture.
Filtration Method For Dissolved Metals and Dissolved Mercury
The samples for dissolved metals and dissolved mercury must be
filtered on site prior to shipping. Mercury is distinguished from the
other metals because of the difference in maximum holding times. The
samples should be filtered as soon as possible after collection.
¦ Equipment Required; 2 Suction Pumps
2-47 mm Millipore Filtration Funnels
2 Filtration Flasks
0.45 Millipore Filters
500 ml Beakers
100 ml Graduated Cylinders
Magnetic Stirrer
Nitric Acid (HN03)
Stirring Bars
pH Meter and Probe
Buffer Solutions
Procedure; 1. Filter a small portion of the composite
sample to rinse the filter flask and discard.
2. Filter 300 ml of the composite sample. The
filter may become clogged if a large amount
of particulate is present. If filtration
slows, change the filter and continue.
3. Pour the filtrate into the 500 ml beaker and
place on the magnetic stirrer. Immerse the
pH probe. While stirring, add nitric acid
(HNO3) until the pH is less than 2.
4. Place the sample in a 500 ml sample bottle.
Preserving Samples
The preservation procedures for the various parameters are discussed
below. Before pouring off each split, insure the suspension of all par-
ticulate matter by stirring the composite sample on the magnetic
stirrer. Table 52 shows which parameters can be combined to reduce the
144
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number of sample bottles. Note that although the preservation pro-
cedures for 304 and fluoride are -different (Cool, 4°C and none
required respectively), they will be combined in one¦bottle because the
shipping box will be cooled with dry ice.
TABLE 52. SAMPLE STORAGE BOTTLES AND CORRESPONDING PARAMETERS
Parameters Sample Bottle Required(*)
Acidity/Alkalinity; TSSj TDS 500 ml
TOC 25 ml
F. S04 500 ml
Total Hardness; Total Metals, Total Hg 500 ml
Dissolved Metals; Dissolved Hg 500 ml
{*) All bottles are plastic.
Equipment Required;
500 ml Beakers
100 ml Beakers '
Magnetic Stirrer
¦Stirring Bars
Pipets
Graduated Cylinder
pH Meter and Probe
Buffer Solutions
25 ml Plastic Bottles
500 ml Plastic Bottles
Nitric Acid (HNO3)
Sulfuric Acid {H2SO4)
Procedure:
Ac idity/Alkalinity
TSS, and TDS:
Pour 300 ml of the composite sample' into a 500
ml sample bottle and keep the bottle cool.
Total Organic
Carbon
Pour 25 ml of the composite sample into the
.100 ml beaker and place on the magnetic
stirrer. Immerse the pH • probe. While
stirring, add sulfuric acid (H2SO4) until a
pH of less than 2 is obtained. Pour the sample
into a 25 ml sample bottle and keep cool.
Sulfate and
Fluoride:
Pour 350 ml of the composite sample directly in-
to a 500 ml sample bottle and keep cool. No pre-
servative is needed.
145
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Total Hardness
Total Metals,
Total Mercury
Pour 300 ml of the composite sample into the 500
ml beaker and place on the magnetic stirrer. Im-
merse the pH probe. While stirring, add nitric
acid (ENO3) until the pH is lowered to less
than 2. Place the preserved sample in a 500 ml
sample bottle.
Field Laboratory Analyses
Acidity/alkalinity, total suspended solids (TSS), and total dis-
solved solids (TDS) will be analyzed in the mobile field laboratory.
The analysis methods as specified in Methods for - Chemical Analysis of
Water and Wastes, EPA—600/4-79-020, March, 1979, will be followed.
These methods are discussed in detail in Appendix H. Acidity and
alkalnity are determined titrimetrically. TSS and TDS analyses are
gravimetric methods.
146
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REFERENCES
1. EPA-600/2-77-199 Sampling and Modeling of Non-Point Sources at a
Coal-Fired Utility by TRC-The Research Corporation of New England for
the Industrial Environmental Research Laboratory, Research Triangle
Park, N.e.
2. University of Florida, stormwater Management Model.User's Manual,
Version II, EPA-670/2-75-Q17, March 1975.
3. U.S. Army Corps of Engineers, Hydrologic Engineering Center,
723-S8-L7520, August 1977
4. Hydrocomp, Inc., "Modeling Pesticides and Nutrients on -Agricultural
Lands", EPA-600/2-76-043, February 1976.
5. EPA, "Pyritic Systems: A Mathematical Model," EPA-R2-72-QC2,
November 1972.
6. Ohio State University, "Resources Allocation to Optimize Mining
Pollution Control," EPA-600/2-76-112, November 1976.
7. Anderson, J.A., Runoff Evaluation and Streamflow Simulation by Com-
puter, U.S. Army Corps of Engineers, Portland, Oregon,'May 1971.
8. Adams, R.T., and Kurish, F.M., "Simulation of Pesticide Movements on
Small Agricultural Watersheds", Sept. 1976.
9. TRC — The Research Corporation of New England, "Sampling and Modeling
of Non-Point Sources at a Coal-Fired Utility", EPA-600/2-77-199,
September 1977.
10. Tennessee Valley Authority, "Characterization of Coal Pile Drainage,"
EPA-600/7—79—051, February, 1979.
11. Anderson, William C., "System Treats Coal Pile Leachate and Municipal
Wastewater Together," Water and Wastes Engineering 15(3), March 1978.
12. Monsanto Research Corporation, "Source Assessment: Water Pollutants
from Coal Storage Areas," EPA 600/2-78-004in, May 1978.
-13. Davis, E.C., Boegly, W.J., "A Review of the Literature on Leachates
from Coal Storage Piles," ORNL/TM/6186, January 1978.
147
-------
.14. Weeter, Dennis W., "Coal'Pile Water Quality Management Results of a
National Survey," Symposium on Ground Water Effects of Power Pro-
duction Activities. "Spring AGO meeting, April 1978.
15. Wewerka, E.M. and J.M. Williams, "Trace Element Characterization of
Coal Wastes — First Annual Report," EPA-600/7-78-028, March 1978.
16. Ohio River Valley Water Sanitation Commission, "Planning and Making
Industrial Waste Surveys," April 1952.
148
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APPENDIX A
COAL FIRED POWER
FOR ASSESSMENT
TREATMENT DESIGN
PLANT QUESTIONNAIRE
OF COAL STOCKS AND
OF COAL PILE RUKOFF
-------
COAL FIRED POWER PLANT Page 1 of 4
QUESTIONNAIRE
for
Assessment of Coal Stocks and Treatment Design
of
COAL PILE RUNOFF
TRC Project: 1119-B80-00
Client: EPA-IERL-RTP and Edison Electric Institute
General Information for Each Plant
Plant Name Utility
Ci ty,State
Type of Plant, Check One: Base Load_ Peaking
Total Plant Capacity MW % Usage Coal
I Coal Pile Information
J Is there segregation between live storage and reserve storage piles? If not, explain_
. Is the coal rotated within the pile? . What
type of surface are the piles constructed on? (Clay, Compacted Coal, Compacted Ash, etc.)
For Reserve or Non Segregated Piles
PILE CHARACTERISTICS
Person Responding to
Questionnaire
Title
Phone No.
Pile Id.
No.
Volume
(tons)
Average Pile
Height Width Length
(ft.) (ft.) (ft.)
Side Slope
(ft.vert./ft.horiz.)
Storage Time
at Plant
(months)
Is the Pile
Compacted
1
5
-------
COAL FIRED POWER PLANT QUESTIONNAIRE Page 2 of 4
COAL CHARACTERISTICS PER PILE
Pile Id. Coal Coal Source Avg. % Avg. BTU Avg. % % Pyritic Avg. % Is the
No. Rank Seam County.State Sulfur Content Moisture Sulfur Ash Coal Cleaned
1
Are there seasonal changes with reserve or nonsegregated pile sizes? Please explain
Additional Comments
>
I
-O
PILE CHARACTERISTICS
Pile Id,
No.
Volume
(tons)
Height
(tons)
For Live Storage Piles
Width
(ft.)
Length
(ft.)
Side Slope
(ft.vert./ft.horiz.)
Storage Time
at Plant
(months)
Is the Pile
Compacted
1
5
-------
COAL FIRED POWER PLANT QUESTIONNAIRE
page j or q
V — —
I COAL CHARACTERISTICS PER PILE~
Pile Id. Coal Coal Source Avg. % Avg. BTU Avg. % % Pyritic Avg. % Is the
No. Rank Seam County,State Sulfur Content Moisture Sulfur Ash Coal Cleaned
1 ,
2 _____
3 ___
4 _________
5
Are there seasonal changes with live pile sizes? Please explain
>
i
Additional Comments:
Coal Pile Runoff Treatment Design
1. Has a treatment or control system been designed for coal pile runoff at this plant? If yes, please
provide the following.
2. Is the runoff from all piles treated? If not, which piles are treated?
3. At what time (month & year) did the treatment system go on line?
4. Provide the name and address of the person responsible for the treatment design:
-------
COAL FIRED POWER PLANT QUESTIONNAIRE
Page 4 or 4
5. Lish the design criteria used at this plant:
Design Storm Size Source of This Design Storm Data
Tech. Paper 40, Local Data, Other
Design Runoff Flow From: __ .
. Rational Formula, On-Site Data, Other
If the rational formula was used, what runoff coefficient was selected?
Do you collect runoff from areas not specifically coal storage?_ If yes, what type of areas?
6. List the types of treatment or control used at this plant:
Are the coal piles diked? ¦ , How
Is the runoff directed through a flow measuring device? What type device_
Is the runoff treated for:
Flow Equalization How
TSS Removal How_
pH Neutralization How_
A, Metals Removal How_
Other
7. List the types of data normally collected on site for control, design or treatment of coal pile runoff.
Coal pile runoff water quality Which parameters
8. Continuous or Periodic Monitoring of
Runoff pH . Precipitation
Runoff Temperature Ground Water Quality
Runoff Conductivity _______________ Ground Water Level
Runoff Flow
Runoff Other
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APPENDIX B
STANDARD METHODS FOR COLLECTION
OP A GROSS SAMPLE OF COAL
"Reprinted, with permission, from the Annual Book of ASTM. Standards,
Part 26. Copyright, American Society for Testing and Materials,
1916 Race Street, Philadelphia, PA 19103."
B-l
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teSSSi ANSl/ASTM D 2234 - 78
Standard Methods for
- ¦ COLLECTION OF A GROSS SAMPLE OF COAL1
This Standard is issued under the fixed designation. D 2234; the number immediately following the designation indicates
the year of original adoption or. in the case of revision the year of Jast revision- A number in parentheses indicates the
year of last reapprovai.
INTRODUCTION
Data obtained from coal samples are used in establishing price, controlling mine
and cleaning plant operations, allocating production costs, and determining plant or
component efficiency. The task of obtaining a sample of reasonable weight to repre-
sent an entire lot presents a number of problems and emphasizes the necessity for
using standard sampling procedures.
Coal is one of the most difficult of materials to sample, varying in composition
from noncombustible particles to those which can be burned completely, with all gra-
dations in between. The task is further complicated by the use to be made of the ana-
lytical results, the sampling equipment available, the quantity to be represented by the
sample and the degree of precision required.
These standard methods give the over-all requirements for the collection of coal
samples. The wide varieties of coal handling facilities preclude the publication of de-
tailed procedures for every sampling situation. The proper collection of the sample
involves an understanding and consideration of the physical character of the coal, the
number and weight of increments, and the over-all precision required.
L Scope
LI These methods cover procedures for the
collection of a gross sample under various
conditions of sampling. The gross sample is to
be crushed and further prepared for analysis
in accordance with Method D 2013,2 How-
ever, the procedures for dividing large gross
samples before any crushing are given in this
standard.
1.2 These methods describe genera! and
special purpose sampling procedures for coals
(/) by size and condition of preparation (for
example mechanically cleaned coal or raw
coal) and (2) by sampling characteristics.
2. Applicable Documents
2.1 ASTM Standards:
D43I Designating the Size of Coal from
Its Sieve Analysis-
D20I3 Preparing Coal Samples for Anal-
ysis2
E 177 Recommended Practice for Use of
the Terms, Precision, and Accuracy as
Applied to Measurement of a Property
of Material3
3. Summary of Methods
3.1 General-purpose sampling procedures
are intended to provide a precision of ±Ko of
the ash content of the coal sampled in 95 out
of 100 cases. To obtain a stated precision in
terms of other constituents, the special pur-
pose sampling procedures should be used. ,
3.2 Special purpose sampling procedures
apply to the sampling of coal when other pre-
cision limits are required, or when other con-
'These methods are under the jurisdiction of ASTM
Committee D-5 on Coa! and Coke nnd are the direct
responsibility of Subcommittee D05.23 on Sampling.
Current edition approved Oct. 29, 1976. Published
December 1976. Ori
-------
D 2234
stituents are used to specify precisian, or for
performance tests.
3.3 For coals of known size and condition
of preparation, tables are given for the deter-
mination of the number and weight of incre-
ments required for a gross sample for both
general and special purpose sampling. For
coals having known sampling characteristics,
as determined by the use of appropriate test
and statistical procedures given in these
methods, the number and weight of the incre-
ments required for either general purpose or
special purpose precision can be determined.
3.4 The procedures appear in the following
order:
Method Section
Sampling of Coals Based on Size and Con-
dition of Preparation ...' 7
General-Purpose Sampling Procedure . 7.1
Number and Weight of Increments 7.1.2
Number of Gross Samples 7J.4
Special Purpose Sampling Procedure .. 7.2
Number and Weight of Increments 7.2.2
Number of Gross Samples 7.2.3
Sampling of Coals Based on Known Sam-
pling Characteristics 8
Principles of Sampling by Sampling
Characteristics 8.1
General Purpose Sampling Procedure . 8.2
Number and Weight of Increments 8.2.1
Number of Gross.Samples 8.2.2
Special Purpose Sampling Procedure .. 8.3
Number and Weight of Increments and
Number of Gross Samples 8.3.2
Division of the Gross Samples Before
¦¦ Crushing ; 9
Sampling of Coal for Moisture Determina-
tion 10
Types of Moisture Samples 10.1
Entire Gross Samples 10.1.1
Special Moisture Subsarnples 10.1.2
Other Subsarnples for Moisture Testing 10.1.3
Special Precautions 10.2
Weight of Increments 10.3
Number of Increments 10.4
Moisture Sampling Based on Known Sam-
pling Characteristics 10.4.1
Moisture Sampling Based Only on Size .. 10.4.2
4. Definitions ' ,
4.1 accuracy;
4.1.1 generally, a term used to indicate the
reliability of a sample, a measurement, or an
observation.
4.1.2 specifically, a measure of closeness of
agreement between an experimental result and
the true value. Example: the observed and
true sulfur content of a coal consignment.
This measure is affected by chance errors as
well as by bias.
4.2 air drying—a process of partial drying
of coal to bring it near to equilibrium with the
atmosphere in the room in which further re-
duction and division of the sample is to take
place. *
4.3 analysts sample—final subsample pre-
pared from the original gross sample but re-
duced to 100 percent through No. 60 (250-
pin) sieve and divided to not less than 50 g.
4.4 bias {systematic error)—an error that
is consistently negative or consistent!}' posi-
tive. The mean of errors resulting from a se-
ries of observations which does not tend to-
wards zero.
4.5 chance error—error that has equal
probability of being positive or negative. The
mean of the chance errors resulting from a
series of observations tends toward zero as the
number of observations approaches infinity.
4.6 consignment—a discrete amount of
coal, such as a shipment, a carload, a unit
train, or a day's production. A consignment
may include more than one lot of coal and
may correspond to a specified period of time
such as a sampling period or billing period. -
4.7 error—difference of an observation or a
group of observations from the best obtain-
able estimate of the true value.
4.8 free impurity—the impurities in a coal
that exist as individual discrete particles that
are not- a structural part of the coal and that
can be separated from it by coal preparation
methods.
4.9 gross sample—a sample representing
one lot of coal and composed of a number of
increments on which neither reduction nor
division has been performed.
4.10 increment—a small portion of the lot
collected by one operation of a sampling de-
vice and normally combined with other incre-
ments from the lot to make a gross sample.
4.11 inherent ash—the residue remaining
from the inherent impurities after ignition
under conditions specified for the ash determi-
nation.
4.12 inherent impurity—the inorganic ma-
terial in coal that is structurally part of the
coal and cannot be separated from it by coal
preparation methods.
4.13 lot—a quantity of coal to be repre-
sented bv a cross sample.
B-3
-------
4.14 precision—a term used to indicate the
capability of' a person, an instrument, or a
method to obtain reproducible results: specifi-
cally, a measure of the chance error as ex-
pressed by the variance, the standard error, or
a multiple of the standard error (see Recom-
mended Practice E 177).
4.15 representative sample—a sample col-
lected in such a manner that every particle in
the lot to be sampled is equally represented in
the gross sample.
4.16 sample—a quantity of material taken
from a larger quantity for the purpose of esti-
mating properties or composition of the larger
quantity.
4.17 sample division—the process whereby
a sample is reduced in 'weight without change
in particle size.
4.18 sample preparation—the process that
may include air drying, crushing, division and
mixing of a gross sample for the purpose of
obtaining an unbiased analysis sample.
4.19 significant loss—any loss that intro-
duces a bias in final results that is of appreci-
able economic importance to the concerned
parties. "
4.20 size consist—the particle size distribu-
tion of a coal.
4.21 standard deviation—the square root of
the variance.
4.22 subsample—a sample taken from an-
other sample.
4.23 systematic error (see 4.4 bias)
4.24 top she—the opening of the smallest
screen in the series upon which is retained less
than 5 percent of the sample (see Method D
431).
4.25 unbiased sample (representative sam-
ple)—a sample free of bias.
4.26 variance—the mean square of devia-
tions (or., errors) of a set of observations: the
sum of squared deviations (or errors) of indi-
vidual observations with respect to their arith-
metic mean divided by the number of obser-
vations less one (degrees of freedom); the
square of the standard deviation (or standard
error).
4.26.1 random variance of increment
collection (unit variance), sr3—the theoretical
variance calculated for a uniformly mixed lot
and extrapolated,..to,J lb.(0.5 kg).increment.
size. For a method of estimating this variance
see Appendix Al.
D 2234
.. 4.26.2 segregation variance of increment
collection, ss*—the variance caused by non-
random distribution of ash content or other
constituent in the lot. For a method of esti-
mating this variance see Appendix Al.
4.26.3 total variance. s0*—the over-all var-
iance resulting from collecting single incre-
ments, and including division and analysis of
the single increments. For a method of esti-
mating this variance see Appendix A2.
5, Increment Collection Classification
5.1 The type of selection, the conditions
under which individual increments are col-
lected, and the_ method of spacing of incre-
ments from the coal consignment or lot are
classified according to the following descrip-
tions and Table 2. These designations are to
be used for sampling specifications and for
descriptions of sampling programs, and sam-
pling equipment.
5.2 Types of Increments—The types of
selection of increments are based on whether
or not there is human discretion in the selec-
tion of the pieces of coal or portions of the
coal stream.
5.2.1 Type I, in which specific pieces or
portions are not subject to selection on a dis-
cretionary basis. This includes that in which
the increment is collected in precise accord
with previously assigned rules on timing or
location that are free of any bias. Type I
selection increments generally yield more ac-
curate results.
5.2.2 Type II, in which some measure of
human discretion is exercised in the selection
of specific pieces of coal or of specific por-
tions of the stream, pile, or shipment.
5.3 Conditions of Increment Collection—
The conditions under which individual incre-
ments are collected are the conditions of the
main body of coal relative to the portion
withdrawn. Four conditions are recognized.
5.3.1 Condition A (Stopped-Belt Cut), in
which a loaded conveyor belt is stopped and a
full cross-section cut with parallel sides is
removed from the coal stream. The distance
between the parallel faces shall not be less
than three times the diameter of the largest
piece.
. 5.3.2 Condition B (Full-Stream Cut), in
which a full cross-section cut is removed from
a moving stream of coal.
B-4
-------
#
5.3-3 Condition C (Pan-Stream Cut), in
which a portion, not a full cross section, is
removed from a moving stream of coal.
5.3.4 Condition D (Stationary Coal Sam-
pling), in which a portion of coal is collected
from a. pile, a rail car, a barge, or a shiphold.
5.4 Spacing of Increments—The spacing of
increments pertains to the kind of intervals
between increments. Two spacing methods are
recognized: systematic and random. System-
atic spacing is usually preferable.
5.4.1 Systematic Spacing 1, in which the
movements of individual increment collection
are spaced evenly in time or in position over
the lot.
5.4.2 Random Spacing 2, in which the in-
crements are spaced at random in time or in
position over the lot.
6. Organization and Planning of Sampling
Operations
6.1 Precaution—It is imperative that every
gross sample be collected carefully and con-
scientiously and in strict .accordance with the
procedures prescribed in these methods; for if
the sampling is done improperly, the sample
will he in error and it may be impossible or
impracticable to take another sample. How-
ever, if the analysis is in error; another anal-
ysis can easily be made of the original sample,
except for moisture.
6.2 Selection of Appropriate Sampling
Procedure—Variations in coal-handling facili-
ties make it impossible to publish rigid rules
covering every sampling situation in complete
and exact details. Proper sampling involves an
understanding and proper consideration of the
minimum number and weight of increments,
the size consist of the coal, the condition of
preparation of the coal, the variability of the
constituent sought, and the degree of preci-
sion required.
6.2.1 Number and Weight of Increments—
The number and weight of increments re-
quired for a given degree of precision depends
upon the variability of the coal. This varia-
bility increases with an increase in free im-
purity. A coal high in inherent impurity and
with comparatively Little free Impurity may
exhibit much less variability than a coal'with
a low inherent impurity and a relatively high
D 2234
proportion of free impurity. For most prac-
tical purposes, an increase in the ash content
of a given coal usually indicates an increase in
variability. It is imperative that not less than
the minimum specified number of increments
of not less than the minimum specified weight
be collected from the lot. For Condition D the
increments shall be of equal weight.
6.2.2 Increment Collection Method to Be
Used—In order to obtain complete represen-
tation of all sizes, it is most desirable that the
sample increments be withdrawn from the full
cross section of the stream. The best possible
increment is a full cross-section cut removed
from a stopped belt; Classification I-A-l in
Table 1. The best possible increment from a
flowing stream of coal is one obtained by
moving a cutter device entirely across the
stream at a uniform speed, the same for each
increment, into one side of the stream and out
of the other, without allowing the receptacle
to overflow (Classification I-B-l in Table 1).
Classification methods given in Table 1 are
listed in order of decreasing reliability. The
highest possible classification . method,
wherever feasible, should be used. Details of
sampling procedures should be agreed upon
in advance by all parties concerned. When-
ever circumstances dictate utilization of incre-
ment collection classifications "Condition C"
or "Condition D" or "Type IF*, details of
sampling procedure shall be agreed upon in
advance by all parties concerned.
6.3 Distribution of Increments—It Is essen-
tial that the Increments be distributed,
throughout the lot to be sampled. This distri-
bution is related to the entire volume of the
lot, not merely its surface or any linear direc-
tion through it, or over it. If circumstances
prevent the sampler from applying this princi-
ple, the lot is sampled only in part, and the
gross sample is representative only' of this
part. The spacing of the increments shall be
varied if the possibility exists that increment
collection may get "in phase" with the se-
quence of coal variability. Example: routine
sampling of commercial coal from a contin-
uous stream (conveyor belt), where increment
collection is automatic and its sequence coin-
cides with the "highs" or "lows" in the con-
tent of fines.
6.4 Dimensions of Sampling Device—The
B-5
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opening of the sampling device shall be at
least 2lh to 3 times the top-size of the coal.
However, for practical reasons if is recom-
mended that the opening of any sampling de-
vice be not less than llU in. (31.8 mm),
regardless of the top size of the coal. In sam-
pling from a moving - stream, the effective
width is the width projected perpendicular to
the relative direction of the stream (Note 1).
The sampling device shall be of sufficient
capacity to completely retain or entirely pass
the increment without loss or spillage.
Note 1: Geometry of Cutting Samples from
Moving Streams—Consider the geometric plane
that is common to the directions of the cutter
movement and of the stream being sampled as
shown in the vector diagram in Fig. L In this plane,
determine a, the angle between these two directions.
Draw the vectors Vc and V.. so that their lengths are
proportional to the velocities of the cutter and of
the stream, in the common plane. See Fig. 1(a)-
Join the origins of these vectors to give Vr the
vector of stream movement relative to the cutter
and to get angle /S. Apply this angle to a scaled
cross section of the sample cutter with Wa being the
actual width in the direction of travel. See Fig. I (h).
Measure Wc, the effective cutter width as the
width in the relative direction of the stream. When
angle fi differs appreciably from 90 deg the height
of the cutter blades must be sufficient to prevent
contamination of sample by particles bounced off
the leading face of the cutter.
6.5 Movement of Sampling Device—In
sampling from moving streams of coal the
sampling device shall be designed to minimize
disturbance of the coal, thereby avoiding sep-
aration of various coal densities and sizes or
both. To prevent segregation and rejection
due to disturbance of the coal stream, practi-
cal evidence indicates that the velocity with
which the sampling instrument travels through
the stream shall not exceed 18 in./s (457
mm/s).
6.6 Preservation of Moisture—The incre-
ments obtained during the sampling period
shall be protected from changes in composi-
tion due to exposure to rain, snow, wind, sun,
contact with absorbent materials, and ex-
tremes of temperature. The circulation of air
through equipment must be reduced to a min-
imum to prevent both loss of fines and mois-
ture-. Samples in which moisture content is
importanT'shall be "protected from excessive
air flow and then shall be stored in moisture-
tight containers. Metal cans with air-tight
D 2234
lids, or heavy vapor-impervious bags, properly
sealed, are satisfactory for this purpose.
6.7 Contamination—The sampling ar-
rangement shall be planned so that contami-
nation of the increments with foreign material
or unrelated coal is avoided.
6.8 Mechanical System Features—'With
mechanized systems, it is essential that the
system as a whole including the sample cutter,
chutes, conveyors, crushers and other devices
be self-cleaning and nonclogging and be de-
signed in a manner that will minimize the
need for maintenance.
6.9 Personnel—Because of the many varia-
tions in the conditions under which coal must
be sampled, and in the nature of the material
being sampled, it is essential that the samples
be collected under the direct supervision of a
person qualified by training and experience
for this responsibility. Where human labor is
employed to collect the increments, it is essen-
tial that samples be collected by a trained and
experienced sampler or under the direct per-
sonal observation of such a- person. This in-
cludes sampling for the purpose of deter-
mining sampling characteristics of a coal or
characteristics of a particular sampling appa-
ratus.
6.10 Criteria of Satisfactory Performance
—A satisfactory sampling arrangement is one
that takes an unbiased sample at the desired
degree of precision of the constituent for
which the sample is to be analyzed. One fun-
damental characteristic of such an arrange-
ment is that the size consist of the sample will
adequately represent the true size consist of
the coal. Sampling systems shall be tested ini-
tially and at regular intervals to determine
whether the sample adequately represents the
coal. In addition, sampling systems should be
given a rough performance check as a matter
of routine. This is done by comparing the
weight or volume of collected sample with
that of the total flow of coal, to assure a con-
stant sampling ratio.
6.11 Relative Location of Sampling and
Weighing—It is preferable that coal be
weighed and sampled at the same point in
time. If there is a lapse in time between these
two events, consideration should be given by
both purchaser and seller to changes in mois-
B-6
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... ®
ttire during this interval and the consequent
shift in relationship of moisture to the true
quality of the coal at the instant when owner-
ship of the coal transfers from one to the
other.
7. Sampling of Coals Based on Size and
Condition of Preparation
7.1 General-Purpose Sampling Procedure:
7.1.1 The general-purpose sampling pic.re-
dure is intended For a precision such that if
gross samples are taken repeatedly from a lot
or consignment and one ash determination is
made on the analysis sample from each gross
sample, 95 out of 100 of these determinations
will fall within ±Ko of the average of al! the
determinations. Under some conditions, as
detailed in 6.2.1 and 6.2.2, Condition C and D
and Type II, this precision may not be ob-
tained.
7.1.2 Number and Weight of Increments—
Obtain the number and weight of increments
as specified in Table 2 except as provided in
7.1.5.2. Determine the minimum number of
increments from the condition of preparation,
and determine the minimum weight of each
increment from the top size of the coal. Clas-
sify the coals to be sampled according to the
genera! purpose procedure into three groups
by top size. Further classify each of these
groups into two subgroups in accordance with
the condition of preparation. These classifica-
tions are shown in Table 2.
7.1.3 Variations in construction of the
sampling device and flow, structure, or size
consist of the coal may make it impracticable
to collect Increments as small as the minimum
weight specified in Table 2. In such cases, col-
lect an increment of greater weight. However,
do not reduce the minimum number of incre-
ments, regardless of large excesses of indi-
vidual increment weights. Table 2 lists the
absolute minimum number of increments for
general purpose sampling which may not be
reduced except as specified in 7.1.5.2. Other "
considerations may make it advisable or nec-
essary to increase this number of increments.
7.1.4 Number of Gross Samples—Under
the general-purpose sampling procedure, for
quantities up to approximately 1000 tons (908
Metric~Toris) (908 Mg) it is recommended
that one gross sample represent the lot. Take
D 2234 -
this gross sample in accordance with the re-
quirements prescribed in Table 2.
7.1.5 For quantities over 1000 tons (90S
Mg), use any of the following alternatives:
7.1.5.1 Take separate gross samples for
each 1000-ton lot of coal or fraction thereof.
7.1.5.2 Use one gross sample to represent
the total tonnage provided the number of in-
crements, as stated in Table 2, are increased
as follows:
/total lot size (tons or Mg) ...
A • — A'T A / — — — — (i)
V 1000 tons or 908.Mg
where:
Ni = number of increments specified in
Table 2, and
A'2 = number of increments required.
For example, a 4000-ton (3632-Mg) lot
will require twice the number of increments
specified in Table 2. Using this technique,
theoretically it is possible to collect one gross
sample to represent a lot of infinite tonnage.
However, practical experience indicates maxi-
mum size of a lot of coal to be represented by
one gross sample should not exceed 10 000
tons (9080 Mg).
7.2 Special-Purpose Sampling Procedure:
7.2.1 This special-purpose sampling proce-
dure shall apply to the sampling of coal when
increased precision is required, and the only
knowledge of the coal is its top size and con-
ditions of preparation.
7.2.2 Number and Weight of Increments—
Take the same number and" weight of incre-
ments per gross sample as specified in Table
2, or as specified in 7.1.5.3.
7.2.3 Number of Gross Samples—To ob-
tain increased precision for the laboratory
result for a given consignment, increase the
number of gross samples collected from that
consignment and analyze each gross sample
separately, reporting the average of results.
To reduce errors to one half, that is, to "dou-
ble" the precision, take four times as many
gross samples. Similarly, -to reduce errors to
one third, to "triple" the precision, take nine
times as many gross samples.
8. Sampling of Coals Based on Known
Sampling Characteristics
8.1 Principles' of Sampling 'by "Sampling
Characteristics:
B-7
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#
8.1.1 The relationship between sampling
characteristics (expressed' as variances ) and
the number of increments which will give a
desired precision (expressed as-the specified
variance of one gross sample) is shown as fol-
lows:
ATf = (s/ + s*/ mRsc* - uS/F) (2)
where:
iVf = the number of increments in one gross
sample,
W = the weight in pounds of each incre-
ment; this is selected for convenience
or by the limitations imposed by the
particular mechanical sampling appa-
ratus,
sr- = the random variance of a 1-Ib (0.5-fcg)
increment; this value is obtained from
the special sampling program given in
Appendix A1 (Note A1),
S32 = the segregation variance, this value is
also obtained from the special sam-
pling program given in Appendix A1
(Note A I),
sda* = the variance of division and analysis-
Procedures for calculating this quan-
tity are given in Appendix A2 of
¦ ASTM Method D 2013.
P = the number of analysis samples (pre-
pared independently from the same
gross sample), and
Jo2 = the specified variance of one gross
sample. The procedure for . deter-
mining this variance is given in 8.1.2
and 8.1.3.
Note 2—The random variance and the segrega-
tion. variance, s,1 and s/. are each inflated by un-
known amounts of variance due to division and
analysis. Since this results in an increased numer-
ator in Eq^ 2, and consequently, a larger calculated
number ot increments, JV,, it can he considered a
"safety factor" for the sampling program. How-
ever, if too many large increments are taken
for the evaluation of s.-z and" s,', the "safety factor"
may become unreasonably large. . .
8.1.2 The relationship between the specified
variance of one gross sample, sa\ and the
precision for the result of several gross sam-
ples in one test period, expressed as the test
period variance, sT2, is given as follows:
5r* - SaVNa (3)
where:
sTz = the test" period variance,
sa2 = the specified variance of one gross
sample, and
¦ D 2234
jVc ¦= the number of gross samples in the test
period.
8.1.3 Fig. 2 shows the relationship between
variance and sampling precision (plus or
minus percent of a given constituent. 95 cases
out of 100). The variance (Fig. 2) can be ei-
ther the test period variance, .vT2, or the spe-
cified variance of one gross sample. sGz, This
choice will depend upon the sampling situa-
tion to be evaluated. The sampling precision
(Fig. 2) can be based on any coal constituent,
provided it is expressed as a percentage of
that constituent. The following example Is an
illustration of the calculations necessary to
determine the number of increments for one
gross sample:
8.1.3.1 Accuracy Limits—Assume a coal of
6.5 percent average ash content. If the desired
accuracy is of the ash content, the sam-
pling accuracy can be expressed as ±0.65 per-
cent ash.
8.1.3.2 Test Period Variance—The accu-
racy limits given in 8.1.3.1 correspond to a
test period variance,- jT2, of 0.112, from Fig.
2 (Line 1).
8.1.3.3 Specified Variance of One Gross
Sample—The specified variance of one gross
sample is equal to the test period of variance,
srz, multiplied by the number of gross sam-
ples in the test period, Nc (Eq 3). Assuming
seven gross samples in the period, the speci-
fied variance for one gross sample is then
equal to 0.112 x Tor 0.784.
8.1.3.4 Number of Increments—Assume
the following Information was obtained from
the special sampling procedures outlined in
Appendix AI of this procedure and Appendix
A2 of ASTM Method D 2013: Jr2 = 12.5, j,1
= 10.2, and sdc* = 0.06 (one analysis sample
per gross sample). The specified variance of
one gross sample, sc\ as found previously, is
0.784. Further, the weight per increment for
this sampling device, is found to be 50 lb (23
kg). Then, substituting into Eq 2:
N, - (10.2 + 12.5/50)/{0.784 - 0.06/1)
= 14.4 or 15 increments
For this coal, 15 increments of 50 lb (23 kg)
each would be required for each gross sample,
and seven gross samples would constitute the
sampling period. The weighted average for the
test "period will be within ±0.65 percent' ash,
95 cases out of 100.
8.1.4 The following variance relationship
B-8
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can be derived from Eq 2. It combines the
random variance, sr% and the segregation
variance, ss2. This derivation is applicable
when the incremental weight is fixed by the
characteristics of the sampling equipment:
fT2 - l(sj - sda*)/NcN,) + [s^/N^) (4)
where:
s,-1 = the over-all variance for single incre-
ments (including division and analysis),
as determined by Appendix A2.
Other terms are as defined in 8.1.1 and 8.1.2.
The following example demonstrates the use
of the overall variance for increments, s„3, in
determining the number of increments for one
gross sample:
8.1.4.1 Test Period Variance—Assume a
required accuracy of ±0.5 percent ash. This
corresponds to a test period variance, sT2, of
0.066 from Fig. 2 (Line 2).
8.1.4.2 Number of Increments—Assume
the following information was obtained from
the special sampling procedures outlined in
Appendix A2 of ASTM Method D 2013,
and Appendix A2 of this procedure: sa2 = 3.5
and sa
-------
#
riod variance. sT2. In, this case, use the new
sampling precision limitations in Fig. 2.
8.3.4 Other precision limits may be used or
other constituents may be used to specify pre-
cision when agreed upon by the parties con-
cerned. The principles outlined in this section
will apply to all special precision limits.
3.3.5 Greater accuracy cannot be obtained
by merely increasing the -weight and number
of increments if significant bias exists.
9. Division of the Gross Sample Before
Crushing
9.1 In the case of very large and unwieldy
gross samples, it is permissible to divide the
gross sample to reduce its weight, provided
the following conditions are fulfilled:
9.1.1 If the entire gross sample is mixed in
a suitable blender (double cone or twin shell
tumbler) it is permissible to divide the sample
using the schedule of Table 2. Test the divided
sample for bias. •
9.1.2 If each very large increment is re-
duced in quantity by secondary sampling,
take at least six secondary increments from
each primary increment: The method of
collection of secondary increments must be
proved to be free from bias. In no case shall
the weight of a secondary increment be less
than shown in the schedule of Table 2.
10. Sampling of Coal for Total Moisture
Determinations
10.1 Types of Moisture Samples—-Mois-
ture determinations as specified in the method
to be employed,, are to be made on the fol-
lowing kinds of samples.
10.LI Entire Gross Sample—For referee
tests, air dry the entire gross sample and
measure"the weight loss from the entire gross
sample during this drying. This procedure can
be carried out an the entire grass sample as a
single batch or on groups of primary incre-
ments, or as separate operations on the indi-
vidual primary increments: but obtain, by one
of these means, the total weight loss from the
entire gross sample. After this air drying, the
sample can be crushed or divided or both as
required by the referee test for moisture.
10.1.2 Special Moisture Subsample—For
D 2234 '
moisture testing, a. special subsample can be
taken from a gross sample before any opera-
tions of air drying or crushing. Take this sub-
sample from the gross sample in accord with
the requirements of Section 9.
10.1.3 Other Subsamples far Moisture
Testing—For moisture testing, a subsample
can be used that is collected after the initial
crushing and dividing of a gross sample. The
procedures for the crushing and dividing, and
for this subsequent stibsampling for moisture,
are given in Method D 2013.
10.2 Special Precautions—Collect samples
and subsamples for moisture in such a
manner that there is no unmeasured loss of
moisture of significant amount. Make ade-
quate weighings before and after drying or
other operations to measure all significant
weight losses. ~ . . _ .
10.3 Weight of Increments—The minimum
weight of each increment must be that which
is sufficient as to be free of bias. This depends
on the top size of the coal in the stream being
sampled, the dimensions of the collection de-
vice, and other factors of the withdrawal of
the increment. Since much of the moisture
tends to be distributed uniformly across the
surface, moisture bias is present when the size
consist of the sample is not the same as the
size consist of the tot sampled. In addition,
when there is no knowledge of the sampling
characteristics for moisture, each increment,
shall weigh not less than the values in Table
2.
10.4 Number of Increments—The number
of increments required for a given degree of
precision depends on the weight of the incre-
ments. the distribution of the moisture, and
the total amount of moisture. However, the
distribution of moisture is not easily evaluated
independent of total moisture; consequently,
the combined effects can be measured by de-
termining the sampling characteristics for
moisture.
10.4.1 Moisture Sampling Based on
Known Sampling Characteristics-—When the
sampling characteristics for moisture are
known, calculate the number of increments
required for a desired degree of precision. The
procedures are those given in Section 8 of this
procedure.
B—10
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D 2234
10.4.2 Moisture Sampling Based Only on
Size—When there Is no knowledge of the
sampling characteristics for moisture, collect
at least the number of increments from the lot
of coal as those given in Table 2. Also, when
a special moisture subsample is taken from
the gross sample before any drying or
crushing operations, collect the number of
increments for the subsample as specified in
Section 9.
TABLE I Iiwrrement Types, CoDditlons, and Spacing
Types of Increment
Condition of Increment Collection
from the Main Bodv of Coal
Type I
No Human Discretion
Is Employed
Type 11
Human Discretion
Is Employed
Spacing of Increments
Spacing of Increments
I.
. Systematic 2, Random
I. Systematic 2. Random
Condition A, stopped belt cut
Condition B. full stream cut
Condition C, part stream cia
Condition D. stationary sampling
. i-A-i l-A-2
1-B-l I-B-2
! C-1 IC 2
l-D-I I-D-2
1J-A-I II-A-2
II-EM II-B-2
II-C-I II-C-2
II-D-1 H-D-2
TABLE 2 Number 2nd Weight of Increments for General Purpose Sampling Procedure®
Top Size
5/b in, (16 mm)
2 in. (SO mm) 6 in. <150 mm)
Mechanically Cleaned Coa!c
Minimum number of increments
Minimum weight of increments, lb
Minimum weight of increments, kg
15
2
I
15 15
6 15
- 3 7
Raw (Uncleaned Coal)c
Minimum number of increments
Minimum weight of increments, lb
Minimum weight of increments, kg
35
2
35 35
6 15
3 - ?
8 Under conditions C and D see 6.2.1 and 6-2.2.
b For coals above 6 in. (150 mm) top size, the sampling procedure should be mutually agreed upon in advance by all
panics concerned.
• c If there ts any doubt as to the condition of preparation of the coal {for example, mechanically cleaned coal or raw
coal) the number of increments for raw coal shall apply. Similarly, although a coal has been mechanically cleaned, it may
still show great variation because of being a blend of two different portions of one seam or a blend of two different seams.
Fn such cases, the number of increments should be as specified for raw (imdeaneri) coal.
B-ll
-------
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8
i 7
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1
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t
i
1 1 1 1
1 i**
t
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, rS
ms»
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1
1
i
1
1
1
. r
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1
I
1 .
o
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oa •• i;o
VARIANCE
FIG. 2 Conversion of SaaipSitig Accuracy to Variance.
B-13
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fl|i5 D 2234
APPENDIXES . ¦ -- . •
At. METHOD FOR DETERMINING THE VARIANCE COMPONENTS
OF A COAL
Al.l Scope
ALL! This method covers a procedure for de-
termining the following variance components of a
coat
Al.l J.I The random variance of a 14b {0.5-kg)
increment, srx, and
A 1.1.1.2 The" segregation variance, the vari-
ance caused by nonrandom distribution of the ash
content in the lot or consignment.
AI J.2 In this method, each different coal will
require a complete experiment, which involves the
collection of two sets of 30 samples from a stopped
conveyor belt. The first set of samples includes 30
very small samples to furnish data for the random
variance; the second set includes 30 large samples
to furnish data for the, segregation variance. Since
one of the important components of variance is that
due to segregation, it is essential that the 30 large
samples be so distributed with respect to time that
coverage of all subtypes of coal are represented.
A 1.2 Apparatus
Al.2.1 The following equipment, in addition to
that equipment normally provided for routine sam-
pling, will be required:
A 1.2.1.1 Two-Section Belt Divider—One of the
sections should be approximately the width corre-
sponding to three times the tap size of the coal, and
should irao a sample of between 4 and 20 lb (2 and
9 kg). the other section should be approximately
the width corresponding to 20 times the top size of
the coal, and should trap a sample of between 80
and 150 lb (36 and 68 kg). The bottom edges of the
divider should be shaped to conform to the surface
of the conveyor belt.
Al.2.1.2 Riffle Splitter, with slots at least 2 Vi to
3 times as wide as the maximum size of the parti-
cles, or, a manual divider and canvas for subdi-
viding the small samples by hand.
A13 Procedure
A1.3.I The fallowing sampling procedure should
be used for each of the two required sets of sam-
ples:
A 1.3.1.1 Stop the loaded belt and insert the belt
divider with the division plates perpendicular to the
direction of belt movement. Scrape off the coal
from each section, and put each section into a sepa-
rate completely labeled container. The container
holding the coal from the small section of the belt
divider should be labeled "A." The container
holding the co:!I from the large section of the belt
divider should be labeled "B."
A!.3.1.2 Collect a subsample from the "A" sec-
tion by riffling or by manual subdivision after
spreading the sample evenly on a smooth fiat sur-
face. Tag the subsample with a label "A", and
weigh to the nearest gram. The weight of the sub-
sample should be between 100 to 200 g.
A 1.3.1.3 Dry the "A" subsample, grind to
minus No. 60 sieve size and determine the ash con-
tent to the nearest 0.1 percent, dry basis.
AL3.L4 Weigh the entire "B" section, dry, and
work down to an analysis sample. Determine the
ash content to the nearest 0.1 percent, dry basis. .
A1.4 Calculation ¦
Al.4.1 Calculate the variance of the "A" and
"B" series (Note Al) as follows:
Variance - (2x2 - (Zr)2/n)/(« _ !) (5)
where:. - . " .
Zx2 = the sum of the squares of ash results,
(2x)* = the square of the sum of ash results, and
n — the number of individual ash results in
the series. .
Al.4.2 The random variance, irJ, is found from:
5/ = [WJT&S - P/2 - H\) (6)
where:
Wi = average weight of small samples, lb orequiv-
' alent kg,
U'\ = average weight of large samples, lb or equiv-
alent kg,
- .variance of small, "A" samples, and
sB' = variance of large "B" samples. .
A 1.4.3 The segregation variance,'j,s, is found
from:
.{7)
Note Al—Ah actual example illustrating the
treatment of data from this sampling experiment is
given in Tables Al to A3 and in Fig. Al.
A 1.4.3.1 Using log-log paper, plot the point cor-
responding to an increment weight h> =¦ I lb (0.5
kg) and variance s.1 = 7.6; draw a straight line
through this point, downward at 45 deg. This line
gives the random component of variance for an in-
crement of any weight. Plot the point corresponding
to an increment weight - 106 lb (48 kg) and
variance s,z - 1.2; draw a straight horizontal line
through this point. This line gives the segregation
component of variance far an increment of any
weight.
A 1.4.3.2 On Fig. Al, find the algebraic sum of
the random component and the segregation compo-
nent of variance for a number of increment weights:
.draw a curve through these points. This curve gives
the total variance of sampling for increments of any
weight, including those used in the "A" and "8"
series.
B-14
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# ¦ D 2234
A2. METHOD FOR ESTIMATING THE OVER-ALL VARIANCE FOR
INCREMENTS '
A2.I Scope
A2.LI This method describes the procedure Tor
estimating the over-all variance for increments of
one fixed weight of a given coal. It is applicable to
mechanical sampling when there is no need to ex-
plore system and random variance components, but
there is a need for obtaining the over-all variance
for increments (the size of increments is dictated by
the sampling equipment),
A2.2 Procedure
A2.2.I The following procedure should be used
to determine the over-all variance for increments:
A2.2J.1 Collect two series of individual incre-
ments at widely spaced intervals; for example, a se-
ries of 10 increments, two each day for five days,
followed by a second series of 10 collected in sim-
ilar fashion. Both series must be from the same
coal.
A2.2.1.2 Collect each increment by using as
much of the equipment and procedure employed in
routine sampling operatioss as passible. Remove
the individual increment from the sampling system
without mixing with or contaminating by any other
increment. Where possible, allow it to pass through
any mechanical crusher or subsampler, or both,
which is located in the system prior to the point of
blending with other increments.
A2.2.1.3 Then weigh the individual increment (if
desired for record purposes) and reduce to a labora-
tory sample by procedures identical as possible to
those employed in the routine preparation and re-
duction of gross samples.
A2.2.1.4 Analyze the sample for the constituents
for which the variance calculations are to be made.
Usually sampling specifications are based on dry
ash; but where total moisture or as-received Btu is
of particular concern, the analyses should be made
for these.
A2.3 Calculation
A2.3.1 For each series, compute a variance value
from the analyses of the ten increments as follows:
j*-(Zr*-(S*)V«)/(»- I) (8)
where:
sz = the variance value for the series,
Xxs = the sum of squares of ash results,
(£x)* = the square of the sum of ash results, and
r. - the number of individual ash results in
the series.
A2.3.2 For the two series, the ratio of the larger
variance to the smaller should not exceed the value
given in Table A4, Column 2. If they differ by less
than this amount, the variances are combined to
give the estimated over-all increment^variance for
the coal as follows:
-t-^2)/2] (9)
where:
s0* - the probable maximum value of the over-all
variance for increments,
F — a factor from Table A5, Column 3, corre-
sponding to the number of increments per
set,
sx3 = j* from first-series, and
5s3 = s* from second series.
A2.3.3 If the ratio of the larger variance to the
smaller does give a greater value than the Table A4,
Column 2 value, the two series are to be considered
in a single set of increments, and another set equal
to this enlarged set is to be taken. For example, if
originally two sets of 10 increments were taken,
these would be combined to give a set of 20. Then
an additional set of 20 increments would be col-
lected, giving two sets of 20 increments each. Vari-
ance values are computed for the two new series
and the test is repeated using the appropriate fac-
tors given in Table A5. IF these results have a ratio
which is less than, the appropriate value in Column
2 of Table A5, they are combined by using Eq 10
and used as the new variance for increments.
A2.3.4 Example—The example given in Table
A5 illustrates the computation of the over-all vari-
ance for increments, s„2- Two series of 10 incre-
ments each are used.
B-15
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® D 2234
TABLE'A1 Schedule 1: Sample Weigte . TABLE A2 Sdsedrie II: Ash SssuJts "A" Series
Set Nombcr
"A" Series, g
"8" Series, lb
Set
Ash,
Asli,
percent
percent-squared
t
89
117,4 •
2 '
126
117.5
i
14.2
201,64
3
152
123.4
2
13-4
179,56
4 .
109
90.7 -
3
13.7
187.69
5
149
101,7
4
15.8
249.64
6
87
89,6
5 ¦
13.7
187.69
7
110
107.7
6
14.1
198.81
' ' 8
142
110.8
7
13.6
184.96
9
123
123.0
8
18,7
349.69
1(1
m
106.2
9
16.3
265-69
U
140
116.4
10
12.4
153.76
12
121
96.7
11
5.8
33.64
13
112
109.0
12 ¦
12.2
148.84
14
122
106.9
13
10.9
118.81
15
158
99.8
14
8.9
7921
16
160
87.6
15
34.5
1190.25
1?
55
88.6
16
8.7
75.69
(8
76
92.3
17
7.5
56.25
19
105
93.0
18
15.7
246.49
20
132
99.8
19
21.8
475.24
21
108
106.6
20
11.8
139^4
22
86
124.2
21
12.2
148.84
23
142
127.8
22
11.8
139.24
24
- 123
111.3
23
7.1
1 50.41
25
' 133
111.6
24
12.8
163.S4 '
' 26
261
107.2
25
14.0
196.00
27
129
106.0
26
6.3
39.69
28
150
102.8
• 27
12.3
151.29
29
108
97.7
28
7.2
51.84
30
99
107.4
29
13.V
171.61
30
11.3
127.69
Sum
3732
3180.7
Average
124.4 g, or 0.27
106.0 lb or 48.1
Sura
391.8
5963-24
lb - »¦, kg - h>,
sA* = [5963.24 - (391.8)!/»l/29 » 29.2
B-16
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TABLE A3 Schedule HI". Ash Results "B" Series
C-,
Ash,
Ash,
percent
percent-squared
1
13.6
184.96
2
132
174.24
3
14.3
204.49
4
153
234.09
5
15.0
225.00
6
14 J
204.49
7
13.6
184.96
8
14.7
216.09
9
14.2
201.64
10
12.5
156.25
11
13.0
169.00
12
143
204.49
13
13J
187.69
14
lig
163.84
15
132
174.24
16
14.0
196.00
17
10-5
110.25
IS
13.5
182.25
19
15.4
237.16
20
15.0
225.00
21
14.4
207.36
22
12.8
163.84
23
13.0
169.00
24
13.0
169.00
25
12-3
151.29
26
13.1
171.61
27
14.2
201.64
28
11,6
134.56
29
13.1
171.6!
30
11.4
129.96
Sum
405.0
5506.00
Sm* - (5506.00 - (405)s/30J
__ _ _
then:
-*.* = 10.27 x 106 (293. - 13)]
_____
= 7.6
and
V" =13- (7.6/106)
- 1J2
D 2234
TABLE A4 Variant Rsiio Limit Values
1
2
3
Increment
Variance
..F.
per Set
Ratio Limit
Factor
10
3.18
1.92
20
2.17
1.53
30
1.86
1.40
40
1.70
1.33
50
1.61
1.29
B-17
-------
D 2234
TABLE A5 Determoaficn of fee OTer-A.II Variance for IncrerrjeEts'1
Series I Series 2
[ncrcment Increment
Number, Dry Ash8 (x) (Dry Ash)" (x)2 Number. Dry Ash6'(x) (Dry Ash)*-* (x)1
l
4.17
17.3889
U
3.07
9.4249
2
3.62
13.1044
12 ¦
4.88 '
23.8144
3
. 1-79
3.2041
13
5.14
26.4196
4 . ,
4.37
19.0969
14
. 3.63
13.1769
5 '
4.64
21.5296
15
" 3.17
10.0489
6
7.03
49.4209
16
7.20
51.8400
7
6.27
39.3129
17
3.52
12.3904
S
3.9!
15.2881
18
0.87
0.7569
9
6.04
36.4816
19
0.72
OS184
10
4.18
17.4724
20
4.78
77 8484
Surra
46.02
232.2998
Sum
36.98
171.2388
""This example Involves Increment weights in the approximate range of 100 to 200 lb (45 to 90 kg).
* 10 percent ash was subtracted from each of the ash results to simplify the calculations.
- <£(*)* - (2W«)/<* - i)
Series I:
St= {232299% - {46.0iy/lQ)/9
- 22795
Series ?:
Sj* = (171.2388 - (36.9S}s/t0i/9
- 3.8319
Variance ratio limit from Table A5 - 3.18
Variance ratio for two test series:
JiY-Sx* s 3.8319/22795 — 1.68 < 3.18
Since tine computed value far the ratio is less than 3.18, variances are combined to give an estimate of the over-all variance
for increments, sa*:
- [\S2 (2-2795 + 3-83!9)]/2 - 5.867
W.-0.2T
Tola! Vortance of Sampling = Random Vonance+fegregolion VariGfi«j
5* « 7.6
W= f.O
S| * 1.3
Wj * IO€
!
Segregofton Variance ss*>i,2
.4 .5 .6 .753
4 5 67SS
i.o io.g teo.o
Weight of Increment, lb. or equivalent kg
3 4 5 6 7 89
10.0
FIG. At Relation of Variance to W«lgbL
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted
in connection wtk any item mentioned m this standard. Users of this standard are expressly advised th^t determination of the
validity of any such patent rights, and the risk of infringement of suck rights, is entirely their own responsibility.
B-18
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APPENDIX C
STANDARD METHOD FOR TOTAL
MOISTURE IN COAL
"Reprinted, with permission, from the Annual Book of A3TM Standards,
Part 26. Copyright, American Society for Testing and Materials,
1916 Race Street, Philadelphia, PA 19103."
C-l
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©
Designation: D 3302 - 74e
i
Standard Test Method for
TOTAL MOISTURE IN COAL1
Til's Standard is issued under the fixed designation D 3302; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year oflast revision. A number in paremheses indicates the year of last
reapproval.
€ Note—Editorial addition of Fig. 1 was made in June 1976.
1. Scope
1.1 This method covers the measurement of
the total moisture ui coal as it exists at the site,
at the time, and under the conditions it is
sampled. It is applicable to coals as mined,
processed, shipped, or utilized in normal com-
mercial' pursuits. Exceptions are coal-water
slurries, sludges, or pulverized products, or
both, under 0.5-mtn diameter sieve size, ft is
applicable to coals of all ranks within the
recognized limitations imposed by oxidation
and decomposition variations of lower rank
coals. Because of its empirical nature, strict
adherence to basic principles and permissive
procedures are required for valid results (see
Appendix). The standard is available to produc-
ers, vendors, and consumers as a total moisture
method when other procedures or modifica-
tions are not mutually agreed on.
1.2 Since coal can vary from extremely wet
(water saturated) to completely dry, special
emphasis must be placed on the sampling,
sample preparation, and the moisture determi-
nation itself to ensure total reliability of mea-
surement. Therefore, this standard is recom-
mended entailing collection of the gross sample,
sample preparation, and the method of deter-
mination.
1.3 While it is recognized that such a stan-
dard may be unwieldy for routine usage com-
mercial operations, it can provide a common
base for agreement in cases of dispute or
arbitration. Also, embodied in the standard are
segments that can be extracted and used as is,
or, with the agreement of the parties, involved,
as the basis for contract specifications.
2. Applicable Documents
2.1 ASTM Standards:
D2013 Preparing Coal Samples for
Analysis2
D 2234 Collection of a Gross Sample of
Coal2
D 3173 Test for Moisture in the Analysis
Sample of Coal and Coke2
3. Summary of Method
3.1 This method is based on the loss in
weight of a coal sample in an air atmosphere
under rigidly'controlled conditions of tempera-
ture, time, and air flow.
3.2 The gross moisture sample is air-dried to
equilibrate it with the atmosphere at each stage
of division arid reduction. Final moisture deter-
mination is made in a heated Forced-air circula-
tion oven under rigidly defined conditions.
33 The total moisture is calculated from
losses (or gains) in air-drying and the residual
moisture as shown in Section 11.
4. Significance
4.1 The collection and treatment of the sam-
ple as specified herein is intended for the
express purpose of determining the total mois-
ture in coal. The standard is available to
producers, vendors, and consumers as a method
of determination when other techniques or
modifications are not mutually agreed on.
4.2 Specific sections of the procedure may be
designated as a valid total moisture determina-
tion upon agreement between or among the
parties involved and designated as such.
1 This method is under the jurisdiction of ASTM Commit-
tee D-5 on Coal and Coke.
Current edition loptova! Feb. 27, 1974. Published April
1974.
* Annual Book of ASTM Standard-,. Part 26.
C-2
-------
5. Definitions
5.1 air drying—a process of partial drying of
coal to bring lo near equilibrium with the
atmosphere in the room in which further reduc-
tion/division of the sample is to take place.
5.2 air dry loss—the loss in weight, ex-
Dressed in percentage, resulting from the partial
drying of coal at each stage of reduction or
division.
5.3 residual moisture—that moisture re-
maining in the sample after determining the
air-dry loss.
5.4 total moisture—the loss in weight in an
air atmosphere under the rigidly controlled
conditions of temperature, time, and air (low as
set in this standard. It is calculated from losses
(or gains) in air-drying and the residual mois-
ture as shown in Section 11.
5.5 gross moisture sample—a sample repre-
senting one lot of coa! and composed of a
number of increments on which neither reduc-
tion nor division has been performed or a
subsample for moisture test ins that, is t ale en m
accordance with Section 10 of Method D 2234.
6. Apparatus
6.1 Drying Floor—A smooth clean floor
area in a room free of contamination by dust or
other material and that permits air circulation
without excessive heat or'air currents. Condi-
tions for an air-drying floor should approach
those established for oven drying as much as
possible.
6.2 Air Drying Oven—A device for passing
slightly heated air over the sample. The oven
should be capable of maintaining a temperature
of 10 to I5°C. (18 to 27°F) above room
temperature with a maximum oven tempera-
ture of 40°C (104°F) unless ambient tempera-
ture is above 4()"C (104°F) in which case
ambient temperature shall be used. In case of
easily oxidized coals, the temperature should
not be over iO°C (18°F), above room tempera-
ture. Air changes should be at the rate of 1 to
4/niin. A typical oven is shown in Fig. 1.
6.3 Drying Pans—Noncorroding metal pans
of sufficient size so that the sample may be
spread to a depth of eat more than 25 mm (1.0
in.) with sides not mere than 38 mm (1-5.in.)
high.
6.4 Scale (Gross Sample)—A scale of suffi-
D 3302
cient capacity and sensitive to 23 g (0.05 lb) in
45 kg (100 lb).
6.5 Laboratory Sample Containers—Heavy
vapor-impervious bags, properly sealed, or non-
corroding cans such as those with an airtight,
friction top or screw top sealed with a rubber
gasket and pressure-sensitive tape for use in
storage and transport of the laboratory sample.
Glass containers, sealed with rubber gaskets,
may be used but care must be taken to avoid
breakage in transport.
7. Precautions
7.1 In collecting, handling, reducing, and
dividing the gross moisture sample, all opera-
tions shall be done rapidly and in as few oper-
ations as possible, since moisture loss depends
on several factors other than total moisture
content, such as time required for crushing,
atmospheric temperature and humidity, and
type of crushing equipment.
7.2 While awaiting preparation, the un-
crushed gross moisture sample shall be pro-
tected from moisture change due to exposure to
rain, snow, wind, and sun, or contact with
absorbant materials.
7.3 The initial weight of the original gross
moisture sample and container shall be re-
corded, and the moisture loss or gain of sample
¦and containers shall be determined before the
sample is reduced.
7.4 Whenever a distinct change of humidity
occurs during the course of preparation of an
air-dried subsample, the subsample should be
weighed and equilibrated with the new atmos-
phere, and the weight loss or gain used in the
calculation of moisture content.
7.5 Whenever subsamples are stored or
transported, the containers and subsamples
shall be weighed, equilibrated to the new atmos-
phere by air-drying, and the weight loss or gain
shall be used in the calculation of moisture
content.
7.6 Since most coals oxidize on exposure to
air, the air drying procedure should not be
prolonged past the time necessary to bring the
sample to equilibrium with the air in the room
in which further reduction and division are to be
made. In no case should the air drying be done
at a temperature over 40°C. The sample shall
be allowed to attain room temperature before
C-3
-------
D 3302
welshing and further reduction. Air drying of
low rank coals should not exceed 18 h because
of oxidation.
8. Sampling
8.! The p rinciples, terms, organization, and
collection as set forth in Method D 2234 shall
apply to the collection of the total moisture
sample. Particular attention is directed to Sec-
tion 10. The increments as established in Table
2 of Method 2234 for mechanically cleaned coal
are deemed adequate for general-purpose sam-
pling for total moisture {see Tabic 1).
9. Sample Preparation (Air-Drying)
9.1 The principles, terms, organization, and
preparation procedures as established in
Method D 2013 shall apply to the handling and
preparation for total moisture. Specific Refer-
ence is made to Sections 1.3.1, Fig. 4, Sections
8.2.1, 8.4.2. One of two procedures must be
used in handling the total moisture sample.
9.2 Procedure A provides for using a drying
floor to reduce the surface moisture to such a
level that the sample can be reduced in size or
amount, or both, without moisture loss during
' the processing.
9.3 Procedure B provides for using an air-
drying oven to equilibrate the sample prior to
reduction in size or amount, or both.
10. Procedure
10.1 Procedure A; Drying Floor—This pro-
. cedure is particularly applicable if the gross
moisture sample is too large in amount to ship
reasonably or is too wet to handle or ship
without loss of moisture.
10.1.1 Weigh the gross moisture sample and
spread on the drying floor to a depth of not
more than twice the top size of the coal. Mix or
. stir the coal from time to time, being careful
not to lose any of the coal particles. Continue
the air-drying and mixing until the surface of
the sample appears dry. Weigh the entire
sample and redistribute over the floor for
additional drying. Continue the drying, stirring,
and weighing until the weight loss of the total
sample is not more than 0.1 %/h,
Note 1—If the sample surface appears dry, and
the time contemplated for reduction and division is
well established, air drying can be stopped when [he
weight loss is less than 0.1 % per twice lie contem-
plated time far processing.
Example—If reduction and division of the sample
is estimated to require 20 min, the air-drying proce-
dure can be stopped when the rate of moisture loss is
less than O.t %/40 rain. If this procedure is used, a
second air-drying is required to establish the 0.1 %/h
rate before the final preparation of the laboratory
sample.
10.1.2 Avoid excess drying. Record the
weight of the gross moisture sample after
drying time. Proceed with sample reduction and
division in accordance with Method D2013.
10.2 Procedure B; Air Dry Oven—Distrib-
ute the gross moisture sample over the required
number of tared pans. Weigh each pan with
sample as it is filled from the gross sample.
Place in the moisture oven that has been
adjusted to the proper temperature and air
flow. The oven temperature should be held at a
temperature of 10 to 15°C (18 to 27°F) above
room temperature (not to exceed 40°C). Air
circulation through the oven should be main-
tained at a rate of at least one air exchange per
minute but in no case should it be sufficiently
high to blow fine particles from the pans.
Gently stir the sample from time to time to
ensure uniform drying throughout the sample.
Continue drying with intermittent stirring until
the coal surfaces appear to be dry. Remove
from oven, weigh, and record the weight.
Return the pans with sample to the oven and
continue the operation. Calculate the percent-
age weight loss. Repeat the drying and weighing
process at 1 to 2-h intervals until the weight loss
is less than 0.1 %/h (Note I). Allow the sample
to reach equilibrium with room temperature
and humidity before the final air dry weight is
recorded.
11. Residual Moisture on Prepared Sample
11.1 The procedure for determining the re-
sidual moisture on the prepared sample is
dependent upon the top size to which the
prepared sample is crushed. Procedure A is
used on samples prepared to a top size of No. 8
(2.36-mm) sieve U.S.A. Standard. Procedure B
is used on samples prepared to a top size of No.
60 (250-/im) sieve U.S.A. Standard.
11.2 Procedure A, Top Size—No, 8 {236-
mm) sieve US.A. Standard:
11.2.1 That portion of the sample used for
C-4
-------
'#
the residual moisture determination shall have
a minimum weight of 500 g.
11.2.2 Determine and record the weight of a
drying pan preconditioned at 107°C. Place the
sample and sample container in the drying pan
and determine the total weight (Note 2). Dis-
tribute the sample uniformly over the pan,
being sure not to exceed a depth of 1 in. (25
mm).
Note 2—If the moisture determination is to be
made in the immediate vicinity of sample prepara-
tion, the sample need not be placed in a container but
can be weighed directly in a tared drying pan. .
11.2.3 Place both the pan containing the
sample and the empty sample container in the
oven at a temperature of 107 ± 3°C. Dry for
1 Vi h, remove from the oven, and weigh
immediately.
11.2.4 Return to the oven for an additional
Vi h, remove, cool, and weigh. Repeat the
drying at Vz-h intervals until the weight loss is
not more than 0.05 % for the Vz-h. period. For
the final weighing, place the dried sample
container on the pan of dried coal and record
the total weight.
11.2.5 Remove any residual coal from the
dried sample container and weigh the empty
container (N ote 2).
11.3 Procedure B—Top Size—No. 60 (250-
fim) sieve US.A. Standard: (This procedure is
the same as that described in Method D 3173.)
11.3.1 Heat an empty capsule under the
conditions, at which the sample is to he dried,
place the cover on the capsule, cool over a
desiecant for 15 to 30 mm, and weigh. Dip out
with a spoon or spatula from the sample bottle
approximately 1 g of the sample. Put this
quickly into the capsule, close, and weigh at
once. Place the capsules in a preheated oven
(107 ± 3°C) through which passes a current of
atr that has been dried by 112^0« (sp gr 1.84} or
other suitable desiecant such as Drierite or
magnesium pe,-chlorate. Close the oven at once
and heat for 1 h. Open the oven, cover the
capsules quickly, cool in a desiccator over
desiecant, and weigh as soon as cold.
12. CaicrfatioBS
12.1 Calculate the percent total moisture,
D 3302
M, as follows:
M - [R (100-^5/100] + A
where:
M = total moisture, %,
A = air-dry loss, %, and
R - residual moisture, %
12.2 Calculate percent air-dry loss. A, as
follows:
A = (£/G)100
where:
A = air-dry loss, %
L - loss in weight in air-drying, and
G = weight of gross sample.
12.3 Calculate percent residual moisture, R,
as follows:
R .. [( W-H)j W] X 100
where:
W — weight of sample used, and
H = weight of sample after heating.
13, Precision
13.1 Repeatability and Reproducibility—
Since the entire sample is subjected to the air-
dry process, there is no opportunity to compare
data for repeatability in the air-drying process.
However, repeatability data between duplicate
subsamples at each reduction and division stage
can be obtained bv analyzl ng duplicate cuts.
Reproducibility data for total moisture is con-
tingent with the taking of two or more samples
simultaneously. Within the above limitations
the repeatability and reproducibility are listed
below:
13.1.1 Repeatability—Results of duplicate
moisture determinations carried out on the
same sample in the same' laboratory by the
same operator using the same equipment
should not differ by more than 0.30 %. (These
limits may not be applicable to low rank coals;
additional data are required to establish such
limits.)
13.1.2 Reproducibility—T he mean of results
of duplicate moisture determinations carried
out by different laboratories on different por-
tions of the sample should not differ by more
than 0.50 %.
C-5
-------
® D 3302
REFERENCES
¦ Brown, G. M_, "The Determination of Moisture in
Coals," National Gas Bulletin, NAGBA Austra-
lia. Vol 17, 1953 pp. 14 -21.
Goodman, J. B.. Gomez, M., Parry, V. F., "Determi-
nation of Moisture in Low-Rank Coals," Bureau
of Mines. XMBUA, R.I. 4969, 1953, p. 20.
Gauger, A. W_, "Condition of Water in Coals of
Various Ranks," Transactions of the TAIMA,
Vol 101, 1932, pp. 148-164.
Barghoorn, E. S., Spackman, W., "Geological and
Botanical Study of the Brandon Lignite and its
Significance in Coal Petrography," Economic
Geological, ECGLA, Vol 45, No. 4, 1950, pp.
344-357.
Hocppncr, J. J., Fowkes, W. W McMurtrie, R„
"Removal of Moisture from Lignite in Inert Gas
¦ Atmospheres," Bureau of Mines, XMBUA.
R.I. 5215, 1956.
TABLE 1 Number and Weight of Increments for General-Purpose Sampling Procedure
Top Size H in. (16 mm) 2 in. (50 mm) 6 in. < 150 mm)
Mechanically Cleaned Coal
Minimum number of increments 15 15 15
Minimum weight of increments, lb . 2 6 15
Minimum weight ofincrements, kg I 3 7
Raw {Undeaned Coal)
Minimum number ofincrements 35 35 35
Minimum weight of increments, lb 2 6 15
Minimum weight of increments, kg 13 7
APPENDIX
XI. ACCURACY DETERMINATION OF MOISTURE IN COAL
XI.I The accurate determination of moisture in
coat of various ranks has long been a subject of
discussion and investigation. As has been pointed out
in the referenced investigations, one of the major
difficulties in assigning absolute merit to a particular
procedure is the multiplicity of conditions under
which water exists in coals and the difficulties in-
volved in obtaining sharp separation and distinction
among these conditions,
XL2 As stated by Gauger, "Water recoverable
from coal is obtained from the following sources: (/)
decomposition of organic molecules (sometimes
called combined water)/(2) surface adsorbed water,
(J) capillary condensed water, (4) dissolved water,
and 0) water of hydration of inorganic constituents
of the coal."
XI.3 Brown further refers to (/) "Free" or "ad-
herent" Moisture (essentially surface adsorbed) pos-
sessing the physical properties of ordinary water, (2)
physically hound or "inherent** moisture of vapor
pressure lowered by the small diameter of the pores of
the coal structure in which it is absorbed, and (J)
chemically bound water of hydration or "combined**
water.
X1.4 It becomes apparent, then, that "total mois-
ture" in principle represents a measurement of all of
the water not chemically combined.
XL5 Traditionally, thermal treatment has pro-
vided the most commonly used basis for attempting
to separate the nonchemically bound water from coal,
and the measurement is normally made by weight
loss. The "absolute" separation of adsorbed moisture
without toss of a portion of chemically bound water is
most difficult, if not impossible. The separation is
particularly difficult in geologically younger coals of
lower rank. Investigators have shown that the amount
of water extracted is a function of both temperature
and time. The problem is further compounded by the
susceptibility of certain coals to oxidation.
Xl.6 Because of such problems, investigators have
proposed a number of schemes to satisfy their
particular objectives in the measurement of water
associated with coal. These include:
XI.6.1 Heating in air at varying temperatures and
for varying time intervals.
X 1.6.2 Heating in inert atmospheres (nitrogen,
helium, argon, etc.).
Xl.6.3 Separation of water by distillation with
benzene, toluene, xylene, kerosine, etc.
X1.5.4 Measurement of water by such chemical
methods as Karl Fischer titrations.
C-6
-------
® D 3302
TOP
Blower
in. (8£.3erj$
5-1/8 in
~113.0cm5
1/2 in (I 27cm)
Celotes Insulating Board
4-500 Watt Strip Heolers
8 in. (20.3 cm)
!/2m. (1.27cm)
Ceieiex insulating
Board Attached
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-------
flPPEHDIX D
STANDARD TEST METHOD FOR
INFILTRATION RATE OF SOILS IN FIELD
USING DOUBLE RING-IMFILTROMETERS
"Reprinted, with permission, from the Annual Book of ASTM Standards,
Part 19. Copyright, American Society for Testing and Materials,
1916 Race Street, Philadelphia, PA 19103."
D-l
-------
Designation: D 3385 - 75
Standard Test Method for
INFILTRATION BATE OF SOILS IN FIELD USING
DOUBLE-RING INFILTROMETERS1
This Standard is issued under the fixed designation D 33S5; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
rtsippravaL
INTRODUCTION
Tills method describes a procedure for field measurement of the infiltration rate of,sails.
Infiltration rate is defined as a soil characteristic determining or describing tie maximum rate at
which water can enter the soil under specified conditions, including the presence of an excess of
water.'Infiltration rates have application to such problems as erosion rates, leaching and drainage
efficiencies, irrigation, water spreading, rainfall runoff, and evaluation of potential septic-tank
disposal fields, among other applications.
Rates determined by ponding of large areas are considered the most reliable method of
determining infiltration rate but the high cost makes the infiltrorneter-ring method more feasible
economically. The infiltration rate is controlled by the least-permeable zone in the subsurface soils.
The double-ring infiltrometer is used to help prevent divergent flow in layered soils by providing an
outer water barrier to encourage only vertical flow from the inner ring. Many other factors2 affect
the infiltration rate in addition to the soil structure, for example, the condition of the soil surface,
the moisture content of the soil, the chemical and physical nature of the soil and of the applied
water, the head of applied water, and the temperature of the water. Thus, tests made at the same
site are not likely to give identical results and the rate measured by the procedure described in this
method is primarily for comparative use. Some aspects of the test, such as tie length of time the
tests should be conducted and the head of water to be applied, must depend upon the experience of
the user, the purpose for testing, and the kind of information that is sought.
1. Scope
LI This method describes a procedure for
field measurement of the rate of infiltration of
water into soils using double-ring infiltrome-
ters. This method is difficult to use and the
resultant data may be unreliable in very coarse
or heavy clay soils, or in frozen or highly
fractured ground. This test may be conducted
at the surface or at given depths in pits, and on
bare soil or with vegetation in place, depending
upon the conditions for which infiltration rates
are desired.
2. Summary of Method
2.1 Infiltration rates can be measured in the
field using double-ring infiltrometers. Two
open cylinders, one inside the other, are drives
Into the ground and partially filled with water
which is then maintained at a constant level
The volume of water added to maintain the
water level constant is fee measure of the
volume of water that infiltrates the soil.'The
volume infiltrated during timed intervals is
converted to an infiltration velocity, usually
expressed in inches per hour (or centimetres per
hour). The maximum infiltration velocity is
1 This method is under the jurisdiction of A ST M Commit-
tee D-18 on Soil and Rock for Engineering Purposes.
Current edition approved Feb. 28, 1975. Published April
1975.
'Johnson, A. t.. A Field Method for Measurement of
Infiltration, U.S. Geological Survey Watcr-Suop'v Paper
1544-F, 1963, pp. 4-9.
D-2
-------
- .. #
equivalent to the infiltration rate.
3. Apparatus
3.1 Injillrometer Rings—Cylinders approxi-
mately 20 in. (50 cm) high and with different
diameters of approximately 32 and 24 in (30
and 60 cm). Cylinders can be made of Vfc-in.
(3-mm), hard-alloy, aluminum sheet or other
materia] sufficiently strong to withstand hard
driving, with the bottom edge beveled From the
outside to the inside edge (see Fig. I). The
beveled edges should be kept sharp. Larger
rings can be calibrated in accordance with
Table 1 and used, if economically feasible.
3.2 Driving Caps—Disks, of %-in. (13-mm)
aluminum alloy with centering pins around the
edge. The diameters of the disks should be
slightly larger than those of the infiltrometer
rings.
3.3 Driving Equipment—A 12-lb (5.5 kg)
mall or sledge and a 2 or 3-ft (60 or 90-cm)
length of wood approximately 2 by 4 in. (5 by
10 cm) or 4 by 4 in. (10 by 10 cm).
3.4 Depth Gage—A hook gage, steel tape or
rule, or length of heavy wire pointed on one
end, for use in measuring and controlling the
depth of water (head) in the infiltrometer ring.
3.5 Splash Guard—Several pieces of rubber
sheet or burlap 6 in. (15 cm) square.
3.6 Rule or Tape—A 6-ft (2-m) steel tape or
1 -ft (30-cm) steel rule.
3.7 Metal Tamp—Pipe, 14 in. (35 cm) long,
with 6-in. (15-em) length of 1 in. (25 mm) wide,
V* in. (6 mm) thick steel strap welded to the
end.
3.8 Shovels—One long-handled shovel and
one trenciung spade.
3.9 Hand Augei—Orchard-type auger with
3 in. (75 mm) in diameter, 9-in. (225-mm) long
barrel and a rubber headed tire hammer for
knocking sample out of the auger.
3.10 Water Containers—One 50-gal (190-
litre) barrel for the main water supply; one
1000-ml graduated cylinder or a graduated
Mariotte tube for measurement of water during
the test: a 12-qt (12.7-Htre) pail for initial filling
of the infiltrometer; and a length of rubber hose
to siphon water from the barrel (see Fig. 2).
3.11 Water Supply—Preferably, water of
the same quality and temperature as that
involved in the problem being examined.
3.12 Stop Watch.
D 3385
3.13 Level—A carpenter's level or bull's-eye
(round) level.
3.14 Recording Materials—Record books
and graph paper, 20 by 20 lines/in. (8 by 8
lines/cm), or special forms with graph section
(see Fig. 3),
4. Test Site
4.1 The test requires an area of approxi-
mately 10 by 10 ft (3 by 3 m), accessible by a
truck.
4.2 The test site should be as. nearly level as
possible, or a level surface should be prepared.
4.3 The test may be set up in a pit if
infiltration rates are desired at depth rather
than at the surface.
4.4 Avoid sites where interference with test
equipment is possible, such as sites near chil-
dren or in pastures with livestock.
5. Procedure
5.1 Driving Infiltration Rings with a Sledge:
Note 1 —Driving rings with a jack is the preferred
method (see 5,2).
5.1.1 Place driving cap on the outer ring and
center it thereon. Place the wood Mock (see 3.3)
on the driving cap.
5.1.2 Drive the outer ring 6 in. (15 cm) into
the soil with blows of a heavy sledge on the
wood block. Use blows of medium force to
prevent fracturing of the soil surface. Move the
wood block around the edge of the driving cap
every one or two blows so that the ring will
penetrate the soil uniformly.
5.1.3 Center the smaller ring inside the
larger ring and drive to a depth of 2 in. (5 cm),
using same technique as in 5.1.2.
5.1.4 Check rings with the level, correcting
the attitude of rings to be vertical, as needed.
5.2 Driving Infiltration Rings with Jacks:
5.2.1 Use a heavy jack and a truck to drive
the rings as an alternative to the sledge method
(see 5.1).
5.2.2 Center the wood block across the driv-
ing cap of the ring. Center a jack on the wood
block. Place the top of the jack and the
assembled items vertically under the previously
positioned end of a truck body and apply force
to the ring by means of the jack and truck
reaction.
5.2.3 In heavy-textured soils, add additional
D-3
-------
weight to the truck if needed to develop suffi-
cient force to drive the ring.
5.2.4' Check rings with the level, correcting
attitude of rings to be vertical, as needed.
_ 5.3 Tamping Disturbed Soit ¦
5.3.1 If the soil is visibly disturbed more
than Va in. (3 mm) from the wall of the ring,
reset the ring with less disturbance of the
sample.
5.3.2 If the soil is visibly disturbed less than
Va in. (3 mm), tamp the disturbed soil adjacent
to the inside wall of the ring with a metal tamp
until'the soil is as firm as it was prior to the
disturbance.
'" 5.4 Maintaining Water Level: ~
5.4.1 Install a depth gage or a Mariotte tube
for each infiltrorneter ring to assist the inves-
tigator visually in maintaining a constant head.
For a depth gage, use a steel tape or rule, if the
soils have high permeability. Use a hook gage,
simple-point gage, or Mariotte tube if the soils
have low permeability.
5.4.2 Install the gages to be used near the
center of the center ring and also in the annular
space midway between the two rings.
5.4.3 Cover the soil surface wihin the center
ring and between the two rings with splash
guards (6-in. (15-cm) square pieces of burlap or
rubber sheet) to prevent erosion of the soil when
the initial water supply is poured into the rings.
5.4.4 Use a pail to fill both rings with water
to the same desired depth in each ring. Do not
record this initial volume of water. Remove the
splash guards.
5.4.5 Choose a head of at least 1 in. (2.5 cm)
and not greater than 6 in. (15 cm) and maintain
the water level at the selected head as near as
possible throughout the test.'The head is se-
lected on the basis of the permeability of the
soil, the higher, heads being required for lower
permeability soils.
5.5 Measurements:
5.5.1 Record all volumes oF water that are
added to maintain a constant head during a
timing interval.
5.5.2 For average soils, record the volume of
water used at intervals of 15 min for the first
hour, 30 min for the second hour, and 60 min
during the remainder of a period of at least 6 h,
or until a maximum rate is obtained.
5.5.3 For high-permeability materials, take
early readings more frequently. The exact
D 3385
schedule of " readings can be determined only
through experience.
5.5.4 For low-permeability materials, use a
longer test interval, possibly 24 h, or more.
Again, the exact" schedule is determined
through experience.
5.5.5 Place the driving cap or some other
covering over the rings during the intervals
between water measurements to minimize evap-
oration.
5.5.6 Upon completion of the test, remove
the rings from the soil assisted by light ham-
mering on the sides with a rubber hammer.
6. Calculations - - -
6.1 Convert the volume of water used during
each measured time interval into the depth of
water per unit of time in inches (or centimetres)
per hour. Table 1 can be used to convert volume
measurements Into equivalent depths of water
by multiplying the volume of water used during
the time interval by the area factor shown in the
table. The' infiltration velocity is obtained by
dividing the depth of water by the time interval,
in hours.
6.2 Make these calculations for the inner
ring, the annular space, and both rings com-
bined.
7. Report
7.1 Record the infiltration velocities in a
record book or on a report form (see Fig. 3).
Record the depth to the water table. If known,
and a description of the soils found between the
rings and the water table, or at least to a 20-ft
(6-m) depth. Plot the data on the cross-sec-
tioned part of the report form (see Fig. 3).
7.1.1 Record the temperature and the pH of
the water used in the test. If available, a full
analysis of the water should be recorded also.
7.2 The rate for the inner ring should be the
value used if the rates for both rings and
annular space differ. The difference in rates is
due to divergent flow.
NOTE 2—Although not considered a required part
of the test, the determination of the moisture pattern
in the moistened sot! beneath the infiltration rings
commonly provides information useful in interpreting
the movement of water through any particular soil
. profile. For example, water movement horizontaliy
may be caused by lower-permeability layers and will
result in a lateral spreading of the wetted zone. Trius.
the exploration of the soils below an infiltration test
in an unfamiliar area caff determine the subsurface
D-4
-------
D 3385
conditions that may affect the test and later applica-
tions of the data.
If the investigator chooses lo make such a study,
dig a trench so that one waif of the trench passes
along the center line of the farmer position of the
rings. Orient the trench so that the other wall is
illuminated fay the sun, if the day is sunny. If feasible,
dig the trench large enough to include all of the newly
moistened area. Collect samples from the shaded wall
of the trench for determination of moisture content.
If preferred, an auger, such as the orchard barrel
type, may be used to determine the approximate
outline of the moistened area below the rings and to
collect samples for moisture content.
Plot the visibly-moistened area on graph paper or
on the cross-section part of the report form {see Fig.
3). If samples were collected and moisture contents
were determined, the contour of moisture content
also can be plotted on the graph.
TABLE I Data for Double-Ring Infiltroraeters
Diameter of
Riug(s),
in. (mm)
Volume of Water
Multiplication Factors tc -
Area of Annular
Area of Rio®, in5
Providing a I-in.
Convert Volume of Water
Space, in2 (cm*)
(cm)2
(2.5-cm) Depth.
Used in ml to Depth of
ml
Water in in. (cm)
12 and 24
(30 and 60)
12(30}
24(60)
339-3
(2189.2)
113.1
(729.7)
452.4
(2918.9)
5561
1854
7415
1.80 x 10—•
(4.57 x 10-*)
5.39 x 10-
(13.70 x 10-*)
1.35 x 10-"
(3.43 x I0-")
30 or 60 cm. din
(12 or 24 in.)
Welded butt
joint
50 cm
(20 in.)
Note—-The material shall fee a !4-in. (3-mm) alurainam-
alloy sheet or material or similar strength.
• '• FIG. I ItittrrocrMcr Construction.
D-5
-------
Shutaff
clamp
Paine
Hook gage
valve
Wa ter
level
£
2.5-r15 cm
(1-6 in-) Wate
Soil
Threaded
hose ¦
connec tor
To water supply-
See detail
of Mariotte tube
at right
Hater level
Support clamp
1.3-cra (i-in.)
steel rod
To
Infiltra tion
. ring
¦ To water supply-
Rubber
stopper
Brass valve
with flare
¦ fitting
Note—Center ring has been eliminated for simplification of the illustration.
FIG. 1 Ring Installation and Mariotte Tube Details,
Brass
elbow
B C
CJ
CD CD
lO CM
Plastic
This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five
years and if not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or
for additional standards and should be addressed to ASTM Headquarters. Your comments wiil receive careful consideration
at a meeting of the responsible technical committee, which you may attend. If you feef that your comments have not received
a fair hearing you should make your views known to the ASTM Committee on Standardst 1916 Race St., Philadelphia, Pa.
1910S, which mil schedule a further hearing regarding your comments. Failing satisfaction there, you may appeal to the
ASTM Board of Directors.
D-6
-------
Date
/0-J4-SS
Technician
73/9^/?' /'Vi<"s
Method 30 ff 6ocjn J}oti&/e-r/r>$Irtfi/trom«t*r
Elapsed
time ,
trtin
Quan-
tity of
water >
/n/
Infil-
tration
rate.
jhr
IS
a ho
/. 3
30
<+u?
2.3
45
S-bO
3.0
60
(a to
i.B
90
\SfoO
4.3
mo
\1S0
4.8
180
'iooo
5-5
£40
J>no
6.3
Sao
3S°0
48
360
ll-to
4.5
i n
, V
J \
t \
1 i^C
^ 1
i
L:-'
CROSS-SECTION OF MOIST AREA AND GRAPH OF INFILTRATION RATE
HORIZONTAL DISTANCE IN meiiers
0.5 1.0 l.ff 2.0
I
too 7.0Q $0 o
ELAPSED TIME IN minutes
Soil
profile
deocrip-
tion
Soil)sandyl
thin (frnss
Snnc/,\/,f.
¦&o k,
dry,host
ki "ti,
k?rs
Basa/i,
dsnst
surface
FIG. 3 Report Form for Infiltration Test With Sample Dntn.
The American Society for Testing and Materials takes no position respecting the validity of anv patent rights asserted
In connection with anv lie/it mentioned in this standard. Users of this standard are expressly advised that determination of the
validity of anv such patent rights, and the risk of Infringement of such rights, Is entirely their own responsibility.
-------
APPENDIX E
STANDARD METHOD OF
SIEVE ANALYSIS OP COAL
"Reprinted, with permission, from the Annual Book of ASTM Standards,
Part 26. Copyright, American Society for Testing and Materials,
1916 Race Street, Philadelphia, PA 19103."
E-l
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©
Designation: D 410-38 (Reapprovsd 1976! American National Standard K2D.S-1S70
American National Standards Institute
Standard Method of .
SIEVE ANALYSIS OF COAL1
' This Standard is issued under the fixed designation D 410; (he number immediately following the designation indicates the
year of angina! adoption or, in the ease af revision, the year of" last revision, A number in parentheses indicates the ye;ir of"
last rcappruvaL
Note—An editorial change in 6.3 was made in June 1947, and the title was changed in July 1969.
1. Scope
1.1 This method for sieve analysis is appli-
cable to all coal except anthracite, powdered
coal as used in boiler plants, and crushed coal
as charged into coke ovens.
Note—The values stated in U.S. customary
units are to be regarded as the standard.
2. Apparatus
2.1 Sieves of the Following series shall be
used conforming to ASTM Specification E
It, for Wire-Cloth Sieves for Testing
Purposes2, or ASTM Specification E 323, for
Perforated-Plate Sieves for Testing Purposes2,
Round-Hole Screens:
8-in.
6-in.
5-in.
4-in.
3-in.
IVi-la.
I- in.
(...)
(...)
(125-mm)
{IOO-mm}
(75-mm)
(63-nim)
(50-mm)
1 Vi-in. (37.5-mm)
I '4-in. (31.5-mm)
l-in. (25.0-mm)
in (19.0-mm)
'/4-in. (12,5-mm)
%-in. (9.5-mm!
Wire-Cloth Steves with Square Openings:
4.75-mm (No. 4)
2.36-mm (No. 8)
1.18-mm (No. 16)
60C M(" (No. 30)
300-^m (No. 50)
150-jira (No. 100)
75-^m (No. 200)
3, Time of Sampling
3.1 Sample coal when it is being loaded
into or unloaded from railroad cars, ships,
barges, or wagons, or when discharged from
supply bins, or from industrial railway cars,
or grab buckets, or from any coa! conveying
equipment, as the case may be. It is not fea-
sible to collect representative samples for
screen analysis from the surface of coal in
piles or from loaded cars or bins.
4. Collection of Gross Sample
4.1 Collect increments regularly and sys-
tematically, so that the entire quantity of coal
sampled will be represented proportionately in
the gross sample, and with such frequency
that a gross sample of the required amount
shall be collected. The-number of increments
collected shall be not less than 20. When the
coa! is passing over a conveyor or down a
chute, increments the full width and thickness
of the stream of coal shall be taken either by
stopping the conveyor and removing all coal
from a transverse section of it, or by momen-
tarily inserting a suitable container into the
stream. If it is impracticable to collect incre-
ments the full width and thickness of the coa!
stream, increments shall be systematically col-
lected from all portions of the stream.
5. Weight of Gross Sample
5.1 The weight of the gross sample col-
lected shall conform to the following:
Run-of-mtne coal
Screened coal with upper
limit larger than 4-in.
(100-mm) round
Coal smaller than 4-in. •
(100-mm) round
Coal smaller than 2-in.
not less than 4000 lb
(1800 kg)
not less than 4000 lb
(1800 kg)
not less than 2000 lb
(900 kg)
not less than 1000 lb
'This method is under ihe Jurisdiction af ASTM Com-
mittee D-5 on Coal and Coke.
Current edition effective Sept. 1, 1938. Originally issued
1935. Replaces D 410 35 T.
* Annual Book of ASTM Standards. Part 26.
By publication of this standard na position is taken with respect to the validity af any patent rights in connection there-
with. and the American Society for Testing and Materials dees riot undertake to insure anyone unit: my the standard
against liability for infringement of any Letters Patent nor assume any such liability.
E-2
-------
D 410
(50-mrn) round
Coal smaller lhai) l-in.
(25-rnrn) round
Coal smaller than V4-in.
(12.5-mm) round
(450 kg)
not less than 500 lb
(215 kg)
not less than 100 lb
(45 kg)
6. Reduction of Gross SaetpJe
6.1 Coal Larger than I-in. {25-mm) Round
—Screen without mixing or dividing.
6.2 Coal Smaller than I-in. Round—Divide
in amount to not less than 125 lb (56.5 kg) by
riffling or by arranging it in a long, flat pile
and successively halving it or quartering it by
the alternate-shovel method as follows: Take
successive shovelfuls in passing around the
pile {advancing a distance equal to the width
of the shovel for each shovelful), and retain
alternate shovelfuls or every fourth shovelful
for the sample.
6.3 Coal Smaller lhar. Vi-iri. (12.5-mm)
Round—Divide to not less than 25 lb (11.4
kg) by passing it through a riffle or equally
accurate dividing device, or by hand-quar-
tering as described in ASTM Method D 346,
Sampling Coke for Analysis.4
6.4 Coal Smaller than No. 4 Sieve—Divide
to not less than 2 lb (1000 g) by riffling or
hand-quartering.
6.5 Coal Smaller than No. S Sieve—Divide
to not less than I lb (500 g) by riffling or
hand-quartering.
7. Drying Sample
7.1 In case the coal is wet, the sample may p Report
be tested on sieves 1 in. (25 mm) round and „ , „ , . . , ,
larger, without drying, but dty the sample of 9J ^ T*** 10
coal smaller than I-in. round (divided in nearest percent as follows.
amount to 125 lb (56.5 kg), as described in
Section 6.2), sufficiently to remove surface Percent
moisture which causes small particles to cling Retained on . . in. round 0
to the larger pieces. In cases of lignite, subbi- Retained on .... in. round, passing
luminous, and high volatile C bituminous rour>d
coals,'take care not to over-dry and cause ^
weathering of the coal.
Retained on No passing in.
8. Sieve Analysis round '
Retained on No , passing No
8.1 Accurately weigh the sample before Passing No. „• _
screening. Starting with the largest sieve,
- c Total
screen the sample in such. amounts as will
allow the pieces to be in direct contact with 9.2 If the sum of the weights shows a loss of
the openings at the completion of the over 2 percent, reject the analysis and make
screening of each amount. Determine the another test.
smallest sieve through which all of the sample
passes by actual test, in accordance with 8.2,
8.3, and 8.4.
8.2 Coal Larger than 2Vt-in. {63-mm)
Round—Try by hand pieces of coal not
passing readily through sieves 2%-in. round
and larger to see if they will pass through the
openings in any position. Do not shake sieves
2 Vt-in. round and larger except for whatever
jiggling may be necessary to clear the sieves
of fine coal.
8.3 Coal Smaller than 2-A-in. Round—
Test coal passing the 2^-in. round sieve with
sieves down to and including I-in. (25-mm)
round as follows: Move the sieve horizontally
a distance of about 8 in. at just sufficient rate
to cause the pieces of coal to tumble or roll
on the sieve. Stop the motion of the sieve
without impact. After ten such shakes (five in
each direction), screening of the increment
shall be considered complete.
8.4 Coal Smaller than I-in. Round—Coal
passing the I-in. round and smaller sieves
may be weighed and then divided in amount
as provided in Section 6 and then dried as
provided in Section 7. Shake sieves smaller
than l-in. round gently with a reciprocating
horizontal motion until practically no more
coal will pass through the openings. When
both 150-/im (No. 100) and 75-fim (No. 200)
sieves are used, use the latter first in order to
facilitate screening.
E-3
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APPENDIX F
STANDAED METHOD FOR ASH IN THE
ANALYSIS SAMPLE OF
COAL AND COKE
"Reprinted, with permission, from the Annual Book of ASTM Standards,
Part 26. Copyright, American Society for Testing and Materials,
19X6 Race Street, Philadelphia, PA 19103."
F-l
-------
41
Designation: D 3174 - 73
Standard Test Method for
ASH IW THE ANALYSIS SAMPLE OF COAL AND
COKE1
This Standard is issued under the fixed designation D 3174; the number immediately following the designation indicates the
year of original adoption or. in the case of revision, the year of last revision. A number in parentheses indicates the year oflast
trapproval,
1. Scope
I. J This method covers determination of the
ash content in the analysis sample of coal or
coke as prepared in accordance with ASTM
Method D 2013 or Method D 346. The results
obtained can be applied as the ash in the
proximate analysis, Method D 3172, and in the
ultimate analysis. Method D 3 i 76. For the
determination of the constituents in ash, refer-
ence is made to Method D 2795.
2. Applicable Documents
2.1 ASTM Standards:
D 346 Collection and Preparation of Coke
Samples for Laboratory Analysis"
D388 Specification for Classification of
Coats hv Rank2
D 2013 Preparing Coal Samples for
Analysis*
D 2795 Test for Analysis of Coal and Coke
Ash2
D3172 Proximate Analysts of Coal and
Coke'
D 3i73 Test for Moisture in the Analysts
Sample of Coal and Coke2
D 3176 Ultimate Analysis of Coal and Coke®
3. Summary of Method
3.1 Ash is determined by weighing the resi-
due remaining after burning the coal under
rigidly controlled conditions of sample weight,
temperature, time, and atmosphere.
4. Apparatus
4.1 Gas or Electric Muffle Furnace for
Coal—For determination of ash of coal, the
furnace shall have an adequate air circulation
and be capable of having its temperature regu-
lated between 700 and 750° C.
4.2 Gas or Electric Muffle Furnace or
Meker Burner for Coke—For determination of
ash of coke, the furnace shall have an adequate
air circulation and be capable of haying its
temperature regulated at the prescribed tern-
perature(s) of 750 and 950°C.
4.3 Porcelain Capsules, about I's in. (22
mm) in depth, and l3/s in. (44 mm) in diameter,
or similar shallow dishes or platinum crucibles.
5. Procedure for Coal
5 J Transfer approximately I g of the sam-
ple to a weighed porcelain capsule with a spoon
or spatula and quickly establish the weight to
the nearest 0.1 mg. An alternative way is to use
the dried coal from the moisture determination
Method D3173. Place the porcelain capsule
containing the sample in a cold muffle furnace,
or on a hearth at a low temperature, and
gradually heat to redness at such a rate as to
avoid mechanical loss from too rapid expulsion
of volatile matter. Finish the ignition to con-
stant weight (±0.001 g) at a temperature be-
tween 700 and 750"C. Cool in a desiccator over
desiceant, and weigh as soon as cold.
Note I—Ash results obtained by this method
differ in composition from the inorganic constituents
present in the original coal. Incineration causes an
expulsion of water from the clays and calcium sulfate,
of carbon dioxide from carbonates, and the conver-
sion of iron pyrites into ferric oxide. Each of these
reactions involves a loss in weight from the original
inorganic material. Formulas and references for
correcting ash results to a mineral matter basis are
1 This method is under (he jurisdiction of ASTM Commit-
tee D-5 on Coal and Coke.
Current edition aoproved Aoril 2f. 19/3. Published
July 1973. * "
* Annual Book of ASTM Standards. Part 26.
1-2
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: #
listed in Method D 388, Section 7. Also, see the
report on Fixed Carbon and Ash.1
Note 2—Difficulty may be experienced in secur-
ing satisfactory check determinations of ash in the
same or different laboratories far coals unusually
high in calcite and pvrite. This is caused by varying
amounts of sulfate sulfur being retained in the ash.
When such difficulty is encountered, or when coals of
relatively high ash content whose mineral matter
composition is unknown are encountered, the ash
should be determined by the following modified
procedures:
(~) Place the capsules containing the dried coal
from the moisture determination in a cold muffle
furnace and heat gradually so that the temperature
reaches 500DC in ! h, and 750"C in 2 h. Heat to
constant weight at 750°C. By this means, pyritic
sulfur will be oxidized and expelled before the calcite
is decomposed. An ample supply of air in the muffle
must be assured at all times to ensure complete oxi-
dation of the pyritic sulfur and to remove the SO,
formed.
(~) The modified procedure described in Para-
graph (a) should be adequate for determining ash
in troublesome commercial samples. However, sam-
ples may be encountered in certain special studies
whose .ash values are quite high and whose mineral
matter contains much greater than normal amounts
of calcite and pyrite. In such cases sulfate sulfur
should be determined on the ash obtained by the
modified cold muffle method and the value properly
corrected, or the Parr* sulfated ash method as modi-
fied by Kees" should be used.
6. Procedure for Coke
6.1 Weigh the sample as described in 5.1.
6.2 Place the capsules containing the coke
sample in a muffle furnace or over a burner,
and heat to redness at such a rate as to avoid
mechanical loss. Finish the ignition to constant
weight (±0.001 g) at a temperature not exceed-
ing 950°C. Cool in a desiccator and weigh.
6.3 For those samples containing an excep-
tionally low ash, a 5-g sample weight is per-
D 3174
missible.
7. Calculations
7.1 Calculate the ash percent in the analysis
sample as follows:
Ash in analysis sample. % - [(A - B)/C] x 100
where: '
A = weight of capsule and ash residue, a,
B ~ weight of empty capsule, g. and
C = weight of analysis sample used, g.
8, Precision
8.1 The Following criteria should be used for
judging the acceptability of results:
8.1.1 Repeatability—Duplicate results by
the same laboratory should not be considered
suspect unless they differ by more than the
following percentages:
Kg carbonates present 0.2
Carbonates present 0.3
Coalswhh more than 12 *£ ash. 0.5
containing carbonates and pyrites
8.2.1 Reproducibility—Results submitted by
two or more laboratories should not be consid-
ered suspect unless they differ by more than the
following percentages:
No carbonates present 03 ' -
Carbonates present 0.5
Coals with more than 12 % ash, 1.0
containing carbonates and pyrites
'Report on Fixed Carbon and Ash, Proceedings- Am.
Soc. Testing Mats., Vol XIV, Fart I (Committee Reports),
1914 p 4^45
4 Parr. S. W_ "Chemical Study of Illinois CoaiT" Bulletin
No, 3, p 35, Illinois Coal Mining Investigations. State
Geological Survey. Urbana. III. (1916).
5 Rees. O. W„ "Determining Ash in High Carbonate
Coals. Study of the Modified Method." Industrial end
Engineering Chemistry. Analytical Edition, Vol 9, 1937, pp.
307-309.
By publication of this standard no position is taken with respect to the validity-of any patent rights in connection therewith*
and the A mcrican Society for Testing and Materials does not undertake to insure anyone utilizing the standard against liability
for infringement of any Letters Patent nor assume anv such liability.
F-3
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APPENDIX G
STANDARD TEST METHODS FOR
TOTAL SULFUR IN THE ANALYSIS SAMPLE
OF COAL AND COKE
"Reprinted, with permission, from the Annual Book of ASTM Standards,
Part 26. Copyright, American Society for Testing and Materials,
1916 Race Street, Philadelphia, PA 19103."
G-l
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#
Designation: D3177 - 75
Standard i est Methods for
TOTAL SULFUR IM THE ANALYSIS SAMPLE OF
¦ GOAL AND COKE1
This Standard is issued under the fixed designation D 3177; the number immediately following the designation indicates the
year of original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last
reappnjval.
1. Scope
1.1 These methods cover three alternative
procedures for the determination of total sulfur
in samples of coal and coke. Sulfur is included
in the ultimate analysis of coal and coke.
1.2 The procedures appear in the following
order.
Sections
Method A—Esdika Method ' 5 to 8
Method B—Bomb Washing Method " 9 to 11
Method C—Higb-Tempemture Combustion
Method -- 12 to 16
2. Applicable Documents
2.1 ASTM Standards:
D 346 Collection and Preparation of Coke
Samples for Laboratory Analysis2
D 1193 Specification For Reagent Water3
D 2013 Preparing Coal Samples for
Analysis2
D2015 Test for Gross Calorific Value of
Solid Fuel by the Abiabatic Bomb
Calorimeter2
D 3173 Test for Moisture in the Analysis
; Sample of Coal2
D 31'76 Ultimate Analysis of Coal and Coke2
D 3180 Calculating Coal and Coke Analyses
from As-Determined to Different Bases2
3. Summary of Methods
3.1 Eschka Method—A weighed sample and
Eschka mixture are ignited together, and the
sulfur is precipitated from the resulting solution
as barium sulfate (BaS04). The precipitate is
filtered, ashed, and weighed.
3.2 Bomb Washing Method—Sulfur is pre-
cipitated as BaSO< from oxygen-bomb calorim-
eter washings, and the precipitate is filtered,
ashed, and weighed.
3.3 High-Temperature Combustion Method
—A weighed sample Is burned in a tube
furnace at a temperature of 1350°C in a stream
of oxygen. The sulfur oxides and chlorine
formed are absorbed in a hydrogen peroxide
(H202) solution yielding hydrochloric (HCI)
and sulfuric (H2S04) acids. The total • acid
content is determined by titration with sodium
hydroxide (NaOH), and the amount of sodium
chloride (NaCl) resulting from the titration of
the HCI is converted to NaOH with a solution
of mercuric osycyanide (Hg(OH)CN). This
sodium hydroxide is determined titrimetrically
and used to correct the sulfur value which is
equivalent to the amount of H2S04 formed
during combustion of the coal.
4. Sample
4.1 The sample shall be the material pulver-
ized to pass No. 60 (250-^rn) sieve in accord-
ance with Method 1) 2013 or Method D346.
4.2 A separate portion of the analysis sam-
ple should be analyzed for moisture content in
accordance with Method D 3173,. so that calcu-
lation to other than the as determined basis can
be made.
4.3 Procedures for converting as determined
sulfur values obtained from the analysis sample
to other bases are described in Method D 3176
and Method D3180.
4.4 Standard Reference Material (SRM)
'These methods are utsiie; the jurisdiction of ASTM
Committee D-5 on Coat asd Coke.
Current edition approved May 30. 1975. Published Au-
gust 1975. Originally published as D 3177 - 73. Last previous
edition 0 3177 - 73*.
3 Annual Book of ASTM Standards. Part 26.
* Annua! Book of ASTM Standards, Part 31.
G-2
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#
1631 -Sulfur in Coal* consists of three different
low-volatile coal samples, each of which has a
certified sulfur content. Sulfur values obtained
by analyzing these coals, using any of the three
methods described in this standard, may be
used for checking the accuracy of analvtical
results.
ALTERNATIVE PROCEDURES
Method A—Eschka Method
5. Apparatus
5.1 Gas {Note 1) or Electric Muffle Furnace,
or Burners, for igniting the sample with the
Eschka mixture and for igniting the barium
sulfate (BaSO<).
Note 1—Gas may contain sulfur compounds.
5.2 Crucibles or Capsules—Porcelain cap-
sules, % in. (22 mm) in depth and 1% in. (44
mm) in diameter, or porcelain crucibles of
30~ml capacity, high or low form, or platinum
crucibles of similar size shall be used for
igniting the sample with the Eschka mixture.
Porcelain, platinum, ahindum, or silica cruci-
bles of 10 to 15-ml capacity, shall be used for
igniting the BaSO,.
6. Reagents
6.1 Purity of Reagents—Reagent grade
chemicals shall be used in all tests. Unless
otherwise indicated, it is intended that all
reagents shall conform to the specifications of
the Committee on Available Reagents of the
American Chemical Society, where such speci-
fications are available.5 Other grades may be
used, provided it is first ascertained that the
reagent is of sufficiently high purity to permit
its use without lessening the accuracy of the
determination.
6.2 Purity of Water—Unless otherwise indi-
cated, references to water shall be understood
to mean reagent water, Type IV conforming
to Specification D J193.
6.3 Barium, Chloride Solution (100 g/litre)
-—Dissolve 100 g of barium chloride
(BaCU-2H20} and dilute to 1 litre with water.
6.4 Bromine Water (Saturated)—Add an ex-
cess of bromine to 1 litre of water.
6.5 Eschka Mixture—Thoroughly mix' 2
parts by weight of light calcined magnesium
oxide (MaO) with 1 part of anhydrous sodium
carbonate (Na2C03). Both materials should be
D 3177
as free as possible from sulfur.
6.6 Hydrochloric Acid (I /)—Mix equal
volumes of concentrated hydrochloric acid
(HC1, sp gr 1.19) and water.
6.7 Hydrochloric Acid (1 + 9)~Mix I vol-
ume of concentrated hydrochloric acid (HC1, sp
gr 1.19) with 9 volumes of water.
6.8 Methyl Orange Indicator Solution {0.2
g/litre)—Dissolve 0.02 g of methyl orange In
100 ml of hot water and filter.
6.9 Sodium Carbonate, Saturated Solution
—Dissolve approximately 60 g of crystallized
sodium carbonate (Na2COs - 10H2O) or 22 g of
anhydrous sodium carbonate (Na-COa) in 100
ml of water, ¦ using a sufficient excess of
NasCOj to ensure a saturated solution.
6.10 Sodium Hydroxide Solution (100 g(
litre)—Dissolve 100 g of sodium hydroxide
(NaOH) in 1 litre of water. This solution may
be used in place of the Na2C03 solution.
7. Procedure
7.1 Preparation of Sample and Mixture—
Thoroughly mix on glazed paper approximately
1 g of the sample, weighed to nearest 0.1 mg,
and 3 g of Eschka mixture. The amount of
sample to be taken will depend on the amount
of BaCi2 solution required in accordance with
7.3. Transfer to a porcelain capsule or porcelain
crucible, or a platinum crucible, and cover with
about 1 g of Eschka mixture.
7.2 Ignition—Heat the crucible over an alco-
hol, gasoline, or gas flame as described in 7.2.1,
or in a gas or electrically heated muffle as
described in 7.2.2 for coal and in 7.2.3 for coke.
The use of artificial gas for heating the sample
and the Eschka mixture is permissible only
when the crucibles are heated in a muffle.
7,2.1 Heat the crucible, placed in a slanting
position on a triangle, over a very low flame to
avoid rapid expulsion of the volatile matter
which tends to prevent complete absorption of
the products of combustion of the sulfur. Heat
the crucible slowly for 30 min. gradually in-
crease the temperature, and occasionally stir
4 Available from the Office of Standard Reference Male-
rials, Room B3I4, Chemistry B!dg.r National Bureau of
Standards, Washington. D.C. 20234.
s "Reagent Chemicals, America Chemical Society
Specification," Am. Chemical Soc., Washington. D.C. For
suggestions on the testing of reasents sot lists! bv the
American Chemical Society, see '"'Reagent Chemicals and
Standards/* by Joseph Rosin. D. Van Nostrand Co.. Inc..
New York. N.Y., and the "United States Pharmacopeia.*"
G-3
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until all black particles have disappeared, which
is an indication of the completeness of the
procedure.
1.22 For Coal—Place the crucible in a
cold muffle and gradually raise the tempera-
ture to 800 ± 25°C in about 1 h. Maintain
this maximum temperature until on stirring
ail black particles have disappeared (about
1 % fa).
7.2.3 For Coke—Place the crucible in a
warm muffle (about 200°C) and gradually raise
the temperature to 800 ± 25aC in about 30
min. Maintain this maximum temperature until
on stirring all black particles have disappeared.
7.3 Subsequent Treatment—Remove the
crucible and empty the contents into a 200-rn 1
beaker and digest with 100 ml of hot water for
Vi to % h, while stirring occasionally. By
decantation, filter, and thoroughly wash the
insoluble matter with hot water. After several
washings in this manner, transfer the insoluble
matter to the filter and wash five times with hot
water, keeping the mixture well agitated. Treat
the filtrate, amounting to about 250 ml, with 10
to 20 ml of saturated bromine water, make
slightly acid with HQ, and boil to expel the
liberated bromine. Make just neutral to methyl
orange with NaOH or Na2C03 solution; then
add 1 ml of HC1 (1 + 9). Boil again and add
slowly from a pipet, while stirring constantly,
10 ml or more of BaCl, solution. The BaCI2
solution must be in excess. If more than 10 ml
of BaClj solution is required, reduce the weight
of sample to about 0.5 g and repeat the ignition
and digestion. Continue boiling for 15 min and
allow to stand for at least 2 h, or preferably
overnight, at a temperature just below boiling.
Filter through an ashless paper and wash with
hot water until 1 drop of silver nitrate (AgN03)
solution produces no more than a slight opales-
cence when added to 8 to 10 ml of filtrate.
7.3;1 Place the wet filter containing the
precipitate of barium sulfate (BaS04) in a
weighed platinum, porcelain, silica, or Alun-
dum crucible, allowing a free access of air by
fotding the paper over the precipitate loosely to
prevent spattering. Smoke the paper off gradu-
ally and at no time allow to burn with flame.
After the paper is practically consumed, raise
the temperature to approximately 925°C and
heat to constant weight.
7.4 Blanks and Corrections—In all cases a
D 3177
correction must be applied. Either a reagent
blank may be run exactly as described above,
using the same amount of all reagents that were
employed in the routine determination, or a
more accurate correction may be made by
analyzing a weighed portion of a standard
sulfate using the prescribed reagents and opera-
tions. If the latter procedure is carried out once
a week, or whenever a new supply of a reagent
is used, for a series of solutions covering the
approximate range of sulfur concentrations m
the samples, it is only necessary to add to or
subtract from the weight of BaSO, determined
for the sample, the deficiency or excess found
by the appropriate "check" determination. This
procedure is more accurate than the simple
reagent blank because, for the amounts of
sulfur in question and the conditions of precipi-
tation prescribed, the solubility error for
BaSO4, is probably the largest one to be
considered. Barium sulfate is soluble11 in acids
and pure water, and the solubility limit is
reached almost immediately on contact with
the solvent. Hence, if very high-purity reagents
are used or extra precaution is exercised, there
may be no sulfate apparent in the "blank." In
other words, the solubility limit for BaSO, has
not been reached or at any rate not exceeded;
consequently, some sulfate in the sample may
remain in solution or redissolve.
8. Calculation
8.1 Calculate the sulfur content as follows:
Sulfur, %, in the analysis sample
13.738
_ ' j-
where;
A — grams of BaS04 precipitated,
B — grams of BaSO., correction, and
C = grams of sample used.
Method B—Bomb Washing Method7
9. Reagents
9.1 Purity of Reagents—(See 6.1.)
9.2 Purity of Water—(See 6.2.)
* Journal of the American Chemical Socien', JACSA, Vol
32. 1910, p. 588; Vol 33, 19\U P 829
TSelvig, W. A., and Fieldner, A. C. "Check Determina-
tions of Sulfur in Cos! and Coke by the Eschka, Bornb-
Wasfcms and Sodium Peroxide Fusion Methods," Industrial
and Engineering Chemistry, JECHA, Vol 29, 1927. pp.
729-733.
G-4
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9.3 Ammonium Hydroxide (sp gr
-¦ 0.90)—Concentrated ammonium hydroxide
(NHjOH).
9.4 Bromine Water (Saturated)—(See 6.4.)
9.5 Hydrochloric Acid (1 4- /)—(See 6.6.)
9.6 Sodium Carbonate Solution—Dissolve
20.90 g of anhydrous sodium carbonate
(Na2C03) in water and dilute to 1 litre. The
Na;C02 should be previously dried for 24 h at
105°C.
9.7 Wash Solution—Dilute 1 ml of a satu-
rated solution of methyl orange to 1 litre with
¦ water.
10. Procedure
10.1 Ignition—Sulfur is determined in the
washings from the oxygen-bomb calorimeter
following the calorimetric determination
(Method D 2015). The type of bomb, amount of
water in the bomb, oxygen pressure, and
amount of sample taken shall be the same as
specified under the calorimetric determination
(Sections 4 to 8 of Method D 2015). The bomb
shall stand in the calorimeter water for not less
than 5 min after firing.
10.2 Subsequent Treatment—Remove the
bomb from the calorimeter water and open the
valve carefully so as to allow the gases to escape
at an approximately even rate so the pressure is
reduced to atmospheric in not less than 1 min.
Bombs equipped with valves other than needle
valves, such as compression valves, shall be
provided with a device so the valve can be
controlled to permit a slow and uniform release
of the gases. Open the bomb and examine the
inside for traces of unburned material or sooty
deposit. If these are found, discard the determi-
nation. Wash carefully all parts of the interior
of the bomb, including the capsule, with a fine
Jet of water containing methyl orange (9.7) until
no acid reaction is observed. It is essential to
wash through the valve opening in the case of
bombs equipped with compression valves, or
other types of valves with large openings, as
considerable spray may collect in such valve
openings.
10.3 Collect the washings in a 250-ml beaker
and titrate with standard sodium carbonate
solution (9.6) to obtain the "acid correction"
for the heating value, as specified under the
calorimetric determination D2015. Adjust the
pH to 5.5 to 7.0 with dilute NH401!. heat the
D 31 77
solution to boiling, and filter through a qualita-
tive paper. Wash the residue and paper thor-
oughly five or six times with hot water. To the
filtrate and washings, amounting to about 250
ml, add 1 ml of saturated bromine water (9.4)
and sufficient HC1 (9.5) to make it slightly acid.
Boil the solution to expel the excess bromine.
Adjust the acidity, precipitate, and determine
the sulfur as specified under the Eschka
method. Sections 5 to 8.
Method C—High-Temperature Combustion
Method*
II. Apparatus
11.1 Tube Furnace—Capable of heating a
tube approximately 34-mm external diameter
over a length of 150 mm to a temperature of
1350°C. It is heated electrically using either
silicon carbide resistance rods or a resistance
wire.
Note 2—Induction furnace techniques may be
used provided it can be shown that they meet the
precision requirements of Section 17.
11.2 Combustion Tube—Approximately
2S-mm internal diameter with a 3-mm wall
thickness and 750 mm in length, which is gas
tight at working temperature. A high-tempera-
ture porcelain or zircon straight refractory tube
has been found most efficient. It requires a
silica (12.12) adaptor with a flared end that
just fits inside the combustion tube and
serves as an exit for the gases. Alternatively,
the combustion may be carried out in a
tapered end tube that is directly connected
to the elbow of the fritted gas bubbler (12.8)
or to a 10/30 standard-taper ground joint
which is attached to a borosilicate glass
right-angle bend. The temperature at the
tapered end of the tube should be high enough
to prevent condensation in the tube itself.
¦11.3 Oxygen Cylinder, fitted with pressure
regulator and needle valve to control flow rate
of oxygen.
11,4 Flowmeter, for measuring an oxygen
flow rate of 300 ml/min.
8 Based on the method of Mott, R. A., and Wilkinson. H.
C.. "Determination of Sulfur -in Coal and Coke By the
Sheffield High Temperature Method," R/eJ, FUEL B, Vol
35. 1956, p. 6. This method is designed for the rapid
determination of suffer in coal and coke. It is not applicable
to coals or coal density fractions that have been subjected to
treatment with chlorinated hydrocarbons because of the
potentially high acidity of the combustion gases.
G-5
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11.5 Sample Combustion Boats—Iran-free,
unglazed porcelain or zircon boats. A con-
venient size is 100 mm long, 19 mm wide, and
11 mm deep.
11.6 Heat-Resistant Wire, 1.5 mm thick
with bent end to remove boats from combustion
tube.
11.7 Silica Pusher or Heat-Resistant Rod,
with a disk end for pushing the combustion boat
into the hot zone. The pusher passes through a
T-piece which is fitted into a rubber stopper at
the inlet end of the combustion tube. The open
end of the T-piece is sealed with a rubber tube
or one-holed stopper to permit movement of the
pusher and prevent escape of oxygen which
enters at the side limb of the T. The rubber
stopper or tube should be changed periodically
to avoid leakage.
11.8 Gas Absorption Bottles with Fritted
Disk, 125-ml capacity, for gas absorption.
Fritted glass end porosity should be 15 to 40
jim. The bottle should be of such a diameter
that the fritted end is covered by peroxide
solution to a depth of at least 50 mm. The
bottles are fitted, in a series of two per combus-
tion tube, to the outlet end of a combustion
tube. Alternatively a single narrow gas ab-
sorber may be used so that the fritted bubbler is
covered to a depth of at least 90 mm.
11.9 Vacuum Regulating Bottle, containing
mercury with an open-ended tube dipping into
it.
11.10 U-tube, packed with soda-asbestos.
11.11 Vacuum Source.
11.12 Silica Adaptor, 300 mm long by 8 mm
in outside diameter and flared at one end to 26
mm.
12. Reagents "
12.1 Purity of Reagents—(See 6.1.)
. 12.2 Purity of Water—(See 6.2.)
12.3 Aluminum Oxide (Al203), finely di-
vided and dried at 1350°C.
12.4 Hydrogen Peroxide (fl:02) Solution
—One volume percent (50 ml of 30 % H202
with 1450 ml of water). The pH is adjusted
(using NaOH or H2S04 as appropriate) to that
which is used for the end point in the titration.
Solutions should be discarded after 2 or 3 days.
12.5 Indicator—Indicators that change
color (titration end point) between pH 4 and 5
D 3177
are recommended, but in no case should the pH
exceed 7. Adequate lighting and stirring to
ensure proper detection of the end point is
essential. A choice of indicators or use of a pH
meter is permitted. Directions for preparing
two acceptable mixed indicators are as follows:
12.5.1 Mix 1 part methyl red solution (dis-
solve 0.125 g in 60 ml of ethanol and dilute to
100 ml with water) with 3 parts bromcresol
green solution {dissolve 0.083 g in 20 ml of
ethanol and dilute to 100 ml with water).
Discard the mixed solution after 1 week.
12.5.2 Mix equal volumes of methyl red
solution (dissolve 0.125 g in 60 ml of ethanol
and dilute to 100 ml with water) and methylene
blue solution (dissolve 0.083 g in 100 ml of
ethanol and store in a dark glass bottle).
Discard the mixed solution after 1 week.
12.6 Mercuric Oxycyanide Hg(OH)CN
(Note 2)—One g/80 ml of water. Prepare
fresh solution every 2 or 3 days.
Note 4—This is a highly poisonous substance and
will explode when touched with a flame or by
percussion.
12.7 Soda-Asbestos, 8 to 20 mesh.
12.8 Sodium Hydroxide (NaOH) Solution,
0.050 N.
12.9 Sulfuric Acid (H^SOt), 0.050 N.
13. Procedure
13.1 Raise the temperature of the furnace
to 1350°C at such a rate that the combustion
tubes will withstand the thermal shock. Mea-
sure 100 ml of 1 % HjOi (12.4) into two gas
absorption bottles so that at least 50 mm of the
fritted disk is covered in the first bottle, or pour
the whole amount into a single absorption
bottle. Assemble the apparatus as shown in Fig.
1 except do not connect the rubber tube from
the oxygen supply to the soda-asbestos U-tube.
Draw air through at about 350 ml/min. The
rate of flow can be adjusted by changing the
depth of penetration into the mercury of the
open-ended glass tube in the vacuum regulating
bottle. Connect the oxygen supply to the U-
tube and adjust the rate of flow of oxygen to
300 ml/min. This flow rate, at a temperature of
1350°C, will prevent the formation of oxides of
nitrogen. The preliminary adjustment to 350
ml/min of air ensures that the connections at
the outlet end of the combustion tube are under
6-6
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D 3177
slightly-reduced internal pressure and no leak of
combustion products will occur.
13.2 Weigh about 0.5 § of the analysis
sample (Note 3) to the nearest 0.1 mg and
spread evenly in a combustion boat previously
lined with a thin layer of AI5Os (0.02 to 0.05 g);
then cover with approximately 0.5 g of A1203.
Note 3—It may be necessary to grind coals of
high mineral matter content to pass through a No.
100 (150-pm) sieve.
13.3 Put the charged boat into the inlet end
of the combustion tube so that the center of the
boat is 270 mm from the center of the combus-
tion tube hot zone, and if necessary readjust the
rate of flow of oxygen to 300 ml/mirt. Move the
boat forward a distance of 30 mm at the
beginning of each minute with the exception of
the sixth minute, for the next 10 rnin. The boat
should be left at the fifth minute position until
the seventh minute to ensure a slow heating
rate. At the end of the 10-min period the
combustion boat will be in the center of the hot
zone. Withdraw the pusher after each move-
ment to prevent distortion of the rod. Keep the
boat in the hot zone for an additional 4 min.
Disconnect the gas absorption bottles and with-
draw the boat onto a sheet of asbestos. This
heating program has been established for all
types of coal, and where it is shortened for a
particular coal, results should be checked
against those obtained by using the longer
heating schedule.
13.4 Pour the content of the absorption
bottles into a suitable titration flask. Wash the
bottles and the interior of the silica adaptor
with water (12.2) and add the washings to the
flask. Add 5 or 6 drops of indicator solution
and titrate with 0,050 N NaOII solution
(12.8). The total acidity, due to oxides of sulfur
and chlorine, is given according to the follow-
ing reactions:
SO* + HjOj - H2S04
CI, H,0. 7 HC1 ¦ O,
13.5 After titration, the chloride ion is pres-
ent in solution as NaCL Convert the NaCl to
NaOH by adding 20 ml of Hg(OH)CN (13.6)
solution (sufficient for coals containing up to
1.2 % chlorine):
NaCI + Hg(OH)CN - HgClCN + NaOH
13.6 Titrate the liberated NaOH with the
0.050 N H,SO. (12.9). Make a blank determi-
nation in the same manner but without sample.
14. Calculation
14.1 Calculate the percentage sulfur in coal
as follows:
S = ' 603 [>. (a-a,)-F,(b-b,)j
W
where:
S — percent sulfur in coal,
a millilitre of NaOH solution used in full
determination,
Oj = millilitre of NaOH solution used in
blank determination,
b = millilitre of H2SO« used in full determi-
nation,
= millilitre of H2S04 used in blank deter-
mination,
Fj = normality of the NaOH solution.
F2 = normality of the H2S04 solution, and
W = grams of coal taken.
15. Report
15.1 The results of the sulfur analysis may be
reported on any of a number of bases, differing
from each other in the manner by which
moisture is treated.
15.2 Use the percentage of moisture in the
sample passing a No. 60 (250-/xm) sieve to
calculate the results of the analysis sample to a
dry basis.
15.3 Procedures for converting the value
obtained on the analysis sample to other bases
are described in Specifications D3I76 and
D 3180. . ^
PRECISION
16. Esehka and Bomb-Washing Methods
16.1 Repeatability—Results of two consecu-
tive determinations carried out on the same
sample in the same laboratory by the same
operator using the same apparatus should not
differ more than the following:
%
Coal containing less than 2 % sulfur ' 0.05
Coil containing 2% sulfur ormote [ . 0.10
Coke 0_03
16.2 Reproducibility—The means of results
of duplicate determinations carried out by
different laboratories on representative samples
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• #
taken from the same bulk sample after the last
stage of reduction should not differ by more
than the following:
%
Coa! containing less than 2 % sulfur 0. JG
Coal containing 2 % sutftir ar more 0.20
¦ Coke 0-05
17. High Temperature Combustion Method
17.1 Repeatability—Results of two consecu-
tive determinations carried oat on the same
sample in the same laboratory by the same
D 3177
operator using the same apparatus should not
differ more than 0.05 % sulfur for all coal and
coke.
17.2 Reproducibility—The means of results
of duplicate determinations carried out by
different laboratories on representative samples
taken from the same bulk sample after the last
stage of reduction should not differ more than
the following:
%
Coals containing less than 2% sulfur 0.15
Coals containing 2 % sulfur or more 0.25
Coke 0.15
Rubber Tubing Connections
/
¦2.8 mm I, D.
Combustfort Tube
125 ml X Gas Absorpt/cn
Softies
Fritted Disks
^Sample See! Pusher
Flare to
cc 2Smm
Tube
Pusfi Sched. Mcrke
\ Stopp
«140 mrn*i
f
To Vcc
NO. 6
Stopper
Silica
Nal Steppe?
ar Rubber Tube
Adaotor
3mm O.D.
X 3GO m m
Rubber
Tube
Combustion
Me'er Pressure Recjuictcr
/ end Needle Valve
FIG, 1 ITigli-Temperature Combustion Tofee Fcraace for the Determination of Total Sulfur is Coal-
The American Society for Testing and Materials takes no position respecting the validity of any patent rights asserted
in connection with anv item mentioned in this standard. Users of this standard are expressly advised that determination of the
validity af any such patent rights, and the risk of infringement of such rights, is entirety their own responsibility.
G-8
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APPENDIX H
ANALYSES PERFORMED IN THE
MOBILE FIELD LABORATORY
H—1
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ALKALINITY
Method 310,1 (Titriuietric, pH 4.5)
STOMET NO. 00410
1. Scope and Application
1.1 TMs method is applicable to drinking, surface, and saline waters, domestic and industrial
wastes.
1.2 The method is suitable for all concentration ranges of alkalinity: however, appropriate
aliquots should be used to avoid a titration volume greater than 50 ml.
1.3 Automated titrimctric analysis is equivalent.
2. Summary of Method
2.1 An unaltered sample is titrated to an electrometrieally determined end point of pH 4.5.
The sample must not be filtered, diluted, concentrated, or altered in any way,
3. Comments
3.1 The sample should be refrigerated at 4°C and ran as soon as practical. Do not open
sample bottle before analysis.
3.2 Substances, such as salts of weak organic and inorganic acids present in large amounts,
may cause interference in the electrometric pH measurements.
3.3 For samples having high concentrations of mineral acids, such as mine wastes and
associated receiving waters, titrate to an electrometric endpoint of pH 3.9, using the
procedure in:
Annual Book of ASTM Standards, Part 31, "Water", p 115, D-1G67, Method D, (1976).
3.4 Oil and grease, by coating the pH electrode, may also interfere, causing sluggish
response.
4. Apparatus
4.1 pH meter or electrically operated titrator that uses a glass electrode and can be read to
0.05 pH units. Standardize and calibrate according to manufacturer's instructions. If
automatic temperature compensation is not provided, make titration at 25 ±2° C.
4.2 Use an appropriate sized vessel to keep the air space above the solution at a minimum.
Use a rubber stopper fitted with holes for the glass electrode, reference electrode (or
combination electrode) and buret.
4.3 Magnetic stirrer, pipets, flasks and other standard laboratory equipment
4.4 . Burets, Pyrex 50,25 and 10 ml.
5. Reagents
5.1 Sodium carbonate solution, approximately 0.05 N: Place 2.5 ±0,2 g (to nearest mg)
Na2C03 (dried at 250°C for 4 hours and cooled in desiccator) into a 1 liter volumetric
flask and dilute to the mark.
Approved for NPDES
Issued 1971
Editorial revision 1978
310.1-1
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where:
A = ml standard acid
N = normality standard acid
7.2 Potentiometric titration of low alkalinity:
Total alkalinity, mg/1 CaCO, = (2B ~ Q x N x 50,000
* ° J ml of sample
where:
B = ml titrant to first recorded pH .
C = total ml titrant to reach pH 0.3 units lower
N = normality of acid
8. Precision and Accuracy
8.1 Forty analysts in seventeen laboratories analyzed synthetic water samples containing
increments of bicarbonate, with the Following results:
Increment as
¦ Alkalinity
mg/liter, CaC03
Precision as
Standard Deviation
mg/liter, CaC03
Accuracy as
Bias, Bias,
% mg/1, CaCO,
9
113
119
1.27
1.14
5.28
5.36
+ 10.61
+22.29
- 8.19
- 7.42
+G.85
+2.0
-9.3
-8.8
(FWPCA Method Study 1, Mineral and Physical Analyses)
8.2 In a single laboratory (EMSL) using surface water samples at an average concentration
of 122 mg CaCOj/1, the standard deviation was ±3.
Bibliography
1. Standard Methods for the Examination of Water and Wastewater, 14th Edition^ p 278,
Method 403, (1975).
2. Annual Book of ASTM Standards, Part 31, "Water", p 113, D-1067, Method B, (1976).
310.1-3
H-3
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ACIDITY
Method 305.1 (Titrimetric)
STORET NO. 70508
1. Scope and Application
1.1 This method is applicable to surface waters, sewages and industrial wastes, particularly
mine drainage and receiving streams, and other waters containing ferrous iron or other
polyvalent cations in a reduced state.
1.2 The method covers the range from approximately 10 mg/1 acidity to approximately
1000 mg/1 as CaC03j using a 50 ml sample.
2. Summary of Method
2.1 The pH of the sample is determined and a measured amount of standard acid is added, as
needed, to lower the pH to 4 or less. Hydrogen peroxide is added, the solution boiled for
several minutes, cooled, and titrated electrometrically with standard alkali to pH8.2.
3. Definitions
3.1 This method measures the mineral acidity of a sample plus the acidity resulting from
oxidation and hydrolysis of polyvalent cations, including salts of iron and aluminum.
4. Interferences
4.1 Suspended matter present in the sample, or precipitates formed during the titration may
cause a sluggish electrode response. This may be offset by allowing a 15-20 second pause
between additions of titrant or by slow dropwise addition of titrant as the endpoint pH is
approached.
5. Apparatus
5.1 pH meter, suitable for electrometric titrations.
6. Reagents
6.1 Hydrogen peroxide (H202,30% solution).
6.2 Standard sodium hydroxide, 0.02 N.
6.3 Standard sulfuric acid, 0.02 N.
7. Procedure
7.1 Pipet 50 ml of the sample into a 250 ml beaker.
7.2 Measure the pH of the sample. If the pH is above 4.0, add standard sulfuric acid (6.3) in
5,0 ml increments to lower the pH to 4.0 or less. If the initial pH of the sample is less than
4.0, the incremental addition of sulfuric acid is not required.
7.3 Add 5 drops of hydrogen peroxide (6.1).
7.4 Heat the sample to boiling and continue boiling for 2 to 4 minutes. In some instances, the
concentration of ferrous iron in a sample is such that an additional amount of hydrogen
peroxide and a slightly longer boiling time may be required.
Approved for NPDES
Issued 1971
Technical revision 1974
305.1-1
E-4
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RESIDUE, FILTERABLE
Method 160.1 (Gravimetric, Dried at 180°C)
STOMET NO. 70300
1. Scope and Application
1.1 This method is applicable to drinking, surface, and saline waters, domestic and industrial
wastes.
1.2 The practical range of the determination is 10 mg/1 to 20,000 mg/1.
2. Summary of Method
2.1 A well-mixed sample is filtered through a standard glass fiber filter. The filtrate is
evaporated and dried to constant weight at 180°C.
2.2 If Residue, Non-Filterable is being determined, the filtrate from that method may be
used for Residue, Filterable.
3. Definitions
3.1 Filterable residue is defined as those solids capable of passing through a glass fiber filter
and dried to constant weight at 180°C.
4. Sample Handling and Preservation
4.1 Preservation of the sample is not practical; analysis should begin as soon as possible.
Refrigeration or icing to 4°C, to minimize microbiological decomposition of solids, is
recommended.
5. Interferences
5.1 Highly mineralized waters containing significant concentrations of calcium, magnesium,
chloride and/or sulfate may be hygroscopic and will require prolonged drying,
desiccation and rapid weighing.
5.2 Samples containing high concentrations of bicarbonate will require careful and possibly
prolonged drying at 180°C to insure that all the bicarbonate is converted to carbonate.
5.3 Too much residue in the evaporating dish will crust over and entrap water that will not
be driven off during drying. Total residue should be limited to about 200 mg.
6. Apparatus
6.1 Glass fiber filter discs, 4.7 cm or 2.1 cm, without organic binder, Reeve Angel type 934-
AH, Gelman type A/E, or equivalent
6.2 Filter holder, membrane filter funnel or Gooch crucible adapter.
6.3 Suction flask. 500 ml.
6.4 Gooch crucibles, 25 ml (if 2.1 cm filter is used).
6.5 Evaporating dishes, porcelain, 100 ml volume. (Vycor or platinum dishes may be
substituted).
6.6 Steam bath.
6.7 Drying oven, 180°C ±2°C.
6.8 Desiccator.
Approved for NPDES
Issued 1971
160.1-1
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RESIDUE, NON-FILTERABLE
Method 160.2 (Gravimetric, Dried at 103-105°Q
STORET NO. 00530
1. Scope and Application
1.1 This method is applicable to drinking, surface, and saline waters, domestic and industrial
wastes.
1.2 The practical range of the determination is 4 mg/1 to 20,000 mg/1.
2. Summary of Method
2.1 A well-mixed sample is filtered through a glass fiber filter, and the residue retained on the
filter is dried to constant weight at 103-105'C.
2.2 The filtrate from this method may be used for Residue, Filterable.
3. Definitions
3.1 Residue, non-filterable, is defined as those solids which are retained by a glass fiber filter
and dried to constant weight at 103-105°C.
4. Sample Handling and Preservation
4.1 Non-representative particulates such as leaves, sticks, fish, and lumps of fecal matter
should be excluded from the sample if it is determined that their inclusion is not desired
in the final result.
4.2 Preservation of the sample is not practical; analysts should begin as soon as possible.
Refrigeration or icing to 4°C, to minimize microbiological decomposition of solids, is
recommended.
5. Interferences
5.1 Filtration apparatus, filter material, pre-washing, post-washing, and drying temperature
are specified because these variables have been shown to affect the results.
5.2 Samples high in Filterable Residue (dissolved solids), such as saline waters, brines and
some wastes, may be subject to a positive interference. Care must be taken in selecting the
filtering apparatus so that washing of the filter and any dissolved solids in the filter (7.5)
minimizes this potential interference.'
6. ' Apparatus
6.1 Glass fiber filter discs, without organic binder, such as Millipore AP-40, Reeves Angel
934-AH, Gelman type A/E, or equivalent.
NOTE: Because of the physical nature of glass fiber filters, the absolute pore size cannot
be controlled or measured. Terms such as "pore size", collection efficiencies and effective
retention are used to define this property in glass fiber filters. Values for these parameters'
vary for the filters listed above.
6.2 Filter support: filtering apparatus with reservoir and a coarse (40-60 microns) fritted
disc as a filter support.
Approved for NPDES
Issued 1971
160.2-1
H-6
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7.6 Carefully remove the filter from the filter support. -Alternatively, remove crucible and
filter from crucible adapter. Dry at least one hour at 103-105°C. Cool in a desiccator and
weigh. Repeat the drying cycle until a constant weight is obtained (weight loss is less than
0.5 mg).
8. Calculations
8.1 Calculate non-filterable residue as follows:
Non-filterable residue, tng/1 = — ^X1»Q00
where:
A = weight of filter (or filter and crucible) + residue in mg
B = weight of filter (or filter and crucible) in mg
C = ml of sample filtered
9. Precision and Accuracy
9.1 Precision data are not available at this time.
9.2 Accuracy data on actual samples cannot be obtained.
Bibliography
1. NCASI Technical Bulletin No. 291, March 1977. National Council of the Paper Industry for
Air and Stream Improvement, Inc., 260 Madison Ave., NY.
160.2-3
H-7
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